JPH0234566A - Aluminum nitride-based powder and production thereof - Google Patents
Aluminum nitride-based powder and production thereofInfo
- Publication number
- JPH0234566A JPH0234566A JP63183490A JP18349088A JPH0234566A JP H0234566 A JPH0234566 A JP H0234566A JP 63183490 A JP63183490 A JP 63183490A JP 18349088 A JP18349088 A JP 18349088A JP H0234566 A JPH0234566 A JP H0234566A
- Authority
- JP
- Japan
- Prior art keywords
- aluminum nitride
- nitride powder
- amount
- powder
- alkoxide
- 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 43
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims description 47
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- 239000002245 particle Substances 0.000 claims abstract description 18
- 150000004703 alkoxides Chemical class 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052751 metal Inorganic materials 0.000 claims abstract description 9
- 239000002184 metal Substances 0.000 claims abstract description 9
- 239000012298 atmosphere Substances 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 230000003301 hydrolyzing effect Effects 0.000 claims abstract 2
- 230000001590 oxidative effect Effects 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims 1
- 238000005121 nitriding Methods 0.000 claims 1
- 239000001301 oxygen Substances 0.000 abstract description 21
- 229910052760 oxygen Inorganic materials 0.000 abstract description 21
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 20
- 238000010438 heat treatment Methods 0.000 abstract description 4
- NREVZTYRXVBFAQ-UHFFFAOYSA-N propan-2-ol;yttrium Chemical compound [Y].CC(C)O.CC(C)O.CC(C)O NREVZTYRXVBFAQ-UHFFFAOYSA-N 0.000 abstract description 3
- 238000005245 sintering Methods 0.000 description 22
- 238000010304 firing Methods 0.000 description 5
- 229910052761 rare earth metal Inorganic materials 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 229910052727 yttrium Inorganic materials 0.000 description 2
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 241001197925 Theila Species 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- MMLSWLZTJDJYJH-UHFFFAOYSA-N calcium;propan-2-olate Chemical compound [Ca+2].CC(C)[O-].CC(C)[O-] MMLSWLZTJDJYJH-UHFFFAOYSA-N 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- HHFAWKCIHAUFRX-UHFFFAOYSA-N ethoxide Chemical compound CC[O-] HHFAWKCIHAUFRX-UHFFFAOYSA-N 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 150000002926 oxygen Chemical class 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
Abstract
Description
【発明の詳細な説明】
〔概 要〕
窒化アルミニウム質粉末及びその製造方法に係り、特に
焼結性の良好な窒化アルミニウム質粉末及びその製造方
法に関し、
焼結助剤を過剰に添加することなく、短時間の焼成で、
窒化アルミニウム粉末粒子の表面に存在する酸化物層を
除去することが可能な窒化アルミニウム質粉末およびそ
の製造方法を提供することを目的とし、
窒化アルミニウム粒子の表面を、ＩＩＩａ族、ＩＩＩａ
族及び希土類金属の各々の酸化物の群から選択された少
なくとも１種により被覆したことを構成とする。[Detailed Description of the Invention] [Summary] This invention relates to an aluminum nitride powder and a method for producing the same, particularly an aluminum nitride powder with good sinterability and a method for producing the same, without adding an excessive amount of a sintering aid. , with a short firing time,
The purpose of the present invention is to provide an aluminum nitride powder capable of removing an oxide layer existing on the surface of aluminum nitride powder particles and a method for producing the same.
oxides of rare earth metals and rare earth metals.
本発明は窒化アルミニウム質粉末及びその製造方法に係
り、特に焼結性の良好な窒化アルミニウム賞粉末及びそ
の製造方法に関する。The present invention relates to an aluminum nitride powder and a method for producing the same, and more particularly to an aluminum nitride powder with good sinterability and a method for producing the same.
窒化アルミニウムは高い熱伝導性とシリコンに近い熱膨
張係数を有するため、ＬＳＩパッケージや多層回路基板
等の材料として有望視されている。Aluminum nitride has high thermal conductivity and a coefficient of thermal expansion close to that of silicon, so it is seen as a promising material for LSI packages, multilayer circuit boards, and the like.
従来より、窒化アルミニウム焼結体の製造には、主成分
となる窒化アルミニウム粉末に、数−１％の焼結助剤を
添加して焼成している。これらの焼結助剤としては、Ｃ
ａ等のＵａ族、Ｙ等のＩＩＩａ族または希土類元素の酸
化物や塩などが有効である。Conventionally, in the production of aluminum nitride sintered bodies, a few to 1% of a sintering aid is added to aluminum nitride powder, which is the main component, and then fired. These sintering aids include C
Oxides and salts of Ua group elements such as a, IIIa group elements such as Y, or rare earth elements are effective.
これらの焼結助剤は、窒化アルミニウム粉末粒子の表面
に存在する酸化物層と反応して、液相を発生し、緻密化
を促進するとともに、蒸発飛散して、窒化アルミニウム
の熱伝導率を阻害する原因となる酸素を系外に排出する
働きを有する。従って、焼結助剤の添加量は、窒化アル
ミニウム粉末中に存在する酸素量と対応していなければ
ならない。These sintering aids react with the oxide layer present on the surface of aluminum nitride powder particles to generate a liquid phase and promote densification, and also evaporate and scatter, increasing the thermal conductivity of aluminum nitride. It has the function of discharging oxygen, which causes inhibition, out of the system. Therefore, the amount of sintering aid added must correspond to the amount of oxygen present in the aluminum nitride powder.
焼結助剤の量が酸素量に対して過少と成る場合は、除去
しきれない酸素が残留することになり、また、過多とな
る場合は、焼結助剤が残留することになり、ともに不純
物となるため、熱伝導率を低下させる原因となる。If the amount of sintering aid is too small relative to the amount of oxygen, oxygen that cannot be removed will remain, and if it is too much, sintering aid will remain. Since it becomes an impurity, it causes a decrease in thermal conductivity.
ところが、これらの焼結助剤を粉末として添加する場合
は、窒化アルミニウム粉末と充分に混合し、分散させた
場合でも、ミクロ的に見れば添加量の少ない焼結助剤は
偏析していることになる。However, when these sintering aids are added as powder, even if they are thoroughly mixed and dispersed with aluminum nitride powder, from a microscopic perspective, the sintering aids added in small amounts are segregated. become.
このため、窒化アルミニウム粒子の一つ一つからそれぞ
れ酸化物層を除去するためには、存在する酸素量に対し
て過剰となる量の焼結助剤を添加することが必要となる
。Therefore, in order to remove the oxide layer from each aluminum nitride particle, it is necessary to add a sintering aid in an amount that is in excess of the amount of oxygen present.
従って、この過剰の焼結助剤は、窒化アルミニウムの焼
結後、粒界に不純物層として析出することになり、熱伝
導率が本来期待される値よりも小さくなるという問題を
生じていた。そのため、高熱伝導率化するためには、最
高温度で極めて長時間に渡って焼成しなければならない
など、特別な方法が必要となる。Therefore, this excessive sintering aid precipitates as an impurity layer at the grain boundaries after sintering the aluminum nitride, causing a problem that the thermal conductivity becomes lower than originally expected. Therefore, in order to achieve high thermal conductivity, special methods are required, such as firing at the highest temperature for an extremely long time.
本発明は、焼結助剤を過剰に添加することなく、短時間
の焼成で、窒化アルミニウム粉末粒子の表面に存在する
酸化物層を除去することが可能な窒化アルミニウム質粉
末およびその製造方法を提供することを目的とする。The present invention provides aluminum nitride powder and a method for producing the same, which can remove the oxide layer present on the surface of aluminum nitride powder particles by short-time firing without adding excessive sintering aids. The purpose is to provide.
上記課題は本発明によれば窒化アルミニウム粒子の表面
を、ＩＩａ族、ＩＩＩａ族の各々の酸化物の群から選択
された少なくとも１種により被覆したことを特徴とする
窒化アルミニウム賞粉末によって解決される。According to the present invention, the above problem is solved by aluminum nitride powder, which is characterized in that the surface of aluminum nitride particles is coated with at least one kind selected from the group of oxides of group IIa and group IIIa. .
更に上記課題は本発明によればＩｌａ族あるいはＩＩＩ
ａ族の金属アルコキシドをアルコール溶液に溶解し、該
溶液に窒化アルミニウム粉末を分散させた後、水を加え
て加水分解し、非酸化性雰囲気中で加熱処理することを
特徴とする窒化アルミニウム質粉末の製造方法によって
解決される。Furthermore, according to the present invention, the above-mentioned problem can be solved by the Ila group or III group.
Aluminum nitride powder, characterized in that a group a metal alkoxide is dissolved in an alcohol solution, aluminum nitride powder is dispersed in the solution, water is added for hydrolysis, and heat treatment is performed in a non-oxidizing atmosphere. The problem is solved by the manufacturing method.
本発明ではＵａ族はカルシウム（Ｃａ）、ＩＩＩａ族は
イツトリウム（Ｙ）が有効に用いられる。また添加量は
、本来、ＡｆｉＮ粉末中の酸素量に対応して決められる
べきであるが、通常使用されているＡＩＮ粉末の場合、
ＩＩａ族、ＩＩＩａ族の少なくとも１種酸化物の量が窒
化アルミニウム粒子の全体に対して０．２〜５重澄％で
あるのが好ましい。In the present invention, calcium (Ca) is effectively used for the Ua group, and yttrium (Y) is effectively used for the IIIa group. In addition, the amount added should originally be determined according to the amount of oxygen in the AfiN powder, but in the case of the commonly used AIN powder,
It is preferable that the amount of at least one oxide of Group IIa or Group IIIa is 0.2 to 5% by weight based on the total aluminum nitride particles.
０、２重量％未満では不足し、酸素が残留となり５重量
％を越えると極度に過剰となるためである。This is because if it is less than 0.2% by weight, it will be insufficient, and if it exceeds 5% by weight, it will be extremely excessive as oxygen will remain.
アルコキシドとしてはイソプロキシド、エトキシド等が
用いられその量も酸化物換算量として決められる。Isoprooxide, ethoxide, etc. are used as the alkoxide, and the amount thereof is determined in terms of the oxide.
（作 用〕
本発明に係る窒化アルミニウム質粉末は窒化アルミニウ
ム粉末粒子の一つ一つに均一に適量の焼結助剤成分が被
覆されているため、不足による酸素の残留が少なく、ま
た過剰による焼結助剤成分の粒界層への析出も生じない
。従って、高い熱伝導率を有する窒化アルミニウム焼結
体を得ることができる。(Function) In the aluminum nitride powder according to the present invention, since each aluminum nitride powder particle is uniformly coated with an appropriate amount of the sintering aid component, there is little residual oxygen due to insufficient oxygen, and less oxygen remains due to excess. The sintering aid component does not precipitate into the grain boundary layer. Therefore, an aluminum nitride sintered body having high thermal conductivity can be obtained.
以下本発明の実施例を図面に基づいて説明する。 Embodiments of the present invention will be described below based on the drawings.
第１図は本発明に係る窒化アルミニウム質粉末粒子の断
面図である。FIG. 1 is a cross-sectional view of aluminum nitride powder particles according to the present invention.
本発明では、第１図に示すように、窒化アルミニウム粉
末の粒子表面に、焼結助剤の働きをする成分の層が被覆
されている。図中の１は窒化アルミニウム粒子であり、
ｌａはその表面を覆っている酸化物層であり、２は被覆
した焼結助剤成分の層である。この層２は、上記焼結助
剤となる元素の金属アルコキシドを用いて形成される。In the present invention, as shown in FIG. 1, the particle surface of aluminum nitride powder is coated with a layer of a component that functions as a sintering aid. 1 in the figure is an aluminum nitride particle,
la is an oxide layer covering the surface, and 2 is a coated layer of a sintering aid component. This layer 2 is formed using the metal alkoxide of the element that serves as the sintering aid.
すなわち、この金属アルコキシドのアルコール溶液に窒
化アルミニウム粉末を分散させ、水を加えて加水分解し
、非酸化性雰囲気下で１０００℃以下の温度に加熱処理
して作製する。金属アルコキシドをその元素の酸化物に
換算して０．１〜３重量％となるようにアルコール溶液
に溶解されるのが好ましい。That is, aluminum nitride powder is dispersed in an alcohol solution of the metal alkoxide, water is added to hydrolyze it, and heat treatment is performed at a temperature of 1000° C. or lower in a non-oxidizing atmosphere. It is preferable that the metal alkoxide is dissolved in the alcohol solution in an amount of 0.1 to 3% by weight calculated as the oxide of the element.
窒化アルミニウム粉末の平均粒子径は３廂以下が好まし
く、２ｎ以下であれば更に好ましい。粒子径が大きくな
ると緻密な焼結体を得るのが困難となるからである。ま
た、粉末に含有される酸素量は１．５重量％以下である
ことが好ましく、１％以下であれば更に好ましい。酸素
は焼結助剤により除去されるものであるが、初期の酸素
量が多い場合は、粒内に固溶している酸素の存在も考え
られ、この酸素を除去することは著しく困難であるから
である。金属アルコキシドの濃度は、使用する窒化アル
ミニウム粉末に含有される酸素量に対応して決定される
。すなわち、酸素量に対して過不足ない量とする。The average particle size of the aluminum nitride powder is preferably 3 squares or less, more preferably 2 nm or less. This is because as the particle size increases, it becomes difficult to obtain a dense sintered body. Further, the amount of oxygen contained in the powder is preferably 1.5% by weight or less, and more preferably 1% or less. Oxygen is removed by a sintering aid, but if the initial amount of oxygen is large, there may be oxygen solidly dissolved within the grains, and it is extremely difficult to remove this oxygen. It is from. The concentration of metal alkoxide is determined depending on the amount of oxygen contained in the aluminum nitride powder used. In other words, the amount should be just the right amount for the amount of oxygen.
実１１」１
平均粒径１．５ Ｉｎａ、酸素含有量１重量％の窒化ア
ルミニウム粉末２００ｇを、イツトリウムイソプロポキ
シドを酸化イツトリウム換算で窒化アルミニウムに対し
て１重量％溶解したエタノール溶液に分散し、水を加え
て加水分解した。これを大気中で乾燥した後、窒素雰囲
気中、８００℃で、４時間加熱処理して、窒化アルミニ
ウム質粉末を作製した。Example 11''1 200 g of aluminum nitride powder with an average particle size of 1.5 Ina and an oxygen content of 1% by weight was dispersed in an ethanol solution in which yttrium isopropoxide was dissolved in an amount of 1% by weight relative to aluminum nitride in terms of yttrium oxide. , and hydrolyzed by adding water. After drying this in the air, it was heat-treated at 800° C. for 4 hours in a nitrogen atmosphere to produce aluminum nitride powder.
この粉末に、アクリル樹脂をバインダとして加えて、さ
らにエタノールを溶媒として、ボールミルにより混練し
た。これをらいかい機で乾燥して、樹脂を被覆した窒化
アルミニウム質粉末を作製した。この粉末を６０℃で金
型成形した後、窒素中、６００℃で４時間脱脂した。次
に、窒素雰囲気中、１８００℃で６時間焼成した。焼成
後、相対密度、およびレーザフラッシュ法により熱伝導
率を測定し、更に焼結体中の残留酸素量およびＹ（イツ
トリウム）量を測定した。結果を第１表に示す。Acrylic resin was added to this powder as a binder, and ethanol was used as a solvent, and the mixture was kneaded using a ball mill. This was dried in a sieve machine to produce resin-coated aluminum nitride powder. After molding this powder into a mold at 60°C, it was degreased at 600°C for 4 hours in nitrogen. Next, it was fired at 1800° C. for 6 hours in a nitrogen atmosphere. After firing, the relative density and thermal conductivity were measured by a laser flash method, and the amount of residual oxygen and Y (yttrium) in the sintered body was also measured. The results are shown in Table 1.
第１表
第２表
上記実施例１と同様の窒化アルミニウム粉末にイツトリ
ウムイソプロポキシド、カルシウムイソプロポキシドを
それぞれ量を変えて用いて、同様に窒化アルミニウム質
粉末を作製した。これらの粉末を用いて、同様に焼結体
を作製して相対密度、熱伝導率、酸素量および助剤元素
量を測定した。Table 1 Table 2 Aluminum nitride powders were similarly prepared using the same aluminum nitride powder as in Example 1 above, but using different amounts of yttrium isopropoxide and calcium isopropoxide. Using these powders, sintered bodies were produced in the same manner, and the relative density, thermal conductivity, oxygen content, and auxiliary element content were measured.
その結果を第２表に示す。The results are shown in Table 2.
辺、下余白
実施例と比較するため実施例１と同様の窒化アルミニウ
ム粉末と、酸化イツトリウム、酸化カルシウムをそれぞ
れ添加量を変えて混合し、更に樹脂などを加えてボール
ミルで混練し、実施例１と同様の方法で焼結体を作製し
、その特性を測定した。その結果を第３表に示す。Side and lower margin In order to compare with the example, aluminum nitride powder similar to Example 1, yttrium oxide, and calcium oxide were mixed in different amounts, and resin etc. were added and kneaded in a ball mill. A sintered body was prepared in the same manner as above, and its properties were measured. The results are shown in Table 3.
第３表
時間で、窒化アルミニウム粉末の表面に存在する酸化物
層を効率よく除去し、また、焼結助剤成分の残留も少な
くできるため、熱伝導率の高い窒化アルミニウム焼結体
を得ることができる。Table 3: It is possible to efficiently remove the oxide layer existing on the surface of aluminum nitride powder and reduce the amount of residual sintering aid components, thereby obtaining an aluminum nitride sintered body with high thermal conductivity. Can be done.
第１図は、焼結助剤成分を被覆した窒化アルミニウム質
粉末粒子である。
１・・・窒化アルミニウム粒子、
１ａ・・・窒化アルミニウム粒子表面の酸化物層、２・
・・被覆した焼結助剤成分。
〔発明の詳細
な説明した様に、
本発明によれば、短い焼成FIG. 1 shows aluminum nitride powder particles coated with a sintering aid component. 1... Aluminum nitride particles, 1a... Oxide layer on the surface of aluminum nitride particles, 2.
...Coated sintering aid component. [As described in the detailed description of the invention, according to the present invention, short firing
Claims (2)
の各々の酸化物の群から選択された少なくとも１種によ
り被覆したことを特徴とする窒化アルミニウム質粉末。1. An aluminum nitride powder characterized in that the surface of aluminum nitride particles is coated with at least one kind selected from the group of group IIa and group IIIa oxides.
コール溶液に溶解し、該溶液に窒化アルミニウム粉末を
分散させた後、水を加えて加水分解し、非酸化性雰囲気
中で加熱処理することを特徴とする窒化アルミニウム質
粉末の製造方法。2. Nitriding characterized by dissolving a group IIa or group IIIa metal alkoxide in an alcohol solution, dispersing aluminum nitride powder in the solution, hydrolyzing it by adding water, and heat-treating it in a non-oxidizing atmosphere. Method for producing aluminum powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63183490A JPH0234566A (en) | 1988-07-25 | 1988-07-25 | Aluminum nitride-based powder and production thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63183490A JPH0234566A (en) | 1988-07-25 | 1988-07-25 | Aluminum nitride-based powder and production thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0234566A true JPH0234566A (en) | 1990-02-05 |
Family
ID=16136730
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63183490A Pending JPH0234566A (en) | 1988-07-25 | 1988-07-25 | Aluminum nitride-based powder and production thereof |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0234566A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5395694A (en) * | 1992-09-21 | 1995-03-07 | Sumitomo Electric Industries, Ltd. | Aluminum nitride powder having surface layer containing oxynitride |
| JPH09157034A (en) * | 1995-12-06 | 1997-06-17 | Denki Kagaku Kogyo Kk | Aluminum nitride sintered body, its production and circuit board |
-
1988
- 1988-07-25 JP JP63183490A patent/JPH0234566A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5395694A (en) * | 1992-09-21 | 1995-03-07 | Sumitomo Electric Industries, Ltd. | Aluminum nitride powder having surface layer containing oxynitride |
| JPH09157034A (en) * | 1995-12-06 | 1997-06-17 | Denki Kagaku Kogyo Kk | Aluminum nitride sintered body, its production and circuit board |
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