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Contract NAS5-270 _-

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NATIONAL AERONAUTICS AND SPACE ADMINISTRATION Goddard Space F l i g h t Center Washington, D.C.

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17 November 1960

ORATION O F AMERICA
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GCA T e c h n i c a l R e p o r t 60- 2

A HIGH VACUUM GAUGE CALIBRATION SYSTEM

Wallace S . K r e i s m a n

C o n t r a c t NAS5-270

NATIONAL AERONAUTICS AND SPACE ADMINISTRATION Goddard S p a c e F l i g h t C e n t e r Washington, D.C.

1 7 N o v e m b e r 1960

GEOPHYS I C s CORPORATION OF AMERICA Bedford, Massachusetts

A HIGH VACUUM GAUGE CALIBRATION SYSTEM

by

Wallace S. Kreisman

SUMMARY
An ultra-high vacuum type metal and glass system has been constructed for the purpose of calibrating vacuum gauges in the pressure
-*

region from 760 to 10

-7

torr. The high vacuum portion of the system is

0

bakeable at temperatures up to 450 C.

A mercury manometer serves as a pressure standard in the region

from 760 to 20 torr, and three specially designed, bakeable McLeod gauges with overlapping pressure ranges serve as pressure standards in the region

0 from 20 torr to 1 x 1

-4

torr. Theoretical accuracies of 1 percent or

better are expected for the McLeod gauge readings in this pressure region. Pressures from 1 x 10-4 torr to 1 0-7 torr region can be measured, but the accuracy of the readings depends on adsorption and outgassing effects. Results pertaining to the reproducibility of measurements and comparisons of various gauge readings are presented. A pressure rise measurement technique is used to determine how the vacuum gauges and other system components are behaving.

CONTENTS

Page

............................................................ INTRODUCTION ....................................................... SYSTEM CONSTRUCTION ................................................ PRESSURE STANDARDS ................................................. OPERATING P R 0 C E D S . ...............................................
Summary

3
10

14
16
22

......................................... PRESSURE R I S E MEASUREMENT TECHNIQUE ................................ ACI<NOWLEDGMENTS.................................................... R e f e r e n c e s .........................................................

SYSTEM AND CmPONENT TESTS

24
27

iii

INTRODUCTION In connection with the design and development of high vacuum gauges and mass spectrometers, it is necessary to have some means of accurately calibrating these instruments for pure gases and mixtures. A specialized system has been constructed to fulfill this requirement and, at the same time, provide a means f o r studying such processes as ionization gauge pumping and outgassing, adsorption, temperature effects, etc. In this way, the system is used not only to calibrate gauges, but to improve calibration procedures as well. The problems of pressure gauge calibration have not received extensive treatment in the literature. Such a treatment requires integration of information about pressure gauges, pumping systems, gas flow, adsorption and desorption, etc. Dushman, for example, (Reference I) treats each of the subjects mentioned above rather extensively, but says little or nothing
-\

about calibration work. The recent book on pressure measurement by Leck (Reference 2) does have a short ( 6 page) chapter on gauge calibration. Guthrie and Wakerling (Reference 3 ) also 'devote some space to a discussion of what the various vacuum gauges actually measure, Each of the three books just mentioned provide references to individual papers concerning vacuum gauges and vacuum measurement. Only a very few vacuum gauge calibration systems have been discussed in the literature. A description o i a demountable type vacuum gauge calibration system is given in a paper by L-Clanc (Reference 4 ) . His system

used waxed and greased connections and was not intended for use at pressures -5 below 10 torr. Alpert (Reference 5) has developed a null-reading absolute manometer that can be used with a pressure reduction technique to measure

low pressures in a closed system. Such an arrangement has not attained wide usage. The high vacuum gauge calibration system described in this paper is basically a glass-metal, ultra-high vacuum system, all essential vacuum components of which may be baked out at temperatures up to 450 C.
0

This

type of design was chosen to minimize the contamination of introduced gases and to facilitate the studies of adsorption, desorption, pumping, etc., previously mentioned. Vacuum gauge calibrations from pressures of 760 torr to pressures below 10
-5

torr can be performed with this apparatus. A mercury manometer

and a set of three mercury McLeod gauges are the primary pressure standards. These units have been developed specially for this purpose. Preliminary tests of system components and system operation have been made and some operating procedures have been established. A description is given of a pressure rise method of testing vacuum gauges and low pressure phenomena.
A great deal of work remains to be done to develop calibration

system components and techniques for measuring low pressures.

There is a

definite need for new low pressure standards and for careful evaluation of existing standards and the methodology of their use.

It is hoped that the

system described herein can be used to make contributions in this area of research.

SYSTEM CONSTRUCTION The c a l i b r a t i o n system is shown s c h e m a t i c a l l y i n t h e block diagram of F i g u r e 1. operation. tion. F i g u r e 2 i s a n o v e r - a l l view of t h e c a l i b r a t i o n system i n

F i g u r e 3 i s a close-up showing some of t h e d e t a i l e d c o n s t r u c -

I n c o n n e c t i o n w i t h t h e d e s c r i p t i o n t h a t f o l l o w s , i t w i l l prove h e l p -

f u l t o r e f e r t o t h e b l o c k diagram and t h e two photographs t h a t f o l l o w . The e n t i r e system i s mounted on a t h r e e s e c t i o n , modular-type electronics cabinet. The major p o r t i o n s of t h e u l t r a - h i g h vacuum system

(which i n c l u d e s t h e McLeod gauges) a r e mounted w i t h i n t h e Veeco motorized l i f t , model F H h i g h t e m p e r a t u r e oven. s i o n s of 23" x 18" x 20", The oven, f e a t u r i n g i n t e r i o r dimenWithin t h e
x 22%", which

i s a n i n t e g r a l p a r t of t h e system.

oven a r e two p a r a l l e l s t a i n l e s s s t e e l mounting b a r s , 3" x

are l o c a t e d j u s t above t h e i n s u l a t e d oven base and are spaced a b o u t 9 i n c h e s

apart. G r a n v i l l e P h i l l i p s type C u l t r a - h i g h vacuum (UHV) v a l v e s are f a s t e n e d

t o t h e s e mounting b a r s , and a l a r g e p a r t of t h e vacuum system i s connected t o , and s u p p o r t e d by, t h e v a l v e s . The McLeod gauges a r e s e a t e d i n p l a s t e r

molds which r e s t on a mounting p l a t e l o c a t e d between, and f a s t e n e d t o , t h e mounting b a r s . I n t h i s way, t h e components w i t h i n t h e oven a r e a l l s u p p o r t e d

by t h e same r i g i d s t u r c t u r e t o minimize r e l a t i v e movements due t o mechanical and t h e r m a l stresses. T i g h t e n i n g t h e UHV valves i s one such mechanical

stress.

The major stresses are caused by t e m p e r a t u r e g r a d i e n t s t h a t b u i l d

up d u r i n g t h e bakeout p e r i o d . The pumping p o r t i o n of t h e vacuum system i s f a i r l y c o n v e n t i o n a l . It c o n s i s t s of a Welch Model 1400B 2 1 l i t e r / m i n . mechanical fore-pump and a n H . S . M a r t i n Company model M-40112 80 l i t e r / s e c . , t h r e e j e t , w a t e r - c o o l e d , g l a s s , mercury d i f f u s i o n pump. The fore-pump i s mounted i n a t r a y t h a t

Bottle bakeout cutoff

7Dessi cant

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Large Reservotr .Volve
'

Small Reservoir

vent bakeout cutoff

cutoff

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Thermocouple Gouge Fore . vocuum Fore Vacuum Reservoir

vent and leak test volve Dessicont

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Mechanical Fore Pump

Mer cur y Diffusion Pump

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C o Id Trap
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GRANVILLE PHILLIPS
HOKE

VALVE

VALVE

VACUUM CONNECTIONS

Figure 1.

Block Diagram of Vacuum Gauge Calibration System

F i g u r e 2.

Overall V.iew of t h e Calibration System

5

Figure 3 .

Close-up V i e w of Oven I n t e r i o r and McLeod Gauge Mercury R e s e r v o i r s

r e s t s e i t h e r on t h e c a b i n e t c a s t e r brackets o r e l s e i s s u p p o r t e d d i r e c t l y
from t h e ;:loor by means of f o u r c o r n e r j a c k s c r e w s .
When supported from t h e

f l o o r , t h e mechanical pump i s e f f e c t i v e l y i s o l a t e d from t h e c a b i n e t , being connected t o t h e vacuum system o n l y by a l e n g t h of rubber t u b i n g . The v i -

b r a t i o n miniii.ization a f f o r d e d by t h i s c o n s t r u c t i o n i s e s s e n t i a l f o r optimum performance of t h e mercury manometer and McLeod gauges.

A fore-vacuum c o l d t r a p (dry i c e ) , a v a l v e , and a l a r g e g l a s s

r e s e r v o i r s e p a r a t e t h e mechanical and d i f f u s i o n pumps. The r e s e r v o i r makes

i t p o s s i b l e t o t u r n o f f t h e mechanical pump completely when r e q u i r e d .

On t h e h i g h vacuum s i d e of the d i f f u s i o n pump t h e r e i s t h e conventional liquid nitrogen cold t r a p . The main pumping l i n e runs from t h i s

t r a p s t r a i g h t up through t h e i n s u l a t e d oven base and connects t o t h e LHV pumping v a l v e . The pumping v a l v e connects t o t h e manifold which, i n t u r n ,

h a s c o n n e c t i o n s t o two r e a g e n t g r a d e , 1 l i t e r gas b o t t l e s and a l a r g e gas c y l i n d e r ( t a n k gas i n F i g u r e 1). The l a t t e r c o n n e c t i o n can be e a s i l y

I t should be n o t e d t h a t each

broken f o r t h e purpose of v e n t i n g the system.

of t h e t h r e e c o n n e c t i o n s j u s t mentioned i s made through a p a i r of v a l v e s r a t h e r than a s i n g l e valve. The t h r e e bakeout c u t o f f v a l v e s a r e Hoke They a r e l o c a t e d a t t h e l e f t hand s i d e

model 411 diaphragm type v a l v e s .

of t h e c a l i b r a t i o n system below t h e i n s u l a t e d oven b a s e . The pumping manifold i s connected t o t h e measuring volume through t h e pumping manifold c o l d t r a p . This t r a p a c t s t o keep condensable m a t e r i a l s

o r i g i n a t i n g i n t h e pumping, v e n t i n g and g a s s a m p l e p o r t i o n s of t h e system. o u t of t h e measuring voluine. The measuring vo1um.e i s a 1 l i t e r , t h r e e neck

s p h e r i c a l f l a s k having a Veeco RG-75 i o n i z a t i o n gauge t u b e a t t a c h e d t o one neck, a H a s t i n g s R a y d i s t model D V - 1 7 , 0 t o 1000 micron p r e s s u r e r a n g e , g l a s s

e n v e l o p e thermocouple gauge a t t a c h e d t o t h e second neck, and t h e t h i r d neck a v a i l a b l e f o r gauges t o be c a l i b r a t e d . The thermocouple gauge i s used t o

g i v e c o n t i n u o u s q u a l i t a t i v e i n d i c a t i o n of p r e s s u r e w i t h i n i t s range. The McLeod gauges a r e mounted i n plaster molds w i t h i n t h e oven,

and t h e i r pumping t a b u l a t i o n s are connected t o g e t h e r and l e a d i n t o t h e

measuring voltgne througb t h e McLeod gauge v a l v e and t h e McLeod gauge c o l d trap, The mercury manometer a l s o leads i n t o t h e McLeod gauge c o l d t r a p

via t h e mercury manometer v a l v e .

The UHV t e s t gauge v a l v e can be used t o connect t h e measuring volume d i r e c t l y t o a gauge b e i n g t e s t e d . This valve has t h e g l a s s tubula-

t i o n s e a l e d when i t i s n o t connected t o a gauge, s o t h a t t h e v a l v e can be l e f t open d u r i n g bakeout.

A UHV gas expansion v a l v e j o i n s a small c a l i b r a t e d volume t o t h e

measuring volume. known p r e s s u r e . I n u s e , t h e c a l i b r a t e d volume i s f i l l e d w i t h a gas a t a The remainder of t h e system (having a known measured volume)

i s t h e n pumped down t o a low background p r e s s u r e , a f t e r which t h e g a s i n t h e

c a l i b r a t e d volume is allowed t o expand i n t o t h e remainder of t h e system.

By m o n i t o r i n g t h e new p r e s s u r e i n t h e system, i t i s p o s s i b l e t o measure

a d s o r p t i o n and perform c a l i b r a t i o n work. The mercury c u t o f f v a l v e s f o r t h e low p r e s s u r e and d u a l medium and h i g h p r e s s u r e McLeod gauges are l o c a t e d below t h e oven e n c l o s u r e where they may be k e p t c o o l w i t h a n a i r blower d u r i n g t h e bakeout p e r i o d . An E a l i n g model 6165 c a t h e t o m e t e r i s used t o r e a d t h e p o s i t i o n s of t h e mercury columns i n t h e McLeod gauges and t h e manometer. The c a t h e -

tometer I s mounted on a metal s t a n d t h a t i s equipped w i t h f o u r c a s t e r s f o r e a s y m o b i l i t y and four jackscrews for s u p p o r t i n g t h e s t a n d i n a f i x e d

position.

The s t a n d may be r i g i d l y joined t o t h e c a l i b r a t i o n system To a i d i n r e a d i n g t h e McLeod

c a b i n e t by means of a n a n g l e i r o n b r a c k e t .

gauges and manometer, i l l u m i n a t i o n boxes are a p p r o p r i a t e l y p o s i t i o n e d on t h e system and c o n t r o l l e d by a s w i t c h a t t h e c a t h e t o m e t e r . F i l l i n g and

emptying of t h e McLeod gauges i s a l s o c o n t r o l l e d by a n e l e c t r i c a l s w i t c h

a t the cathetometer.
Mercury i s brought i n t o and t a k e n o u t of t h e McLeod gauges by r a i s i n g and lowering vacuum-tight, s t a i n l e s s s t e e l r e s e r v o i r s t h a t a r e coupled t o t h e McLeod gauge via f l e x i b l e m e t a l h o s e s . Mercury c a n b e i n -

t r o d u c e d i n t o t h e s e r e s e r v o i r s through small v a l v e s l o c a t e d a t t h e t o p s of the reservoirs. J u s t below t h e s e v a l v e s a r e l o c a t e d closed-end mercury

manometers t o i n d i c a t e t h e s t a t e of vacuum e x i s t i n g above t h e r e s e r v o i r mercury.

A m o t o r i z e d l i f t i s used t o raise and lower t h e mercury reser-

voirs.

The l i f t i s a modified v e r s i o n of a commercially a v a i l a b l e b e l l

It makes u s e of a 1/15 horsepower double r e d u c t i o n g e a r motor

jar l i f t .

t h a t t u r n s a saginaw screw.

A saginaw n u t , which i s f i r m l y a t t a c h e d t o
The two

two p a r a l l e l u p r i g h t s t e e l r o d s , r i d e s up and down on t h e screw.

r o d s are c o n s t r a i n e d t o move v e r t i c a l l y by f i x e d - p o s i t i o n b a l l b u s h i n g s .
A h o r i z o n t a l r e c t a n g u l a r b a r , which may b e a d j u s t e d i n p o s i t i o n , i s clamped

t o t h e s t e e l r o d s n e a r t h e i r upper end.

Two heavy aluminum r e s e r v o i r h o l d e r s

a r e suspended from t h e r e c t a n g u l a r bar by T - s l o t b r a c k e t arrangements s o

t h a t t h e y may b e e a s i l y removed. Brackets a r e also provided t o suspend

t h e r e s e r v o i r h o l d e r s a t a f i x e d l e v e l below t h e mercury c u t o f f v a l v e s . T h i s i s done s o t h a t t h e mercury of the McLeod gauges c a n b e lowered below t h e c u t o f f valves and t h u s i s o l a t e d from t h e vacuum system d u r i n g b a k e o u t .

There are f o u r c o n t r o l panels on t h e c a l i b r a t i o n system.

One i s

f o r c o n t r o l of t h e mechanical and d i f f u s i o n pumps; t h e second i s a modified Veeco c o n t r o l u n i t f o r t h e i o n i z a t i o n gauge ( p r o v i s i o n has been made t o r e d u c e t h e i o n i z i n g e l e c t r o n c u r r e n t t o v e r y small v a l u e s and t o measure t h e s e c u r r e n t s ) ; t h e t h i r d is a standard f i v e - p o s i t i o n Hastings Raydist c o n t r o l u n i t f o r t h e thermocouple gauges; and t h e f o u r t h p a n e l c o n t r o l s t h e s p e e d w i t h which t h e mercury r e s e r v o i r s are r a i s e d o r lowered. These

f o u r u n i t s are i n a d d i t i o n t o t h e oven t e m p e r a t u r e , f a n , and l i f t c o n t r o l s t h a t are on t h e oven i t s e l f .

PRESSURE STANDARDS

The mercury manometer i s t h e fundamental primary p r e s s u r e s t a n d a r d of t h e c a l i b r a t i o n system. For p r e s s u r e s above 20 t o r r , t h e manometer

i s used d i r e c t l y as a s t a n d a r d .

In the p r e s s u r e r e g i o n j u s t below 20 t o r r ,

t h e manometer i s used t o check t h e p r e s s u r e r e a d i n g s of t h e h i g h p r e s s u r e McLeod gauge. The h i g h p r e s s u r e McLeod gauge range o v e r l a p s t h a t of t h e

medium p r e s s u r e McLeod gauge, so t h a t t h e l a t t e r gauge r e a d i n g s may a l s o be r e f e r e n c e d t o t h o s e of t h e manometer. F i n a l l y , t h e medium p r e s s u r e McLeod

gauge r a n g e o v e r l a p s p a r t of t h e range of t h e low p r e s s u r e McLeod gauge, s o t h a t t h e s e r e a d i n g s a l s o may be r e f e r r e d t o t h o s e of t h e manometer. The mercury manometer i s of t h e c o n v e n t i o n a l U-tube v a r i e t y , and

i s c o n s t r u c t e d of 3 / 4 i n c h I.D. p r e c i s i o n - b o r e g l a s s t u b i n g .

Each l e g of

t h e manometer i s connected v i a a Hoke 440 bellows t y p e vacuum v a l v e t o t h e mercury manometer valve w i t h i n t h e oven. Mercury w a s c a r e f u l l y vacuum

d i s t i l l e d i n t o t h e manometer so t h a t no trace of g a s bubbles a l o n g t h e g l a s s

w a l l s is evident.

The m n o m e t e r i s kept c o n t i n u o u s l y under h i g h vacuum ex-

c e p t when i t i s i n u s e .

10

The manometer i s r e a d w i t h a c a t h e t o m e t e r which i s equipped w i t h

a micrometer screw f o r a c c u r a t e l y measuring d i s t a n c e s up t o 30 m i l l i m e t e r s .

The smallest d i v i s i o n on t h e micrometer s c a l e r e p r e s e n t s 5 microns, and

estimates t o t h e n e a r e s t micron may be made.

For a c o n s t a n t p r e s s u r e i n

t h e system, a series o f measurements of t h e mercury column h e i g h t d i f f e r e n c e ( w i t h t h e columns b e i n g hand tapped between r e a d i n g s ) y i e l d e d s t a n d a r d dev i a t i o n s of a b o u t 10 t o 20 microns. i f t h e columns are n o t hand tapped. The t h r e e McLeod gauges were c o n s t r u c t e d t o cover t h e p r e s s u r e range from 20 t o r r down t o t h e 10 10 Deviations less t h a n t h i s a r e o b t a i n e d

-7

t o r r r e g i o n , w i t h p r e s s u r e s between

-4

t o r r and 20 t o r r being measured with 1 p e r c e n t a c c u r a c y o r b e t t e r .

P a s t e x p e r i e n c e has i n d i c a t e d t h a t one c o u l d n o t hope t o s a t i s f y more s t r i n g e n t low p r e s s u r e requirements a t t h e p r e s e n t s t a t e - o f - t h e - a r t . The McLeod gauges were designed i n such a way t h a t t h e y c o u l d be mounted w i t h i n t h e oven e n c l o s u r e and baked o u t a t h i g h temperature w i t h t h e o t h e r system components. This requirement l i m i t e d t h e gauge dimensions The medium and h i g h p r e s s u r e gauges were

as i n d i c a t e d i n F i g u r e s 4 and 5 .

combined i n a s i n g l e u n i t t o conserve space and p e r m i t one mercury reserv o i r t o f i l l b o t h gauges s i m u l t a n e o u s l y . The h i g h p r e s s u r e McLeod gauge measures p r e s s u r e s from 20 t o r r

-1 t o 2.00 x 10 t o r r w i t h a c a l c u l a t e d a c c u r a c y of 1 p e r c e n t , and lower

p r e s s u r e s w i t h c o r r e s p o n d i n g l y less accuracy. gauge measures p r e s s u r e s from 4.00 x 10 The medium p r e s s u r e McLeod t o r r with 1 The low p r e s s u r e t o r r with

-1

t o r r t o 4.00 x

p e r c e n t a c c u r a c y , and lower p r e s s u r e s w i t h less a c c u r a c y . McLeod gauge measures p r e s s u r e s from 8.00 x 10

-3

t o 8.00 x

a c a l c u l a t e d a c c u r a c y of 1 p e r c e n t , and lower p r e s s u r e s w i t h less a c c u r a c y .

11

Not Over

I" 15,-

Figure 4.

Low Pressure McLeod Gauge

12

A
OVER
I

c
--W" --Figure 5.
13

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D u a l Medium and High Pressure McLeod Gauge

The dimensions of t h e l a t t e r gauge a r e such, t h a t i n s q u a r e l a w o p e r a t i o n ,

1 mm c o r r e s p o n d s t o a p r e s s u r e of 2 x 10

-7

torr.

The d e l i b e r a t e o v e r -

l a p p i n g of t h e 1 p e r c e n t a c c u r a c y p r e s s u r e ranges of t h e t h r e e gauges i s

a f e a t u r e which e n a b l e s gauge measurements t o be compared, t h u s r e v e a l i n g

s y s t e m a t i c e r r o r s that depend on gauge geometry. Mercury i s vacuum d i s t i l l e d i n t o t h e two McLeod gauge s t a i n l e s s

s t e e l r e s e r v o i r s and i s k e p t under vacuum c o n t i n u o u s l y t o minimize o u t gassing during operation. The mercury s u r f a c e i s always c l e a n and b r i g h t ,

and t h e r e have never been any gas bubbles v i s i b l e a t t h e mercury g l a s s interface. The h e i g h t s of t h e McLeod gauge mercury columns are normally measured t o 0.05 mm w i t h t h e c a t h e t o m e t e r . D i f f e r e n c e s between t h e h e i g h t s

o f t h e columns t h a t do n o t exceed 30 m c a n b e measured t o a few microns w i t h t h e micrometer v e r n i e r adjustment of t h e c a t h e t o m e t e r .

OPERATING PROCEDURES
S t a r t i n g w i t h t h e complete c a l i b r a t i o n system a t atmospheric p r e s s u r e , t h e system i s evacuated i n the f o l l o w i n g manner in o r d e r t o keep
i t a s c l e a n as p o s s i b l e .

F i r s t , dry i c e i s p l a c e d on t h e fore-vacuum c o l d When t h e f o r e p r e s s u r e

t r a p dewar and t h e mechanical pump i s t u r n e d on.

reaches a v a l u e of t h e o r d e r of 10 microns, b o t h t h e pumping valve and t h e

fore-vacuum i s o l a t i o n v a l v e are c l o s e d , t h e dewar i s removed from t h e f o r e vacuum t r a p , and t h e t r a p i s warmed up t o d r i v e o f f t h e v a p o r s t h a t have condensed t h e r e . When t h e t r a p i s c l e a n , t h e dewar w i t h d r y i c e i s a g a i n The mercury d i f f u -

p l a c e d i n p o s i t i o n , and t h e i s o l a t i o n v a l v e i s opened.

s i o n pump i s t u r n e d on, and t h e d i f f u s i o n pump c o l d t r a p i s h a l f - f i l l e d

14

with liquid nitrogen.

The pumping v a l v e i s opened, and tho ov n p o r t i o n When the g l a s s thermocouple gaugl r e a d s

of t h e s y s t e m i s pumped down.

e s s e n t i a l l y z e r o , t h e i o n i z a t i o n gauge i s turned on s o t h a t t h e ;:ystem p r e s s u r e can be monitored c o n t i n u o u s l y . When t h e p r e s s u r e i n t h e s y s t e m A f t e r bakeout and c o o l i n g ,

i s s u f f i c i e n t l y l o w , bakeout may be commenced.

t h e d i f f u s i o n pump c o l d t r a p i s f i l l e d t o t h e top w i t h l i q u i d n i t r o g e n , and t h e s y s t e m i s ready f o r u s e . A f t e r t h e bakeout p e r i o d , the s y s t e m i s u s u a l l y allowed t o pump down t o a l i m i t i n g p r e s s u r e of about 2 x 10
-I

torr.

A t this point, liquid

n i t r o g e n i s i n t r o d u c e d i n t o t h e dewars t h a t surround t h e pumping manifold c o l d t r a p and t h e McLeod gauge c o l d t r a p . The l e v e l of t h e l i q u i d n i t r o g e n

i n t h e s e dewars should be k e p t f a i r l y c o n s t a n t , With t h e system a t a low p r e s s u r e , t h e g a s b o t t l e s can be opened, and t h e t u b i n g up t o t h e now c l o s e d G r a n v i l l e P h i l l i p s g a s v a l v e s can be f i l l e d with gas.
By c l o s i n g t h e gas bakeout c u t o f f v a l v e s , s m a l l amounts

of g a s a r e i s o l a t e d between t h e v a l v e s and can be used f o r c a l i b r a t i o n work. The G r a n v i l l e P h i l l i p s u l t r a - h i g h vacuum v a l v e s can be used t o admit g a s i n t o t h e system from low leak r a t e s t o v e r y h i g h l e a k r a t e s . Un-

f o r t u n a t e l y , f i n e a d j u s t m e n t of t h e leak r a t e w i t h t h e s e v a l v e s i s d i f f i cult. wrench. S e t t i n g s could be o n l y roughly reproduced w i t h t h e a i d of a torque

N e w G r a n v i l l e P h i l l i p s s e r i e s 9100 v a r i a b l e l e a k s a r e being used

t o replace these gas valves. The normal c a l i b r a t i o n procedure c o n s i s t s of t h e f o l l o w i n g s t e p s : The system i s f i r s t pumped down and baked o u t at a t e m p e r a t u r e of between

15

300 and 45OoC f o r one hour o r more.

System pumping i s continued u n t i l t h e

p r e s s u r e i n t h e measuring volume, as read by t h e i o n i z a t i o n gauge, i s a t

a l e v e l t h a t i s w e l l below t h e p r e s s u r e a t which c a l i b r a t i o n s are t o be

made.

A t t h i s t i m e , a continuous flow of t h e c a l i b r a t i n g g a s i s e s t a b -

l i s h e d s o t h a t t h e lowest c a l i b r a t i o n p r e s s u r e e x i s t s i n t h e measuring

vo lume

.
A s e r i e s of p r e s s u r e r e a d i n g s i s t a k e n w i t h b o t h t h e a p p r o p r i a t e

p r e s s u r e s t a n d a r d McLeod gauge and t h e gauge being c a l i b r a t e d .

The gas

flow i s t h e n i n c r e a s e d s t e p by s t e p t o o b t a i n h i g h e r p r e s s u r e s i n t h e measuring volume and t h e measuring procedure i s r e p e a t e d a t each s t e p .

It

i s i m p o r t a n t t h a t s u f f i c i e n t t i m e be allowed f o r t h e e n t i r e system t o r e a c h
i t s new h i g h e r p r e s s u r e each t i m e t h e gas flow i s i n c r e a s e d . SYSTEM AND COMPONENT TESTS Only a l i m i t e d amount of experimental work h a s been c a r r i e d o u t t o d a t e w i t h t h i s system. Most of t h e work h a s been concerned w i t h t e s t i n g

t h e o p e r a t i o n of t h e v a r i o u s system components

--

e s p e c i a l l y t h e McLeod

gauges , mercury manometer, t h e continuous flow of v a r i o u s g a s e s through t h e measuring volume a t d i f f e y e n t p r e s s u r e l e v e l s , and t h e procedures f o r baking t h e system and pumping down t o low background p r e s s u r e s . Background p r e s s u r e s a s low a s 5 x 10
-9

t o r r i n t h e measuring

volume, as r e a d by t h e Veeco i o n i z a t i o n gauge, have been a c h i e v e d by u s i n g o n l y a moderate bakeout a t 300 C f o r one h o u r , followed by o v e r n i g h t i o n gauge pumping. The system h a s a l s o been baked o v e r n i g h t a few t i m e s a t
-7 Background p r e s s u r e s of 2 x 10 t o r r , as r e a d
0

4500C w i t h no d i f f i c u l t y .

by t h e i o n i z a t i o n gauge, a r e r o u t i n e l y e s t a b l i s h e d i n t h e measuring volume ( w i t h t h e McLeod gauges and t h e i r mercury i n t h e s y s t e m ) w i t h o u t any bakeout 16

Continuous flows of pure, reagent grade nitrogen have been established in the system corresponding to pressures ,in the low 1 0 region, as read by the ion gauge.
-7

torr

Steady flows of prepurified nitrogen

from the high pressure cylinder and pressure regulator have been obtained, corresponding to system pressures as high as 20 torr, as read by the manometer. The diffusion pump is turned off, of course, during these relatively high pressure measurements,
A series of experiments were performed to test the operation of

the McLeod gauges. The gauges were filled at various speeds, and the optimum rate of filling, as determined from observation of the mercury motion in the capillaries, was established. Experiments were made to determine the effect of hand tapping and mechanically vibrating the capillaries at low frequencies of the order of 60 cycles per second. This matter is not settled yet, but it appears that the vibration technique, while yielding more reproducible readings, tends to raise the mercury t o nonequilibrium positions, from which it may not recover in the case of small bore (1 mm dia. or less) capillaries. Since hand tapping gives rise to poor reproducibility of readings, the only acceptable method appears to be a controlled filling
of the capillaries under conditions of minimum vibration. For the high

pressure gauge with its 2 mm dia. bore capillary, the equilibrium position of the mercury columns is reached in a matter of seconds. For the medium and low pressure gauges with their small bore capillaries, the equilibrium position is attained after several minutes. The initial comparison of the readings of the mercury manometer with those of the high pressure McLeod gauge was made by bleeding laboratory air into the system through a filter, desiccant, external liquid

17

n i t r o g e n c o l d t r a p , and a V a c t r o n i c Vari-Vac a d j u s t a b l e l e a k . o f t h e s e measurements are g i v e n i n Table I .

The r e s u l t s

The i n c r e a s e i n t h e e r r o r f o r

p r e s s u r e s of a b o u t 6 t o r r and h i g h e r a r e b e l i e v e d t o be due t o poor i l l u m i n a t i o n of t h e mercury m e n i s c i i n the manometer, when t h e levels become s e p a r a t e d by t h i s amount. one. This comparison i s c o n s i d e r e d o n l y a p r e l i m i n a r y

The p r e l i m i n a r y comparison between t h e r e a d i n g s of t h e h i g h and

medium p r e s s u r e McLeod gauges w a s performed w i t h a continuous flow of p r e p u r i f i e d n i t r o g e n from t h e h i g h p r e s s u r e c y l i n d e r through a n e x t e r n a l l i q u i d n i t r o g e n c o l d t r a p and t h e V a r i - V a c a d j u s t a b l e l e a k . R e s u l t s of

t h i s comparison are summarized i n Table 11. The medium p r e s s u r e gauge gave c o n s i s t e n t l y lower r e a d i n g s t h a n t h e h i g h p r e s s u r e gauge by amounts t h a t are d e f i n i t e l y g r e a t e r t h a n the systematic and e x p e r i m e n t a l e r r o r s of t h e two gauges.

It i s p o s s i b l e t h a t a d s o r p t i o n and d e s o r p t i o n e f f e c t s are

responsible f o r t h i s systematic difference i n the readings. When medium and low p r e s s u r e McLeod gauge r e a d i n g s were t a k e n of f o u r d i f f e r e n t p r e s s u r e s of pure n i t r o g e n i n a continuous flow f a s h i o n , t h e s a m e s o r t of r e s u l t s were o b t a i n e d as d i s c u s s e d above.

In t h i s case,

t h e low p r e s s u r e gauge y i e l d e d readings t h a t w e r e 8 t o 10 p e r c e n t below t h o s e o b t a i n e d w i t h t h e medium p r e s s u r e gauge. i n Table 1 1 1 . There a r e a t l e a s t t h r e e p o s s i b l e e x p l a n a t i o n s f o r t h e s e r e s u l t s . The f i r s t i s that w a t e r vapor i s p r e s e n t i n t h e McLeod gauges and i s b e i n g condensed o u t by t h e low p r e s s u r e gauge. The second i s t h a t t h e n i t r o g e n These r e a d i n g s are shown

i s b e i n g adsorbed i n t h e gauges
gauge.

--

t o a g r e a t e r e x t e n t i n t h e low p r e s s u r e

The t h i r d e x p l a n a t i o n i s t h a t o u t g a s s i n g from t h e mercury more

COMPARISON O F MERCURY MANOMETER AND HIGH PRESSUR McLEOD GAUGE READINGS FOR A CONTINUOUS FLOW O F DRlD LABORATORY A I R

(och pressure value below i s an overage o f

five

readings)

AVRAG

PRESSURE

VALUES

STANDARD D E V l A TIONS OF AVERAG PRSSUR VALUS

Mercury Monometer Pressure

McLeod Gouge Pressure

Me r cury Monometer De viaf ion

Mc L eod
Gouge Dev i 0 t ion

HPG

1 . 4 2 3 mm f f g
2.300 3.385

I . 4.20 mm ffg

- 0.21 %

0.009 mm Hg

0 . 0 0 3 mm Hg
0.003

2.301
3.386

+ 0.04

0.037

+ 0.03
- 0.8/
4- 1 . 6 7
-I-1 . 2 5

0.019 0.016 0.0/6

0.009

0.007

5.826

5.779
9.721 15.756

0.015
0.038 0 . 010

9.562
5.561

/9

COMPAR/SON O f HIGH PRESSURE AND MEDIUM PRSSUR McLOD GAUGtF RAD/NGS FOR A CONTINUOUS FLOW O F PRPUR/F/D NITROGEN

(Each pressure value below i s an averoge o f

five

readings 1

AYERAG

PRSSUR

VALUES
- .

High Pre ssure Gauge Reading

Me dium Pressure Gauge Reading

%PG

Error

%#PG- ffPG
HPG

High Pr e ssure Gauge Deviation

M e dium Pressure Gouge Deviation

PHPG

0 . 0 8 8 mm ffg

I i
0 . 0 8 5 5 mm ffg

2.89%

0 . 0 0 1 mm ffg

O . O O / mm ffg

0 .f77
0.294

0./ ? 4
0.290
0.350

2.08
f

0.002

0.002

.50

0. OOf
0.003

o.oo/
0.003

0.363

3.58

20

COMPAR/SON OF AifD/UM PRS.SUR AND LOW PRESSURE McLEOD GAUG ffAD/NGS FOR A CONTINUOUS FLOW O F PUR N/TffOGAf

1
MD/UM PRESSUR GAUGE READ/NG MPG

I
LOW PffSSUR G A M RAD/NG
LPG

/.46

mm Hg

1.32

mm Hg

9.59 %

3.5/ 3.76
4 . /5

3.2/
3.45

8.55

8.25 8.20

3.8/

2/

e f f e c t i v e l y i n c r e a s e s t h e p r e s s u r e i n the s m a l l e r oiediuzn p r e s s u r e gauge.

PRESSURE RISE MEASUREMENT TECHKIQL'E

It may be of i n t e r e s t t o d e s c r i b e b r i e f l y a technique which w e

are c u r r e n t l y u s i n g f o r d i a g n o s t i c purposes, t h a t i s , t o h e l p u s determine

how t h e gauges and o t h e r system components a r e behaving.

In t h i s t e c h n i q u e

t h e system i s f i r s t baked and then pumped down t o a low background p r e s s u r e . With t h e pumping v a l v e open, a s m a l l gas flow from a 1 l i t e r gas b o t t l e i s e s t a b l i s h e d i n t h e pumping m a n i f o l d , and t h e e q u i l i b r i m p r e s s u r e i n t h e measuring chanber i s n o t e d .
A t a convenient time, thP piimping v a l v e i s

c l o s e d and t h e p r e s s u r e i s allowed t o r i s e i n t h z s y s t e m .

I f the leak is

m o l e c u l a r , t h e p r e s s u r e i n t h e systeni w i l l r i s e I n a n e x p o n e n t i a l f a s h i o n , t h e i n i t i a l phase of which i s p r a c t i c a l l y l i n e a r . Dttring t h i s p e r i o d of

r i s i n g p r e s s u r e , v a r i o u s measurements a r e trade w i t h t h e d i f f e r e n t gauges. Measurements of t h e r i s i n g p r e s s u r e a s a a d e w i t h a n i o n i z a t i o n gauge a r e shown i n F i g u r e 6 . Curve A r e p r e s e n t s t h e r e a d i n g s o b t a i n e d v i a The gauge i s turned on f o r 15

i n t e r m i t t e n t u s e of t h e i o n i z a t i o n gaage. seconds e v e r y 10 m i n u t e s . f i r s t 60 m i n u t e s .

The measured pressL.re r i s e i s l i n e a r d u r i n g t h e

By way of c o n t r a s t , curve B r e p r e s e n t s t h e r e a d i n g s Although t h e i o n i z i n g

o b t a i n e d w i t h t h e i o n i z a t i o n gauge on c o n t i n u o u s l y .

e l e c t r o n c u r r e n t w a s m a i n t a i n e d a t the low v a l u e of 100 microamperes i n each c a s e , t h e e E f e c t of i o n i z a t i o n gauge panping i s s t r i k i n g l y e v i d e n t . When McLeod gauges a r e i n c l u d e J i n t h e c l o s e d s y s t e m i n which t h e p r e s s u r e i s r i s i n g , one can measure t h e e v o l u t i o n o f condensables from t h e s e gauges by t a k i n g i n t e r m i t t e n t i o n i z a t i o n gauge r e a d i n g s w i t h and w i t h o u t a l i q u i d n i t r o g e n c o l d t r a p s e p a r a t i n g t h e McLeod .1nd i o n i z a t i o n gauges

22

NGUR

6 -

MEASURSEMENT O F RISING PRSSUff /N A CLOSED SYSTM WITH AN /ON/ZAT/ON GAUGE USED E I ~ H E Rc o w I N u o u s u OR IN TERM r TENTL Y

AI

BI

INTERMITTENT READINGS CON r/wous READINGS

TIME (minutes)
0
'

20

40

60

80

/oo

120

/40

/60

/BO

as shown in Figure 7. Without the cold trap, the ionization gauge measures the partial pressures of the mercury vapor, water vapor, and other condensables as well as the nitrogen pressure, as shown in curve C. The rate

of rise of this total pressure, however, can be compared with that of the pure nitrogen rate of pressure rise. Using the pressure rise technique, the readings of an ionization gauge can be compared with those of a McLeod gauge. Such a Comparison is shown in Figure 8 . No cold traps were present in the system. This par-

ticular experiment showed that the total rate of pressure rise of both condensable and noncondensable gases was measured to be the same with a McLeod gauge and an intermittently operated ionization gauge.

In this case both

the ionization and McLeod gauges measure the pressure of the condensables as well as the pure nitrogen. The ionization gauge also measures the mercury vapor pressure, and this must be subtracted out in order to compare the readings. When the evolution of condensable gases is small enough, a cold trap would be used to keep mercury vapor out of the ionization gauge during this comparison of gauge readings. ACKNOWLEDG?lENTS

I would like to express my thanks to Dr. R.F.K. Herzog for his

many contributions to this project and to A. Suprenard and F. Robert for technical assistance in the construction and maintenance of the system. This work was performed under the sponsorship of the National Aeronautics and Space Administration.

24

28 26

24
22 20 l8

/6
/4

/2
/O
8

.6
4

2
0
0

30

60

90

/20

/ 50

/BO

50
48
46

44 42
40 38

36

34
32
30

28 26 24 22

20
/8
I6

/4 /2

/O
8 6
4

2
0
0

30

60
26

90

/2 0

I50

180

REFERENCES

1.
2.

Dushmn, S., Scientific Foundations of Vacuum Technique (.Tohn Wiley & Sons, Inc., New York, 1949). Leck, J.H., Pressure Measurements In Vacuum Systems (The Institute of Physics, London, 19571, pp. 132-7. Guthrie, A., and Wakerling, R . K . , Vacuum Equipment and Techniques (M:,GrawHill Book C o . , Inc., New York, 1949), pp. 141-3, LeBlanc, .I .A., "Vacuum Gauge Calibration System" in National Symposium on Vacuum Technology Transactions, (Pergamon Press, New York, 1956), pp. 78-81. Alpert, D., "New DeVelOFlnentS in The Production and Measurement of Ultra High Vacuum", J. App1. Phys. 2 4 ( 7 ) : 869-870, July 1953.

3.

4.

5.

27