JPS5951483B2 - Aluminum nitride manufacturing method - Google Patents
Aluminum nitride manufacturing methodInfo
- Publication number
- JPS5951483B2 JPS5951483B2 JP2408376A JP2408376A JPS5951483B2 JP S5951483 B2 JPS5951483 B2 JP S5951483B2 JP 2408376 A JP2408376 A JP 2408376A JP 2408376 A JP2408376 A JP 2408376A JP S5951483 B2 JPS5951483 B2 JP S5951483B2
- Authority
- JP
- Japan
- Prior art keywords
- oxide
- aluminum nitride
- weight
- heating
- nitrogen atmosphere
- 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.)
- Expired
Links
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims description 20
- 238000004519 manufacturing process Methods 0.000 title claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 15
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 12
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims description 10
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 10
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 239000003575 carbonaceous material Substances 0.000 claims description 8
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 6
- 239000006229 carbon black Substances 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 6
- 239000000395 magnesium oxide Substances 0.000 claims description 6
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 6
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 6
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 5
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 claims description 5
- 229910000423 chromium oxide Inorganic materials 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 229910000480 nickel oxide Inorganic materials 0.000 claims description 5
- 229910000484 niobium oxide Inorganic materials 0.000 claims description 5
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims description 5
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims description 5
- 229910001935 vanadium oxide Inorganic materials 0.000 claims description 5
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 4
- 239000000292 calcium oxide Substances 0.000 claims description 4
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 4
- 229910000428 cobalt oxide Inorganic materials 0.000 claims description 4
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims description 3
- 239000000571 coke Substances 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 description 12
- 238000000034 method Methods 0.000 description 11
- 238000005121 nitriding Methods 0.000 description 11
- 239000002245 particle Substances 0.000 description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 239000008187 granular material Substances 0.000 description 4
- MXRIRQGCELJRSN-UHFFFAOYSA-N O.O.O.[Al] Chemical compound O.O.O.[Al] MXRIRQGCELJRSN-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000013067 intermediate product Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 150000001247 metal acetylides Chemical class 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 2
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 description 1
- 229910001515 alkali metal fluoride Inorganic materials 0.000 description 1
- 229910001618 alkaline earth metal fluoride Inorganic materials 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
- 229910001634 calcium fluoride Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 150000004673 fluoride salts Chemical class 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 description 1
- 229910001635 magnesium fluoride Inorganic materials 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000011698 potassium fluoride Substances 0.000 description 1
- 235000003270 potassium fluoride Nutrition 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000011775 sodium fluoride Substances 0.000 description 1
- 235000013024 sodium fluoride Nutrition 0.000 description 1
- 239000004449 solid propellant Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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
- C01B21/0726—Preparation by carboreductive nitridation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Ceramic Products (AREA)
Description
【発明の詳細な説明】
本発明は窒化アルミニウムの製造方法に関するものであ
る。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing aluminum nitride.
窒化アルミニウムは溶融金属にぬれにくく、しかも２０
００℃までの高温でも機械的強度に優れ、熱衝撃抵抗も
高いことから工業的にその発展が期待されている耐火材
料であり、また常温での熱伝導性の大なることからも電
子工業材料としての応用が強く期待されている。Aluminum nitride is difficult to wet with molten metal, and
It is a fireproof material that is expected to be developed industrially because it has excellent mechanical strength even at high temperatures up to 00°C and high thermal shock resistance, and it is also a material for the electronics industry because of its high thermal conductivity at room temperature. There are strong expectations for its application as
これまで、窒化アルミニウムの製造方法としては、多く
の提案がなされているが、それらを大別すると次の２つ
の方法に分けることができる。Until now, many proposals have been made as methods for producing aluminum nitride, but these can be roughly divided into the following two methods.
すなわち、第１の方法は、金属アルミニウムに窒素又は
アンモニアを直接反応させる方法であり、第２の方法は
、アルミナとカーボンとの混合物を窒素雰囲気中で加熱
する方法である。That is, the first method is a method in which metal aluminum is directly reacted with nitrogen or ammonia, and the second method is a method in which a mixture of alumina and carbon is heated in a nitrogen atmosphere.
しかし、第１の方法では溶融した金属アルミニウムと窒
素とが約４００℃から反応を開始し、約１４００℃まで
の昇温期間において生成した窒化アルミニウムが金属ア
ルミニウムの表面を覆うため以後の反応の進行が妨げら
れる。However, in the first method, the reaction between molten metal aluminum and nitrogen starts at about 400°C, and the aluminum nitride produced during the heating period up to about 1400°C covers the surface of metal aluminum, which hinders the progress of the subsequent reaction. is hindered.
また、金属アルミニウムとしては粉末を使うため比較的
多量の酸化物が混入することは避けえず、窒化アルミニ
ウム生成効率、純度共に低い。Furthermore, since powder is used as aluminum metal, it is inevitable that a relatively large amount of oxides will be mixed in, and both aluminum nitride production efficiency and purity are low.
また、第２の方法では１６００℃から１８００℃までの
高温を必要とするばかりでなく、複雑な反応が生起する
ため窒化アルミニウムの純度、生成効率は低い。Furthermore, the second method not only requires a high temperature of 1,600° C. to 1,800° C., but also involves complex reactions, resulting in low purity and production efficiency of aluminum nitride.
本発明者は、水酸化アルミニウムに炭素質物質を混合し
、その混合物を窒素雰囲気中で１３００〜１６００℃に
加熱することにより、従来方法では考えられない低温で
高純度の窒化アルミニウムを高収率で製造しうること、
また上記混合物に対し、さらに弗化カリ、弗化ソーダ等
の弗化アルカリ金属、弗化マグネシウム、弗化カルシウ
ム等の弗化アルカリ土金属などの弗化物、鉄、酸化マグ
ネシウム、酸化力ルシュム、Ｆｅ０１Ｆｅ２０３、Ｆｅ
３Ｏ４ノ鉄の酸化物、ニッケルの酸化物、コバルトの酸
化物、クロムの酸化物、マンガンの酸化物、バナジウム
の酸化物、ニオブの酸化物の１種又は２種以上の化合物
を０．２〜１０重量％添加混合すると窒化反応は促進さ
れ、加熱温度が約１００℃低下するので加熱温度を１２
００〜１５００℃にすることができると共に、加熱時間
が短縮されることを知見した。By mixing a carbonaceous substance with aluminum hydroxide and heating the mixture to 1,300 to 1,600°C in a nitrogen atmosphere, the present inventor was able to produce high-purity aluminum nitride in a high yield at a low temperature unimaginable with conventional methods. that can be manufactured with
In addition, to the above mixture, fluorides such as potassium fluoride, alkali metal fluorides such as sodium fluoride, alkaline earth metal fluorides such as magnesium fluoride and calcium fluoride, iron, magnesium oxide, oxidizing force, Fe01Fe203 , Fe
One or more compounds of 3O4 iron oxide, nickel oxide, cobalt oxide, chromium oxide, manganese oxide, vanadium oxide, and niobium oxide at 0.2 to When 10% by weight is added and mixed, the nitriding reaction is accelerated and the heating temperature is lowered by about 100°C.
It has been found that the temperature can be raised to 00 to 1500°C and the heating time can be shortened.
本発明は上記知見に基づくものであって、第１の発明は
水酸化アルミニウムと炭素質物質との混合物を窒素雰囲
気中で１３００−１６００℃に加熱することを特徴とす
る窒化アルミニウムの製造方法であり、第２の発明は水
酸化アルミニウムと炭素質物質との混合物に弗化物、鉄
、酸化マグネシウム、酸化カルシウム、鉄の酸化物、ニ
ッケルの酸化物、コバルトの酸化物、クロムの酸化物、
マンガンの酸化物、バナジウムの酸化物及びニオブの酸
化物より選ばれた１種又は２種以上の化合物０．２〜１
０重量％を添加混合して窒素雰囲気中で１２００−１５
００℃に加熱することを特徴とする窒化アルミニウムの
製造方法である。The present invention is based on the above findings, and the first invention is a method for producing aluminum nitride, which comprises heating a mixture of aluminum hydroxide and a carbonaceous substance to 1300-1600°C in a nitrogen atmosphere. In the second invention, fluoride, iron, magnesium oxide, calcium oxide, iron oxide, nickel oxide, cobalt oxide, chromium oxide,
One or more compounds selected from manganese oxide, vanadium oxide and niobium oxide 0.2 to 1
1200-15 in a nitrogen atmosphere by adding and mixing 0% by weight.
This is a method for producing aluminum nitride, which is characterized by heating to 00°C.
本発明において、アルミナ製造の中間生成物である水酸
化アルミニウムを使用することもできる。In the present invention, aluminum hydroxide, which is an intermediate product of alumina production, can also be used.
本発明における炭素質物質としては、カーボンブラック
、オイルコークス、グラファイト等の炭素粉末で、この
ものを１８〜２４重量％、好ましくは２０〜２２重量％
、水酸化アルミニウムに対し内側で混合する。The carbonaceous material used in the present invention is carbon powder such as carbon black, oil coke, graphite, etc., and the content thereof is 18 to 24% by weight, preferably 20 to 22% by weight.
, mix inside against aluminum hydroxide.
なお、炭素質物質を１８重量％未満混合したときは、窒
化反応が円満に進行せず、酸化アルミニウムを残存した
窒化アルミニウムとなり、また２４重量％を超すときは
炭素および炭化物が共存した窒化アルミニウムとなって
しまう。Note that when less than 18% by weight of carbonaceous material is mixed, the nitriding reaction does not proceed smoothly, resulting in aluminum nitride with residual aluminum oxide, and when it exceeds 24% by weight, aluminum nitride containing carbon and carbides coexists. turn into.
次に、弗化物、鉄、酸化マグネシウム、酸化カルシウム
、鉄の酸化物、ニッケルの酸化物、クロムの酸化物、マ
ンガンの酸化物、バナジウムの酸化物又はニオブの酸化
物の添加混合量は、水酸化アルミニウム７６〜８２重量
％と炭素質物質２４〜１８重量％との混合物に対し、０
．２〜１０重量％、好ましくは０．３〜５重量％である
。Next, the mixing amount of fluoride, iron, magnesium oxide, calcium oxide, iron oxide, nickel oxide, chromium oxide, manganese oxide, vanadium oxide or niobium oxide is For a mixture of 76-82% by weight of aluminum oxide and 24-18% by weight of carbonaceous material, 0
．． 2 to 10% by weight, preferably 0.3 to 5% by weight.
この添加範囲をはずれ、上記化合物を０．２重量％未満
添加した場合は、窒化反応に与える影響は低下し、１０
重量％を超える場合は窒化反応の促進効果は低減するば
かりでなく、過剰の物質が窒化アルミニウム中に残留し
純度が低下する。If the above-mentioned compound is added at less than 0.2% by weight outside of this addition range, the influence on the nitriding reaction will be reduced, and 10
If the amount exceeds % by weight, not only will the effect of promoting the nitriding reaction be reduced, but an excessive amount of the substance will remain in the aluminum nitride, resulting in a decrease in purity.
加熱温度は化合物を添加混合しないときは１３００〜１
６００℃、化合物を０．２〜１０重量％添加混合したと
きは１２００〜１５００℃であるが、いずれの場合も下
限よりも低い温度で加熱すると反応が容易に完結せず未
反応物が残留し、上限よりも高い温度で加熱するとＡｌ
４Ｃ３、Ａ１２．ＯＣ，Ａ１４０４Ｃなどの炭化物を副
生する。The heating temperature is 1300-1 when no compound is added and mixed.
600℃, and 1200 to 1500℃ when 0.2 to 10% by weight of the compound is added and mixed, but in any case, if heated at a temperature lower than the lower limit, the reaction will not be completed easily and unreacted materials will remain. , when heated at a temperature higher than the upper limit, Al
4C3, A12. Carbides such as OC and A1404C are produced as by-products.
最後に、本発明の方法における加熱時間は数時間程度で
ある。Finally, the heating time in the method of the invention is on the order of several hours.
本発明の方法によれば、加熱反応過程で金属アルミニウ
ムが生成することはないので、溶融アルミニウムの窒化
反応のように、反応速度が遅くなることがない。According to the method of the present invention, metal aluminum is not generated during the heating reaction process, so the reaction rate does not slow down unlike the nitriding reaction of molten aluminum.
またアルミナとカーボンとの混合物を窒化する場合のよ
うな高温度での加熱を必要としないし、窒化物の収率の
低下も全く認められない。Further, unlike the case of nitriding a mixture of alumina and carbon, heating at a high temperature is not required, and no decrease in the yield of nitride is observed.
これは水酸化アルミニウムが低温度域で加熱、脱水され
る過程で、結晶が極めて小さな細片に分割され、構造も
未編成のまま乱れた活性なアルミナとなり、このものが
窒素を吸着することによって窒化反応が促進されるもの
と考えられる。This is a process in which aluminum hydroxide is heated and dehydrated in a low temperature range, and the crystals are split into extremely small pieces, resulting in disordered active alumina with an unorganized structure, which adsorbs nitrogen. It is thought that the nitriding reaction is promoted.
本発明を実施するに際しての熱源は気体、液体、固体燃
料または電気などのいずれれでもよく、これにより加熱
された窒化炉中に本発明の原料混合物を粉末又は粒状に
して静置又は流動状態にして窒化することができる。The heat source used in carrying out the present invention may be gas, liquid, solid fuel, or electricity, and the raw material mixture of the present invention is made into powder or granules and allowed to stand still or in a fluid state in a heated nitriding furnace. can be nitrided.
実施例 １
水酸化アルミニウム粉末（試薬、粒径２０μ以下）にオ
イルコークス粉末（平均粒径１０μ）を内側で２１重量
％混合した混合物をパンペレタイザーにて５〜８ｍｍ径
に造粒し、該造粒物を窒素雰囲気中で１５００℃、３時
間３０分加熱することにより窒化率１００％で高純度の
窒化アルミニウムを得た。Example 1 A mixture of aluminum hydroxide powder (reagent, particle size 20 μm or less) and oil coke powder (average particle size 10 μm) mixed inside at 21% by weight was granulated to a diameter of 5 to 8 mm using a pan pelletizer. High purity aluminum nitride with a nitriding rate of 100% was obtained by heating the particles at 1500° C. for 3 hours and 30 minutes in a nitrogen atmosphere.
実施例 ２
アルミナ製造の際の中間生成物である水酸化アルミニウ
ム粉末（粒径６０μ以下）にカーボンブラック（平均粒
径３μ）を内側で２０重量％混合した混合物を実施例１
と同様に造粒し、該造粒物を窒素雰囲気中で１５００Ｃ
１３時間加熱することにより窒化率９９％で高純度の窒
化アルミニウムを得た。Example 2 Example 1 A mixture in which 20% by weight of carbon black (average particle size 3μ) was mixed inside aluminum hydroxide powder (particle size 60μ or less), which is an intermediate product during alumina production, was prepared.
Granulate in the same manner as above, and heat the granules at 1500C in a nitrogen atmosphere.
By heating for 13 hours, high purity aluminum nitride with a nitriding rate of 99% was obtained.
比較のためのアルミナ（粒径６０μ以下）にカーボンブ
ラック（平均粒径３μ）を２０重量％混合したものの造
粒物は窒素雰囲気中で１６５０’Ｃで１２時間加熱して
も窒化率が７０％であった。For comparison, the granulated product made by mixing 20% by weight of carbon black (average particle size 3μ) with alumina (particle size 60μ or less) had a nitriding rate of 70% even when heated at 1650'C for 12 hours in a nitrogen atmosphere. Met.
実施例 ３
アルミナ製造の際の中間生成物である水酸化アルミニウ
ム粉末（粒径６０μ以下）カーボンブラック（平均粒径
３μ）を内削で２０重量％加えた混合物に対し、さらに
弗化アンモン、鉄、酸化マグネシウム、酸化カルシウム
、Ｆｅ２Ｏ３、ニッケルの酸化物、コバルトの酸化物、
クロムの酸化物、マンガンの酸化物、バナジウムの酸化
物、ニオブの酸化物、鉄及び酸化マグネシウムのそれぞ
れを下表の如く外側で添加混合し、実施例１と同様に造
粒した造粒物を窒素雰囲気中で１４００℃に加熱して窒
化アルミニウムを製造した結果は下表のとおりである。Example 3 To a mixture in which 20% by weight of aluminum hydroxide powder (particle size 60 μm or less) and carbon black (average particle size 3 μm), which are intermediate products during alumina production, were added by internal grinding, ammonium fluoride and iron were added. , magnesium oxide, calcium oxide, Fe2O3, nickel oxide, cobalt oxide,
Chromium oxide, manganese oxide, vanadium oxide, niobium oxide, iron and magnesium oxide were added and mixed on the outside as shown in the table below, and the granules were granulated in the same manner as in Example 1. The results of producing aluminum nitride by heating to 1400° C. in a nitrogen atmosphere are shown in the table below.
Claims (1)
２４〜１８重量％との混合物を窒素雰囲気中で１３００
〜１６００℃に加熱することを特徴とする窒化アルミニ
ウムの製造方法。 ２ 炭素質物質がカーボンブラック、オイルコークス、
グラファイトの粉末である特許請求の範囲第１項記載の
窒化アルミニウムの製造方法。 ３ 水酸化アルミニウム７６〜８２重量％と炭素質物質
２４〜１８重量％との混合物に対し、弗化物、鉄、酸化
マグネシウム、酸化カルシウム、鉄の酸化物、ニッケル
の酸化物、コバルトの酸化物、クロムの酸化物、マンガ
ンの酸化物、バナジウムの酸化物及びニオブの酸化物よ
り選ばれた１種又は２種以上の化合物を０．２〜１０重
量％重量％添加室素雰囲気中で１２００〜１５００℃に
加熱することを特徴とする窒化アルミニウムの製造方法
。 ４ 炭素質物質か勿−ボンブラック、オイルコークス、
グラファイトの粉末である特許請求の範囲第３項記載の
窒化アルミニウムの製造方法。[Claims] 1. A mixture of 76 to 82% by weight of aluminum hydroxide and 24 to 18% by weight of carbonaceous material was heated to 1300% by weight in a nitrogen atmosphere.
A method for producing aluminum nitride, comprising heating to ~1600°C. 2 The carbonaceous material is carbon black, oil coke,
The method for producing aluminum nitride according to claim 1, which is graphite powder. 3. Fluoride, iron, magnesium oxide, calcium oxide, iron oxide, nickel oxide, cobalt oxide, One or more compounds selected from chromium oxide, manganese oxide, vanadium oxide, and niobium oxide are added in an amount of 0.2 to 10% by weight in a nitrogen atmosphere. A method for producing aluminum nitride, which comprises heating to ℃. 4 Carbonaceous substances, such as carbon black, oil coke,
The method for producing aluminum nitride according to claim 3, which is graphite powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2408376A JPS5951483B2 (en) | 1976-03-08 | 1976-03-08 | Aluminum nitride manufacturing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2408376A JPS5951483B2 (en) | 1976-03-08 | 1976-03-08 | Aluminum nitride manufacturing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS52107299A JPS52107299A (en) | 1977-09-08 |
| JPS5951483B2 true JPS5951483B2 (en) | 1984-12-14 |
Family
ID=12128501
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2408376A Expired JPS5951483B2 (en) | 1976-03-08 | 1976-03-08 | Aluminum nitride manufacturing method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5951483B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0629124B2 (en) * | 1989-09-13 | 1994-04-20 | 東京タングステン株式会社 | Aluminum nitride powder manufacturing method, aluminum nitride sintered body and manufacturing method thereof |
-
1976
- 1976-03-08 JP JP2408376A patent/JPS5951483B2/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| JPS52107299A (en) | 1977-09-08 |
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