Manufacture of Large Nuclear and Fossil Components Using Powder Metallurgy and Hot Isostatic Proce Ssing Technologies

Program on Technology Innovation: Manufacture of
Large Nuclear and Fossil Components Using Powder

Metallurgy and Hot Isostatic Processing Technologies
2012 TECHNICAL REPORT
Program on Technology
Innovation: Manufacture of
Large Nuclear and Fossil
Components Using Powder
Metallurgy and Hot Isostatic
Processing Technologies
EPRI Project Manager

D. Gandy
3420 Hillview Avenue

Palo Alto, CA 94304-1338
USA
PO Box 10412
Palo Alto, CA 94303-0813
USA
800.313.3774
650.855.2121
askepri@epri.com
www.epri.com
1025491
Final Report, May 2012
DISCLAIMER OF WARRANTIES AND LIMITATION OF LIABILITIES

THIS DOCUMENT WAS PREPARED BY THE ORGANIZATION(S) NAMED BELOW AS AN ACCOUNT OF
WORK SPONSORED OR COSPONSORED BY THE ELECTRIC POWER RESEARCH INSTITUTE, INC. (EPRI).
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IMPLY ITS ENDORSEMENT, RECOMMENDATION, OR FAVORING BY EPRI.
THE FOLLOWING ORGANIZATIONS PREPARED THIS REPORT:
Electric Power Research Institute (EPRI)
Carpenter Technology Corporation
X-Gen Engineering
NOTE
For further information about EPRI, call the EPRI Customer Assistance Center at 800.313.3774 or
e-mail askepri@epri.com.
Electric Power Research Institute, EPRI, and TOGETHERSHAPING THE FUTURE OF ELECTRICITY are
registered service marks of the Electric Power Research Institute, Inc.
Copyright 2012 Electric Power Research Institute, Inc. All rights reserved.
Acknowledgments
The following organizations prepared this report:

Electric Power Research Institute (EPRI)
1300 West W.T. Harris Blvd.
Charlotte, NC 28262
Principal Investigators
D. Gandy
J. Siefert
J. Shingledecker
Carpenter Technology Corporation
600 Mayer Street
Bridgeville, PA 15017
Principal Investigators
L. Lherbier
D. Novotnak
X-Gen Engineering
7173 Queensbridge Way
San Jose, CA 95120
Contributing Author
D. Sandusky
This report describes research sponsored by EPRI.
This publication is a corporate

document that should be cited in the
literature in the following manner:
Program on Technology Innovation:
Manufacture of Large Nuclear and
Fossil Components Using Powder
Metallurgy and Hot Isostatic
Processing Technologies.
EPRI, Palo Alto, CA: 2012.
1025491.
iii
The following individuals from the EPRI NDE Center in Charlotte,

North Carolina, are gratefully acknowledged for their efforts in
preparing the inspection summary that constitutes Appendix E of the
report, and for their continued support of this project: W. Ratliff,
R. Salisbury, and M. Dennis.
iv
Product
Description
An alternative manufacturing method, powder metallurgy coupled

with hot isostatic processing (PM/HIP), is being explored for the
manufacture of large, pressure-retaining components that will be
required to meet the demanding needs of nuclear, fossil, combined
cycle, ultra-supercritical, and oxy-combustion power applications
over the next few decades. This report provides an in-depth review of
the new manufacturing process, discusses why the PM/HIP
technology is ripe for the power industry to consider, highlights a
feasibility study on a test product, and finally reviews a data package
assembled for the ASME Boiler & Pressure Vessel Code to support
use of the technology for stainless steel valve bodies, pump housings,
piping elbows, flanges, and other pressure-retaining components.
Background
Large PM/HIP-produced components have not been utilized in the
power generation industry to date primarily because of three
technical barriers: 1) the sizes and shapes for near-net shape
components have only recently reached a point for consideration and
have not been tailored for the compositions/alloys that are of most
interest to the power industry; 2) materials and processes used to
manufacture pressure-retention or high-temperature power plant
components are generally subject to, in the United States, the ASME
Boiler and Pressure Vessel Code, which currently does not allow the
use of PM/HIP-produced components for the desired applications;
and 3) for iron-based steel alloy systems, the PM/HIP production
route has generally been more expensive than traditional forging and
casting routes.
Objectives
This report is targeted primarily at utility engineering teams and
original equipment manufacturers responsible for selection and
procurement of new or replacement pressure-retaining components
for power generation applications. The challenges met in this
research cover demonstration of the manufacturing method over four
component articles (including three 316L stainless steel valves and
one tee-section) necessary to define the technology for manufacture
of future pressure-retaining components. The objectives of this effort
are to develop sufficient data and interest as well as to assess the
manufacturing technology for future use in the power industry.
v
Approach
EPRI, in conjunction with partner organizations, evaluated the
feasibility of PM/HIP for pressure-retaining applications and
performed the necessary testing and validation steps to introduce the
new manufacturing process to ASME. This report describes the
results of both phases of this assessment.
Results
PM/HIP exhibits several attributes that immediately make it
attractive to the power generation industry, including the following:
1) it eliminates inspectability issues and concerns associated with cast
components; 2) it enables manufacture of large, complex components
using near-net shape technologies; 3) it enables new alloy systems
and targeted chemistries; 4) it enhances weldability; 5) it enables an
alternate supply route for long-lead time components; and 6) it
eliminates rework or repair of large cast components. The research
described in the report highlights the development and assessment of
sufficient mechanical, microstructural, inspection, and processing
information to fully describe the PM/HIP technology for power
generation applications.
Applications, Value, and Use
Primary applications of the manufacturing technology described
include 316L stainless steel: valve bodies, pump housings, piping
elbows and sweep-o-lets, and flanges. Other pressure-retaining
components may also be considered for application. In the future,
other materials may also be accepted for use once the technology is
fully vetted for these alloys, including Grade 91/92 steels, nickelbased alloys, and various low-alloy steels.
Keywords
Powder metallurgy
Hot isostatic processing
Valves and valve bodies
Pump housings
Piping elbows
vi
Abstract
The manufacture of large, complex components for nuclear, fossil,
combined-cycle, ultra-supercritical, and oxy-combustion applications
will be costly for the power industry over the next few decades as
many of these components will be produced from high-strength alloy
castings and forgings. The current EPRI study investigates the use of
an alternative manufacturing method, powder metallurgy and hot
isostatic processing (PM/HIP), to produce high-qualityand
potentially less expensivepressure-retaining components for power
generation applications. Benefits of the process include manufacture
of components to near-net shapes, precise chemistry control, a
homogeneous microstructure, increased material utilization, good
weldability, and most importantly, improved inspectability.
In the current study, a number of large valve body components
including three 316L stainless steel valve bodies, three Grade 91 steel
valve bodies, and one IN625 valve body have been produced and are
under assessment. This work represents a follow-on to an earlier
feasibility assessment in which a 780-kg (1716-lb), 300-mm
(12-inch) diameter 316L stainless steel valve body was manufactured
using the PM/HIP process. Microstructural and mechanical test
results are provided for the stainless steel valve body materials.
Mechanical test results obtained at room temperature and at 50F
(28C) increments up to 1000F (538C) suggest that the PM/HIP
process is capable of producing properties superior to those of
conventional cast and forged components in the time-independent
mechanical property regime. Based on these results, a data package
has been developed for the 316L stainless steel. A second data
package, for the Grade 91 steel (time-dependent), is being assembled
in 2012 for submittal to the ASME Boiler & Pressure Vessel Code.
vii
Table of Contents
Section 1: Introduction ............................................1-1
Research Context ............................................................. 1-1
References....................................................................... 1-3
Section 2: What Is Powder Metallurgy? ...................2-1
Process Overview............................................................. 2-1
Component Design ..................................................... 2-1
Powder Production ...................................................... 2-2
Molding (or Container) ................................................ 2-4
Powder Consolidation, Vacuum Processing, and Hot
Isostatic Pressing ......................................................... 2-5
Characteristics of PM/HIP Products (Produced from Inert
Gas Atomized Powders) ................................................... 2-8
Oxide Inclusions and Porosity ...................................... 2-8
Mechanical Properties ................................................. 2-9
Microstructure and Corrosion Properties ........................ 2-9
Process and Product Controls........................................... 2-12
Process Controls ....................................................... 2-12
Product Controls ....................................................... 2-14
References..................................................................... 2-14
Section 3: Why Consider PM/HIP for Large
Nuclear and Fossil Components?..............3-1
Section 4: Valve Body Feasibility Assessment ...........4-1
Manufacture of a 316L Valve Body .................................... 4-1
Inspection and Weldability Results ..................................... 4-2
Valve Body AssessmentMechanical and
Metallographic Characterization ....................................... 4-7
Chemical Composition.................................................... 4-11
Mechanical Testing ........................................................ 4-11
ix
Section 5: Manufacture and Characterization of

Multiple Valve Bodies .............................. 5-1
316L Stainless Steel Valve Body Development and
Testing ............................................................................ 5-1
Grade 91 Valve Body Development and Testing .................. 5-4
IN625 Valve Body Development and Testing ...................... 5-6
Section 6: Results and Discussion ............................. 6-1
Section 7: Conclusions ............................................. 7-1
Appendix A: Process and Product Controls for
Material Produced by PM/HIP..................A-1
Appendix B: Draft ASME BPVC Section III Code
Case and Supporting Data Package ......... B-1
Appendix C:
Stress Analysis .................................. C-1
Appendix D: Corrosion Data Supplied by

Rolls-Royce .............................................. D-1
Appendix E: Inspection Summary.......................... E-1
Initial Component Inspectability Assessment ........................ E-1
Overview ................................................................... E-1
Equipment.................................................................. E-1
Sample Preparation .................................................... E-1
Examinations.............................................................. E-2
Results ....................................................................... E-2
Ultrasonic Examinations of Installed Reflectors ................... E-23
Overview ................................................................. E-23
Equipment................................................................ E-23
Sample Preparation .................................................. E-24
Examinations............................................................ E-27
Results ..................................................................... E-28
Comparison of PM/HIP Stainless Steel and Cast
Stainless Steel Inspectability ............................................ E-50
Overview ................................................................. E-50
Equipment................................................................ E-50
Examinations............................................................ E-50
Results ..................................................................... E-53
Inspection Summary ....................................................... E-56
List of Figures
Figure 2-1 Typical powder production sequence ....................... 2-3
Figure 2-2 Inert gas atomization chamber ................................ 2-3
Figure 2-3 Powders produced by gas atomization (figure
courtesy of Carpenter Powder Products) .............................. 2-4
Figure 2-4 Container for a stainless steel valve body (figure
courtesy of Carpenter Powder Products) .............................. 2-5
Figure 2-5 HIP furnace/vessel arrangement (figure courtesy
of Carpenter Powder Products) .......................................... 2-7
Figure 2-6 Large commercial HIP furnace/vessel (figure
courtesy of Avure.com) ..................................................... 2-7
Figure 2-7 Comparison of microstructures of PM/HIP 316L
and wrought 316L ......................................................... 2-10
Figure 4-1 Sectional drawing of a 316L stainless steel valve
body used as a demonstration piece in this feasibility
assessment ...................................................................... 4-1
Figure 4-2 780-kg (1716-lb) 316L prototype stainless steel
valve body produced during the feasibility assessment
(photo on the right shows valve body sectioned along its
center line to reveal its ability to produce a sound,
dimensionally stable component configuration) .................... 4-2
Figure 4-3 Inspection flaws installed at various locations
around the diameter of one flange from the valve body ........ 4-3
Figure 4-4 Inspection flaws described in Figure 4-3 installed
at various depths around the diameter of one flange
from the valve body.......................................................... 4-4
Figure 4-5 Photograph showing manual inspection of the
valve body in process ....................................................... 4-4
Figure 4-6 Photograph showing automated inspection of the
valve body in process ....................................................... 4-5
Figure 4-7 12-inch-diameter 316L stainless steel stock
fabricated for weldability testing ........................................ 4-6
xi
Figure 4-8 Cross-sectional view of an autogenous weld in

the 316L stainless steel slice removed from the end of
the stock shown in Figure 4-7 ............................................ 4-6
Figure 4-9 Cross-sectional view of a multiple-pass weld
overlay applied to the 316L stainless steel coupon ............... 4-7
Figure 4-10 Closer view of the valve body diagrammed in
Figure 4-1, demonstrating the ability of the process to
produce intricate shapes or configurations .......................... 4-8
Figure 4-11 Section of the valve body flange that was used
to remove metallographic and mechanical specimens
along three different directions .......................................... 4-9
Figure 4-12 Photomicrographs of the valve body
microstructure along three different directions: a) hoop;
b) longitudinal; c) transverse............................................ 4-10
Figure 5-1 One of the 316L stainless steel valves
manufactured by Carpenter Technology to
drawing/specifications provided by Tyco Crosby: a) the
finished valve body; b) the valve body sectioned into
halves ............................................................................. 5-2
Figure 5-2 Tensile test results for three Type 316L stainless
steel valve bodies manufactured during this project .............. 5-3
Figure 5-3 Yield strength test results for three Type 316L
stainless steel valve bodies manufactured during this
project ............................................................................ 5-3
Figure 5-4 Grade 91 alloy steel valve manufactured by
Carpenter Technology to drawing/specifications
provided by Dresser (photo on the right shows valve
body sectioned into halves) ............................................... 5-5
Figure 5-5 IN625 valve body manufactured by Carpenter
for feasibility purposes ...................................................... 5-7
Figure E-1 Valve sample as received ........................................ E-3
Figure E-2 Valve sample after glass bead blasting and
flange sanding................................................................. E-3
Figure E-3 360-151-053 on main flange OD looking at the
back wall ........................................................................ E-4
Figure E-4 UltraVision screen shot of 360-151-053 on main
flange OD looking at the back wall .................................... E-4
xii

ID corner ......................................................................... E-5
flange OD looking at the ID corner .................................... E-5
Figure E-7 360-151-053 on main flange back side looking
at the ID corner ................................................................ E-6
flange back side looking at the ID corner ............................ E-6
at the OD corner .............................................................. E-7
Figure E-10 UltraVision screen shot of 360-151-053 on
main flange back side looking at the OD corner .................. E-7
Figure E-11 360-151-053 on main flange mating surface
looking at the OD corner .................................................. E-8
main flange mating surface looking at the OD corner........... E-8
looking at the back wall.................................................... E-9
main flange mating surface looking at the back wall ............ E-9
Figure E-15 360-151-053 on side flange OD looking at the
back wall ...................................................................... E-10
Figure E-16 UltraVision screen shot of 360-151-053 on side
flange OD looking at the back wall .................................. E-10
ID corner ....................................................................... E-11
Figure E-18 UltraVision screen shot of 360-151-053 on side
flange OD looking at the ID corner .................................. E-11
Figure E-19 360-151-053 on valve body looking at the
back wall ...................................................................... E-12
valve body OD looking at the back wall ........................... E-12
Figure E-21 360-151-054 on main flange OD looking at
back wall ...................................................................... E-13
Figure E-22 UltraVision screen shot of 360-151-054 L-wave
on main flange OD looking at the back wall ..................... E-13
xiii

ID corner ....................................................................... E-14
on main flange OD looking at the ID corner ...................... E-14
Figure E-25 UltraVision screen shot of 360-151-054 S-wave
on main flange OD looking at the ID corner ...................... E-15
at the ID corner .............................................................. E-15
on main flange back side looking at the ID corner ............. E-16
on main flange back side looking at the ID corner ............. E-16
at the OD corner ............................................................ E-17
on main flange back side looking at the OD corner ........... E-17
looking at the OD corner ................................................ E-18
on main flange mating surface looking at the OD corner .... E-18
on main flange mating surface looking at the OD corner .... E-19
looking at the back wall.................................................. E-19
on main flange mating surface looking at the back wall ..... E-20
ID corner ....................................................................... E-20
Figure E-37 UltraVision screen shot of 360-151-054 L wave
on side flange OD looking at the ID corner ....................... E-21
back wall ...................................................................... E-21
on valve body OD looking at the back wall ...................... E-22
main flange OD corner on the bounce.............................. E-22
xiv

on valve body OD looking at the main flange OD corner
on the bounce................................................................ E-23
Figure E-42 Drawing of flaw locationssheet 1 of 3 ............... E-25
Figure E-45 Flaw location table ............................................. E-26
Figure E-46 Scanning setup for UT examinations on the OD ..... E-27
Figure E-47 Scanning setup for UT examinations on the
flange face .................................................................... E-28
Figure E-48 Flaw 1 seen with a 50 L-wave looking positive ..... E-31
Figure E-49 Flaw 1 seen with a 50 S-wave looking positive .... E-31
Figure E-50 Flaw 1 seen with a 50 L-wave looking negative.... E-32
Figure E-51 Flaw 1 seen with a 50 S-wave looking
negative ........................................................................ E-32
Figure E-52 Flaw 2 seen with a 45 L-wave looking down........ E-33
Figure E-53 Flaw 2 seen with a 48 S-wave looking down ....... E-33
Figure E-54 Flaw 3 seen with a 46 L-wave looking down........ E-34
Figure E-55 Flaw 3 seen with a 45 S-wave looking down ....... E-34
Figure E-56 Flaw 5 seen in a 30 merge L-wave looking
negative ........................................................................ E-35
positive ......................................................................... E-35
Figure E-58 Flaw 5 seen in a 30 merge S-wave looking
negative ........................................................................ E-36
positive ......................................................................... E-36
Figure E-60 Flaw 5 seen off a bounce in a 4045 S-wave
merge from the scan looking up ....................................... E-37
negative ........................................................................ E-37
positive ......................................................................... E-38
negative ........................................................................ E-38
xv

positive ......................................................................... E-39
Figure E-65 Approximate location of array while imaging
Flaw 1 .......................................................................... E-39
Figure E-66 Flaw 1 seen with a 49 L-wave ............................ E-40
Figure E-67 Flaw 1 seen with a 48 S-wave ........................... E-40
Flaw 2 .......................................................................... E-41
Figure E-70 Flaw 2 seen with a 44.5 S-wave ........................ E-42
Flaw 3 .......................................................................... E-42
Figure E-73 Flaw 3 seen with a 50 S-wave ........................... E-43
Figure E-74 Approximate location of array looking negative
while imaging Flaw 5 ..................................................... E-44
Figure E-75 Flaw 5 seen with an 18.5 L-wave looking
negative ........................................................................ E-44
Figure E-76 Flaw 5 seen with a 32 S-wave looking
negative ........................................................................ E-45
Figure E-77 Approximate location of array looking positive
Figure E-78 Flaw 5 seen with a 29.5 L-wave looking
positive ......................................................................... E-46
Figure E-79 Flaw 5 seen with a 32 S-wave looking positive .... E-46
Figure E-80 Approximate location of array looking negative
Figure E-81 Flaw 6 seen with an 18 L-wave looking
negative ........................................................................ E-47
Figure E-82 Flaw 6 seen with a 31.5 S-wave looking
negative ........................................................................ E-48
Figure E-83 Approximate location of array looking positive
Figure E-84 Flaw 6 seen with an 18 L-wave looking
positive ......................................................................... E-49
xvi
Figure E-85 Flaw 6 seen with a 30.5 S-wave looking

positive ......................................................................... E-49
Figure E-86 Drawing of calibration block K8939-1 ................. E-51
Figure E-87 End view of calibration block K8939-1................. E-52
Figure E-88 Bottom view of calibration block K8939-1 ............ E-52
Figure E-89 Photograph of the grain structure for calibration
block K8939-1 .............................................................. E-53
Figure E-90 Image comparing PM/HIP and CSS L-wave
corner reflectors ............................................................. E-54
Figure E-91 Image comparing PM/HIP and CSS S-wave
corner reflectors ............................................................. E-54
Figure E-92 Image comparing PM/HIP and CSS L-wave
EDM notch reflectors ...................................................... E-55
Figure E-93 Image comparing PM/HIP and CSS S-wave
EDM notch reflectors ...................................................... E-55
xvii
List of Tables
Table 4-1 Chemical composition for the 316L stainless steel
valve body (values in wt%) .............................................. 4-11
Table 4-2 Room temperature tensile test results for the 316L
stainless steel valve body ................................................ 4-12
Table 4-3 Elevated temperature (600F) tensile test results
for the 316L stainless steel valve body .............................. 4-12
Table 5-1 Chemical composition of S31603 (316L)
manufactured components................................................. 5-2
Table 5-2 Chemical composition for one Grade 91 valve
body manufactured during this project (values in wt%) ......... 5-5
Table 5-3 Elevated temperature tensile test results for one
Grade 91 valve body manufactured during this project ........ 5-6
Table 5-4 Chemical composition for the IN625 valve body
manufactured during this project (values in wt%).................. 5-7
Table 5-5 Elevated temperature tensile test results for the
IN625 valve body manufactured during this project ............. 5-8
Table A-1 Representative quality controls ................................ A-2
Table E-1 Automated examination detection results.................. E-29
Table E-2 Manual examination detection results ...................... E-30
xix
Section 1: Introduction
Research Context
Powder metallurgy (PM) technology, integrated with advanced modeling/design
capabilities and applied in conjunction with state-of-the-art hot isostatic
processing (HIP) technology, can have a significant impact on the energy
industrys goals of increased efficiency, reduction of emissions, and lower
installation and operating costs. The manufacturing of large, pressure-retaining
components with PM/HIP technology can provide an alternative method to
current processes such as forging and casting for complex parts. Benefits of
making near-net shapes (NNSs) via PM/HIP include precise chemistry control
for any stainless steel, low-alloy steel, and nickel/cobalt alloys; increased material
utilization; elimination of many welding repairs; and improvement in
inspectability.
The purpose of the research effort documented in this report is to conduct the
necessary processing, manufacturing, and evaluation studies of this novel method
for manufacturing very large, complex near-net shapes for use in electrical power
generation equipment. This technology has the potential to increase plant
reliability and safety, reduce manufacturing energy use and processing waste, and
provide a new domestic supply base for the electrical generation industry. The
proposed process will demonstrate a significant advancement in manufacturing
methodology for the large, pressure-retaining components required for current
and advanced fossil and nuclear power plants. The technology is transformational
in nature and would shift the current technology base for manufacturing these
components from forging and/or casting to a more cost-effective powder
metallurgy processing technology. It is anticipated that fabrication and processing
energy costs can be reduced by more than 20% over conventional processes, while
deployment of these components can be significantly accelerated.
The project goals are consistent with industry and the Electric Power Research
Institutes (EPRIs) Sector Council strategic objectives to meet the growing
energy demand through promotion of both advanced coal and nuclear power
plants, improvement in plant efficiency and safety (via inspection), and
enhancement of plant availability. It is anticipated that large, complex
components could be produced for nuclear, fossil, ultra-supercritical, heat
recovery steam generator, and oxy-combustion plant applications including pump
housings, valve bodies, sweepolets, tees, flanges, steam chests, nozzles, elbows,
turbine casings, canister plugs, and other components that are currently cast for
power plant use.
1-1
Successful development and demonstration of the PM/HIP technology will

benefit other industries that use large components, including gas, oil, chemical,
process, steel, transportation, and shipping industries. Furthermore, entirely new
markets could be created with the new PM/HIP process, as parts/components
can be designed in an NNS condition for a specific use or application. It is
anticipated that the sustainable manufacturing technology will enable new
markets in the United States and abroad exceeding hundreds of millions of
dollars annually.
PM technology would minimize or eliminate current issues associated with
microstructural and mechanical property uniformity, welding difficulties, heat
treatment problems, and inspectability in large components. It would also
provide an ideal path for manufacturing, addressing a short-term need for
domestic fabrication of complex components. In addition, PM technology would
increase material utilization (thereby reducing energy utilization on a per
component basis), reduce machining operations, and significantly reduce
manufacturing and delivery times. PM technology could allow the use of new
alloy systems with high-temperature strength, creep resistance, and
corrosion/erosion resistance that will enable power generation systems to operate
at higher temperatures and pressures and for longer periods of time, which will
measurably increase plant efficiency and availability. Once accepted, PM
technology would provide additional longer-term transformation opportunities
by custom tailoring alloy compositions or manufacturing bi-metallic components
for specific applications.
It is important to highlight the considerable research that has been completed
over the last decade to characterize PM/HIP for potential use in nuclear
applications. Specifically, Rolls-Royce has conducted research on the
development of data for 316L stainless steel (SS) to be used in nuclear
components [15]. The Rolls-Royce research has shown that 316L SS
components (thick-section tees, large valves, valve seat inserts, thin-walled
toroids, and so on) can be effectively produced with the PM/HIP process,
resulting in high-quality components with superior mechanical and
microstructural properties. Rolls-Royce has also explored the use of Inconel 600
and 690 powders for component manufacture [6].
Carpenter Technology, in addition to supplying gas atomized powder for many
PM/HIP applications, has evaluated consolidated PM components with regard
to mechanical properties, corrosion resistance, and other aspects. The
components were manufactured from stainless steels, borated stainless steels,
duplex stainless steels, and various high-temperature alloys. In all cases, the PM
materials met or exceeded the capabilities of cast or cast and wrought materials.
Numerous examples are available [712].
1-2
Research has also been undertaken by the VTT Technical Research Centre of
Finland and Helsinki University [13,14]. Their research includes manufacture
and assessment of duplex stainless steels for paper machine roll applications,
nitrogen-containing austenitic stainless steels for wear applications, and 316LN
austenitic stainless steels for light water reactor applications, as well as
investigation of oxide dispersion strengthened (ODS) alloys.
ASTM currently recognizes two standards for producing HIP alloy (ASTM
A989-11) and stainless steel (ASTM A988-11) flanges, fittings, valves, and parts
for high-temperature service applications [15,16]. Finally, a number of EPRI
papers present information on powder metallurgy and HIP applications in the
power industry [1720].
References
1. W.B. Burdett, P. Hurrell, and A. Gilleland, Hot Isostatic Pressing of Type
316L Powder for Pressure Retaining Components, ASME PVP-2004,
July 2529, 2004, San Diego, California, MK-04-031.
2. W.B. Burdett and C.T. Watson, Hot Isostatic Pressing of Type 316L
Powder for Pressure Retaining Components, ASME PVP-2005,
July 1721, 2005, Denver, Colorado, PVP 2005-71711, p. 7.
3. J.L. Sulley and I.D. Hookham, Justification and Manufacturing Quality
Assurance for the Use of Hot Isostatically Pressed, Reactor Coolant System
Components in PWR Plants, Proceedings of ICAPP08, Anaheim,
California, June 812, 2008, Paper 8110, pp. 820.
4. I. Hookham, B. Burdett, K. Bridger, and J.L. Sulley, Hot Isostatically
Pressed (HIPed) Thick-Walled Component for a Pressurized Water Reactor
(PWR) Application, Proceedings of ICAPP09, Tokyo, Japan, May 1014,
2009, Paper 9389, p. 7.
5. J.L. Sulley, I.D. Hookham, B. Burdett, and K. Bridger, Introduction of Hot
Isostatically Pressed Reactor Coolant System Components in PWR Plants,
Proceedings of the 18th International Conference on Nuclear Engineering,
ICONE 18, Xian China, May 1721, 2010, ICONE 18-30253.
6. T. Jelfs and B. Burdett, Hot Isostatic Pressing of Inconel 600 and 690
Powders for Pressure Retaining Components, ASME PVP 2011,
July 1721, 2011 Baltimore Maryland, PVP2011-57194.
7. L.W. Lherbier and J.F. Radavich, An Evaluation of PM Waspaloy,
Proceeding of 11th International Symposium on Advanced Superalloys
Production and Application, May 2125, 2007, Shanghai, China.
8. L.W. Lherbier and D.J. Novotnak, Effect of Thermal History on the
Properties and Microstructure of Large Hiped PM Superalloy Billet,
Proceedings of 11th International Symposium on Superalloys, September
1418, 2008, Champion, Pennsylvania.
9. A. Eklund et al., Corrosion Properties of PM Hiped Stainless Steel, 15th
Nordic Corrosion Congress, May 1921, 2010, Stockholm, Sweden.
1-3
10. J. Scanlon et al., Mechanical Properties of PM Hiped Stainless Steel A

Comparison to Conventional/Rolled Material, PowderMet 2010
Conference, June 2730, 2010, Hollywood, Florida.
11. B. Bengston et al., Mechanical Properties of PM Hiped Stainless Steels,
Stainless Steel World Conference, October 57, 2010, Houston, Texas.
12. D.J. Novotnak, L.W. Lherbier, and D.W. Gandy, Manufacturing Large
Complex PM HIP Shapes, Euro PM 2011 Conference, October 912,
2011, Barcelona, Spain.
13. S. Tahtinen, In-Vessel Materials Studies at VTT, VTT Industrial Systems,
Association Euratom-Tekes, Annual Seminar, Paasitorni, Helsinki,
May 3031, 2005.
14. A. Pertti and H. Hanninen, personal communication, July 4, 2011.
15. ASTM Standard A988/A 988M-07, Standard Specification for Hot
Isostatically-Pressed Stainless Steel Flanges, Fittings, Valves, and Parts for
High Temperature Service.
16. ASTM Standard A989/A 989M-07, Standard Specification for Hot
Isostatically-Pressed Alloy Steel Flanges, Fittings, Valves, and Parts for High
Temperature Service.
17. D. Gandy et al., Powder Metallurgy Methods for Producing Nuclear and
Fossil Components, EPRI Advanced Materials Conference, Santa Fe, New
Mexico, October 2010.
18. D. Gandy et al., Powder Metallurgy Methods for Producing Nuclear and
Fossil Components, ATI Corrosion Solutions Conference, 2011
Proceedings, Lake Louise, Alberta, Canada, Paper 7E.
19. D. Gandy, J. Siefert, and J. Shingledecker, Overcoming the Barriers for
PM/HIP Technology in Large Nuclear and Fossil Components, ASM
InternationalAdvanced Materials & Processes, Volume 170, No. 1,
January 2012.
20. D. Gandy et al., Powder Metallurgy Methods for Producing Components,
Stainless Steel World, November 2011.
1-4
Section 2: What Is Powder Metallurgy?

Powder metallurgy (PM) is a metal forming process that generates a product
form different from the more familiar forms such as forgings, plate, and castings.
In this process, metal powder is formed into a specific shape, compacted, and
sintered by heating to fuse the metal particles together. Historically the resulting
product was limited in density and internal coherence by the quality of the metal
powder used. However, modern processing by inert gas-shielded atomization of
the metal to powder followed by hot isostatic pressing (HIP) allows production
of near-net shapes to near maximum theoretical density. The resulting products
can have mechanical properties as good as or better than forgings or castings of
the same alloy. This process is often used for high-strength alloys and refractory
alloys that are difficult or impossible to form by forging or rolling. The process
consists of a forming and fabrication technique that is performed in multiple
stages, which include 1) component design, 2) manufacturing of a metallic
powder, normally by gas atomization, 3) loading of the powder into a mold or die
with a packing density of 6070%, 4) degassing and sealing the mold with the
contained powder, and 5) consolidation by applying high temperature and
pressure (hot isostatic pressing). During the HIP process the metal powder is
consolidated by a solid state diffusion process that produces fully dense
microstructures with no porosity.
Process Overview
Component Design
Component design includes creation of a 3-D model for the desired component
or shape. In some cases, such as for production of high-strength tool steels, the
shape can be a simple rectangular solid from which the finished tool shapes are
created by subsequent machining. However, it is also possible to make complex
shapes such as pump or valve bodies for which the amount of machining required
to produce the final form is very limited. Consequently, the process can be very
efficient with respect to the amount of raw material used. With the model
completed, a mold or container that replicates the final component can be
produced to contain the powder (more information on this subject follows later).
Through utilization of the PM/HIP process, the manufacturer is able to target a
specific composition that allows for fine control of specific elements to achieve
desired materials attributes.
2-1
Powder Production
Metal powders are produced for various applications such as metal forming by
powder metallurgy techniques and welding processes such as plasma arc welding
and laser welding. Metal powders can be produced by mechanical or chemical
methods. Processes commonly used include gas or water atomization, milling,
mechanical alloying, electrolysis, and chemical reduction of oxides. However,
some of these processes introduce contaminants into the powder, particularly
metal oxides. Over the last 50 years, atomization by the various techniques has
become the dominant process of metal powder production. Atomization is
simply the breakup of a liquid into fine droplets. Most atomization of metals is
performed as either water atomization or gas atomization with the gas being air,
nitrogen, argon, or helium. Other atomization techniques include centrifugal
atomization, vacuum or soluble-gas atomization, and ultrasonic atomization.
Water atomization is most commonly used because of high productivity and low
cost. In water atomization, jets of high-pressure water are directed at a stream of
molten metal flowing from a reservoir (called a tundish). Atomization occurs
from momentum transfer as water droplets impinge on the molten metal stream.
The metal droplets are rapidly quenched, and the metal particle/water mixture
forms a slurry in the bottom of the chamber. The slurry is subsequently subjected
to drying operations to produce the metal powder. Although the process is
efficient, the powder produced consists of relatively irregularly shaped particles
with some oxide contamination. Gas atomization, on the other hand, tends to
produce spherically shaped particles that, if inert gas is used, are oxide free.
However, gas atomization tends to be more expensive because of the process
media (water costs less than argon, for example), and productivity can be limited
by such things as gas nozzle plugging.
Currently, high-quality powders are routinely manufactured by inert gas
atomization. A typical powder production sequence is illustrated schematically in
Figure 2-1. Continuous improvements in gas nozzle design and other features of
the gas atomization equipment have resulted in processes that can perform
reliably on a daily basis. The produced powders are generally free of oxides and
other contaminants. In this process, a material is induction melted at a high
temperature and forced through an orifice (nozzle) at moderately high pressures
(see Figure 2-2). A gas is introduced into the molten metal stream just as it leaves
the nozzle, creating significant turbulence as the entrained gas expands (from
heating). The gas/metal mixture exits into a large collection volume outside of
the orifice. The collection volume is filled with inert gas to promote further
turbulence of the molten metal and avoid the introduction of oxygen. As
individual liquid metal droplets are formed, they tend to become spherical from
surface tension and then solidify in that shape. Gravity or cyclonic separation is
used to separate the resulting powder particles of varying sizes from the gas. The
resulting powders are predominantly spherical particles of a size range dictated by
the nozzle design and the gas/metal flow ratio. Particle size typically follows a log
normal distribution.
2-2
Figure 2-1
Typical powder production sequence
Figure 2-2
Inert gas atomization chamber
After removal from the atomization chamber, the metal powder is sieved through
size-graded screens to separate the powder into various size ranges (see Figure
2-3). Different size ranges of powders are optimum for different forming
processes or welding processes. For example, metal injection molding (MIM)
requires relatively fine powders, whereas for plasma or laser welding relatively
large particle sizes are preferred. For parts formed by HIP, the raw powder is
screened to remove oversize particlestypically particles greater than 500 m
(0.020 inch) in diameter. Other applications may require sieving to both a
maximum and minimum diameter particle size. The sieved powder is then
blended to produce a uniform powder size distribution. At this point, if a large
volume of material is required, more than one heat of material having the same
nominal chemistry may be blended.
2-3
Figure 2-3
Powders produced by gas atomization (figure courtesy of Carpenter Powder
Products)
It is important to note that powders produced by inert gas atomization are

consistently higher in quality than those produced through powder milling or
most other processes. Accordingly, oxidation issues (porosity, oxide inclusions,
lack of bonding of particles) associated with earlier powder metallurgy processes
are significantly reduced and in most cases eliminated entirely.
Molding (or Container)
The third step in the PM/HIP process is the manufacture of a mold or container
that is used to contain the atomized powder during the HIP operation. This
container is often referred to as a can and in fact is defined as such in Paragraph
3.1.1 of ASTM A988. The can is manufactured to the desired shape of the
finished part, but somewhat larger than the finished dimensions to allow for
compaction and consolidation of the powder in the HIP process. The container
design and dimensions are based on the component design drawings established
at the beginning of the process. For stainless steel and nickel base alloys, a thin
mild steel (typically 0.01% maximum carbon) is most commonly used to
construct the container. This material is very ductile at HIP temperatures and is
thus able to move inward with the powder as it consolidates into a solid piece.
Carbon content of the mild steel may be limited to reduce potential for
carburization of the stainless steel or nickel alloy. A container used to produce a
Type 316L valve body is shown in Figure 2-4. Following the HIP process, the
mild steel container is readily removed by acid etching. The acids used have no
2-4
effect on the stainless steel or nickel alloy other than passivation of the surface.
Removal can also be done by machining if the part is of a shape amenable to
machining. Carburization of stainless steel or nickel alloy surfaces is not a
concern because the carbon content of the can material is maintained at such a
low level. With a very low carbon gradient across the interface there will be very
little carbon transport, and what does occur could be toward the can material
rather than into the stainless steel or nickel alloy.
Figure 2-4
Container for a stainless steel valve body (figure courtesy of Carpenter Powder
Products)
Powder Consolidation, Vacuum Processing, and Hot Isostatic

Pressing
Metal powders are consolidated without melting by a number of processes,
including cold pressing, forging, extrusion, and sintering. However, most of these
processes produce materials that are free of voids and defects; these materials
approach 100% theoretical density. Hot isostatic pressing, on the other hand, is
capable of fully fusing clean metal powders to maximum density. It is well known
that if bare metal surfacesthat is, surfaces free of oxidesare brought into close
contact in an inert atmosphere at a sufficiently high temperature, bonding will
occur. This bonding takes place by diffusion of metal atoms across the interface
such that they become intermixed and atomically bonded. In the process, the
interface boundary is eliminated. Melting, as occurs in welding processes, is not
required to create a diffusion bond, but mechanical pressure can facilitate the
process. HIP was originally developed by Battelle Memorial Institute in 1955 for
the purpose of creating a diffusion bond between dissimilar materials (zircaloy
bonded to uranium dioxide for nuclear fuel elements) [1]. Subsequently, in the
1960s the process was adapted to production of parts and shapes of beryllium,
refractory alloys, ceramics, and other materials that are difficult or impossible to
hot form. In the 1970s large-scale commercial furnaces were developed that
allowed expansion of the process to tool steels, titanium alloys, stainless steels,
and nickel alloys. In addition to being used in consolidation of powder metallurgy
products, HIP is routinely used to improve casting quality by reducing and fusing
2-5
voids and porosity. The PM/HIP process is heavily used by the aerospace
industry, particularly for producing titanium alloy and superalloy components for
aircraft engines. For pressure-retaining applications, ASTM has issued a
standard for PM/HIP processing of stainless steel alloys [2]. It is noteworthy that
this specification requires completed parts to have density of at least 99% of the
same alloy in wrought form. Alternately, in a microstructural examination, no
voids or porosity are allowed.
The powder consolidation and HIP process is described as follows: The inert gas
atomized powder is packed into the mold/container that has been constructed to
the desired shape and dimensions as described above. Typically, mechanical
vibration is used to tightly pack the powder into the container to about 70%
density. For HIP processing, powders having a range of sizes are preferred, to
allow smaller-diameter particles to pack in tightly between larger particles.
Spherical particles, as produced by inert gas atomization, are preferred for this
application because they flow and compact to a higher density than irregularly
shaped powders. The container is then evacuated of air by a vacuum pump and
sealed. After leak checking, the vacuum sealed container is then placed in the
HIP furnace. This furnace is specially designed and constructed to
simultaneously heat the container(s), and the metal powder therein, and at the
same time apply a high isostatic gas pressure. Consequently, the furnace is also a
high-temperature pressure vessel. A typical HIP furnace arrangement is shown
schematically in Figure 2-5, and a large commercial furnace is shown in Figure
2-6. In the process version illustrated in Figure 2-5, water jacket cooling is used
to moderate the temperature of the pressure vessel wall. Argon is normally used
to apply the isostatic pressure. After loading of the containers into the furnace, it
is sealed, flooded with argon, brought to temperature, and pressurized.
2-6
Figure 2-5
HIP furnace/vessel arrangement (figure courtesy of Carpenter Powder Products)
Figure 2-6
Large commercial HIP furnace/vessel (figure courtesy of Avure.com)
2-7
Depending on alloy type, holding temperatures in the HIP furnace range from
500 to 1200C (900 to 2200F). Again, depending on alloy type, argon pressures
can range from 7,000 psi to 45,000 psi (48 MPa to 310 MPa), with 15,000 psi
(103 MPa) being the most common for stainless steels and nickel alloys as well as
alloy steels. The furnace is held at the assigned temperature and pressure for a
time sufficient for the powder to compact and the powder particles to bond to
each other, creating a solid metal part. Initially, as the powder is mechanically
compacted under the isostatic pressure, some plastic deformation of the powder
particles occurs, thereby reducing the void spaces that exist between spherical
particles. Thereafter, necks begin to form by solid state diffusion between
particles where the interfaces have been brought into close contact. This bonding
readily occurs at the HIP furnace temperature because the oxide-free particles
produced by the inert gas atomization process are in vacuum. Contact between
the particles is pure metal-to-metal under pressure, and diffusion rates are
relatively high. At the same time, some creep deformation is occurring, bringing
more and more of the particle surfaces into contact. As the particles grow
together in the final densification stage, randomly distributed voids are
eliminated. In the final phase of consolidation, a polycrystalline structure
develops, and some grain growth occurs. The old interface boundaries between
the powder particles are completely eliminated in the process. Following cooldown and removal from the HIP furnace, the parts may be subjected to
additional heat treatment if required. ASTM A988 requires that austenitic
stainless steels such as 316L be subjected to a final solution anneal at 1900F
(1040C) minimum followed by liquid quenching to below 500F (260C). Other
alloys may require different final heat treatments. For example, a low-alloy steel
such as ASME SA-508, Grade 3, Class 1 would be reaustenitized, quenched,
and tempered.
Characteristics of PM/HIP Products (Produced from Inert Gas
Atomized Powders)
Oxide Inclusions and Porosity
As discussed above, powders produced by inert gas atomization are essentially
free of surface oxidation on individual particles. Consequently, the only source of
oxides in the finished product is any oxidation that may occur at ambient
temperatures prior to the powder being put in the mold/container for the HIP
operation. If excessive surface oxidation of powder particles were to occur, it
could interfere with the consolidation process, leading to lack of bonding of
particles, residual voids and porosity, and oxide inclusions. For stainless steels and
nickel alloys, there is no concern, because these alloys contain significant
quantities of chromium. When exposed to air, alloys containing chromium
rapidly form a thin chromium oxide layer (called a passive layer) on the surface
that stops oxygen transport to the metal interface. This prevents further oxide
growth. This chromium oxide layer, when formed at ambient temperature in air,
is on the order of 13 nm (130 angstroms) thick [3]. This is much less than the
wavelength of visible light and as such cannot be seen with the naked eye. In fact,
this oxide layer is too thin to be observed with optical metallography. As a result,
when inert gas atomized stainless steels or nickel alloy powders are consolidated
2-8
under vacuum in an HIP furnace, the amount of oxide incorporated into the
finished part is small, is widely dispersed, and cannot be seen by conventional
optical metallography. For low-alloy steels with relatively low chromium content,
oxidation (rusting) in ambient air can occur. The rate is dependent on the
ambient temperature and humidity. This is usually not a concern, because after
powder production the low-alloy steel powder is most often immediately moved
on to the canning operation described above, whereby the loaded can is sealed
under vacuum. However, because oxidation can occur in a relatively short time
with low-alloy steels, in-house controls are applied to powder handling. For
example, if the powder will not be canned within a set time, storage under an
inert atmosphere may be required. As with stainless steel and nickel alloys,
significant oxide inclusions or porosity are not observed by optical metallography
in low-alloy steel parts produced by PM/HIP using inert gas atomized powders.
Mechanical Properties
Mechanical properties of parts produced by PM/HIP are essentially the same as
those observed for the same alloy in wrought form. ASTM A988 requires the
same minimum ultimate strength, yield strength, and ductility for Types 304,
304L, 316, or 316L required for A182 forgings or A240 plate. Actual testing of
Type 316L, as described later in this report, produced mechanical properties that
easily exceeded the minimum properties specified by ASME for several heats of
material [4]. This is most likely attributable to the fine grain structure observed
for parts produced by PM/HIP. Also, the fine grain structure contributes to a
higher bulk hardness than typically observed for annealed 316L. However,
elevated surface hardness will not be present as may be found if the surface layer
is carburized, because as discussed above, the potential for carburization of
surfaces is very limited by the specified low carbon content of the can material.
Given these observations, it is expected that other austenitic alloys will exhibit
similar behavior. That is, the properties will meet or exceed the minimums
specified for wrought versions of the same alloy. For low-alloy steels, assuming
complete consolidation and recrystallization occurs, mechanical properties of the
finished parts will be controlled by the final heat treatment applied
(reaustenitizing, quenching, and tempering) rather than by the PM/HIP process.
Microstructure and Corrosion Properties
When examined by optical microscope, the microstructure of material produced
by PM/HIP shows a fine-grained, equiaxed structure that is very similar to a
wrought product of the same alloy. This is particularly true for austenitic stainless
steels. On the other hand, there are no similarities between the microstructure of
a PM/HIP processed austenitic stainless steel and an as-cast microstructure of
the same alloy type, and in particular there is a complete absence of ferrite. Figure
2-7 compares a micrograph of wrought 316L and a micrograph of 316L
produced by PM/HIP. Both show a microstructure typical of an unstabilized
wrought 300 series stainless steel. The structure shows equiaxed austenitic grains
with some twinning. The PM/HIP sample shows complete fusion of the
2-9
individual particles with no residual voids, porosity, or grain boundary oxides.

Although there is a minor difference in magnification in these two micrographs,
it can be seen the PM/HIP processed material has much finer grain size than the
wrought 316L.
a) 316L produced by PM/HIP
b) Typical wrought 316L (note minor difference in magnification, approximately 12%)
Figure 2-7
Comparison of microstructures of PM/HIP 316L and wrought 316L
2-10
There are a number of other features associated with the material produced by
PM/HIP that compare favorably relative to wrought product:
The structure is isotropic in all directions. That is, there is no texturing,

layering, or laminations as are often seen in heavy forgings or plate.
Consequently, the mechanical properties are the same in all directionsthat
is, there is no reduced strength in the short transverse direction as is
frequently seen in some plate and forgings.
There are no significant non-metallic inclusions such as manganese sulfides

as are often seen in plate and forgings. Such inclusions can affect mechanical
properties and act as sites for corrosive attack.
The chemistry is entirely uniform through the whole piece. Because the
material is not melted in forming the part, there is no potential for
segregation to occur. In wrought products the melted material is first cast
into an ingot where chemical segregation can occur as the ingot freezes (the
center freezing last). This segregation can carry over into the wrought form
as the material is hot worked into the final shape, especially if the working
ratios are not high. As the ingot is freezing, non-metallic impurities are
concentrated in the liquid that freezes last, thereby concentrating higher
levels of inclusions and impurities in the center. This cannot occur in a piece
produced by PM/HIP.
No residual delta ferrite as can be found in wrought products. Delta ferrite

forms at high temperatures as the stainless steel is freezing. Although it is not
stable at lower temperatures, wrought products may retain some delta ferrite,
depending on hot working temperatures and working ratios.
As noted above, the grain size of the PM/HIP piece is fine and very uniform.
Heavy section wrought products can develop large, non-uniform grain sizes
as the material is subjected to multiple heat-up cycles for hot working.
Large-grained material, or material with regions of large grains, can have
reduced mechanical properties and be difficult to inspect ultrasonically.
Stainless steel produced by PM/HIP has been demonstrated to be very
transparent to ultrasound and therefore very amenable to ultrasonic
inspection.
Although relevant corrosion data such as stress corrosion crack (SCC) growth
rates are not currently available for austenitic alloys produced by PM/HIP,
corrosion properties can be inferred from observations of the chemistry and
microstructure. Because the chemistry is the same as in wrought versions of the
alloys in question, general corrosion resistance may be expected to be essentially
the same. Chromium-bearing alloys in particular may be expected to readily form
a protective chromium oxide film on the surface that will retard further oxidation
and corrosion. The general lack of non-metallic inclusions, particularly sulfides,
in the PM/HIP processed material also means that there is an absence of
pathways for corrosive attack at exposed surfaces. With respect to stress corrosion
cracking behavior, it is expected that the PM/HIP processed material will
certainly be no more susceptible than the comparable wrought version of the
2-11
alloy. Because of the favorable microstructural features described above, including

the uniform fine grain size, one may in fact expect somewhat superior behavior
relative to the typical wrought alloy. Fine grain size is generally considered to be
beneficial with respect to SCC resistance [5,6].
Process and Product Controls
There are basically two types of controls that may be applied to the PM/HIP
process: in-process controls and end product controls. From the point of view of the
purchaser, the most straightforward controls are those applied by specification of
measurable attributes of the end productfor example, chemistry, mechanical
properties, density, and microstructure. The requirements for these attributes are
dictated by the demands that will be placed on the material when it is put in
service and are known to the material purchaser. In-process controls, on the other
hand, are typically developed and applied by the material manufacturer. The
material manufacturer may not necessarily know the operating conditions
(temperature, loads, environment, and so on) that the material will experience,
but the manufacturer does know the material attributes required by the
purchaser. Therefore, the manufacturer applies in-house controls that have been
found to be necessary to be assured that the material produced will comply with
the purchaser-specified end product requirements.
Process Controls
It is the objective of the material manufacturer to produce a product that
conforms to the purchasers specification as efficiently as is practical. As a
material manufacturing process is developed and initially applied at a specific
facility, the material manufacturer identifies process variables and steps that need
to be controlled in order to consistently produce a product of acceptable quality.
Such controls may vary depending on the specific techniques being applied and
the equipment being used in the individual manufacturing shop. Detailed
controls will also vary depending on the specific material being processed. As the
process matures, these in-house controls are refined and entered into the material
processing procedures used on the shop floor. With a few exceptions, it is
impractical for the material purchaser to specify these kinds of controls, because
it requires knowledge unique to the manufacturing shop and process being used.
In-process controls for production of PM/HIP processed parts may include, but
are not limited to, the following:
Powder Processing
Analysis of raw stock to verify that the chemistry complies with end product
requirements
Cleaning/maintenance/inspection of the atomization mechanism
Sieving of powder to a specific mesh size to remove oversize particles
Restricted blending of powders (each heat of powder in the blend must

comply with final chemistry requirements)
Storage of powder under a nitrogen or inert gas atmosphere

2-12
Canning
Controlled carbon content of can material to limit potential for carburization

of parts
Limiting of can welding to non-flux processes with inert gas back purge to
avoid slag and oxide entrapment
Visual inspection of can welds, including the root side, to verify absence of
oxidation
Vibratory compaction of powder in the can
Specified vacuum level in can prior to sealing
Helium leak check of can after evacuation and sealing
HIP Process
Control, monitoring, and recording of furnace temperature using calibrated

thermocouples
Control, monitoring, and recording of argon pressure using calibrated

pressure gauges
Analysis of sample from fill tube for argon ingress
Visual examination of can for abnormalities after removal from furnace
Dimensional check of parts after can removal
The controls listed above may vary between different material manufacturers or
within an individual manufacturing shop, depending on the material type being
processed. For example, superalloys for aerospace components may require
sieving to a finer powder size. Application of inert atmospheres for handling and
storage of powder may vary considerably for specific material types and local
atmospheric conditions. In any case, each material manufacturer applies the inprocess controls the manufacturer deems necessary to be certain the parts
produced will conform to all the customer-specified requirements. Conversely,
end product requirements specified by the purchaser for the same material and
component will not vary between manufacturers.
Although the material purchaser tends to specify end product requirements, there
are often some process requirements that are considered to be universal and
important enough to include in the purchase requirements. For example, final
heat treatment after PM/HIP processing may be required; heat treatment
parameters are specified (see Table 2 of ASTM A988). Another example may be
(for austenitic stainless steel and nickel alloys) specification of the maximum
carbon content of the can material. For a more complete listing of typical
PM/HIP process and product controls, see Appendix A.
2-13
Product Controls
As noted above, product controls are normally defined by the material purchaser,
either directly in the purchasing documentation or by invoking a standard
specification, or both. These controls usually specify measurable attributes of the
material or require nondestructive examinations. They may be as simple as
verifying that all specified dimensions have been met, or as involved as a detailed
100% ultrasonic examination. Many of these types of product controls are
typified by those contained in the ASTM specification for PM/HIP processed
stainless steel, A988. Common product controls that the purchaser may apply are
listed below. For specific applications, material types, or products, additional
requirements may be applied.
Verification of dimensions using calibrated measuring instruments and tools.
Chemical analysis of samples taken from finished parts or prolongations of

finished parts.
Density checking to verify freedom of microporosity (density > 99% wrought

product density).
Examination of microstructure at high magnification to confirm that the

parts are free of voids, laps, cracks, or porosity (A988 requires examination at
2050X, 100200X, and 10002000X).
Mechanical properties tests with minimum requirements the same as for the
equivalent wrought version of the alloy.
Hardness test with maximum hardness specified.
Grain size control with maximum grain size specified.
Corrosion tests (for example, for austenitic stainless steel ASTM A262,
Practice A or E, or ASTM Method G48).
Surface examination by liquid penetrant or magnetic particle testing as

appropriate to the material type (for example, ASME Section III, NB-2545
or NB-2546).
Ultrasonic testing (for example, for pressure boundary parts ASME Section
III, NB-2540 or NB-2550 as required). Radiographic testing may be applied
in some cases as an alternate.
Hydrostatic testing of pressure boundary parts.
References
1. ASM Handbook, Volume 7, Powder Metal Technologies and
Applications, ASM International, 1998.
2. ASTM A988, Standard Specification for Hot Isostatically-Pressed Stainless
Steel Flanges, Fittings, Valves, and Parts for High Temperature Service.
3. What Makes Stainless Stain-less,
http://www.estainlesssteel.com/corrosion.shtml, accessed March 2012.
4. ASME Boiler and Pressure Vessel Code, Section II, Part D, 2010 Edition.
2-14
5. G. Palumbo, P.J. King, P.C. Lichtenberger, K.T. Aust, and U. Erb, Grain
Boundary Design and Control for Intergranular Stress-Corrosion
Resistance, Scripta Metallurgica et Materialia (USA). Vol. 25, no. 8,
pp. 17751780. August 1991.
6. C. Cheung, U. Erb, and G. Palumbo, Application of grain boundary
engineering concepts to alleviate intergranular cracking in Alloys 600 and
690, Materials Science and Engineering, A185 (1994) 3943.
2-15
Section 3: Why Consider PM/HIP for

Large Nuclear and Fossil
Components?
Large power generation components are commonly fabricated by conventional
tried-and-true metallurgical processing methods, including casting, rolling,
drawing, forging, extrusion, welding, and heat treatment. These processes have
been used to fabricate components since the early part of the 20th century. As
materials processing practices have improved, higher-quality components have
also resulted, such as superclean forged rotor and disc steels, directionally
solidified and single-crystal blade alloys, controlled residual element alloys, creepstrength enhanced ferritic piping/headers, and improved component surfacing
techniques. One area that has seen remarkable improvements in processing
technology is powder metallurgy, with dramatic increases in component quality,
availability, and size over the past 25 years.
Atomized powder production facilities currently exist to manufacture large
quantities (tonnage) of powder for high-quality alloy steels, stainless steels, and
nickel base alloy parts. HIP facilities are also available to manufacture large
shapes, which have been demonstrated to a limited extent for specialized
aerospace, oil exploration, tools, and other niche applications. High-quality
components showing good structural uniformity, no segregation, superior
mechanical properties, and ease of inspectability have been produced from a
number of stainless steels and nickel base alloys.
Large PM-produced components have not been utilized in the power generation
industry to date, primarily because of three technical barriers:
The sizes and shapes for near-net shaped components have only recently
reached a point for consideration and have not been tailored for the
compositions/alloys that are of most interest to the power industry.
Materials and processes used to manufacture pressure-retention or hightemperature power plant components are generally subject to (in the United
States) the ASME Boiler and Pressure Vessel Code, which currently does
not allow the use of PM-produced components for the desired applications.
3-1
For iron base steel alloy systems, the PM/HIP production route is generally
more expensive than traditional forging and casting routes. For stainless
steels and nickel base alloys, where raw material costs are much higher,
PM/HIP appears to be a cost-effective solution.
These barriers can be overcome through focused research. EPRI, in conjunction

with partners Carpenter Technology, Rolls-Royce, Tyco Valves, and GEDresser, has set out to explore how and where PM technologies might be
brought to the power industry. PM technologies exhibit several attributes that
make them attractive to the power industry:
They eliminate inspectability issues and concerns.
They enable manufacture of large, complex components using near-net shape

(NNS) technologies.
They enable new alloy systems and targeted chemistries.
They enhance weldability.
They provide an alternate supply route for long-lead-time components.
They eliminate rework or repair of large cast components.
Inspectability. Inspection of large cast components such as pump housings, valve

bodies, elbows, flanges, sweepolets, steam chests, turbine casing shells, nozzles,
and canister plugs is challenging because of the non-homogenous microstructure
within castings. Castings can contain voids, pockets, segregation of tramp
elements, inclusions, hot tears, secondary phases, and non-metallic particles.
These irregularities in the microstructure make inspection of cast components
difficult. The use of PM to produce alloys and components results in uniform,
homogeneous microstructures that are demonstrated to be very inspectable in
terms of both detection and sizing.
Near-Net Shape (NSS) Components. One of the highly desirable attributes of
producing components via PM/HIP processing methods is the ability to produce
components in an NNS condition that requires only minimal machining and
clean-up. Cast components are commonly fabricated in an over-sized condition
to allow for irregularities that may occur through thickness of the component.
Components produced with PM/HIP can be produced in very near final shape,
resulting in reduced component weight, reduced machining, and ultimately dollar
savings in the overall production of the component. Manufacture by NNS
technologies also reduces energy and processing waste during the fabrication
process.
New Alloy Systems and Chemistries. Another attribute of PM/HIP processing
methods is the ability to alter (or design) the chemistry of a specific component
on a component-by-component basis. A melter/fabricator does not have to
produce a large (several ton) heat of material to fabricate an individual
component. Fabricators will now be able to produce individual components (or
heats of material) cost-effectively using a specified chemistry. Furthermore,
3-2
PM/HIP technologies now enable the production of new alloy systems. For
example, if one wants to control a particular element such as boron or carbon or a
residual element such as sulfur or phosphorous, PM/HIP allows for specific
control of one or more of these elements.
Enhanced Weldability. Cast components are often difficult to weld because of
the irregularities in microstructure of the component. Even within one specific
alloy system (or materials specification), the weldability of a cast component can
vary greatly. The homogeneity of PM/HIP-produced alloys eliminates the
weldability concerns almost entirely. Once a particular chemistry has been
selected, it can readily be reproduced over and over again with minimal
differences in weldability.
Alternate Supply Route For Long-Lead-Time Components. Long lead times
are commonly encountered for new power plant construction since only a limited
number of manufacturers are available to produce components for the power
industry. Introduction of PM/HIP technologies within the ASME BPV Code
will allow utilities to access an alternate supply route for components.
Manufacturing times will be significantly decreased, and overall costs will be
reduced.
Elimination of Rework or Repair of Large Cast Components. One additional
attribute of PM/HIP technology that cannot be overlooked is its ability to
produce homogeneous microstructures, which substantially reduces the number
of repairs required in castings. Discussions with various valve manufacturers
reveal that it is not uncommon for large cast components to require 1050%
repairs to eliminate casting defects, depending on the casting house used. This
represents considerable rework and overall life-cycle cost to the manufacturer,
which is often not taken account of in the purchase of the casting. Such findings
also bring into question the integrity of cast components, which leads to
overdesign in many cases. PM/HIP can eliminate the need for this rework.
As can be seen from the many potential advantages/attributes described above,
PM technologies are ripe for the power industry to consider. The feasibility study
and the subsequent work described in this report were initiated with this
consideration in mind.
3-3
Section 4: Valve Body Feasibility

Assessment
Manufacture of a 316L Valve Body
The initial feasibility assessment performed by EPRI in 2010 involved the
production of a single 316L stainless steel valve body. A general valve body
design for a 12-inch (305-mm) diameter valve was provided to Carpenter
Technology for the production of the demonstration valve. A sectional drawing
of the valve body is provided in Figure 4-1.
Figure 4-1
Sectional drawing of a 316L stainless steel valve body used as a demonstration
piece in this feasibility assessment
Upon completion of the container (or can), manufactured from low-carbon

(C<0.01) mild steel, the powder was introduced into the container, and the
assembly was subjected to HIP processing. The resulting component is shown in
Figure 4-2. The valve body was provided in the annealed condition and weighed
780 kg (1716 lb). Upon receipt of the valve body from Carpenter Technology,
EPRI provided the component to its inspection team for characterization. The
following subsection summarizes the inspection results, and Appendix E provides
additional details on the inspection results.
4-1
Figure 4-2
780-kg (1716-lb) 316L prototype stainless steel valve body produced during the
feasibility assessment (photo on the right shows valve body sectioned along its
center line to reveal its ability to produce a sound, dimensionally stable component
configuration)
Inspection and Weldability Results

Upon receipt of the PM-manufactured valve body from Carpenter Technologies,
the valve body was photographed and marked for inspection validation. The
inspection assessment involved manual and automated ultrasonic techniques
aimed at detection and sizing of various flaws embedded into one of the outboard
flanges. Both longitudinal and shear wave assessment techniques were employed
using a 1.5-MHz transducer. A total of six flaws were inserted into the flange
using electro-discharge machining (EDM) techniques. A composite of the
embedded flaws is provided in Figures 4-3 and 4-4. Figures 4-5 and 4-6 show
the operators performing manual and automated inspection of the valve body.
4-2
Figure 4-3
Inspection flaws installed at various locations around the diameter of one flange
from the valve body
4-3
Figure 4-4
Inspection flaws described in Figure 4-3 installed at various depths around the
diameter of one flange from the valve body
Figure 4-5
Photograph showing manual inspection of the valve body in process
4-4
Figure 4-6
Photograph showing automated inspection of the valve body in process
The results of the inspection testing determined that the valve body was highly
inspectable and presented no inspection challenges to the ultrasonic inspection
process. Inspection results comparable to those associated with a clean forging
were observed. Additional details are provided in Appendix E.
Another factor considered paramount to the success of producing components
from PM/HIP is weldability. No welding was completed on the actual valve body
manufactured in this feasibility assessment; however, several test coupons (three
in all) were produced using PM/HIP to the 316L stainless steel specification.
12-inch (305-mm) diameter, 1-foot (305-mm) long 316L SS stock was
manufactured and then sectioned as shown in Figure 4-7. Sectioning involved
slicing the coupon into several slices so that various autogenous welds and welds
with 308L filler metals could be performed. A cross-sectional view of an
autogenous weld is provided in Figure 4-8. Single and multiple-pass welds
(Figure 4-9) were applied to the surface of the coupons. In terms of weldability,
the welders indicated that the material welded similarly to rolled and welded 304
or 316 austenitic stainless steels. No adverse weldability traits were observed. It
was also stated that the material welded better than cast stainless steels of a
similar grade.
4-5
Figure 4-7
12-inch-diameter 316L stainless steel stock fabricated for weldability testing
Figure 4-8
Cross-sectional view of an autogenous weld in the 316L stainless steel slice
removed from the end of the stock shown in Figure 4-7
4-6
Figure 4-9
Cross-sectional view of a multiple-pass weld overlay applied to the 316L stainless
steel coupon
Valve Body AssessmentMechanical and Metallographic

Characterization
Mechanical testing and metallographic characterization were performed upon
completion of the inspection characterization performed by EPRIs NDE
Center. The testing began with sectioning of the valve body along its center line
(shown earlier in Figure 4-1). A closer view of the sectioned valve body is shown
in Figure 4-10 to provide some perspective on the ability of the process to
produce intricate shapes and configurations.
4-7
Figure 4-10
Closer view of the valve body diagrammed in Figure 4-1, demonstrating the ability
of the process to produce intricate shapes or configurations
It should be noted that no finish machining was performed on the part and that
the external and internal shapes and surface finish were obtained from the
PM/HIP process. Additional sectioning was performed to remove one of the
flanges for mechanical testing and metallographic characterization.
Characterization of the microstructure was performed along three different
directions to ascertain the uniformity in structure along all directions, as shown in
Figure 4-11. The homogeneity of the structure within these three directions is
shown in Figures 4-12a through 4-12c at a magnification of 200X. Note that
little difference exists in the views along each of the three directions. The
microstructure was predominantly austenitic, with some isolated carbides
observed throughout the matrix.
The grain size of the specimens was also recorded for each orientation. An
ASTM grain size of 67 was measured for each, which is consistent with what
would be expected for a solution heat-treated stainless steel alloy.
4-8
Figure 4-11
Section of the valve body flange that was used to remove metallographic and
mechanical specimens along three different directions
4-9
a)
b)
c)
Figure 4-12
Photomicrographs of the valve body microstructure along three different directions:
a) hoop; b) longitudinal; c) transverse
4-10
Chemical Composition
The chemical composition was measured and compared with the 316L ASTM
chemistry for the alloy, as shown in Table 4-1. Note that no attempt was made to
develop a special controlled chemistry, because it was elected to use atomized
powders already in hand at Carpenter Technologies to develop the valve body
demonstration piece. All elements measured were within the ASTM
specification.
Table 4-1
Chemical composition for the 316L stainless steel valve body (values in wt%)
Element
Valve Body
316L Specification
Carbon
0.019
0.030 max
Manganese
0.99
2.00 max
Phosphorus
0.006
0.045 max
Sulfur
0.005
0.030 max
Silicon
0.73
0.75 max
Nickel
12.10
10.0014.00
Chromium
17.25
16.0018.00
Molybdenum
2.52
2.003.00
Mechanical Testing
Mechanical testing performed for the valve body included tensile tests at room
temperature and elevated temperature (600F [316C]), as well as Charpy impact
toughness testing. The tensile test results are provided in Tables 4-2 and 4-3.
Note that tests were performed along the longitudinal and transverse directions
of the valve body flange.
4-11
Table 4-2
Room temperature tensile test results for the 316L stainless steel valve body
Sample
0.2% Offset
Yield
Strength
(psi)
Ultimate
Tensile
Strength
(psi)
Elongation
(%)
Reduction
in Area
(%)
A Long
46,900
90,900
52.3
74.6
B Long
45,300
90,400
51.4
75.3
C Long
44,700
90,200
52.3
74.4
A Trans
49,800
90,800
50.6
74.6
B Trans
47,100
89,700
53.1
73.9
C Trans
49,000
90,600
50.4
74.0
1 psi = 6.895 kPa
Table 4-3
Elevated temperature (600F) tensile test results for the 316L stainless steel valve
body
Sample
0.2% Offset
Yield
Strength
(psi)
Ultimate
Tensile
Strength
(psi)
Elongation
(%)
Reduction
in Area
(%)
A Trans
30,800
71,900
42.1
72.3
B Trans
29,200
71,400
39.7
71.7
C Trans
30,100
71,300
40.7
71.4
A Long
29,200
71,600
40.5
73.2
B Long
29,700
71,300
40.9
70.7
C Long
29,500
71,600
41.8
72.3
1 psi = 6.895 kPa
Charpy impact tests were initiated for specimens removed from the valve body
flange. The initial test results determined the toughness to exceed 195 ft-lb or
the capacity of the machine. No additional testing was conducted.
Overall, the results of the demonstration coupon and testing were considered
very encouraging, showing good inspectability, high strength and toughness, and
good microstructural uniformity. Furthermore, the valve body was free of
porosity and provided good weldability.
4-12
Section 5: Manufacture and

Characterization of Multiple
Valve Bodies
During the second half of 2010, and based on the promising results of the initial
studies described in Section 4 of this report, EPRI initiated a more targeted
research program to focus on the development of several additional valve bodies
of varying materials to support ASME Boiler and Pressure Vessel Code (BPVC)
Code Cases. A variety of valve body configurations were manufactured from
three different alloys: Type 316L stainless steel (for nuclear applications), Grade
91 (for fossil and heat recovery steam generator applications), and IN625 (for
ultra-supercritical applications).
316L Stainless Steel Valve Body Development and Testing
EPRI and Carpenter elected to team with Tyco Valves to manufacture and test
three 316L SS valve bodies. The three valve bodies were manufactured to Tycos
drawings/specifications, which allowed them to place the valve bodies through
their rigorous testing criteria and production machining process. Photographs of
one of the valve bodies are provided in Figure 5-1. Mechanical tests and
metallographic characterization were completed for each valve body and were
used in the assembly of an ASME Code data package. The chemical
composition is presented in Table 5-1, and tensile test results and yield strength
test results for the three valve bodies are provided in Figures 5-2 and 5-3,
respectively.
5-1
a)
b)
Figure 5-1
One of the 316L stainless steel valves manufactured by Carpenter Technology to
drawing/specifications provided by Tyco Crosby: a) the finished valve body; b)
the valve body sectioned into halves
Table 5-1
Chemical composition of S31603 (316L) manufactured components
Heat
Size
S31603 (316L)
Specification*
Product Form
814520
815111
Y1620B
1892 lb
1200 lb
1200 lb
Valve
Valve
Valve
0.030 max
0.013
0.021
0.004
Mn
2.00 max
0.90
0.95
1.41
0.045 max
0.014
0.009
0.005
0.030 max
0.003
0.004
0.005
Si
1.00 max
0.70
0.80
0.55
Ni
10.014.0
12.1
13.2
13.3
Cr
16.018.0
17.3
17.3
16.87
Mo
2.03.0
2.55
2.50
2.37
0.10 max
0.10
0.14
0.038
Others
N/A
O: 0.010
N/A
N/A
*Specification = ASTM A988/A988M
5-2
Figure 5-2
Tensile test results for three Type 316L stainless steel valve bodies manufactured
during this project
Figure 5-3
Yield strength test results for three Type 316L stainless steel valve bodies
manufactured during this project
5-3
As mentioned above, the 316L stainless steel valve body results were used to
develop an ASME BPVC data package. The data package, along with a draft
Code Case, is provided in Appendix B. Information regarding the three valve
bodies, along with information regarding a fourth component, a 316L SS teesection provided by Rolls-Royce, was used to assemble the data package and
included the following:
Chemical composition
Grain size measurements
Hardness measurements
Drawings and images
Microstructure
Density
Inclusion content
Toughness
Tensile properties (701000F [21538C])
Yield stress-strain curves
Weldment properties
Fatigue properties
Corrosion results
A discussion of the results of the 316L SS testing and data package is provided in
Section 6.
Grade 91 Valve Body Development and Testing
In parallel, EPRI and Carpenter also initiated production of three Grade 91 valve
bodies in conjunction with another major valve manufacturer, GE-Dresser.
Teaming with GE-Dresser allowed for component testing and production
machining characterization in a manner similar to the one that would be
employed for actual valve production. Photographs of one of the valve bodies are
shown in Figure 5-4. Initial mechanical tests and metallographic characterization
are underway for each valve body and will be used in the assembly of a Code data
package. Chemical composition for one of the valve bodies is presented in Table
5-2, and some preliminary tensile results are presented in Table 5-3. A rigorous
test matrix has been developed for creep and stress-rupture testing including tests
beyond 20K hours that are underway, to support a potential 2012 Code package
for this alloy.
5-4
Figure 5-4
Grade 91 alloy steel valve manufactured by Carpenter Technology to
drawing/specifications provided by Dresser (photo on the right shows valve body
sectioned into halves)
Table 5-2
Chemical composition for one Grade 91 valve body manufactured during this
project (values in wt%)
Element
Carbon
Manganese
Phosphorus
Sulfur
Silicon
Nickel
Chromium
Molybdenum
Vanadium
Columbium
Nitrogen
Aluminum
Titanium
Boron
Zirconium
Iron
Valve Body
0.10
0.36
0.004
0.009
0.20
0.08
8.89
0.93
0.20
0.08
0.04
<0.01
<0.01
<0.01
<0.01
Bal
5-5
Grade 91 Specification
0.080.12
0.300.60
0.020 max
0.010 max
0.200.50
0.40 max
8.009.50
0.851.05
0.180.25
0.060.10
0.030.07
0.02 max
0.01 max
NA
0.01 max
Bal
Table 5-3
Elevated temperature tensile test results for one Grade 91 valve body
manufactured during this project
Temperature
(F)
0.2% Offset
Yield
Strength
(ksi)
Ultimate
Tensile
Strength
(ksi)
Elongation
(%)
Reduction
in Area
(%)
RT
100
200
300
400
500
600
700
800
900
1000
1100
1200
1300
67.7
68.4
65.4
65.7
64.0
59.6
58.8
58.5
56.4
53.9
49.8
42.3
31.6
20.4
93.2
92.5
87.6
85.2
82.2
78.6
76.3
75.8
72.5
66.9
59.9
47.4
35.3
25.3
26.5
26.5
25.5
24.0
23.5
23.0
21.0
20.5
22.5
25.5
25.5
35.5
40.5
45.5
71.5
73.5
73.0
73.5
67.5
74.0
71.5
70.5
70.0
75.5
79.5
89.0
92.5
94.5
C = 5/9(F32)
1 ksi = 6.895 MPa
IN625 Valve Body Development and Testing

Ultra-supercritical applications will require the use of solid-solution strengthened
and precipitation hardened nickel base alloys to meet the demanding
temperatures and pressures required for such applications. As a feasibility
assessment (there are no immediate plans to submit a Code Case at this time),
one IN625 valve body was manufactured to assess component manufacturing
potential. A photograph of the IN625 valve body is presented in Figure 5-5, and
a few of the results for the component are shown in Tables 5-4 and 5-5.
5-6
Figure 5-5
IN625 valve body manufactured by Carpenter for feasibility purposes
Table 5-4
Chemical composition for the IN625 valve body manufactured during this project
(values in wt%)
Element
Carbon
Manganese
Phosphorus
Sulfur
Silicon
Nickel
Chromium
Molybdenum
Cobalt
Iron
Aluminum
Titanium
Cb + Tantalum
Valve Body
0.01
0.41
0.003
0.003
0.45
Bal
21.9
8.2
<0.1
3.6
<0.05
0.006
3.48
5-7
IN625 Specification
0.10 max
0.50 max
0.015 max
0.015 max
0.50 max
58.0 min
20.023.0
8.010.0
1.0 max
5.0 max
0.40 max
0.40 max
3.154.15
Table 5-5
Elevated temperature tensile test results for the IN625 valve body manufactured
during this project
Temperature
(F)
0.2% Offset
Yield
Strength
(ksi)
Ultimate
Tensile
Strength
(ksi)
Elongation
(%)
Reduction
in Area (%)
RT
100
200
300
400
500
600
700
800
900
1000
1100
1200
1300
1400
1500
1600
66.3
67.3
61.5
59.9
55.2
53.9
52.9
50.1
52.1
48.4
48.7
50.3
49.1
50.1
48.9
42.4
28.3
133.9
131.7
122.8
123.8
122.4
115.4
114.3
115.3
118.9
116.0
114.7
111.0
102.2
86.4
67.0
47.6
30.7
30.5
30.0
31.5
30.5
32.5
27.0
27.0
27.0
41.0
43.5
40.5
31.5
31.0
41.5
40.0
51.5
56.5
24.5
27.5
27.0
27.5
24.0
22.5
26.0
27.0
40.5
38.5
33.5
28.0
26.5
29.5
35.0
37.5
54.0
C = 5/9(F32)
1 ksi = 6.895 MPa
5-8
Section 6: Results and Discussion

This section of the report focuses only on the results of the 316L SS assessment
through April 2012. As noted in the previous section, testing of Grade 91 and
IN625 is currently still in process. For the 316L SS, results and discussion for
each measured property follow. The specific components involved (representing
four heats of 316L SS) were three valve bodies manufactured by Carpenter
(described in Section 5 of this report and in the supporting data package in
Appendix B) and one tee-section from Rolls-Royce.
Chemical Composition. All four components manufactured in this project fully
met the ASTM 316L SS (S31603) compositional requirements. Only one minor
exception was documented: the nitrogen content of heat 815111 was slightly out
of specification, with the content measuring at 0.14 wt% versus the specified
0.10 wt%. Discussions with Carpenter suggested that the nitrogen percent could
be controlled to even lower levels, but this was not originally considered
significant for the EPRI evaluation.
Grain Size Measurements. Grain size was measured for the four components,
with measurements ranging from 5.3 to 7.0 average for the four. The ASTM
specification (SA-965/SA965M) suggests that the grain size should be a number
6 or coarser.
Hardness. Ten Rockwell B hardness traverses were made across the four
components, resulting in average values of 89.9, 84.4, 84.7, and 87.9 Rb. The
ASTM specification (SA965/SA965M) for a forged component does not provide
a suggested hardness range.
Microstructure, Density, and Inclusion Content. Microstructures recorded for
each of the four components were very homogeneous and exhibited no
anomalies. 100X and 500X images were examined for each valve body section.
Density ratios provided for three of the four components (they were not recorded
for the Rolls-Royce tee-section) suggest that ratios exceeding 99.9% could be
readily achieved. No voids were seen in multiple cross-sections examined during
this effort. The inclusion content measurements (ASTM E45) included
measurements for four different types of inclusions: A, B, C, and D. Neither of
the first three types of inclusions were observed. The D-type inclusions were l.0
or less.
6-1
Toughness. Charpy impact toughness values recorded for two heats exceeded
192 ft-lb in all three directions. A third heat exceeded 151 ft-lb, while the fourth
exceeded 121 ft-lb in all three test orientations. In all cases, the toughness was
excellent.
Tensile Properties. Tensile properties were recorded at 50F (28C) increments
beginning with RT, and in the range of 100F (37.8C) and all the way up to
1000F (537.8C). Slightly above the service temperature (roughly 700F [37C]),
the tensile values for the four heats measured 70.5, 74.8, 61.0. and 66.7 ksi
(486.1, 515.7, 420.6, and 459.9 MPa), while the yield strengths were recorded at
29.9, 30.8, 27.1, and 23.4 ksi (206.1, 212.4, 186.8, and 161.3 MPa). Elongation
at the same test temperature was measured at 42.5, 41.5, 40.0, and 43.0, again all
good values. Finally, reduction of area values were measured at 69.5, 66.5, 68.5,
and 71.0. These results are consistent with (or better than) what might be
measured for a wrought or forged product form. SA-965/SA965M suggests that
the minimum tensile strength should be 65 ksi for F316L tested at room
temperature. The yield strength for F316L should be 30 ksi at this same
temperature, while the elongation and reduction of area are 30 and 45. As can be
seen, even at service temperature, the PM/HIP-produced valve bodies exceed the
room temperature requirements for the F316L specification.
Stress Analysis. A detailed stress analysis was also conducted under this project
and is provided in Appendix C. The results of this effort were used to produce
the stress allowables supplied to ASME BPVC Section III for review.
Weldment Properties. Two weldments were completed for the ASME data
packageone SMAW weldment and one GTAW weldment. The results
suggested that good weldability was achieved, along with acceptable properties.
Hardness, bends, and cross-weld tensile tests were performed. The results
suggested that both weldments readily met ASME BPVC Section IX
requirements.
Fatigue Properties. The fatigue results presented in this report were measured by
Rolls-Royce for the tee-section that was used as one of the four heats of
materials. EPRI did not perform testing as part of the data package, but currently
has additional testing underway. Figure 26 of the data package (Appendix B of
this report) provides fatigue results recorded at 572F (300C) and plotted against
the ASME design curve for a wrought austenitic stainless steel. As can be seen,
the fatigue properties for the PM alloy easily exceeded the design curve
properties.
6-2
Corrosion. Corrosion results were also measured by Rolls-Royce for the teesection that was used as one of the four heats of material. Those results are
shown in Appendix D of this report. Test results for a variety of corrosion tests
were compared with wrought 316L. The tests included the following:
ASTM G36Evaluating Stress-Corrosion Resistance of Metals and Alloys

in Boiling Magnesium Chloride Solution
ASTM G35-88Determining the Susceptibility of Stainless Steels and

Related Nickel-Chromium-Iron Alloys to Stress-Corrosion Cracking in
Polythionic Acids
Crevice corrosion evaluation under test conditions designed to represent

layup worst-case scenario
ASTM G48-97Pitting and Crevice Corrosion Resistance of Stainless

Steels and Related Alloys by Use of Ferric Chloride Solution
ASTM A A262Detecting Susceptibility to Intergranular Attack in

Austenitic Stainless Steels
Slow strain-rate tests in primary and secondary water chemistries with

NaOH additions.
EAC/crevice tests
The results of the testing suggest that the PM-fabricated components performed
as well as or better than a wrought and forged 316L SS in all cases. Excellent
microstructural, mechanical, and corrosion properties were consistently measured
throughout the testing phase of this project. Additional details of the testing are
provided in Appendix D.
6-3
Section 7: Conclusions
The research conducted in this project was performed first to assess the feasibility
of using a combination of powder metallurgy and HIP to produce large, near-net
shaped (NNS), complex components for potential use in the power industry, and
second to develop data for ASME Code packages to be submitted such that large
pressure-retaining components can be fabricated. The PM/HIP technique is
targeted at components currently manufactured using various casting and forging
methods for use in nuclear, supercritical, advanced supercritical, and oxycombustion plants. These components may include (but are not limited to)
valves, pump housings, flanges, elbows, sweepolets, steam chests, turbine casing
shells, nozzles, and canister plugs. Attributes of the PM/HIP process that make
it attractive to the power industry include the following:
Elimination of inspectability issues and concerns
Capacity to manufacture large, complex components using near-net shape

technologies
Capacity to employ new alloy systems and targeted chemistries
Enhanced weldability
Alternate supply route for long-lead time components
Elimination of rework or repair of large cast components
This feasibility study determined that PM/HIP can indeed produce NNS
components that exhibit acceptable metallurgical and mechanical properties
meeting or exceeding those of conventionally cast or forged components.
Mechanical properties produced in testing under this evaluation showed a 10
15% improvement over cast components of the same alloy (in terms of tensile
strength), as well as exceptional toughness properties. Furthermore, it was
demonstrated that significantly enhanced inspectability was achieved for the
316L stainless steel valve body produced in this effort, as compared to
conventional casting components. No weldability issues were encountered during
weldability testing of the valve body.
7-1
The second half of the study demonstrated that large components (valve bodies)
can be effectively manufactured using the PM/HIP process with 316L stainless
steel, Grade 91 steel, and IN625 nickel-based alloys. Mechanical test data is
provided for one heat (melt) of each material for these three alloys. This report
focused on the development of an ASME Code Data package and a Code Case
for 316L stainless steel. Four component articles (including three 316L SS valve
bodies and one 316L SS tee-section) were manufactured via the PM/HIP
process, then tested at up to 1000F to ascertain properties. In all cases, the
tensile properties measured for these alloys easily met or exceeded the Code
requirements and provided excellent toughness. Homogeneous microstructures
were observed for each component along with good inspectability. Furthermore,
excellent fatigue and corrosion properties were demonstrated. Based upon these
results, EPRI, in conjunction with Tyco Valve, Carpenter Technology, and
Rolls-Royce, supported the development of an ASME Code Case within
Section III.
7-2
Appendix A: Process and Product Controls

for Material Produced by
PM/HIP
As with any material fabrication process, there are basically two types of controls
that may be applied to the PM/HIP process: in-process controls and end product
controls. From the point of view of the purchaser, the most straightforward
controls are those applied by specification of measurable attributes of the end
productfor example, chemistry, mechanical properties, density, and
microstructure. That is, the purchaser defines the characteristics of the material
that are needed for the material to perform adequately in a specific application.
Some of these requirements may vary considerably depending on the operating
conditions to which the material will be exposed (atmosphere, loads,
temperature, cyclic loading, and so on). In any case, the purchaser should define
to the material manufacturer what the characteristics of the finished material
must be. The purchaser is generally less concerned with the detailed processing
requirements needed to achieve the specified criteria. Conversely, the material
manufacturer frequently has no knowledge of how the material will be used or
what the operating conditions are, but does know how to control the
manufacturing process to achieve specific properties and quality level in a
material. Therefore, in-process controls are typically developed and applied by
the material manufacturer. These in-house controls are those that the
manufacturer has found to be necessary to be assured that the material produced
will comply with the purchaser-specified end product requirements. While the
end product requirements (for example, chemistry, strength, and NDE
requirements) may be common to several product forms of the same alloy type,
in-process controls are mostly unique to the specific material fabrication process.
Consequently, many of the in-process controls for PM/HIP are unique to that
material fabrication technique. On the other hand, many in-process controls that
are critical to the outcome of other materials processes such as forging are
irrelevant to PM/HIP.
As described above, the attributes and quality of a material produced by PM/HIP
are determined by both specification of end product requirements and
inspections, and application of in-process controls. Both of these sets of controls
will vary depending on the material type and the end use of the material, so it is
impractical to describe them for all materials and circumstances. However, to
illustrate the types of controls that may be applied to a PM/HIP processed
A-1
material, the following table (Table A-1) is provided. It lists quality controls that
may be applied to production of Type 316L for high-temperature, pressureretaining service as defined in ASTM A988, along with consideration of
potential application to an ASME Section III component.
Table A-1
Representative quality controls
Process Step
Quality Operation
Rationale
Step Controlled in
ASTM A988-11
Powder Production
Steel Formulation
Chemical analysis. Melt

virgin raw stockproduced by
induction furnace.
To ensure that melt will meet the

specification requirements.
YesSection 6.1 and

manufacturer
specification
Inert Gas
Atomized
Powder
Manufacture
Atomization machine cleaning

and inspection.
To ensure that cross contamination

of the powder does not occur.
Inert gas used to ensure powder
quality and hence final material
qualityfor example, to prevent
powder oxidation.
Manufacturer
specification only
Sieving of
Powder
All powder sieved using a

maximum 0.5-mm mesh size.
To promote improved packing

density and to minimize the
possibility of non-metallic
inclusions. Note: a finer mesh size
may need to be specified,
depending upon the application.
Manufacturer
specification only
Blending
Blending is allowed only to

achieve the required quantity of
powder for large components
that cannot be accommodated
from a single heat. Each heat
to be blended together must
comply with the powder
specification prior to blending.
Blending of heats is not
allowed to enable the overall
final blend to meet the
specification (that is, this
control is in place to prevent an
individual heat that doesnt
meet specification from being
improved by blending with
another). The final blend shall
be a homogeneous batch of
powder with regard to
composition, particle size, and
other properties.
To ensure good, overall powder

quality and section properties
throughout the component.
Manufacturer
specification only
Cleansing batch of raw

material.
A-2
Manufacturer
specification only
Table A-1 (continued)

Process Step
Quality Operation
Rationale
Step Controlled in
ASTM A988-11
Powder Production (continued)

HIP Powder
(Compact)
Sampling
Standard sample of powder

HIPped, then mechanically and
chemically tested and
metallographically examined to
confirm properties.
To perform a check ensuring that

powder HIP consolidates.
YesSection 6.1
Powder Storage
Storage takes place under

positive nitrogen or argon
atmosphere following gas
atomization.
To ensure that no contamination or

oxidation of the powder occurs in
storage.
Manufacturer
specification only
Density/volumetric shrinkage
from previous experience.
To perform a tap density check on

powder in order to ensure that it
meets the requirement.
YesSections 5.1.1
and 8.1.1.1
Low carbon content can

material to be used (0.01%C
max.).
To minimize the possibility of

carbon diffusion into the HIP
material affecting skin properties.
Manufacturer
specification only
Gas tungsten arc welding to be

employed with inert argon
protection on the inside.
To provide a high-quality weld to

reduce the risk of can failure and to
minimize the risk of oxidation and
hence of slag becoming detached
into the powder during can fill.
Manufacturer
specification only
Visual inspection of can welds.
To confirm freedom of reverse side

weld oxidation and freedom from
loose particles that could become
detached into the powder during
can fill.
Manufacturer
specification only
Helium leak check on can.
To ensure that can is leak-tight,

particularly can welds.
Manufacturer
specification only
Vibratory filling.
To ensure that powder is evenly

distributed throughout the capsule
and to ensure optimum packing
density to control shrinkage.
Powder fill weight.
Fill weight to design. The fill weight

is to be recorded.
Manufacturer
specification only
Achievement of vacuum.
To ensure required consolidation.
Manufacturer
specification only
Helium leak check following

powder fill of can.
To confirm that can welds are

intact.
Manufacturer
specification only
Canning
Can Design and
Manufacture
Can Fill
A-3

Process Step
Quality Operation
Rationale
Step Controlled in
ASTM A988-11
Hot Isostatic Processing

HIP
Time, temperature, and

pressure to be controlled,
monitored, and recorded (to
include ramp-up, hold time,
and cool-down rate).
Temperature to be monitored,
controlled, and recorded by
calibrated thermocouples in all
vessel zonesbottom to top.
Pressure to be monitored,
controlled, and recorded by
calibrated pressure gauge.
To verify that conditions of the HIP

cycle meet process requirements
full consolidation achieved.
Manufacturer
specification only
Visual appearance of the

component.
To confirm normal shrinkage of the

can achieved. Also visually inspect
to make sure the can welds are
100%.
Manufacturer
specification only
Argon (pressure media used in

the HIP vessel) ingress
detection. Chromatographic
chemical analysis conducted
on samples from the filling
tube.
To determine that can welds have

not ruptured during HIP cycleto
ensure required consolidation.
Manufacturer
specification only
Post-HIP Processing and Inspection

Solution Anneal
Time and temperature record.
To confirm process parameters

achieved. Eliminates residual
stresses.
YesSections 7.1
through 7.4
Can Removal
Visual examination.
To ensure full removal of can, with

no ferritic contamination present.
Pickling or machining/grinding can
be employed. For pickling, a visual
inspection after 24 hours is to be
performed to search for signs of
discolorationrepeat pickling steps
if found.
YesSection 5.1.5
Microporosity
and Density
Checks
Density measurements and

microstructural examination.
To verify that component (part) is

free of microporosity.
YesSections 8.1 and

8.2
Finished
Component
Dimensional inspection.
Full dimensional check against

design requirements.
Manufacturer
specification only
A-4

Process Step
Quality Operation
Rationale
Step Controlled in
ASTM A988-11
Post-HIP Processing and Inspection (continued)

Inspection
Visual inspection.
To detect discontinuities, flaws,

cracks, poor finish, corrosion,
pitting, fretting, staining, and any
mechanical failure.
Manufacturer
specification only
Ultrasonic inspection.
UT inspection is performed via

Section S7.
Supplemental, via
Section S7.
Material
Acceptance
Testing
Chemical analysis.
To confirm that specification is

achieved.
YesSection 6.1
Mechanical and metallurgical

testing.
To establish that mechanical

properties and metallographic
properties (for example, grain
structure, density, porosity, and
inclusion content) are within
requirements.
YesSections 8.1,
8.2, and 9.1 through
9.7
Final Material
Removal
The as-HIPped surface is to be

removed by machining to a
minimum depth of 0.2 mm
(200 microns) for all wetted
surfaces.
To protect against any skin

hardening effects due to carbon
diffusion from the can into the HIP
material, and any powder profile
geometric effects affecting fatigue
performance.
Manufacturer
specification only
Archival
Archive HIPped material
To maintain availability for future

testing.
Optional, per
agreement with user
A-5
Appendix B: Draft ASME BPVC Section III

Code Case and Supporting
Data Package
This appendix reproduces a draft of a proposed Code Case for the introduction
of powder metallurgy to produce Type 316L stainless steel components, and test
data and information that was assembled and submitted to ASME in early
November 2011 in support of the Code Case. (As of the time this report was
written, only the draft version of the Code Case has been submitted. The final
Code Case is to be submitted in early 2012.)
The draft Code Case appears on pages B-2 through B-4 of this appendix, and
the data package begins on page B-5.
B-1
B-2
B-3
B-4
B-5
B-6
B-7
B-8
B-9
B-10
B-11
B-12
B-13
B-14
B-15
B-16
B-17
B-18
B-19
B-20
B-21
B-22
B-23
B-24
B-25
B-26
B-27
B-28
B-29
B-30
B-31
B-32
B-33
B-34
B-35
Appendix C: Stress Analysis
C-1
C-2
C-3
C-4
C-5
Appendix D: Corrosion Data Supplied by

Rolls-Royce
This appendix presents test data and information assembled and submitted by
Rolls-Royce. It documents corrosion testing of a 316L stainless steel tee-section.
D-1
D-2
D-3
D-4
Appendix E: Inspection Summary

Initial Component Inspectability Assessment
Overview
The purpose for this investigation was to determine the inspectability of
components manufactured using powder metallurgy (PM) and hot isostatic
processing (HIP) technologies using ultrasonic methods. The sample under
consideration is a 316L stainless valve with three flanges (see Figure E-1).
Equipment
Dell XPS Laptop
Zetec UltraVision 3.1R9 Data Acquisition and Analysis Software
Zetec DYNARAY 256/256PR (controlled via UltraVision)
General Electric Inspection Technologies (GEIT) Array # 115-000-592
(1.5MHz, 16x1)
GEIT Wedge # 360-151-053 and Wedge # 360-151-054
GEIT Phasor to Hypertronics Adapter # 112-140-401
Sample Preparation
Upon initial receipt of the sample, the surface was found to be too rough to
conduct an ultrasonic (UT) examination. Initially the part was sent out for glass
bead blasting in order to smooth out the surface. Although there was some
improvement in the surface texture, the sample was still not adequate for
ultrasonic examination. The decision was then made to sand down the flanges of
the sample. A 4-inch angle grinder fitted with an abrasive flap wheel was used for
this process, and it created an acceptable surface finish to conduct the ultrasonic
exams. It should be noted that there were still many surface irregularities (raised
lips, waviness, and inclined surfaces) that challenged the UT examination. Figure
E-2 provides an image of the sample post-sanding.
E-1
Examinations
The sample was initially examined manually using the 115-000-592 probe
coupled to the 360-151-053 wedge. 085 longitudinal waves were used to scan
through the part. However, it became necessary to extend the angle range back to
-15 in order to image some back wall signals due to existing incline angles on
the valves surface. At this point, the entire surface of the flanges was not
examined. The goal was to attempt to identify back wall and corner signals to
evaluate the potential effectiveness of UT examinations on the part.
Next, the part was manually examined again using the 115-000-592 probe
coupled to the 360-151-054 wedge. The main purpose of the scan was to observe
the ultrasonic responses from the shear waves. For the inspection, two channels
were utilized. One channel was set up for -1585 longitudinal waves, while a
second channel was added for 3565 shear waves. During the second
examination, the same back walls and corners were looked at as in the first exam.
Results
The initial manual ultrasonic phased array inspection using the 115-000-592
probe coupled to the 360-151-053 wedge showed that the longitudinal waves did
not appear to have trouble penetrating the part and providing good-quality
ultrasonic images of back walls and corner signals. Figures E-3 through E-20
show the probe position and the corresponding data image screen capture for the
back wall and corner signal that were imaged.
A second manual ultrasonic examination was performed to see how well this
approach would image reflectors utilizing shear waves. The sample material did
not impede the ultrasounds capability to transmit shear waves and image
reflectors. The shear waves were not able to image back walls and some corner
reflectors due to the angles used and the component geometry. Figures E-21
through E-41 show the probe position and the corresponding longitudinal
(L-wave) and shear (S-wave) (when available) wave signals.
E-2
Figure E-1
Valve sample as received
Figure E-2
Valve sample after glass bead blasting and flange sanding
E-3
Figure E-3
360-151-053 on main flange OD looking at the back wall
Back Wall
Indication appears late in time

(below the inside surface).
Indication is usually present around
the full circumference.
Figure E-4
UltraVision screen shot of 360-151-053 on main flange OD looking at the back
wall
E-4
ID Corner
Figure E-5
360-151-053 on main flange OD looking at the ID corner
Back Wall
ID Corner
Figure E-6
UltraVision screen shot of 360-151-053 on main flange OD looking at the ID
corner
E-5
Figure E-7
360-151-053 on main flange back side looking at the ID corner
Back Wall
ID Corner
Figure E-8
UltraVision screen shot of 360-151-053 on main flange back side looking at the
ID corner
E-6
OD Corner
Figure E-9
360-151-053 on main flange back side looking at the OD corner
Back Wall
OD Corner
Figure E-10
UltraVision screen shot of 360-151-053 on main flange back side looking at the
OD corner
E-7
OD Corner
Figure E-11
360-151-053 on main flange mating surface looking at the OD corner
Back Wall
OD Corner
Figure E-12
UltraVision screen shot of 360-151-053 on main flange mating surface looking at
the OD corner
E-8
Figure E-13
360-151-053 on main flange mating surface looking at the back wall
Back Wall
Figure E-14
UltraVision screen shot of 360-151-053 on main flange mating surface looking at
the back wall
E-9
Figure E-15
360-151-053 on side flange OD looking at the back wall
Back Wall
Figure E-16
UltraVision screen shot of 360-151-053 on side flange OD looking at the back
wall
E-10
ID Corner
Figure E-17
360-151-053 on side flange OD looking at the ID corner
Back Wall
ID Corner
Figure E-18
UltraVision screen shot of 360-151-053 on side flange OD looking at the ID
corner
E-11
Figure E-19
360-151-053 on valve body looking at the back wall
Back Wall
Figure E-20
UltraVision screen shot of 360-151-053 on valve body OD looking at the back
wall
E-12
Figure E-21
360-151-054 on main flange OD looking at back wall
Back Wall

Figure E-22
UltraVision screen shot of 360-151-054 L-wave on main flange OD looking at the
back wall
E-13
ID Corner
Figure E-23
360-151-054 on main flange OD looking at the ID corner
Back Wall
ID Corner
Figure E-24
UltraVision screen shot of 360-151-054 L-wave on main flange OD looking at the
ID corner
E-14
ID Corner
Figure E-25
UltraVision screen shot of 360-151-054 S-wave on main flange OD looking at the
ID corner
Figure E-26
360-151-054 on main flange back side looking at the ID corner
E-15
Back Wall
ID Corner
Figure E-27
UltraVision screen shot of 360-151-054 L-wave on main flange back side looking
at the ID corner
ID Corner
Figure E-28
UltraVision screen shot of 360-151-054 S-wave on main flange back side looking
at the ID corner
E-16
OD Corner
Figure E-29
360-151-054 on main flange back side looking at the OD corner
Back Wall
OD Corner
Figure E-30
UltraVision screen shot of 360-151-054 L-wave on main flange back side looking
at the OD corner
E-17
OD Corner
Figure E-31
360-151-054 on main flange mating surface looking at the OD corner
Back Wall
OD Corner

Figure E-32
UltraVision screen shot of 360-151-054 L-wave on main flange mating surface
looking at the OD corner
E-18
OD Corner
Figure E-33
UltraVision screen shot of 360-151-054 S-wave on main flange mating surface
looking at the OD corner
Figure E-34
360-151-054 on main flange mating surface looking at the back wall
E-19
Back Wall
Figure E-35
UltraVision screen shot of 360-151-054 L-wave on main flange mating surface
looking at the back wall
ID Corner
Figure E-36
360-151-054 on side flange OD looking at the ID corner
E-20
Back Wall
OD Corner
Figure E-37
UltraVision screen shot of 360-151-054 L wave on side flange OD looking at the
ID corner
Figure E-38
360-151-054 on valve body looking at the back wall
E-21
Back Wall
Figure E-39
UltraVision screen shot of 360-151-054 L-wave on valve body OD looking at the
back wall
OD Corner
Figure E-40
360-151-054 on valve body looking at the main flange OD corner on the bounce
E-22
OD Corner
Figure E-41
UltraVision screen shot of 360-151-054 S-wave on valve body OD looking at the
main flange OD corner on the bounce
Ultrasonic Examinations of Installed Reflectors

Overview
As documented in the preceding section of this appendix, the ultrasonic
transducer was able to adequately transmit longitudinal and shear waves to
effectively image back wall and corner reflector signals from the stainless steel
valve. The next step was to determine if machined reflectors could be detected
using ultrasonic techniques. A series of surface-connected reflectors (10%
through-wall) were introduced into one of the flanges through the use of
electrical discharge machining (EDM). Both automated and manual ultrasonic
data was acquired in an attempt to detect the reflectors.
Equipment
Dell XPS Laptop
GEIT Array # 115-000-592 (1.5MHz, 16x1)
GEIT Wedge # 360-151-054
GEIT Wedge # 360-152-230, 36-inch diameter contoured for circumferential
scanning
Atco LPS-1000 two-axis pipe scanner
R/D Tech MCDU-02 (motion controller for the scanner)
E-23
Sample Preparation
Although the sample had a smooth finish from the grinding operations, the
surface was still uneven and very wavy. At times this surface condition caused
some contact issues while scanning during the first phase of this investigation.
The decision to install reflectors into the middle flange was made after a visual
exam with a wedge was conducted to see which flange appeared to be the most
flat. A total of six reflectors were installed into the middle flange. Three reflectors
were to be installed on the inner diameter (ID) of the flange so they could be
imaged by scanning axially and circumferentially on the outer diameter (OD).
The three reflectors would be a circumferential EDM notch, an axial EDM
notch, and a 0.25-in. (6.25-mm) round bottom hole; all three reflectors were
selected to be a height of 10% (0.566 in/14.4 mm). Similarly, three reflectors
were installed on the back side of the flange, to be imaged by scanning on the
mating surface of the flange. The three reflectors were a circumferential notch
that would be seen by scanning the part radially outward, an axial notch that
would be seen scanning in an annular sequence, and a 0.25-in. round bottom
hole that could potentially be imaged in both directions. Again, the heights of
the reflectors were chosen to be 10% (0.350 in./8.9 mm) of the 3.5-in.
(88.9-mm) flange thickness.
The EDM reflector installation was performed in-house by the EPRI machine
shop. During the installation of Flaw 4, the circumferential EDM notch to be
seen from the OD was burned axially, making it impossible to be imaged
ultrasonically given its location. Additionally, Flaws 5 and 6 were installed into
the part at an angle instead of normal to the ID of the flange. This would create a
few examination issues, as the reflectors would not be a full 10% height, and
would also be imaged differently while scanning with the ultrasonic transducer
looking in the positive and negative directions. Figures E-42 to E-44 show the
final installed locations of all of the reflectors implanted into the flange. Figure
E-45 provides a numerical table for the location of the start and stop points of
each of the reflectors.
E-24
Figure E-42
Drawing of flaw locationssheet 1 of 3
Figure E-43
E-25
Figure E-44
Figure E-45
Flaw location table
E-26
Examinations
Two main sets of ultrasonic examinations were performed for this phase of the
project. First, automated phased array examinations were performed on both of
the major scan surfaces of the middle flange. Second, manual phased array exams
were performed in an effort to better capture sector scan images of the flaws.
The automated ultrasonic phased array examinations consisted of eight data sets
collected from the OD and flange mating surfaces. GEIT probe 115-000-592
was used for all of the exams. For the axial scans the probe was coupled to GEIT
wedge 360-151-054. Longitudinal waves covering angles from -15 to 70 and
shear waves covering angles 35 to 65 were used to generate data sets with the
probe looking in both the positive and negative directions. The probe was then
coupled to GEIT wedge 360-152-230 (36-inch diameter contoured wedge) for
the circumferential data. Longitudinal waves covering angles 0 to 70 and shear
waves covering angles 25 to 65 were used to generate data sets with the 360152-230 wedge looking in both the positive and negative directions. Figure E-46
shows the setup used for the UT examinations on the OD of the flange.
Figure E-46
Scanning setup for UT examinations on the OD
For the exams that were conducted on the mating face of the flange, the probe
was coupled to GEIT wedge 360-151-054 for all of these inspections. For the
axial exams (conducted radially outward from/inward to the center of the
flange), longitudinal waves covering angles from -15 to 70 and shear waves
covering angles 35 to 65 were used to generate data sets with the probe looking
E-27
in both the positive and negative directions. For the circumferential exams
(conducted annularly around the center of the flange) longitudinal waves
covering angles from 0 to 70 and shear waves covering angles 25 to 65 were
used to generate data sets with the probe looking in both the positive and
negative directions. Figure E-47 shows the setup used for the UT examinations
on the flange face.
Figure E-47
Scanning setup for UT examinations on the flange face
The manual examinations were conducted using the same probe and wedge
combinations used for the automated scans. The purpose for the manual
examinations was to see if some of the flaws could be imaged better using manual
scanning techniques, which would allow for different skew angles and probe
placements. The manual exams also allowed for the operator to optimize the
probe contact to obtain better flaw images. Much like the automated scans, these
were performed with longitudinal wave angles ranging from -15 to 70, and
shear wave angles ranging from 25 to 65.
Results
The results of the automated and manual scans to detect the 10% flaws that were
EDM machined into the part were positive. All of the reflectors were detected in
at least one of the scans, and all flaws were also detectable using longitudinal and
shear waves, the exception being Flaw 4, which was not detected due to its
installation location, as previously noted. Table E-1 displays the results from the
automated scans. It outlines which scans and wave modes were able to detect the
E-28
flaws. Figures E-48 through E-64 show the screen shots for all the automated
detections marked with a YES. Table E-2 presents the same information for
the manual scans. Figures E-65 through E-85 show the screen shots for all the
manual detections marked with a YES, as well as the approximate array
location used to obtain the screen shots. In Figures E-65, E-68, E-71, E-74,
E-77, E-80, and E-83, the approximate flaw locations are indicated with red
pencil marks. Table E-2 shows detections in both the positive axial and negative
circumferential directions, since Figures E-71 and E-73 were captured while the
probe was skewed approximately 135 (see Figure E-73).
Table E-1
Automated examination detection results
Flaw
Number
Flaw
Location
Flaw
Type
Flaw
Detected in
Positive
(Down) Axial
Direction
Flaw
Detected in
Negative
(Up) Axial
Direction
Flaw Detected
in Positive
Circumferential
Direction
Flaw Detected
in Negative
Circumferential
Direction
LWave
SWave
LWave
SWave
LWave
SWave
LWave
SWave
Axial
Notch
YES
YES
YES
YES
Circ.
Notch
YES
YES
NO
NO
Round
Bottom
Hole
YES
YES
NO
NO
NO
NO
NO
NO
Axial
Slot
Round
Bottom
Hole
NO
NO
NO
YES
YES
YES
YES
YES
Axial
Slot
YES
YES
YES
YES
1
2
Back
Side of
Flange
ID of
Flange
E-29
Table E-2
Manual examination detection results
Flaw
Number
Flaw
Location
Flaw
Type
Flaw Detected
in Positive
(Down) Axial
Direction
Flaw Detected
in Negative
(Up) Axial
Direction
Flaw Detected
in Positive
Circumferential
Direction
Flaw Detected
in Negative
Circumferential
Direction
LWave
SWave
LWave
SWave
LWave
SWave
LWave
SWave
Axial
Notch
YES*
YES*
YES
YES
Circ.
Notch
YES
YES
Round
Bottom
Hole
YES
YES
YES*
YES*
YES
YES
Axial
Slot
Round
Bottom
Hole
YES
YES
YES
YES
Axial
Slot
YES
YES
YES
YES
1
2
Back
Side of
Flange
ID of
Flange
* No screen shots were captured for these detections because negative circumferential data was
adequate.
E-30
Flaw 1 Automated: Axial Notch on the Back Side of the Flange
Flaw 1
Flaw 1
Figure E-48
Flaw 1 seen with a 50 L-wave looking positive
Flaw 1
Flaw 1
Figure E-49
Flaw 1 seen with a 50 S-wave looking positive
E-31
Flaw 1
Flaw 1
Figure E-50
Flaw 1 seen with a 50 L-wave looking negative
Flaw 1
Flaw 1
Figure E-51
Flaw 1 seen with a 50 S-wave looking negative
E-32
Flaw 2 Automated: Circumferential Notch on the Back Side of the Flange
OD Corner
Flaw 2
Back Wall
Figure E-52
Flaw 2 seen with a 45 L-wave looking down
OD Corner
Flaw 2
Figure E-53
Flaw 2 seen with a 48 S-wave looking down
E-33
Flaw 3 Automated: Round Bottom Hole Flaw on the Back Side of the Flange
OD Corner
Flaw 3
Back Wall
Figure E-54
Flaw 3 seen with a 46 L-wave looking down
OD Corner
Flaw 3
Figure E-55
Flaw 3 seen with a 45 S-wave looking down
E-34
Flaw 5 Automated: Round Bottom Hole Flaw on the ID of the Flange
Flaw
Flaw 55
Figure E-56
Flaw 5 seen in a 30 merge L-wave looking negative
Flaw55
Flaw
Figure E-57
Flaw 5 seen in a 30 merge L-wave looking positive
E-35
Flaw55
Flaw
Figure E-58
Flaw 5 seen in a 30 merge S-wave looking negative
Flaw55
Flaw
Figure E-59
Flaw 5 seen in a 30 merge S-wave looking positive
E-36
Figure E-60
Flaw 5 seen off a bounce in a 4045 S-wave merge from the scan looking up
Flaw 6 Automated: Round Bottom Hole Flaw on the ID of the Flange
Flaw 56
Flaw
Figure E-61
Flaw 6 seen in a 30 merge L-wave looking negative
E-37
Flaw 6
5
Flaw
Figure E-62
Flaw 6 seen in a 30 merge L-wave looking positive
Flaw65
Flaw
Figure E-63
Flaw 6 seen in a 30 merge S-wave looking negative
E-38
Figure E-64
Flaw 6 seen in a 30 merge S-wave looking positive
Flaw 1 Manual: Axial Notch on the Back Side of the Flange
Flaw 1
Figure E-65
Approximate location of array while imaging Flaw 1
E-39
Flaw 1
Figure E-66
Flaw 1 seen with a 49 L-wave
Figure E-67
Flaw 1 seen with a 48 S-wave
E-40
Flaw 2 Manual: Circumferential Notch on the Back Side of the Flange
Flaw 2
Figure E-68
Flaw 2
Figure E-69
E-41
Flaw 2
Figure E-70
Flaw 2 seen with a 44.5 S-wave
Flaw 3 Manual: Round Bottom Hole Flaw on the Back Side of the Flange
Flaw 3
Figure E-71
E-42
Flaw 3
Figure E-72
Flaw 3
Figure E-73
Flaw 3 seen with a 50 S-wave
E-43
Flaw 5 Manual: Round Bottom Hole Flaw on the ID of the Flange
Flaw 5
Figure E-74
Approximate location of array looking negative while imaging Flaw 5
Flaw 5
Figure E-75
Flaw 5 seen with an 18.5 L-wave looking negative
E-44
Figure E-76
Flaw 5 seen with a 32 S-wave looking negative
Figure E-77
Approximate location of array looking positive while imaging Flaw 5
E-45
Flaw 5
Figure E-78
Flaw 5 seen with a 29.5 L-wave looking positive
Flaw 5
Figure E-79
Flaw 5 seen with a 32 S-wave looking positive
E-46
Flaw 6 Manual: Round Bottom Hole Flaw on the ID of the Flange
Flaw 6
Figure E-80
Approximate location of array looking negative while imaging Flaw 6
Flaw 6
Figure E-81
Flaw 6 seen with an 18 L-wave looking negative
E-47
Figure E-82
Flaw 6 seen with a 31.5 S-wave looking negative
Figure E-83
Approximate location of array looking positive while imaging Flaw 6
E-48
Figure E-84
Flaw 6 seen with an 18 L-wave looking positive
Figure E-85
Flaw 6 seen with a 30.5 S-wave looking positive
E-49
Comparison of PM/HIP Stainless Steel and Cast Stainless Steel

Inspectability
Overview
As described in the preceding sections of this appendix, the first two phases of
the project demonstrated the inspectability of the 316L stainless steel valve.
Phase one demonstrated that the ultrasonic transducer was able to adequately
transmit longitudinal and shear waves to image back wall and corner reflector
signals. Phase two demonstrated the ability of ultrasonic longitudinal and shear
waves to detect certain machined flaws down to 10% thickness in height. While
this information is positive, it is also important to compare these results to the
inspectability of another traditionally manufactured cast stainless steel (CSS)
material.
Equipment
Dell XPS Laptop
GEIT Array # 115-000-592 (1.5MHz, 16x1)
GEIT Wedge # 360-152-231, 36-inch diameter contoured for axial scanning
Examinations
For this examination, a cast stainless steel calibration block was selected to be
examined with phased array ultrasonic techniques. The calibration block chosen
was K-8939-1, which was made of 2.48-inch (63-mm) thick 304LH cast
stainless steel. Figures E-86 through E-88 show a drawing and two photographs
of the calibration block. Figure E-89 displays the grain structure for an etched
and polished section of the original pipe that was used to fabricate the calibration
block.
The inspection performed on the calibration block was set up to be as close as
possible to the exams on the 316L stainless steel valve. The same GEIT 115000-592 array was used and coupled to GEIT wedge 360-152-231 (contoured
for axial scanning). The exam was conducted using 070 longitudinal waves and
3565 shear waves. The target reflectors were a corner reflector at the edge of
the calibration block and the 30% (0.74 in./18.8 mm) EDM notch.
E-50
Figure E-86
Drawing of calibration block K8939-1
E-51
Figure E-87
End view of calibration block K8939-1
Figure E-88
Bottom view of calibration block K8939-1
E-52
Figure E-89
Photograph of the grain structure for calibration block K8939-1
Results
The examination of the K8939-1 calibration block revealed that it was
challenging to detect a corner reflector in the 304LH cast stainless steel material
with a longitudinal wave. The ultrasonic L-wave signal was not able to detect the
30% (0.74 in./18.8 mm) EDM notch. The ultrasonic S-wave signal was not able
to detect either the corner reflector or the EDM notch. A series of ultrasonic
data images were generated showing side-by-side comparisons of the sector scans
from the PM/HIP stainless steel valve and the CSS calibration block (see Figures
E-90 through E-93). The color palette used to represent the ultrasonic signal
displays low amplitudes as blue and high amplitudes as red. Defect signal
responses that are much higher in amplitude (closer to red) when compared to
the background noise (blue) are easier for an ultrasonic technician to identify.
Conversely, ultrasonic signal responses with a small signal to noise ratio (usually
represented by blue) are difficult to characterize. As a result, this comparison
demonstrated that the ultrasonic signal to noise ratios for the 316L component
fabricated using PM/HIP were superior to those obtained from the 304LH cast
stainless steel calibration block for similar reflectors.
E-53
Figure E-90
Image comparing PM/HIP and CSS L-wave corner reflectors
Figure E-91
Image comparing PM/HIP and CSS S-wave corner reflectors
E-54
Figure E-92
Image comparing PM/HIP and CSS L-wave EDM notch reflectors
Figure E-93
Image comparing PM/HIP and CSS S-wave EDM notch reflectors
E-55
Inspection Summary
A 316L stainless steel valve manufactured using powder metallurgy and hot
isostatic processing technologies was examined to determine the feasibility of
applying ultrasonic techniques to similar components. Using both longitudinal
and shear waves generated by a 1.5-MHz transducer, reflectors were adequately
imaged even through very thick portions of the flange. These preliminary results
show that this particular manufacturing process did not significantly challenge
the ultrasonic methods. Additionally, the 316L PM/HIP material had superior
ultrasonic inspectability when compared with the 304LH cast stainless steel
calibration block. Applying ultrasonic inspection techniques to cast stainless steel
components has traditionally been difficult for transducer frequencies of
1.5 MHz and greater, due to the materials microstructure. This new process for
component fabrication provides enhanced inspectability for ultrasonic techniques
and would be of great benefit to the industry.
There are a few items that were discovered during this investigation that should
be noted. The surface condition should be essentially smooth and flat for
adequate ultrasonic inspection. Because of the flange geometry and the surface
condition, the manual ultrasonic examinations, which allowed for more operator
control, performed better than the automated techniques. There was one
reflector (Flaw 4) that was installed incorrectly such that this particular direction
of sound propagation could not be evaluated. This can be very important because
it is possible to observe different ultrasonic responses when the sound travels in
different directions due to the material properties.
While this preliminary evaluation was overall successful, there are a few items
that should be considered for future work. Additional components manufactured
using this new approach should also be examined ultrasonically to identify any
inspection challenges. During this investigation, only a 1.5-MHz transducer was
used; however, higher-frequency transducers (2.25 MHz to 7.5 MHz) should
also be considered for the detection of defects. Additional reflectors should be
installed to conduct a more comprehensive ultrasonic evaluation. Finally, the
component surfaces should be polished and etched to facilitate observation of the
grain structure.
E-56
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Manufacture of Large Nuclear and Fossil Components Using Powder Metallurgy and Hot Isostatic Proce Ssing Technologies

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Program on Technology Innovation: Manufacture of

Large Nuclear and Fossil Components Using Powder

2012 TECHNICAL REPORT

EPRI Project Manager

3420 Hillview Avenue

DISCLAIMER OF WARRANTIES AND LIMITATION OF LIABILITIES

The following organizations prepared this report:

This publication is a corporate

The following individuals from the EPRI NDE Center in Charlotte,

An alternative manufacturing method, powder metallurgy coupled

Section 5: Manufacture and Characterization of

Stress Analysis .................................. C-1

Appendix D: Corrosion Data Supplied by

Figure 4-8 Cross-sectional view of an autogenous weld in

Figure E-5 360-151-053 on main flange OD looking at the

Figure E-23 360-151-054 on main flange OD looking at the

Figure E-41 UltraVision screen shot of 360-151-054 S-wave

Figure E-64 Flaw 6 seen in a 30 merge S-wave looking

Figure E-85 Flaw 6 seen with a 30.5 S-wave looking

Successful development and demonstration of the PM/HIP technology will

10. J. Scanlon et al., Mechanical Properties of PM Hiped Stainless Steel A

Section 2: What Is Powder Metallurgy?

It is important to note that powders produced by inert gas atomization are

Powder Consolidation, Vacuum Processing, and Hot Isostatic

individual particles with no residual voids, porosity, or grain boundary oxides.

a) 316L produced by PM/HIP

b) Typical wrought 316L (note minor difference in magnification, approximately 12%)

The structure is isotropic in all directions. That is, there is no texturing,

There are no significant non-metallic inclusions such as manganese sulfides

No residual delta ferrite as can be found in wrought products. Delta ferrite

alloy. Because of the favorable microstructural features described above, including

Cleaning/maintenance/inspection of the atomization mechanism

Sieving of powder to a specific mesh size to remove oversize particles

Restricted blending of powders (each heat of powder in the blend must

Storage of powder under a nitrogen or inert gas atmosphere

Controlled carbon content of can material to limit potential for carburization

Vibratory compaction of powder in the can

Specified vacuum level in can prior to sealing

Helium leak check of can after evacuation and sealing

Control, monitoring, and recording of furnace temperature using calibrated

Control, monitoring, and recording of argon pressure using calibrated

Analysis of sample from fill tube for argon ingress

Visual examination of can for abnormalities after removal from furnace

Dimensional check of parts after can removal

Verification of dimensions using calibrated measuring instruments and tools.

Chemical analysis of samples taken from finished parts or prolongations of

Density checking to verify freedom of microporosity (density > 99% wrought

Examination of microstructure at high magnification to confirm that the

Hardness test with maximum hardness specified.

Grain size control with maximum grain size specified.

Surface examination by liquid penetrant or magnetic particle testing as

Hydrostatic testing of pressure boundary parts.

Section 3: Why Consider PM/HIP for

These barriers can be overcome through focused research. EPRI, in conjunction

They eliminate inspectability issues and concerns.

They enable manufacture of large, complex components using near-net shape

They enable new alloy systems and targeted chemistries.

They enhance weldability.

They provide an alternate supply route for long-lead-time components.

They eliminate rework or repair of large cast components.

Inspectability. Inspection of large cast components such as pump housings, valve

Section 4: Valve Body Feasibility

Upon completion of the container (or can), manufactured from low-carbon

Inspection and Weldability Results