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GB2127709A - Manufacture of aluminium nitride - Google Patents
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GB2127709A - Manufacture of aluminium nitride - Google Patents

Manufacture of aluminium nitride Download PDF

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Publication number
GB2127709A
GB2127709A GB08228522A GB8228522A GB2127709A GB 2127709 A GB2127709 A GB 2127709A GB 08228522 A GB08228522 A GB 08228522A GB 8228522 A GB8228522 A GB 8228522A GB 2127709 A GB2127709 A GB 2127709A
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United Kingdom
Prior art keywords
aluminium
reaction
rod
levitated
charge
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
GB08228522A
Inventor
Peter Mcallister Dryburgh
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University of Edinburgh
Original Assignee
University of Edinburgh
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by University of Edinburgh filed Critical University of Edinburgh
Priority to GB08228522A priority Critical patent/GB2127709A/en
Publication of GB2127709A publication Critical patent/GB2127709A/en
Withdrawn legal-status Critical Current

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Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00Feed or outlet devices; Feed or outlet control devices
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J10/00Chemical processes in general for reacting liquid with gaseous media other than in the presence of solid particles, or apparatus specially adapted therefor
    • B01J10/005Chemical processes in general for reacting liquid with gaseous media other than in the presence of solid particles, or apparatus specially adapted therefor carried out at high temperatures in the presence of a molten material
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00Nitrogen; Compounds thereof
    • C01B21/06Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
    • C01B21/072Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with aluminium
    • C01B21/0722Preparation by direct nitridation of aluminium

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

High purity aluminium nitride is manufactured by levitating a charge of molten aluminium (112) in a reaction zone (100) by means of electromagnetic induction in a levitation coil (111) in an oxygen-free atmosphere, reacting the levitated molten aluminium with nitrogen gas at a temperature effective to form aluminium nitride, e.g. 1800 to 2300 DEG C, and recovering the resulting aluminium nitride in an oxygen-free atmosphere. The size of the levitated charge can be monitored and the charge replenished under the control of the monitor. The aluminium to be melted can be stripped of its Al2O3 film by heating to cause Al2O3 to react with Al to form Al2O which is volatile and removed by evacuation. <IMAGE>

Description

SPECIFICATION Manufacture of aluminium nitride The present invention is concerned primarily with the manufacture of aluminium nitride, although in some of its aspects it has applications extending beyond aluminium nitride manufacture.
Aluminium nitride potentially has particular value in electronic devices depending on the manipulation of surface acoustic waves, because it has a large electro-mechanical coupling and high resistivity as well as a high propagation velocity for surface acoustic waves. It is also valuable as a substitute gem material and is known to have potential as a light-emitting diode material in the near ultra-violet and as a phosphor at the blue end of the visible spectrum. It has exceedingly high thermal conductivity and high strength and would be useful as an industrial refractory in the form of powder or polycrystalline blocks because it is not attacked by molten aluminium. It is a piezoelectric material of high transparency which could be of use in transducers and in the electro-optical field.
It has been proposed to grow aluminium nitride in the form of an epitaxial film on a corundum support by reaction of an aluminium halide with ammonia at about 1 2000C or by reaction of an organo-aluminium compound such as trimethylaluminium with ammonia. However, both processes have disadvantages and the products obtained tend to contain impurities. Neither process has yet been commercialised despite intense interest in the compounds. The production of aluminium nitride by reaction of nitrogen gas with aluminium selenide has also been proposed but requires more detailed study before it can yield a commercially viable process.
It is not possible to grow aluminium nitride crystals from a melt because the compound decomposes at about 25000C before melting, so that crystals can be grown only by direct sublimation, and for this operation it is of crucial importance to use a starting material of high purity.
The present invention seeks, in one of its aspects, to provide a method for the production of aluminium nitride which can form a basis of a commercial process. In particular it seeks to provide a method of producing high-purity aluminium nitride from which crystals can be obtained by direct sublimation.
According to this first aspect of the invention there is provided a process for the manufacture of high-purity aluminium nitride comprising levitating a charge of molten aluminium in a reaction zone by means of electromagnetic induction in a levitation coil in an oxygen-free atmosphere, reacting the levitated molten aluminium at a functionaliy effective temperature with nitrogen gas and recovering the resulting aluminium nitride in an oxygen-free atmosphere.
The reaction temperature employed must be sufficiently high that the protective surface layer of aluminium nitride which is formed initially is disrupted and does not inhibit further reaction.
Generally speaking, temperatures in excess of 1 5000C will therefore be required. On the other hand the temperature should be below the aluminium nitride decomposition temperature, i.e.
generally speaking below about 25000C.
Preferably, temperatures of about 1 800 to 23000 C, e.g. about 20000 C, are used. At temperatures above 20000C the vapour pressure of aluminium nitride is about 0.1 bar and evaporation takes place freely.
The levitation of the molten aluminium is achieved by means of electromagnetic induction in a levitation coil, which is designed to provide a field pattern creating both an upward levitating force and a radially inward, stabilising force.
Various designs of levitation coils have been proposed in the literature, for example in "Levitation Melting - a survey of the State of the Art" by W. A. Peifer, Journal of Metals, May 1965, pages 487-493, and "Electromagnetic Levitation and its use in Physico-Chemical Studies at High Temperature" by A. E. Jenkins, B. Harris and L. Baker, Symposium on Metallurgy at High Pressures and High Temperatures, Met. Soc.
Conf., 22, New York (1964), pages 23-43. These designs may be used for the process of the present invention. The use of electromagnetic levitation prevents contact between the molten aluminium, which is extremely reactive, and metals or refractories which it would otherwise attack at about 20000 C.
In order to provide good control of the rate of reaction between nitrogen gas and the molten aluminium and to control the temperature of the latter it is desirable to employ a mixture of nitrogen gas and an inert gas, preferably helium, and to control the proportion of nitrogen depending on changes in the aluminium temperature and reaction rate.
It is also important, in order to avoid contamination of the product, that collection of the product should be carried out in an oxygenfree atmosphere.
In a second aspect, the present invention seeks to improve the supply of molten material to a levitation coil. Conventional levitation coiis currently in use are limited to a charge of 10 to 20 g, which is insufficient, in the case of molten aluminium, to produce a worthwhile yield of aluminium nitride from a single run without replenishment of the charge. Although it has been proposed to drop pellets onto a levitated charge to replenish the charge, this is not entirely satisfactory.
According to the second aspect of the present invention apparatus for use in carrying out a chemical reaction in which a levitated mass of non-gaseous material is reacted at elevated temperature with a gas to form a gaseous product, comprises a reaction zone having an inlet for the gaseous reactant and an outlet for the gaseous product and is characterised in that means are provided for the constant replenishment of the levitated mass, said replenishment means comprising an automatic sensor for sensing the size of the levitated mass and drive means controlled by the sensor for protruding an additional quantity of the non-gaseous reactant into the levitation field to maintain a constant size of the levitated mass.
Conveniently the sensor is a television camera or other device producing an image of the levitated mass and controlling the drive means by suitable electronic processing. Especially where the levitated mass of non-gaseous reactant is a molten solid, the drive means may be linked to a solid rod of the non-gaseous reactant so as to cause its tip to protrude into the levitation field, where the tip is heated and melts and thus replenishes the levitated mass, in response to the progess of the reaction.
This apparatus is particularly suited to use in the reaction of molten metals such as aluminium and others. However when a metal rod, particularly an aluminium rod, is used, difficulties may arise owing to the existence of a layer of metal oxide on the surface of the rod, which leads to the introduction of impurities into the levitated mass and hence into the final product.
The third aspect of the invention seeks to provide a method of removing aluminium oxide films from aluminium metal which method can be combined conveniently with the apparatus according to the second aspect of the invention.
According to the third aspect of the invention a method of stripping an aluminium oxide (Al203) film from an aluminium metal rod comprises supporting an aluminium metal rod from both ends in an evacuated reaction zone, providing local heating in one region of the reaction zone to melt the surface portion of the aluminium rod in that region and cause the Awl203 film on that portion of the rod to react with aluminium to form volatile aluminium sub-oxide (A120), which is evacuated, effecting relative movement between the local heating region and the aluminium rod to strip the Awl203 film from the rod along at least part of its length in the reaction zone without destroying the rod, and maintaining the stripped rod under oxygen-free conditions.
This method may be combined with the apparatus according to the second aspect and the method according to the first aspect of the invention by using the same reaction zone in each case and maintaining oxygen-free conditions throughout.
The reaction of the Awl203 film with aluminium metal occurs at temperatures above 1 2000C according to the equation Awl203 + 4AI = 3at20 and the local heating must be sufficient for this purpose without destroying the entire structure of the rod. Conveniently the local heating is provided by electro-magnetic induction.
The invention is further illustrated in the accompanying drawings, in which Fig. 1 is a diagrammatic sketch of apparatus suitable for performing the invention in its first aspect, Fig. 2 is a diagrammatic sketch of apparatus according to the invention in its second aspect, and Fig. 3 is a diagrammatic sketch of apparatus suitable for performing the invention in its third aspect.
Referring to Fig. 1 of the drawings, the apparatus comprises a vertical reaction tube 100 of silica fitted with a cooling jacket 101 for the circulation of cooling water between an inlet 102 and an outlet 103 and with a water-cooled end cap 104 of stainless steel. An inlet 105 for a gaseous mixture of nitrogen and helium is provided in the base of the tube and a lateral outlet 106 removes gaseous products and residual gas to a cyclone separator or other dust catcher 108 where waste gas is separated and removed overhead at 109, product falling into an oxygen-free handling enclosure 110 for recovery or use. A radio-frequency levitation coil 111 .surrounds the reaction tube 101 just below the outlet 106 and a charge of molten aluminium 112 is maintained in the levitation field for conversion into aluminium nitride.This charge may be supplied or supplemented via retractable pedestal 113.
Referring to Fig. 2 of the drawings a vertical reaction tube 201 (which may be identical with the reaction tube 101 of Fig. 1) is equipped with a radio-frequency levitation coil 202 (which may be identical with the coil 112 of Fig. 1) able to maintain a molten charge 203, for example of aluminium. A sensor 204 in the form of a television camera is positioned to take pictures of the charge 203 and this controls, via integrator 205, control amplifier 206 and power controller 207, an electrically driven mechanical feed 208.
The feed 208 drives a vertical stainless steel driving rod 209, passing through a sliding seal (not shown) and a stainless steel end cap 210, into a stainless steel tube 211 attached below the reaction tube 201. The driving rod 209 terminates inside the tube 211 in a silica insulator 212 which carries a chuck 213 which in turn carries a metal rod 21 4 to provide replenishment for the charge 203. Movement of the rod 214 into the field generated by the levitation coil 202 is governed by the size of the charge 203 observed by the sensor 204.
Referring now to Fig. 3 of the drawings, a vertical reaction tube 301 (which may be identical with the tubes 101 and 201) is evacuated via outlet 302 and is fitted with an induction heating coil 303 (which may be identical with the levitation coil 112 and 202). An aluminium rod 304 passes vertically through the reaction tube 301 and its end caps 305 and 306, the upper of which is provided with a gate valve 307, and into stainless steel tubes 308 and 309 above and below the reaction tube 301. At each end it is mounted in an insulated chuck 310,311 and the upper chuck supports a refractory dump tube 31 2 running externally of the rod 304 down to the lower chuck.Support rods 31 3 and 314 extend beyond the chucks 310,311 and are driven by means (not shown) enabling the rod 304 to move vertically relative to the coil 303.
To use the apparatus the rod 304 is moved to its uppermost position with the bottom of the rod (adjacent to the chuck 311) in the heating field provided by the coil 303 and the system is evacuated. The coil is then switched on and the surface of the rod 304 in the region of the coil is rendered molten to provide a "floating" molten zone 31 5 and strip off the Awl203 layer as volatile A120 which is removed via the outlet 302. The system of rods 313,304 and 314 is then moved downwards until the top end of the rod 304 is in the region of the coil 303, the "floating" molten zone 31 5 rising up the rod to strip off the Al203 layer along its entire length. The lower support rod 314 is then held stationary whilst the upper support rod 313 is moved upwards, thus causing the rod 304 to break in the region of the "floating" molten zone 31 5. The upper chuck 310 and dump tube 312 are lifted into the upper tube 308 and isolated by closing the gate valve 307. Melting in the region of the coil 303 is completed and the rod is ready for use, for example according to the procedure described above in connection with Figs. 1 and 2.

Claims (14)

1. A process for the manufacture of high-purity aluminium nitride comprising levitating a charge of molten aluminium in a reaction zone by means of electromagnetic induction in a levitation coil in an oxygen-free atmosphere, reacting the levitated molten aluminium at a functionally effective temperature with nitrogen gas and recovering the resulting aluminium nitride in an oxygen-free atmosphere.
2. A process as claimed in claim 1 wherein the reaction is carried out at a temperature of from 1800 to 23000 C.
3. A process as claimed in claim 1 wherein the reaction is carried out at a temperature of about 20000C.
4. A process as claimed in any of claims 1 to 3 wherein the reaction is carried out in the presence of a mixture of nitrogen gas and an inert gas.
5. A process as claimed in claim 4 wherein the proportion of nitrogen gas and inert gas is varied in response to changes in the temperature and rate of reaction in order to maintain substantially constant temperature and reaction rate.
6. A process as claimed in any of claims 1 to 5 wherein the levitated charge of molten aluminium is replenished during the reaction by sensing the size of the remaining charge with a sensor and protruding an additional quantity of aluminium into the levitation field under the control of the sensor in order to maintain a constant size of the levitated charge.
7. A process as claimed in claim 6 wherein the charge is replenished from a solid aluminium rod one end of which is protruded into the levitation field under the control of the sensor whereupon it melts.
8. A process as claimed in any of claims 1 to 7 wherein the aluminium for the reaction is freed from a surface Al203 film by heating solid aluminium in an evacuated reaction zone to cause the surface of the aluminium to melt and the surface Awl203 film thereon to react with aluminium to form Awl20 which is evacuated, and the thus purified aluminium is maintained under oxygenfree conditions until levitated.
9. A process as claimed in claim 8 wherein the heating of the aluminium is carried out by electromagnetic induction to a temperature above 12000C.
1 0. A process for the manufacture of high purity aluminium nitride carried out substantially as hereinbefore described with reference to Figure 1 or Figure 2 of the accompanying drawings.
11. Apparatus for use in carrying out reaction between a levitated mass of molten aluminium and gaseous nitrogen to produce gaseous aluminium nitride, comprising a reaction zone having an inlet for gaseous nitrogen and an outlet for gaseous aluminium nitride, and a levitation coil arranged to levitate the mass of molten aluminium in the reaction zone.
12. Apparatus as claimed in claim 11 including an automatic sensor for sensing the size of the levitated mass and drive means, controlled by the sensor, for protruding an additional quantity of aluminium into the levitation field generated by the levitation coil to replenish the levitated mass.
13. Apparatus as claimed in claim 11 and substantially as hereinbefore described or illustrated in Figure 1 or Figure 2 of the accompanying drawings.
14. A method of stripping an Awl203 film from an aluminium metal rod to be used in a process as claimed in claim 1, comprising supporting the aluminium metal rod from both ends in an evacuated reaction zone, providing local heating in one region of the reaction zone to melt the surface portion of the rod in that region and cause the Al203 film on that portion of the rod to react with aluminium to form volatile Al2O, which is evacuated, effecting relative movement between the local heating region and the aluminium rod to strip the Awl203 film from the rod along at least part of its length in the reaction zone without destroying the rod, and maintaining the stripped rod under oxygen-free conditions until it is used in a process as claimed in claim 1.
1 5. A method as claimed in claim 14 carried out in apparatus substantially as hereinbefore described or illustrated in Figure 3 of the accompanying drawings.
GB08228522A 1982-10-06 1982-10-06 Manufacture of aluminium nitride Withdrawn GB2127709A (en)

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Application Number Priority Date Filing Date Title
GB08228522A GB2127709A (en) 1982-10-06 1982-10-06 Manufacture of aluminium nitride

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Application Number Priority Date Filing Date Title
GB08228522A GB2127709A (en) 1982-10-06 1982-10-06 Manufacture of aluminium nitride

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Cited By (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4713360A (en) * 1984-03-16 1987-12-15 Lanxide Technology Company, Lp Novel ceramic materials and methods for making same
US4853352A (en) * 1984-07-20 1989-08-01 Lanxide Technology Company, Lp Method of making self-supporting ceramic materials and materials made thereby
US4859640A (en) * 1986-08-13 1989-08-22 Lanxide Technology Company, Lp Method of making ceramic composite articles with shape replicated surfaces
GB2215714A (en) * 1988-03-18 1989-09-27 Vaw Ver Aluminium Werke Ag Tubular reactor for the high-temperature decomposition of bauxite
US4923832A (en) * 1986-05-08 1990-05-08 Lanxide Technology Company, Lp Method of making shaped ceramic composites with the use of a barrier
US5017526A (en) * 1986-05-08 1991-05-21 Lanxide Technology Company, Lp Methods of making shaped ceramic composites
US5077245A (en) * 1987-01-30 1991-12-31 Kyocera Corporation Aluminum nitride-based sintered body and process for the production thereof
US5154863A (en) * 1985-10-31 1992-10-13 Kyocera Corporation Aluminum nitride-based sintered body and process for the production thereof
US5212124A (en) * 1986-08-13 1993-05-18 Lanxide Technology Company, Lp Ceramic composite articles with shape replicated surfaces
US5236786A (en) * 1986-05-08 1993-08-17 Lanxide Technology Company, Lp Shaped ceramic composites with a barrier
WO1993014027A3 (en) * 1992-01-10 1993-10-14 Dow Chemical Co Process for preparing ultrafine aluminum nitride powder
US5306677A (en) * 1984-03-16 1994-04-26 Lanxide Technology Company, Lp Ceramic materials
US5306676A (en) * 1993-03-09 1994-04-26 Lanxide Technology Company, Lp Silicon carbide bodies and methods of making the same
US5314850A (en) * 1985-10-31 1994-05-24 Kyocera Corporation Aluminum nitride sintered body and production thereof
US5340655A (en) * 1986-05-08 1994-08-23 Lanxide Technology Company, Lp Method of making shaped ceramic composites with the use of a barrier and articles produced thereby
US5358914A (en) * 1986-05-08 1994-10-25 Lanxide Technology Company, Lp Methods of making shaped ceramic composites
GB2326160A (en) * 1997-06-11 1998-12-16 Hitachi Cable Making group III metal nitride crystals; crystal growth methods
RU2312060C2 (en) * 2005-01-28 2007-12-10 Общество с ограниченной ответственностью "Центр научно-технических разработок" (ООО "Центр научно-технических разработок") Method for preparing aluminum nitride powder

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB711034A (en) * 1950-01-04 1954-06-23 Nat Res Dev Apparatus for the treatment of fluids comprising a bed of particulate material
GB1103633A (en) * 1965-08-13 1968-02-21 Tokyo Shibaura Electric Co Preparation of molded and sintered aluminium nitride
GB2057910A (en) * 1979-09-07 1981-04-08 Exxon Research Engineering Co A process for the separation of contaminants from feed streams using magnetic beds

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB711034A (en) * 1950-01-04 1954-06-23 Nat Res Dev Apparatus for the treatment of fluids comprising a bed of particulate material
GB1103633A (en) * 1965-08-13 1968-02-21 Tokyo Shibaura Electric Co Preparation of molded and sintered aluminium nitride
GB2057910A (en) * 1979-09-07 1981-04-08 Exxon Research Engineering Co A process for the separation of contaminants from feed streams using magnetic beds

Cited By (22)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4713360A (en) * 1984-03-16 1987-12-15 Lanxide Technology Company, Lp Novel ceramic materials and methods for making same
US5306677A (en) * 1984-03-16 1994-04-26 Lanxide Technology Company, Lp Ceramic materials
US4853352A (en) * 1984-07-20 1989-08-01 Lanxide Technology Company, Lp Method of making self-supporting ceramic materials and materials made thereby
US5154863A (en) * 1985-10-31 1992-10-13 Kyocera Corporation Aluminum nitride-based sintered body and process for the production thereof
US5314850A (en) * 1985-10-31 1994-05-24 Kyocera Corporation Aluminum nitride sintered body and production thereof
US5356720A (en) * 1986-05-08 1994-10-18 Lanxide Technology Company, Lp Shaped self-supporting ceramic composite bodies comprising silicon nitrides
US5358914A (en) * 1986-05-08 1994-10-25 Lanxide Technology Company, Lp Methods of making shaped ceramic composites
US5017526A (en) * 1986-05-08 1991-05-21 Lanxide Technology Company, Lp Methods of making shaped ceramic composites
US5236786A (en) * 1986-05-08 1993-08-17 Lanxide Technology Company, Lp Shaped ceramic composites with a barrier
US4923832A (en) * 1986-05-08 1990-05-08 Lanxide Technology Company, Lp Method of making shaped ceramic composites with the use of a barrier
US5436209A (en) * 1986-05-08 1995-07-25 Lanxide Technology Company, Lp Set up for making shaped ceramic composites with the use of a barrier means and articles produced thereby
US5340655A (en) * 1986-05-08 1994-08-23 Lanxide Technology Company, Lp Method of making shaped ceramic composites with the use of a barrier and articles produced thereby
US5212124A (en) * 1986-08-13 1993-05-18 Lanxide Technology Company, Lp Ceramic composite articles with shape replicated surfaces
US4859640A (en) * 1986-08-13 1989-08-22 Lanxide Technology Company, Lp Method of making ceramic composite articles with shape replicated surfaces
US5077245A (en) * 1987-01-30 1991-12-31 Kyocera Corporation Aluminum nitride-based sintered body and process for the production thereof
GB2215714A (en) * 1988-03-18 1989-09-27 Vaw Ver Aluminium Werke Ag Tubular reactor for the high-temperature decomposition of bauxite
WO1993014027A3 (en) * 1992-01-10 1993-10-14 Dow Chemical Co Process for preparing ultrafine aluminum nitride powder
US5306676A (en) * 1993-03-09 1994-04-26 Lanxide Technology Company, Lp Silicon carbide bodies and methods of making the same
US5436208A (en) * 1993-03-09 1995-07-25 Lanxide Technology Company, Lp Silicon carbide bodies and methods of making the same
GB2326160A (en) * 1997-06-11 1998-12-16 Hitachi Cable Making group III metal nitride crystals; crystal growth methods
GB2326160B (en) * 1997-06-11 1999-11-03 Hitachi Cable Nitride crystal fabricating method
RU2312060C2 (en) * 2005-01-28 2007-12-10 Общество с ограниченной ответственностью "Центр научно-технических разработок" (ООО "Центр научно-технических разработок") Method for preparing aluminum nitride powder

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