JPS6311506A - Production of aluminum nitride powder - Google Patents
Production of aluminum nitride powderInfo
- Publication number
- JPS6311506A JPS6311506A JP15573586A JP15573586A JPS6311506A JP S6311506 A JPS6311506 A JP S6311506A JP 15573586 A JP15573586 A JP 15573586A JP 15573586 A JP15573586 A JP 15573586A JP S6311506 A JPS6311506 A JP S6311506A
- Authority
- JP
- Japan
- Prior art keywords
- powder
- aluminum nitride
- alumina
- boehmite
- 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.)
- Pending
Links
- 239000000843 powder Substances 0.000 title claims abstract description 25
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims description 15
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910001593 boehmite Inorganic materials 0.000 claims abstract description 10
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 claims abstract description 10
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 10
- 238000005121 nitriding Methods 0.000 claims abstract description 6
- 239000011812 mixed powder Substances 0.000 claims abstract description 4
- 239000007858 starting material Substances 0.000 claims abstract description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 238000003786 synthesis reaction Methods 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 17
- 239000002245 particle Substances 0.000 abstract description 8
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract 2
- 239000000203 mixture Substances 0.000 abstract 1
- 238000000034 method Methods 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 9
- 229910052593 corundum Inorganic materials 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 230000002411 adverse Effects 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- -1 aluminum alkoxide Chemical class 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000002829 reductive effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Ceramic Products (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
この発明は、高熱伝導性を有する窒化アルミニウム焼結
体を得るための窒化アルミニウム粉末の製造方法に関す
る。DETAILED DESCRIPTION OF THE INVENTION (Industrial Application Field) The present invention relates to a method for producing aluminum nitride powder for obtaining an aluminum nitride sintered body having high thermal conductivity.
（従来の技術）
ＩＣＳＬＳＩなどの基板、サイリスタの放熱板として窒
化アルミニウム焼結体からなる基板が注目されている。(Prior Art) Substrates made of aluminum nitride sintered bodies are attracting attention as substrates for ICSLSIs and heat sinks for thyristors.
窒化アルミニウム粉末そのものを製造する方法としては
、従来法として次のようなものが知られている。The following conventional methods are known as methods for producing aluminum nitride powder itself.
１、アルミニウムを窒素雰囲気中、１３００〜１５００
℃で熱処理する直接窒化法。1. Aluminum in nitrogen atmosphere, 1300-1500
Direct nitriding method with heat treatment at ℃.
２、Ａｌ２Ｏ３に炭素粉末を混合し、これを窒素雰囲気
中１４００〜１７００℃で熱処理する還元窒化法。2. Reductive nitriding method in which carbon powder is mixed with Al2O3 and heat treated at 1400 to 1700°C in a nitrogen atmosphere.
３、アルミニウムのアルコキシドを窒素中で熱処理する
ＣＶＤ法。3. CVD method in which aluminum alkoxide is heat treated in nitrogen.
（発明が解決しようとする問題）
第１の方法では、安価な製造方法ではあるが、この方法
により得られた粉末には不純物が多く含まれるという問
題がある。(Problems to be Solved by the Invention) Although the first method is an inexpensive manufacturing method, there is a problem in that the powder obtained by this method contains many impurities.
また、第２の方法では、不純物が多く含有されるという
品質上の問題はみられないが、量産性に乏しく、工業上
の利用価値が低い。In addition, in the second method, there is no quality problem such as high content of impurities, but it is poor in mass productivity and has low industrial utility value.
さらに、第３の方法では、原料として高価なアルコキシ
ドを用いるために、コストが高くなる。Furthermore, the third method uses an expensive alkoxide as a raw material, which increases the cost.
（発明の目的）
したがって、この発明は高純度で、粉末の粒径が細かく
、かつ均一な窒化アルミニウム粉末の製造方法を提供す
ることを目的とする。(Objective of the Invention) Therefore, an object of the present invention is to provide a method for producing aluminum nitride powder with high purity, fine powder particle size, and uniformity.
（発明の構成）
この発明によれば、まず、出発材料としてベーマイト（
ＡＩＯＯＨ）を用いる。そして、 このベーマイトにカ
ーボン粉末を混合し、この混合粉末を窒素雰囲気中で５
００〜Ｉ Ｃｏｏ″Ｃ温度で熱処理する。(Structure of the Invention) According to the present invention, first, boehmite (
AIOOH) is used. Then, carbon powder is mixed with this boehmite, and this mixed powder is heated for 50 minutes in a nitrogen atmosphere.
Heat treatment at a temperature of 00 to I Coo''C.
次に、前記工程で得られた粉末を窒素雰囲気中で１４５
０〜１７００℃の温度で窒化合成する工程からなる。Next, the powder obtained in the above step was heated to 145% in a nitrogen atmosphere.
It consists of a step of nitriding synthesis at a temperature of 0 to 1700°C.
ベーマイトとカーボン粉末との混合割合は、ベーマイト
をＡｌ２Ｏ３に換葦し、重量比でＡｌ２Ｏ３を基準とし
てカーボン粉末が０．３５〜１．５の範囲が好ましい。The mixing ratio of boehmite and carbon powder is preferably such that boehmite is replaced with Al2O3, and the weight ratio of carbon powder is 0.35 to 1.5 based on Al2O3.
これは、カーボン粉末が０．３５未満ではα−Ａ１２０
３が残存し、１．５を想えるとカーボン粉末に含まれる
不純物が悪影響を与えることになる。This means that if the carbon powder is less than 0.35, α-A120
If 3 remains and 1.5 is considered, the impurities contained in the carbon powder will have an adverse effect.
また、第１次の熱処理はベーマイトの水和した水を除去
するための工程であり、第２次の熱処理は窒化合成のた
めの工程である。Further, the first heat treatment is a process for removing water in which boehmite is hydrated, and the second heat treatment is a process for nitriding synthesis.
（効果）
この発明方法によれば、出発材料として、ａ−アルミナ
、７−アルミナを用いて窒化アルミニウム粉末を製造す
る方法に比べて、比表面積が大きく、平均粒径が小きく
、粒径も均一である。したがって、この窒化アルミニウ
ム粉末を用いて焼結体としたとき、焼結密度の高いもの
が得られる。(Effects) According to the method of this invention, compared to the method of producing aluminum nitride powder using a-alumina and 7-alumina as starting materials, the specific surface area is larger, the average particle size is smaller, and the particle size is also smaller. Uniform. Therefore, when this aluminum nitride powder is used to form a sintered body, a sintered body with high density can be obtained.
（実施例） 以下に、この発明を実施例に従フて詳細に説明する。(Example) The present invention will be described in detail below with reference to examples.
実施例
ベーマイト（ＡＩＯＯＨ）とカーボン粉末を重量比１：
０．４となるように調合し、アルミナボットにアルミナ
ポールとともに投入した。このアルミナボットを第１図
に示すような熱処理炉に設置した。Example boehmite (AIOOH) and carbon powder in a weight ratio of 1:
It was mixed to a concentration of 0.4 and put into the Alumina Bot together with the Alumina Pole. This alumina bot was placed in a heat treatment furnace as shown in FIG.
第１図に示した熱処理炉について説明すると、１は炉の
本体、この炉１の内壁側にはヒーター２が配置されてお
り、炉１の内部に設置されたアルミナボット３を加熱す
る。アルミナボット３はそれ自体が回転可能にローラー
４．５で支承されている。６は炉の内部にガスを投入す
るためのパイプ、７は炉の内部温度を測定するための熱
電対、８は炉の内部のガスを排気するためのパイプであ
る。To explain the heat treatment furnace shown in FIG. 1, reference numeral 1 denotes a main body of the furnace, and a heater 2 is arranged on the inner wall side of the furnace 1, and heats an alumina bot 3 installed inside the furnace 1. The alumina bot 3 is itself rotatably supported on rollers 4.5. 6 is a pipe for introducing gas into the inside of the furnace, 7 is a thermocouple for measuring the internal temperature of the furnace, and 8 is a pipe for exhausting the gas inside the furnace.
上記したように、第１図の熱処理炉に設置きれたアルミ
ナボット３は、ローラー４．５により回転されるととも
に、ヒーター２により、５００℃〜１０００℃の温度で
加熱される。As described above, the alumina bot 3 installed in the heat treatment furnace shown in FIG. 1 is rotated by the rollers 4.5 and heated by the heater 2 at a temperature of 500°C to 1000°C.
次に、熱処理済の混合粉末を別の雰囲気熱処理炉を用い
て１６００℃の温度で５時間、窒素雰囲気中で熱処理し
た。さらに、熱処理された粉末に残存する過剰のカーボ
ンを除去するために、６゜０〜７００℃の温度で２時間
、空気中で熱処理した。Next, the heat-treated mixed powder was heat-treated in a nitrogen atmosphere at a temperature of 1600° C. for 5 hours using another atmospheric heat treatment furnace. Furthermore, in order to remove excess carbon remaining in the heat-treated powder, it was heat-treated in air at a temperature of 6.0 to 700.degree. C. for 2 hours.
このようにして得られた窒化アルミニウム粉末は、ａ−
アルミナ、７−アルミナ粉末を原料として処理した窒化
アルミニウム粉末よりも、比表面積がおおきく、平均粒
径が小きく、均一であるという特ｉ歇を有している。The aluminum nitride powder thus obtained is a-
It has the characteristics of a larger specific surface area, smaller average particle size, and more uniformity than aluminum nitride powder processed using alumina or 7-alumina powder as a raw material.
第１表は、この発明の実施例で得られた窒化アルミニウ
ム粉末と、従来例のうち７−アルミナを窒素雰囲気中で
熱処理して得られたによる窒化アルミニウム粉末との比
表面積、平均粒径の各特性を示したものである。Table 1 shows the specific surface area and average particle size of the aluminum nitride powder obtained in the example of the present invention and the aluminum nitride powder obtained by heat-treating 7-alumina in a nitrogen atmosphere among the conventional examples. This shows each characteristic.
第 １ 表
この発明の実施例により得られた窒化アルミニウム粉末
を用い、この粉末にＹ２Ｏ３を１．０重量％添加し、こ
れを成形して焼結したところ、上の表に示すような焼結
密度の値を示した。なお、＃考として従来例で得られた
窒化アルミニウム粉末を用い、同様に焼結体を得たとこ
ろ上の表から明らかなように焼結密度は９７．５χであ
った。Table 1 Using aluminum nitride powder obtained in accordance with an example of the present invention, 1.0% by weight of Y2O3 was added to the powder, which was then molded and sintered. Density values are shown. As a #consideration, a sintered body was similarly obtained using the aluminum nitride powder obtained in the conventional example, and as is clear from the above table, the sintered density was 97.5χ.
【図面の簡単な説明】
第１図はこの発明方法を実施するときに使用する熱処理
炉の概略断面図である。
１は炉の本体、２はヒーター、３はアルミナポット、４
．５はローラー、６．８はバイブ、７は熱電対。BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a schematic sectional view of a heat treatment furnace used in carrying out the method of the present invention. 1 is the main body of the furnace, 2 is the heater, 3 is the alumina pot, 4
．． 5 is a roller, 6.8 is a vibrator, and 7 is a thermocouple.
Claims (1)
、このベーマイトにカーボン粉末を混合し、この混合粉
末を窒素雰囲気中で５００〜１０００℃の温度で熱処理
し、前記工程で得られた粉末を窒素雰囲気中で１４５０
〜１７００℃の温度で窒化合成することを特徴とする窒
化アルミニウム粉末の製造方法。(1) Boehmite (AIOOH) is used as a starting material, carbon powder is mixed with this boehmite, this mixed powder is heat-treated at a temperature of 500 to 1000°C in a nitrogen atmosphere, and the powder obtained in the above step is heated in a nitrogen atmosphere. Inside 1450
A method for producing aluminum nitride powder, characterized by nitriding synthesis at a temperature of ~1700°C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP15573586A JPS6311506A (en) | 1986-07-01 | 1986-07-01 | Production of aluminum nitride powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP15573586A JPS6311506A (en) | 1986-07-01 | 1986-07-01 | Production of aluminum nitride powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS6311506A true JPS6311506A (en) | 1988-01-19 |
Family
ID=15612302
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP15573586A Pending JPS6311506A (en) | 1986-07-01 | 1986-07-01 | Production of aluminum nitride powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6311506A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0272493A2 (en) * | 1986-11-28 | 1988-06-29 | Kawasaki Steel Corporation | Method for producing aluminium nitride powder |
| JPH01301505A (en) * | 1988-05-30 | 1989-12-05 | Tokuyama Soda Co Ltd | Aluminum nitride powder and production thereof |
| JPH0353066A (en) * | 1989-07-20 | 1991-03-07 | Sekiyu Kodan | Sputtering device |
-
1986
- 1986-07-01 JP JP15573586A patent/JPS6311506A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0272493A2 (en) * | 1986-11-28 | 1988-06-29 | Kawasaki Steel Corporation | Method for producing aluminium nitride powder |
| JPH01301505A (en) * | 1988-05-30 | 1989-12-05 | Tokuyama Soda Co Ltd | Aluminum nitride powder and production thereof |
| JPH0563406B2 (en) * | 1988-05-30 | 1993-09-10 | Tokuyama Soda Kk | |
| JPH0353066A (en) * | 1989-07-20 | 1991-03-07 | Sekiyu Kodan | Sputtering device |
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