JPH0455370A - Production of aluminum nitride powder - Google Patents
Production of aluminum nitride powderInfo
- Publication number
- JPH0455370A JPH0455370A JP2167731A JP16773190A JPH0455370A JP H0455370 A JPH0455370 A JP H0455370A JP 2167731 A JP2167731 A JP 2167731A JP 16773190 A JP16773190 A JP 16773190A JP H0455370 A JPH0455370 A JP H0455370A
- Authority
- JP
- Japan
- Prior art keywords
- aluminum nitride
- powder
- nitride powder
- firing
- 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 59
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims description 57
- 238000004519 manufacturing process Methods 0.000 title claims description 12
- 239000012298 atmosphere Substances 0.000 claims abstract description 16
- 229930195733 hydrocarbon Natural products 0.000 claims abstract description 8
- 150000002430 hydrocarbons Chemical class 0.000 claims abstract description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 19
- 230000002829 reductive effect Effects 0.000 claims description 11
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 7
- 238000007740 vapor deposition Methods 0.000 claims description 7
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract description 10
- 238000000034 method Methods 0.000 abstract description 7
- 239000002245 particle Substances 0.000 abstract description 5
- 238000004544 sputter deposition Methods 0.000 abstract description 2
- 239000002344 surface layer Substances 0.000 abstract description 2
- 238000001771 vacuum deposition Methods 0.000 abstract description 2
- 239000004215 Carbon black (E152) Substances 0.000 abstract 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract 1
- 229910052593 corundum Inorganic materials 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- 238000010304 firing Methods 0.000 description 20
- 239000000758 substrate Substances 0.000 description 17
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 13
- 239000007789 gas Substances 0.000 description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 9
- 239000001301 oxygen Substances 0.000 description 9
- 229910052760 oxygen Inorganic materials 0.000 description 9
- 229910021529 ammonia Inorganic materials 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 5
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 5
- 238000005245 sintering Methods 0.000 description 5
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 description 4
- 238000007796 conventional method Methods 0.000 description 4
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 4
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 3
- 239000000292 calcium oxide Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 3
- 239000011163 secondary particle Substances 0.000 description 3
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000005121 nitriding Methods 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000011882 ultra-fine particle Substances 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 229910003437 indium oxide Inorganic materials 0.000 description 1
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 230000002040 relaxant effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 description 1
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
この発明は、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 Field of Application] The present invention relates to a method for producing aluminum nitride powder.
ＩＣ等に代表される半導体素子の高集積化や大電力化が
進み、これに従って、放熱性の非常に良い電気絶縁基板
が必要になってきた。この要望に応じて、各種の高熱伝
導性絶縁基板が提案されている。中でも窒化アルミニウ
ム（セラミック）基板は熱伝導性、電気絶縁性、熱膨張
性等の点て優れているために、実用化が進められている
。BACKGROUND ART As semiconductor devices such as ICs and the like have become more highly integrated and have more power, electrically insulating substrates with very good heat dissipation properties have become necessary. In response to this demand, various high thermal conductivity insulating substrates have been proposed. Among these, aluminum nitride (ceramic) substrates are being put into practical use because they are excellent in terms of thermal conductivity, electrical insulation, thermal expansion, etc.
しかしながら、従来、十分な熱伝導率（例えば、２６０
Ｗ／ｍ−１（程度）をもつ窒化アルミニウム基板は製造
が容易でなかった。製造工程で高温かつ長時間の焼成が
必要だからである。上記例示程度の熱伝導率の窒化アル
ミニウム基板を得る場合、窒化アルミニウム粉末に酸化
イツトリウム、酸化カルシウム等の粉末状の焼結助剤等
を少量添加し成形してから、１８００℃以上、２０時間
以上、常圧還元雰囲気下で焼成し焼結させるようにする
。However, conventionally, sufficient thermal conductivity (e.g. 260
Aluminum nitride substrates with W/m-1 (about) were not easy to manufacture. This is because the manufacturing process requires high-temperature and long-time firing. To obtain an aluminum nitride substrate with a thermal conductivity similar to the example above, add a small amount of powdered sintering aid such as yttrium oxide or calcium oxide to aluminum nitride powder, and then mold it at 1800°C or higher for 20 hours or more. , the material is fired and sintered in a reducing atmosphere at normal pressure.
このように高温・長時間の焼成を必要とするのは、窒化
アルミニウム粉末が表面を中心に１ｉｆｔ％程度の不純
物酸素（通常、Ａｌ１ｘＯ＊の形で含まれる）を含んで
いるからである。不純物酸素は熱伝導率を劣化させるた
め、除去しなければならない。焼成工程では、酸化イツ
トリウム、酸化カルシウム等の焼結助剤とアルミニウム
およびＷ＆素との間で複合酸化物液相を粒界に現出し、
不純物酸素をトラップしつつ窒化アルミニウム結晶粒間
の三重点および四重点のところに液相を集中させること
により、酸化物からなる粒界層によるフォノン伝導の阻
害・散乱を出来るだけ低減させているのである。加えて
、還元雰囲気中の１８００°Ｃ以上の長時間焼成の間、
液相中の酸化物が徐々に揮発して除かれる結果、十分な
熱伝導率を有する焼結体になる。焼成時の温度・時間が
不十分だと、不純物酸素のトラップや酸化物の揮発除去
が不十分にしかできずに、十分な熱伝導率をもたせられ
ない。The reason why such high-temperature and long-time firing is required is that the aluminum nitride powder contains about 1 if% impurity oxygen (usually contained in the form of Al1xO*) mainly on the surface. Impurity oxygen degrades thermal conductivity and must be removed. In the firing process, a complex oxide liquid phase appears at grain boundaries between sintering aids such as yttrium oxide and calcium oxide, and aluminum and W& element.
By trapping impurity oxygen and concentrating the liquid phase at the triple and quadruple points between aluminum nitride crystal grains, the inhibition and scattering of phonon conduction by the grain boundary layer made of oxide is reduced as much as possible. be. In addition, during long-term firing at 1800°C or higher in a reducing atmosphere,
The oxide in the liquid phase is gradually volatilized and removed, resulting in a sintered body with sufficient thermal conductivity. If the temperature and time during firing are insufficient, trapping of oxygen impurities and volatilization of oxides will be insufficient, and sufficient thermal conductivity will not be achieved.
このように、従来、窒化アルミニウム粉末表面の不純物
酸素を除去するために高温・長時間の焼成が必要であり
、粉末で添加した焼結助剤があるために高温焼成が必要
であった。製造工程の高温・長時間焼成は、基板コスト
の上昇を招くので窒化アルミニウム基板の利用がなかな
か進まない。As described above, in the past, high-temperature and long-time firing was required to remove impurity oxygen on the surface of aluminum nitride powder, and high-temperature firing was necessary because of the sintering aid added in the form of powder. The use of aluminum nitride substrates has been slow because the high-temperature, long-time firing in the manufacturing process increases substrate costs.
この発明は、上記事情に鑑み、従来よりも緩やかな焼成
温度条件あるいは焼成時間条件で十分な熱伝導率の窒化
アルミニウム基板を作れる窒化アルミニウム粉末が得ら
れる方法を提供することを課題とする。In view of the above circumstances, it is an object of the present invention to provide a method for obtaining aluminum nitride powder that can produce an aluminum nitride substrate with sufficient thermal conductivity under firing temperature conditions or firing time conditions that are gentler than conventional ones.
前記課題を解決するため、請求項１記載の窒化アルミニ
ウム粉末の製造方法では、原料粉末たる窒化アルミニウ
ム粉末を、炭化水素および窒素を含む雰囲気で還元処理
した後、この窒化アルミニウム粉末の表面に窒化アルミ
ニウム蒸着膜を形成するようにしている。In order to solve the above problem, in the method for producing aluminum nitride powder according to claim 1, aluminum nitride powder, which is a raw material powder, is reduced in an atmosphere containing hydrocarbons and nitrogen, and then aluminum nitride is coated on the surface of the aluminum nitride powder. A vapor deposited film is formed.
この発明で得た窒化アルミニウム粉末を用いて基板を作
る場合、従来と同じであり、例えば、得た粉末に焼結゛
助剤をバインダー、溶剤等と共に添加混合し成形してお
いて、焼成し焼結させるようにする。When making a substrate using the aluminum nitride powder obtained in this invention, it is the same as the conventional method. For example, a sintering aid is added and mixed with the obtained powder together with a binder, a solvent, etc., the mixture is shaped, and then fired. Let it sinter.
添加する焼結助剤としては、希土類酸化物、アルカリ土
類酸化物等が挙げられる。複数種の希土類酸化物を併用
したり、複数種のアルカリ土類酸化物を併用したり、あ
るいは、１ないし複数種の希土類酸化物と１ないし複数
種のアルカリ土類酸化物を併用したりしてもよい。希土
類酸化物としては、酸化インドリウム（ｙｔ ｏｓ ）
等があり、アルカリ土類酸化物としては、酸化カルシウ
ム（Ｃａｂ）等がある。Examples of the sintering aid to be added include rare earth oxides and alkaline earth oxides. Multiple types of rare earth oxides are used together, multiple types of alkaline earth oxides are used together, or one or more types of rare earth oxides and one or more types of alkaline earth oxides are used together. It's okay. As a rare earth oxide, indium oxide (yt os )
Examples of alkaline earth oxides include calcium oxide (Cab).
続いて、この発明をより具体的に説明する。Next, this invention will be explained in more detail.
まず、第１図にみるように、酸化アルミニウムの多い表
面Ｊｉｉｌａのある窒化アルミニウム粉末（原料粉末）
１を、炭化水素および窒素を含む雰囲気で熱処理して還
元する。First, as shown in Figure 1, aluminum nitride powder (raw material powder) has a surface with a large amount of aluminum oxide.
1 is reduced by heat treatment in an atmosphere containing hydrocarbons and nitrogen.
原料粉末の粒径は、通常、０．１〜１ｎ程度である。０
．１〜０．３ｎの小粒径の場合には焼成温度が下げられ
るが、還元処理後の製造過程等で再酸化し易くなるため
、取扱難くなる傾向がある。The particle size of the raw material powder is usually about 0.1 to 1n. 0
．． In the case of small particle diameters of 1 to 0.3 nm, the firing temperature can be lowered, but the particles tend to be difficult to handle because they are likely to be re-oxidized during the manufacturing process after reduction treatment.
炭化水素および窒素を含む雰囲気としては、炭化水素用
としてのメタン、エチレン、アセチレン等の各ガスの少
なくともひとつと、窒素用としての窒素ガス、アンモニ
アガス等の少なくともひとつからなる混合ガス雰囲気が
例示される。還元処理で使う加熱炉としては、各窒化ア
ルミニウム粉末を等しく十分に混合ガスと接触させるこ
とが望ましいので、例えば、混合ガスをオーバーフロー
させて処理粉末を舞わせ（流動化させ）ながら熱処理で
きる流動層型の炉か、あるいは、処理粉末を機械的に攪
拌しながら熱処理できる横型回転炉を用いることが好ま
しい。An example of an atmosphere containing hydrocarbons and nitrogen is a mixed gas atmosphere consisting of at least one of methane, ethylene, acetylene, etc. for hydrocarbons and at least one of nitrogen gas, ammonia gas, etc. for nitrogen. Ru. As for the heating furnace used in the reduction treatment, it is desirable to bring each aluminum nitride powder into equal and sufficient contact with the mixed gas. It is preferable to use a type furnace or a horizontal rotary furnace that can perform heat treatment while mechanically stirring the treated powder.
熱処理中、使用ガスの種類に応じて、主として下記のよ
うなＡｌｘＯｓの還元窒化反応が起こる（１１ Ａ
ｓｒｓ ＋ ３Ｃ）＋４ 十Ｎｚ→２＾ＩＮ＋３ＣＯ
＋６１１！（２） ＡｔＯｓ ＋３Ｃ）１４ ＋
２ＮＩＩｓ→２八ＩＮ ＋ ３ＣＯ＋ ９Ｌ（３）
Ａ ！０１＋３／２Ｃ！Ｉ＋！ ＋Ｎ！−２ＡＩＮ＋３
ＣＯ＋３／２Ｈ！（４） ＾ＩｔＬ ＋３／２ＣＪ
ｔ ＋２Ｎｌ’ｌｘ→２＾ＩＮ＋３ＣＯ＋９／２１１
゜（５） 八 ！Ｏｓ ＋３／２ＣＩＨ４＋ Ｎ
！→２八ｌＮ＋３ｃＯ＋３１１゜（６） Ａ ！
０１＋３／２ＣＩＨ，＋２８１１．→２ＡＩＮ＋３ＣＯ
＋９Ｈ。During the heat treatment, depending on the type of gas used, the following reductive nitriding reaction of AlxOs mainly occurs (11 A
srs + 3C) + 4 10Nz→2^IN+3CO
+611! (2) AtOs +3C)14 +
2NIIs → 28 IN + 3CO+ 9L (3)
A! 01+3/2C! I+! +N! -2AIN+3
CO+3/2H! (4) ^ItL +3/2CJ
t +2Nl'lx→2^IN+3CO+9/211
゜(5) Eight! Os+3/2CIH4+N
! →28lN+3cO+311°(6) A!
01+3/2CIH, +2811. →2AIN+3CO
+9H.
熱処理温度は、使用ガスの種類に応じて若干具なるが、
通常、６００〜１２００℃程度の温度範囲で反応が良好
に進行する。The heat treatment temperature varies slightly depending on the type of gas used, but
Usually, the reaction proceeds well in a temperature range of about 600 to 1200°C.
第２図にみるように、還元窒化された窒化アルミニウム
粉末１′は、酸化アルミニウムの多い表面層がなくなっ
ている。As shown in FIG. 2, the reduced-nitrided aluminum nitride powder 1' has no surface layer containing a large amount of aluminum oxide.
還元処理工程の次ぎに、窒化アルミニウム蒸着膜の形成
工程に移り、第３図にみるように、窒化アルミニウム蒸
着膜１″ａを表面に形成した窒化アルミニウム粉末１″
を作る。Next to the reduction treatment step, the process moves to the step of forming an aluminum nitride vapor deposited film, and as shown in FIG.
make.
蒸着膜形成方法としては、真空蒸着法、スパッタリング
蒸着法、ＣＶ Ｄ （Ｃｈｅｎ＋１ｃａｌ Ｖａｐｏｕ
ｒ Ｄｅｐ。Vapor deposition film forming methods include vacuum evaporation method, sputtering evaporation method, and CVD (Chen+1 cal vapor deposition method).
r Dep.
５ｉｔｉｏｎ）法等が例示されるが、まわり込みがよく
均一な膜形成が行えるＣＶＤ法が適当である。蒸着の際
、例えば、ファンで攪拌して処理粉末を舞わせたり、容
器を回転させて処理粉末を舞わせたりする機械的攪拌を
併用するようにすることが好ましい。Examples include the CVD method, which can form a uniform film with good wraparound. During vapor deposition, it is preferable to use mechanical stirring, for example, stirring with a fan to cause the treated powder to fly, or rotating a container to cause the treated powder to flutter.
窒化アルミニウム蒸着膜は、蒸着条件の調整により、例
えば、アモルファス状の完全単一層の状態としたり、多
数の超微粒子が集合した状態としたりできる。By adjusting the deposition conditions, the aluminum nitride vapor-deposited film can be made into, for example, an amorphous complete single layer state or a state in which a large number of ultrafine particles are aggregated.
還元処理工程と蒸着膜形成工程は、それぞれ別々にバッ
チ式に行ってもよいが、ひとつの装置で連続して行う方
が、還元窒化後の窒化アルミニウム粉末の酸化防止の上
からも好ましい。Although the reduction treatment step and the deposited film formation step may be performed separately in a batch manner, it is preferable to perform them continuously in one apparatus from the standpoint of preventing oxidation of the aluminum nitride powder after reductive nitridation.
この発明は、勿論、上記例示の材料や処理条件を使うこ
とに限らないことは言うまでもない。It goes without saying that the present invention is not limited to the use of the materials and processing conditions exemplified above.
この発明の製造方法では、原料粉末の窒化アルミニウム
粉末を、炭化水素および窒素を含む雰囲気で還元処理す
るので、例えば、雰囲気がメタンとアンモニアを含む場
合、ＡＩｔｏｓ ＋ ３ＣＨ４＋ ２ＮＬ→２ＡＩＮ＋
３ＣＯ＋９）１．という還元窒化反応が起こり粉末表面
の酸化アルミニウムが還元窒化され不純物酸素量が激減
する。そのため、焼成時間を短くすることができる。焼
成時間条件を緩和できるようになるのである。In the manufacturing method of the present invention, aluminum nitride powder as a raw material powder is reduced in an atmosphere containing hydrocarbons and nitrogen. For example, when the atmosphere contains methane and ammonia, AItos + 3CH4+ 2NL→2AIN+
3CO+9)1. A reductive nitriding reaction occurs, and the aluminum oxide on the powder surface is reductively nitrided, and the amount of impurity oxygen is drastically reduced. Therefore, the firing time can be shortened. This allows the firing time conditions to be relaxed.
各窒化アルミニウム粉末表面には、アモルファス状ある
いは超微粒子の集合した窒化アルミニウム蒸着膜がある
。この蒸着膜は非常に活性であるため、従来より低目の
焼成温度で十分に焼結させられる。焼成温度条件を緩和
できるようになるのである。On the surface of each aluminum nitride powder, there is an aluminum nitride vapor deposited film that is amorphous or has an aggregate of ultrafine particles. Since this deposited film is very active, it can be sufficiently sintered at a lower firing temperature than conventional ones. This makes it possible to relax the firing temperature conditions.
以下、この発明の詳細な説明する。 The present invention will be explained in detail below.
実施例１−
窒化アルミニウム粉末（徳山曹達！！！Ｆグレード 酸
素含有率０．８９ｗｔ％ −次粒子径０．６μ）を透明
石英製管を用いた縦型管状炉にて還元処理した。雰囲気
は、メタン、アンモニア、窒素の混合ガス雰囲気である
。混合ガスをオーバフローさせながら処理粉末を流動化
させておいて、１０００℃、３０分間熱処理した。Example 1 - Aluminum nitride powder (Tokuyama Soda!!! F grade, oxygen content 0.89 wt% - secondary particle size 0.6 μm) was reduced in a vertical tube furnace using a transparent quartz tube. The atmosphere is a mixed gas atmosphere of methane, ammonia, and nitrogen. The treated powder was fluidized while overflowing the mixed gas, and heat-treated at 1000° C. for 30 minutes.
続いて、炉内温度を６００℃まで落とし、トリメチルア
ルミニウムとアンモニアを用いて、各窒化アルミニウム
粉末表面にＣＶＤ法で窒化アルミニウム蒸着膜をコーテ
ィング形成した。Subsequently, the temperature inside the furnace was lowered to 600° C., and an aluminum nitride vapor deposited film was coated on the surface of each aluminum nitride powder by CVD using trimethylaluminum and ammonia.
このようにして得た窒化アルミニウム粉末に酸化イツト
リウム粉末を３ｗｔ％添加混合し常法により成形して、
１６５０℃、Ｎ、雰囲気中、１時間焼成し、直径Ｌｏｗ
、厚み３鶴の窒化アルミニウム基板を得た。3 wt% of yttrium oxide powder was added to the aluminum nitride powder obtained in this way and mixed, and molded by a conventional method.
Fired at 1650°C in N atmosphere for 1 hour, resulting in a low diameter
An aluminum nitride substrate having a thickness of 3 mm was obtained.
一実施例２−
還元処理時の混合ガスをアセチレン、アンモニア、窒素
の混合ガスとし、処理温度を８０（ｌとした他は、実施
例１と同様にして、窒化アルミニウム基板を得た。Example 2 - An aluminum nitride substrate was obtained in the same manner as in Example 1, except that the mixed gas during the reduction treatment was a mixed gas of acetylene, ammonia, and nitrogen, and the treatment temperature was 80 (l).
実施例３−
窒化アルミニウム粉末（徳山曹達製 Ｆグレード 酸素
含有率０．８９ｗｔ％ −次粒子径０．６ｎ）を透明石
英製管を用いた縦型管状炉にて還元処理した。雰囲気は
、メタン、アンモニア、窒素の混合ガス雰囲気である。Example 3 - Aluminum nitride powder (manufactured by Tokuyama Soda, F grade, oxygen content 0.89 wt% - secondary particle size 0.6 n) was reduced in a vertical tube furnace using a transparent quartz tube. The atmosphere is a mixed gas atmosphere of methane, ammonia, and nitrogen.
混合ガスをオーバフローさせながら処理粉末を流動化さ
せておいて、１０００℃、３０分間熱処理した。The treated powder was fluidized while overflowing the mixed gas, and heat-treated at 1000° C. for 30 minutes.
続いて、炉内温度を８００℃まで落とし、三塩化アルミ
ニウムとアンモニアを用いて、各窒化アルミニウム粉末
表面にＣＶＤ法で窒化アルミニウム蒸着膜をコーティン
グ形成した。蒸着後の粉末を透過型電子顕微鏡で観察し
たところ、粒径０．６μｍ前後（０，４〜１．０μｍ程
）の１次粒子の表面に１０〜２０ｎｍの非常に細かい粒
子で出来た蒸着膜が形成されていた。Subsequently, the temperature inside the furnace was lowered to 800° C., and an aluminum nitride vapor deposited film was coated on the surface of each aluminum nitride powder by CVD using aluminum trichloride and ammonia. When the powder after vapor deposition was observed using a transmission electron microscope, a vapor deposited film made of very fine particles of 10 to 20 nm was observed on the surface of primary particles with a particle size of around 0.6 μm (approximately 0.4 to 1.0 μm). was formed.
このようにして得た窒化アルミニウム粉末に酸化イツト
リウム粉末を３ｅｖｔ％添加混合し常法により成形して
、１７００℃、Ｎ２雰囲気中、１時間焼成し、直径１０
ｎ、厚み３龍の窒化アルミニウム基板を得た。The thus obtained aluminum nitride powder was mixed with 3 evt% of yttrium oxide powder, molded by a conventional method, and fired at 1700°C in an N2 atmosphere for 1 hour.
An aluminum nitride substrate having a thickness of 3 mm and a thickness of 3 mm was obtained.
一比較例１−
窒化アルミニウム粉末（徳山曹達製 Ｆグレード 酸素
含有率０．８９ｗｔ％ −次粒子径０．６ ｐ烏）に酸
化イツトリウム粉末を３ｗｔ％添加混合し常法により成
形して、１７００℃、Ｎ２雰囲気中、１時間焼成し、直
径１０鰭、厚み３鶴の窒化アルミニウム基板を得た。Comparative Example 1 - 3 wt% of yttrium oxide powder was added to and mixed with aluminum nitride powder (manufactured by Tokuyama Soda, F grade, oxygen content: 0.89 wt% - secondary particle size: 0.6 p), molded by a conventional method, and heated to 1700°C. , in a N2 atmosphere for 1 hour to obtain an aluminum nitride substrate with a diameter of 10 fins and a thickness of 3 fins.
実施例１〜３および比較例１の各窒化アルミニウム基板
の熱伝導率をレーザフラッシュ法により測定した。測定
結果を、第１表に記す。The thermal conductivity of each aluminum nitride substrate of Examples 1 to 3 and Comparative Example 1 was measured by a laser flash method. The measurement results are shown in Table 1.
第 １ 表
第１表にみるように、実施例１〜３で得た窒化アルミニ
ウム粉末を用いた場合、従来はどの高温・長時間焼成で
なくとも十分な熱伝導率の窒化アルミニウム基板を得る
ことが出来ることが分かる。実施例１と比較例１を比べ
ると、この発明による窒化アルミニウム粉末を用いれば
、焼成温度が５０℃低く、焼成時間が１／３で十分な熱
伝導率の窒化アルミニウム基板が得られることが分かる
粉末の模式的断面図である。Table 1 As shown in Table 1, when the aluminum nitride powders obtained in Examples 1 to 3 were used, it was not possible to obtain an aluminum nitride substrate with sufficient thermal conductivity without any high-temperature, long-time firing. It turns out that it is possible. Comparing Example 1 and Comparative Example 1, it can be seen that by using the aluminum nitride powder according to the present invention, an aluminum nitride substrate with sufficient thermal conductivity can be obtained at a 50° C. lower firing temperature and 1/3 the firing time. FIG. 2 is a schematic cross-sectional view of powder.
１・・・原料粉末の窒化アルミニウム粉末 １′・・・
還元処理後の窒化アルミニウム粉末 １″・・・窒化ア
ルミニウム蒸着膜形成後の窒化アルミニウム粉末
代理人 弁理士 松 本 武 彦
〔発明の効果〕
以上に述べたように、この発明の製造方法によれば、焼
成温度条件あるいは焼成時間条件を従来よりも緩めて安
価に良熱伝導率の窒化アルミニウム基板を作れる窒化ア
ルミニウム粉末を得ることができる。1... Aluminum nitride powder as raw material powder 1'...
Aluminum nitride powder after reduction treatment 1″...Aluminum nitride powder after aluminum nitride vapor deposition film formation Representative Patent attorney Takehiko Matsumoto [Effects of the invention] As described above, according to the manufacturing method of the present invention It is possible to obtain aluminum nitride powder that can be used to produce aluminum nitride substrates with good thermal conductivity at low cost by relaxing firing temperature conditions or firing time conditions compared to conventional ones.
第１図は、原料粉末である窒化アルミニウム粉末の模式
的断面図、第２図は、還元処理後の窒化アルミニウム粉
末の模式的断面図、第３図は、窒化アルミニウム蒸着膜
形成後の窒化アルミニウム手続補正書（自発
第
図
第２
図
１゜
２゜
３゜
４゜
事件の表示
特願平２−１６７７３１、
発明の名称
窒化アルミニウム粉末の製造方法
補正をする者
事件との関係 特許出願人
住 所 大阪府門真市大字門真１０４８番地名
称（５８３）松下電工株式会社Fig. 1 is a schematic cross-sectional view of aluminum nitride powder, which is a raw material powder, Fig. 2 is a schematic cross-sectional view of aluminum nitride powder after reduction treatment, and Fig. 3 is a schematic cross-sectional view of aluminum nitride powder after forming an aluminum nitride vapor deposition film. Procedural amendment (procedural amendment Figure 2 Figure 1゜2゜3゜4゜ case) Japanese Patent Application No. 167731/1999, Name of the invention: Person amending the manufacturing method of aluminum nitride powder Relationship with the case Patent applicant address 1048 Kadoma, Kadoma City, Osaka Prefecture Name (583) Matsushita Electric Works Co., Ltd.
Claims (1)
よび窒素を含む雰囲気で還元処理した後、この窒化アル
ミニウム粉末の表面に窒化アルミニウム蒸着膜を形成す
るようにする窒化アルミニウム粉末の製造方法。1. A method for producing aluminum nitride powder, in which aluminum nitride powder, which is a raw material powder, is reduced in an atmosphere containing hydrocarbons and nitrogen, and then an aluminum nitride vapor deposition film is formed on the surface of the aluminum nitride powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2167731A JPH0455370A (en) | 1990-06-25 | 1990-06-25 | Production of aluminum nitride powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2167731A JPH0455370A (en) | 1990-06-25 | 1990-06-25 | Production of aluminum nitride powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0455370A true JPH0455370A (en) | 1992-02-24 |
Family
ID=15855106
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2167731A Pending JPH0455370A (en) | 1990-06-25 | 1990-06-25 | Production of aluminum nitride powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0455370A (en) |
-
1990
- 1990-06-25 JP JP2167731A patent/JPH0455370A/en active Pending
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