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Microwave Energy Applied to Processing of High-Temperature Materials

Microwave energy is an emerging, innovative, property-improving, energyconserving, ecology-friendly, time-saving technology that can be used to process a variety of ceramic, composite and metallic materials at lower costs.
Dinesh Agrawal, Jiping Cheng, Hu Peng, Larry Hurt and Kuruvilla Cherian

Top photo: Ceramic products fabricated using high-temperature microwave method: (A) dinner plate and tea bag holder (left) before and (right) after processing; (B) ceramic decorative Chinese egg; and (C) Al2O3 components.

Application of microwave energy is emerging as an innovative technology for the processing of a variety of products and materials at faster rates, cheaper processing cost and, in most cases, with better properties. Moreover, the process is ecology friendly. The first application of microwave energy was during World War II for radar. It since has found utility in numerous diverse fields, making it the most versatile form of energy for materials processing. Microwave energy has been successfully applied in many low-temperature (<500C) applications, such as rubber pretreatment and vulcanization, food processing, wood curing, textiles, poly-

mers and biochemistry. In most of these areas the technology has been successfully commercialized, and low-temperature industrial microwave furnaces are available worldwide. During the past two decades, many new developments have occurred worldwide in microwave research that have made it attractive for high-temperature applications (>500C) that involve ceramics, composites and metals. New companies in China, the United States and Japan have been set up that provide microwave systems for high-temperature applications. Microwave processing has many advantages over conventional methods:

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Microwave Energy Applied to Processing of High-Temperature Materials

V (volts)

Current (amps) Large-sized Al2O3 ring sintered in high-tempertaure microwave batch system at 1600C with 60% decrease in dimensional deformation compared with conventional sintering. Comparison of voltagecurrent response between microwave-sintered and conventionally sintered ZnO varistor.

substantial enhancement in reaction and diffusion kinetics; much shorter process time; finer microstructures; higher-quality products; and ecology friendliness. Use of the microwave process for sintering and synthesis offers the following unique features. Rapid material/volumetric heating and one-tenth the processing time make energy consumption lower than conventional methods. Up to 90% energy savings are possible. Enhancements in sintering and reaction kinetics provide much finer and uniform microstructures in the sintered product, which yields much better mechanical properties. Microwavematter interaction and anisothermal situations often produce better quality and new materials that are normally not possible with conventional methods. All the ceramics, composites and metallic materials described here have been processed using 2.45 GHz microwave multimode systems.

cessing is used. Small-disk alumina samples microwave sintered at 1400C, with no hold time, were 98% of theoretical density (TD)1,2 with relatively low grain size. Conventional heating requires at least 1600C and 2 h of holding time to achieve the same degree of densification but with substantial grain growth. This work has been extended to fabricate some commercial alumina products with substantial improvement in the quality of the sintered product. For example, solgel-prepared alumina grit has been sintered to full density using a continuous microwave-sintering process.3 The microwave sintering of this material at 1500C for 15 min provides near TD and exhibits much higher abrasion index and hardness values than the standard material. In Japan, Sato et al.4 have reported successful sintering of large commercial alumina products for substrate, high-temperature optics and structural applications. An alumina ring, 15 in. in diameter, was sintered to full density using a microwave process in only 20% of total cycle time and only one-tenth of the energy consumed using a conventional process. Furthermore, the bending strength was improved by almost 30% and the shrinkage distortion was ~60% less than the conventionally produced product. Zirconia (ZrO2) is a refractory oxide ceramic that often requires high sintering temperatures and soaking time to obtain a high degree of densification. Fine-grained zirconia ceramics have been sintered using microwaves at

1360C for 2 min that yield 98% of TD and average grain size of 0.25 m. Binner et al.5 have reported from the United Kingdom the fabrication of transparent zirconia ceramics using nanopowders and microwave hybrid heating at 1600C. Lead zirconate titanate (PbZr0.52Ti0.48O3; PZT) is a common ferroelectric material that belongs to the perovskite family. It is generally fabricated conventionally at temperatures >1200C for several hours of soaking time. One serious problem associated with PZT fabrication is the high loss of lead oxide (PbO) because of lengthy sintering/calcination soaking time. This is a serious environmental issue. Single-phase PZT has been obtained using a microwave-assisted process6 at 600C with nonstoichiometric titanium oxide (TiO2x). The use of TiO2x enhances microwave absorption and increases reaction kinetics substantially. The use of nonstoichiometric precursors also leads to different reaction pathways for the formation of PZT. In another study, PZT samples have been microwave sintered at temperatures 150C lower than the conventional process,7 which has resulted in finer grain size and minimal PbO loss. Barium titanate (BaTiO3; BT) can be synthesized using barium carbonate (BaCO3) (a poor microwave absorber) and TiO2x (an excellent microwave absorber) as precursors. Because microwave absorption is material dependent, it is possible to exploit this

Ceramics
Alumina (Al2O3) is the most common ceramic and has been widely used in microwave-sintering research by many scientists. Because of its highly refractory nature, it is difficult to sinter to full densification unless suitable sintering aids or some special processing techniques are adopted. Almost full sintering of alumina has been achieved much faster and at lower temperature when microwave pro40

American Ceramic Society Bulletin, Vol. 87, No. 3

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Transparent materials fabricated using microwave sintering: (A) pure Al2O3; (B) Cr-doped Al2O3 ruby; (C) spinel; (D) AlON; and (E) AlN.

situation to enhance reaction kinetics. The reaction of the mixture of these two phases in a microwave field occurs radically different from the conventional isothermal heating situation. In the microwave case, hexagonal-BT appears at 250C and no soak time and almost phase-pure tetragonal-BT is formed at 900C in 5 min. The conventional process, even at 1300C for 1 h soak time, does not produce XRDdetectable tetragonal-BT phase.8 In another study, nanosized BT powders were synthesized using microwave processing with barium titanyl oxalate as a precursor at 680C in phase-pure cubic form. The average grain size of microwave-synthesized BT powder is ~70 nm. Vanadium nitride (VN) is used extensively in the steel industry for surface hardening through a nitridation process. The rapid heating rate and the microwave effect on the materials being synthesized drive the reactions much faster and consume significantly less energy than other processes. This leads to a lower cost of production. VN synthesis using microwaves requires 5 h, whereas the conven(A)

tional process requires 30 ha substantial savings in energy consumption.9 Positive-temperature-coefficient (PTC) ceramics (titanates) are useful materials in household- and industrial-heating devices. A continuous microwave process for sintering PTC ceramic parts has gone into production recently at SynoTherm Co., China. The ceramics are sintered at the relatively low temperature of 1225C in 15 min in a microwave pusher furnace capable of sintering kilograms of product per hour. The process produces >7000 household PTC ceramic heating elements in 24 h and consumes only threefifths of the energy needed using a conventional method. Zinc oxide (ZnO) varistors are electronic ceramic devices that possess highly nonlinear currentvoltage characteristics, which enable them to be used as voltage surge suppressors. Various types of ZnO varistors produced under various processing conditions have been sintered using microwave heating10 in significantly shorter cycle time and with substantial improvements in electrical properties. Microwave-processed ZnO varistors exhibit better densities, finer grain size

and more uniform microstructure relative to those conventionally processed. Electrical characterization of the microwave-sintered samples shows higher voltage and better clamping properties as compared with conventionally sintered samples. Higher volt/mm response in the microwave samples signifies that smaller devices with similar electrical properties can be used, which enables less material consumption to develop similar devices obtained through conventional processes. Transparent ceramics are specialty ceramics that are fabricated conventionally using multistep processes that involve long sintering cycles and, often, high-pressure methods. The microwave method has been successfully used to fabricate transparent ceramics because of its ability to produce a fully dense ceramic in a short time without using high-pressure conditions.11 Hydroxyapatite has been fully sintered as a transparent ceramic at 1100C in 10 min using microwave processing.12 Reasonably transparent spinel and alumina ceramics have been fabricated1315 using highly pure and submicron-sized powders sintered at 1700C for 15 min. Fully transparent aluminum oxynitride (AlON) ceramics have been made using a multimode microwave system at 1800C.16 Translucent aluminum nitride (AlN) ceramic, which is a well-known high-thermal-conductivity material, has been developed using microwaves at 1900C for 60 min.17 Zinc oxide (ZnO) is a promising material for ultraviolet- and blue-light-emitting devices, because it has several advantages over its chief competitor gallium nitride (GaN). ZnO has a bandgap of 3.37 eV, with a 60 meV binding energy of the free exciton, and it permits
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WCCo-based cemented carbide commercial products fabricated using microwave firing: (A) cutting, polishing and drilling components; and (B) WCCo matrix imbedded with thermally stabilized diamond (TSD).
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Microwave Energy Applied to Processing of High-Temperature Materials

tions favor undesirable grain growth. Full sintering of WCCo green bodies has been achieved using microwave processing21 in only 2 h. The sintered products exhibit better mechanical properties than conventional parts. The microwave-sintering process exhibits an unprecedented improvement in abrasion resistance (1530%), erosion resistance (22%) and corrosion resistance in 15% nitric acid (20 times) without noticeable loss in hardness or fracture toughness. These improvements in the properties are believed to be caused by the fine microstructure, uniform cobalt-phase distribution and pure cobalt-phase at the grain boundaries in the microwave-sintered samples.22 Commercial WCCo parts have been fabricated successfully using microwave technology. Collaboration between Dennis Tool Co., Houston, Texas, and The Pennsylvania State University, University Park, Pa., has resulted in an industrial fullscale technology to produce high-quality WCCo and diamond composite products. Multilayer ceramic capacitors (MLCCs) are used in almost all electronic devices. Microwave sintering of nickel-electrode MLCCs has been conducted in an intermediate reducing atmosphere (oxygen partial pressure of ~106 atm). At a temperature of ~1250C, X7R MLCC chips are well sintered, which results in dense and uniform parts without delaminations or cracks.23 Directionally solidified eutectics of oxide and non-oxide ceramic compositions are attractive composite materials because of their unique thermodynamics, mechanical properties and electrical properties. In general, these materials have excellent thermal stability, hightemperature strength and high fracture toughness, which make them attractive candidates for ultra-high-temperature structural materials. Microwave energy has been used to melt and resolidify oxide and non-oxide refractory ceramic eutectic compositions in yttrium aluminum garnet (Al2O3 Y3Al5O12; YAG) (Tm = 1827C) and boron carbidetitanium boride (B4CTiB2) (Tm = 2310C) systems in a multimode 2.45 GHz microwave furnace.24 Microwave experiments show a stability of eutectic melt temperature and the uniformity of subsequent eutectic microstructure across the sample diameter during the resolidification. The ability to reach ultrahigh temperatures (~2400C) and prevent the formation of significant thermal gradient across the sample confirms the potential of using microwave energy for processing of directionally solidified refractory ceramic eutectics.

Typical microstructure of microwave-produced solidified eutectic of TiB2B4C composition, where B4C is matrix and TiB2 is acicular-shaped grains.24

Metallic Materials
Until 2000, microwave processing of materials mostly had been confined to ceramic, semimetallic, inorganic and polymeric materials. The main reason for this had been a misconception that all metals reflect microwaves and/or cause plasma formation. Hence, they could not be heated in a microwave field. It since has been proved that all metallic materials in powder form (or compacted into green porous bodies) do absorb microwave radiation at room temperature and can be sintered effectively. Even bulk metals, if preheated to ~400C, also begin coupling in a microwave field and are heated rapidly, so much so that they can be melted. Many recent reports have successfully demonstrated that a wide variety of metals and alloysincluding refractory metals, ferrous alloys and tungsten heavy alloyscan be sintered to high densification with better properties using microwave energy. Some metal powders also have been synthesized using microwaves. Molybdenum synthesis and sintering Recently, attempts to extract molybdenum from molybdenum sulfide (MoS2) ore have been successful by direct use of microwave energy in an argon atmosphere in a single-step process. The current multistep state-of-the-art process involves roasting, chemical treatment and reduction under hydrogen. The microwave process transforms the ore directly to pure metal in one-tenth of the process time. Molybdenum nanopowders also have been sintered to 99% of TD at 1400C in 30 min, whereas conventional processing requires
American Ceramic Society Bulletin, Vol. 87, No. 3

Microwave-sintered coppersteel automotive gear.

excitonic emission at room temperature. To date, most ZnO single crystals have been fabricated in the form of bulk crystals, thin films or nanowires/nanorods. ZnO single-crystal microtubes have been grown recently using microwave heating. They are colorless, fully transparent, contamination-free and nearperfect crystallinity.18 ZnO single-crystal microtubes exhibit strong near-bandedge emission, highly selective ultraviolet light response, excellent electron field emission and interesting piezoelectric properties.19,20

Composites
Tungsten carbidecobalt- (WCCo-) based cemented carbides exhibit a unique combination of properties, including high strength, hardness and Youngs modulus. This makes them universally applicable for metal cutting, rock cutting and underground drilling operations in the oil industry. Conventional methods for sintering WCCo involve high temperature and lengthy sintering cycles (~24 h) to achieve high densification. Such condi42

PbO Loss during Firing of PZT Powders

Open crucible method Fast conventional firing (25C/min) Microwave at 2.45 GHz (25C/min) Microwave at 30 GHz (3050C/min) Conventional firing (10C/min) MEGAC (%) 3 1.35 0 0 TRS 200 TRS 200B (%) (%) 5.7 <0.5 2.3 13.3 0.2 0.10.5

Properties of Al2O3 Abrasive Grit

Heating process Specific gravity 3.96 3.94 Abrasion index 100 65

Microwave

Vickers hardness (kg/mm2) 2388 1026

Conventional
Processing

conditions: 1400C for 45 min.

1400C for 10 h to obtain 98% of TD.25 Powdered-metal sinteringThe first attempt of microwave sintering of powdered metals26 was reported in 1999. Since then many researchers have reported successful sintering of many metallic materials. Microwave sintering of powdered metals produces a superior product. Commercial parts of FC208 and FN208 steel have been sintered to near net shape. A commercial gear of FN208 steel has been sintered in a microwave field. Many commercial powdered-metal components of various compositions including iron and steel, copper, aluminum, nickel, molybdenum, cobalt, titanium, tungsten, tungsten carbide, tin and their alloysalso have been sintered using microwaves. They have produced almost fully dense bodies.2730 SteelmakingKyoto Protocol mandates all the signatory member nations to decrease carbon emission for all future technologies. Steel is a basic and highly important material needed for all infrastructure-related components and is a critical material for the economic growth of any country. However, it also contributes to the carbon dioxide (CO2) buildup in the greenhouse effect in a substantial manner. Therefore, a new process to make steel with less CO2 emission is desired. Recently, Hwang et al.31 have succeeded in combining microwaves with the electric-arc furnace to develop a new clean and green steelmaking technology in which CO2 emission and energy conAmerican Ceramic Society Bulletin, Vol. 87, No. 3

sumption (by 25%) decreased compared with conventional basic oxygen furnace (BOF) technology. The unique aspect of this technology uses the advantages of rapid volumetric heating, high energy efficiency and enhanced reaction kinetics that microwaves offer. In another study, Nagata et al.32,33 have succeeded in developing pure microwave-based technology to direct steelmaking with 50% decrease in CO2 emission. They have succeeded in producing highly pure pig irons in a multimode microwave reactor from powdered iron ores with carbon as a reducing agent under a nitrogen atmosphere.

(www.mino-ceramic.co.jp/eng/products /plant/micro/01.html)

Future Prospects
It is believed that the future of microwave technology is promising. This belief considers all aspects of microwave technology for high-temperature materials processinginherent limitations and reluctance of industry to adopt new technology for fear of losing capital investment in existing conventional technology. New microwave high-temperature system manufacturers in China, Japan and the United States are expected to dominate and change the scene during the next five years. In fact, all the successes so far achieved have been with continuous microwaveprocessing systems for specialty materials, such as cemented carbides, ferrites, varistors and metal products. The coming decade will witness more such systems to be built for many other materials and products. There are many other areas where microwave technology will be applied in the future because of its selective heating of powdered metal and highly absorbing ceramics. These applications may include brazing/joining of metals, sintering of metal coating onto steel substrates, and recovery of oil and gas from oil shale and from used tires. I

Microwave Equipment
The successful design and building of microwave systems applicable for hightemperature microwave applications is challenging and demanding. It involves a multidisciplinary approach in which electrical engineers, mechanical engineers, materials scientists and software engineers are important. There are many issues that need to be addressed and resolved: temperature measurement; insulation/susceptor around the workpiece; continuous/batch processes; and frequency. These issues are not serious for low-temperature application. However, at higher temperatures and as larger-sized workpieces are processed, temperature accuracy and uniformity become important for producing a quality product. Continuous microwave processing as an industrial operation is the only feasible, viable and economic approach for almost all the ceramic, metal and composite products mentioned herein. Several companies now have begun to manufacture such systems and have found niche markets for specialty product:. Syno-Therm Co. Ltd., Changsha, China (www.syno-therm.cn); Dennis Tool Co., Houston, Texas (www.dennistoolcompany.com/Microwave .htm); Spheric Technologies Inc., Phoenix, Ariz. (www.spherictechnologies.com); and Mino Ceramic, Mizunami, Japan

About the Authors

Dinesh Agrawal is a professor at The Pennsylvania State University, University Park, Pa., and director of the Microwave Processing and Engineering Center(www.mri.psu.edu/centers/mpec). J. Cheng is senior research associate at The Pennsylvania State University. Hu Peng is vice president and CTO of SynoTherm Co. Ltd., Changsha, China. Larry Hurtt is international marketing manager of Syno-Therm. K. Cherian is director of applied research of Spheric Technologies Inc., Phoenix, Ariz.
This article appears on The American Ceramic Society Bulletin web site (www .ceramicbulletin.org) in pdf format and includes links to additional online resources. 43

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