EP0220283A1 - Procede de preparation de nitrure d'aluminium de grande purete - Google Patents

Procede de preparation de nitrure d'aluminium de grande purete

Info

Publication number
EP0220283A1
EP0220283A1 EP19860903060 EP86903060A EP0220283A1 EP 0220283 A1 EP0220283 A1 EP 0220283A1 EP 19860903060 EP19860903060 EP 19860903060 EP 86903060 A EP86903060 A EP 86903060A EP 0220283 A1 EP0220283 A1 EP 0220283A1
Authority
EP
European Patent Office
Prior art keywords
aluminum
reaction
aluminum nitride
high purity
ammonia
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Withdrawn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
EP19860903060
Other languages
German (de)
English (en)
Inventor
Ibrahim Sekercioglu
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Battelle Development Corp
Original Assignee
Battelle Development Corp
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 Battelle Development Corp filed Critical Battelle Development Corp
Publication of EP0220283A1 publication Critical patent/EP0220283A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/06—Binary 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
    • C01B21/072—Binary 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity

Definitions

  • This invention relates to the preparation of high purity aluminum nitride from ammonia, nitrogen, hydrogen or oxygen.
  • a high quality, vacuum-tight glove box was used to store and manipulate the aluminum sulfide powder.
  • Thermocouples were connected through a gland of one end plate 102, one of which was used to monitor the temperature and the other to monitor a reference sample of aluminum nitride. Gas from a gas supply (not shown) enters at 114,115. Because aluminum sulfide is sensitive to atmospheric water vapor the powder used in this work was received from the supplier in sealed glass ampoules. The sealed ampoules were placed in an argon glove box before being opened. Once the ampoules were opened, the aluminum sulfide was stored in the glove box and the material for each experiment was weighed into a molybdenum boat in the glove box. To limit contact with the ambient atmosphere, the aluminum sulfide samples were placed in a plastic box before being removed through the airlock of the glove box.
  • Oxygen, nitrogen, and sulfur analyses were performed using an inert gas fusion technique. Surface analysis of some powders was performed using Electron Spectroscopy for Chemical Analysis (ESCA). X-ray diffraction spectra were collected on a standard Norelco diffractometer with a vertical axis goniometer, spinning sample holder, and theta compensation slits. Several tests were made using ammonia that are summarized in Table 1. X-ray diffraction (XRD) spectra were measured on all samples and those above 1000°C gave good agreement with the JCPDS reference pattern (25-1133) for aluminum nitride. The pattern from the 1250°C run is compared to the reference pattern in Table 2. All of those lines not accounted for by aluminum nitride are due to a minor alpha alumina impurity ( JCPDS 10-123). The only significant differences between the XRD patterns of the samples treated at
  • Aluminum nitride can be prepared by the reaction of aluminum sulfide with ammonia at temperatures above 1100°C. Below 1100°C, reactions occur but the product is not pure aluminum nitride, although the x-ray diffrac- tion pattern is very similar. Even reaction times of up to 46 hours at 900°C were not sufficient to Complete the reaction.
  • aluminum nitride is the product of the reaction between aluminum sulfide and ammonia and the product has a crystallite size in the range which causes x-ray line broadening. These grains are formed into dense agglomerates with a wide range of particle size which should give a high packing density in green bodies.
  • the pressure is preferably at about atmospheric pressure although a higher pressure may increase the reaction rate.
  • reaction time is preferably at about atmospheric pressure although a higher pressure may increase the reaction rate.
  • reaction time will vary depending on operating conditions above or below 1250°C, the pressure used and the degree to which the reaction is required to go to completion. To achieve reasonable rates of reaction, reaction times of 2-30 hours are preferred.
  • reaction (6) also requires temperatures above 1100°C with a temperature range of about 1200°C to 1750°C being preferred.
  • the pressure may be at atmospher ⁇ ic pressure although higher pressures are preferred. The reaction rate is thereby increased and the reaction products are favored since four moles of reacting gases produce three moles of H2S.
  • reaction time 19.5 hours
  • reaction time will vary depending on operating conditions above or below 1350°C, the pressure used and the degree to which the reaction is required to go to completion.
  • reaction times of 2-30 hours are preferred.
  • a powder, of a fine texture, that is adapted to give adequate reaction rates and adapted to produce suitable sintering charac- teristics as a final product should be chosen for the supply of aluminum sulfide.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Ceramic Products (AREA)

Abstract

Procédé de production de nitrure d'aluminium de grande pureté en faisant réagir le sulfure d'aluminium avec de l'ammoniac ou de l'azote gazeux et de l'hydrogène à une température dépassant 1100oC. Lorsqu'on utilise de l'ammoniac les conditions de réaction préférées se situent entre environ 1200oC et 1500oC et à la pression atmosphérique pendant environ 2 à 30 heures. Lorsqu'on utilise de l'azote gazeux et de l'hydrogène, les conditions de réaction préférées se situent entre environ 1200oC et 1750oC et à des pressions supérieures à la pression atmosphérique pendant environ 2 à 30 heures. Est ainsi produite une poudre de grande pureté, de faible teneur en oxygène et s'écoulant librement.
EP19860903060 1985-04-29 1986-04-23 Procede de preparation de nitrure d'aluminium de grande purete Withdrawn EP0220283A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US72799385A 1985-04-29 1985-04-29
US727993 1985-04-29

Publications (1)

Publication Number Publication Date
EP0220283A1 true EP0220283A1 (fr) 1987-05-06

Family

ID=24924987

Family Applications (1)

Application Number Title Priority Date Filing Date
EP19860903060 Withdrawn EP0220283A1 (fr) 1985-04-29 1986-04-23 Procede de preparation de nitrure d'aluminium de grande purete

Country Status (3)

Country Link
EP (1) EP0220283A1 (fr)
JP (1) JPS63500167A (fr)
WO (1) WO1986006360A1 (fr)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2643069B1 (fr) * 1989-02-10 1993-04-23 Univ Rennes Procede d'obtention de poudres oxynitrurees et leur application a la preparation de ceramiques

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE346122C (fr) *

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO8606360A1 *

Also Published As

Publication number Publication date
JPS63500167A (ja) 1988-01-21
WO1986006360A1 (fr) 1986-11-06

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Inventor name: SEKERCIOGLU, IBRAHIM