JPH02141410A - Surface treatment of aluminum nitride powder - Google Patents
Surface treatment of aluminum nitride powderInfo
- Publication number
- JPH02141410A JPH02141410A JP1183886A JP18388689A JPH02141410A JP H02141410 A JPH02141410 A JP H02141410A JP 1183886 A JP1183886 A JP 1183886A JP 18388689 A JP18388689 A JP 18388689A JP H02141410 A JPH02141410 A JP H02141410A
- Authority
- JP
- Japan
- Prior art keywords
- aluminum nitride
- nitride powder
- pts
- powder
- organophosphoric acid
- 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.)
- Granted
Links
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims abstract description 84
- 239000000843 powder Substances 0.000 title claims abstract description 67
- 238000004381 surface treatment Methods 0.000 title claims description 6
- -1 Alkali metal salts Chemical class 0.000 claims abstract description 25
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 20
- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Substances OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 39
- 239000002253 acid Substances 0.000 abstract description 21
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 16
- 239000001301 oxygen Substances 0.000 abstract description 16
- 229910052760 oxygen Inorganic materials 0.000 abstract description 16
- 239000002904 solvent Substances 0.000 abstract description 11
- 239000000203 mixture Substances 0.000 abstract description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 6
- 239000000945 filler Substances 0.000 abstract description 6
- 239000011347 resin Substances 0.000 abstract description 4
- 229920005989 resin Polymers 0.000 abstract description 4
- 229910052783 alkali metal Inorganic materials 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- 239000003566 sealing material Substances 0.000 abstract description 3
- 238000004898 kneading Methods 0.000 abstract 1
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 21
- 238000010438 heat treatment Methods 0.000 description 16
- 239000006185 dispersion Substances 0.000 description 13
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 12
- 238000000465 moulding Methods 0.000 description 11
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 229910021529 ammonia Inorganic materials 0.000 description 6
- FJTUUPVRIANHEX-UHFFFAOYSA-N butan-1-ol;phosphoric acid Chemical compound CCCCO.OP(O)(O)=O FJTUUPVRIANHEX-UHFFFAOYSA-N 0.000 description 6
- 229910019142 PO4 Inorganic materials 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 239000010452 phosphate Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 239000012756 surface treatment agent Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- ABLZXFCXXLZCGV-UHFFFAOYSA-N Phosphorous acid Chemical compound OP(O)=O ABLZXFCXXLZCGV-UHFFFAOYSA-N 0.000 description 2
- 125000003342 alkenyl group Chemical group 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- OOYGSFOGFJDDHP-KMCOLRRFSA-N kanamycin A sulfate Chemical group OS(O)(=O)=O.O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CN)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O[C@@H]2[C@@H]([C@@H](N)[C@H](O)[C@@H](CO)O2)O)[C@H](N)C[C@@H]1N OOYGSFOGFJDDHP-KMCOLRRFSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000005121 nitriding Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- LJKDOMVGKKPJBH-UHFFFAOYSA-N 2-ethylhexyl dihydrogen phosphate Chemical compound CCCCC(CC)COP(O)(O)=O LJKDOMVGKKPJBH-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- DBVJJBKOTRCVKF-UHFFFAOYSA-N Etidronic acid Chemical group OP(=O)(O)C(O)(C)P(O)(O)=O DBVJJBKOTRCVKF-UHFFFAOYSA-N 0.000 description 1
- OLBVUFHMDRJKTK-UHFFFAOYSA-N [N].[O] Chemical compound [N].[O] OLBVUFHMDRJKTK-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 229920005822 acrylic binder Polymers 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 150000007860 aryl ester derivatives Chemical class 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 description 1
- XPPKVPWEQAFLFU-UHFFFAOYSA-N diphosphoric acid Chemical compound OP(O)(=O)OP(O)(O)=O XPPKVPWEQAFLFU-UHFFFAOYSA-N 0.000 description 1
- 238000007606 doctor blade method Methods 0.000 description 1
- RSNDQTNQQQNXRN-UHFFFAOYSA-N dodecyl dihydrogen phosphite Chemical compound CCCCCCCCCCCCOP(O)O RSNDQTNQQQNXRN-UHFFFAOYSA-N 0.000 description 1
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 238000007580 dry-mixing Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 125000001117 oleyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])/C([H])=C([H])\C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- CMPQUABWPXYYSH-UHFFFAOYSA-N phenyl phosphate Chemical compound OP(O)(=O)OC1=CC=CC=C1 CMPQUABWPXYYSH-UHFFFAOYSA-N 0.000 description 1
- UEZVMMHDMIWARA-UHFFFAOYSA-M phosphonate Chemical compound [O-]P(=O)=O UEZVMMHDMIWARA-UHFFFAOYSA-M 0.000 description 1
- 150000003014 phosphoric acid esters Chemical class 0.000 description 1
- 150000003016 phosphoric acids Chemical class 0.000 description 1
- 229920000137 polyphosphoric acid Polymers 0.000 description 1
- 229940005657 pyrophosphoric acid Drugs 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000565 sealant Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- DQZNLOXENNXVAD-UHFFFAOYSA-N trimethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OC)(OC)OC)CCC2OC21 DQZNLOXENNXVAD-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
本発明は、窒化アルミニウム粉末の表面処理方法に関す
る。DETAILED DESCRIPTION OF THE INVENTION Field of the Invention The present invention relates to a method for surface treatment of aluminum nitride powder.
従来の技術及び発明が解決しようとする問題点窒化アル
ミニウムが高熱伝導性を有していることは公知であり、
その焼結体は高熱伝導性セラミックスとして利用されて
いる。また、その粉末をＩＣ用封止材や接着剤を含めた
樹脂混線材用のフィラーとして使用することも提案され
ている。Problems to be Solved by the Prior Art and the Invention It is known that aluminum nitride has high thermal conductivity.
The sintered body is used as a highly thermally conductive ceramic. It has also been proposed to use the powder as a filler for resin hybrid materials including IC sealants and adhesives.
しかしながら、窒化アルミニウムは水との反応性が強く
、水と接触すると加水分解を受け、アンモニアを発生し
なから水和アルミナに分解される性質を有している。こ
のため、下記のような問題が生ずる。However, aluminum nitride has a strong reactivity with water, and when it comes into contact with water, it undergoes hydrolysis and has the property of being decomposed into hydrated alumina without generating ammonia. This causes the following problems.
ａ） 窒化アルミニウム粉末を成形、焼結して窒化アル
ミニウム焼結体を作成する場合、成形媒体として水を使
用することができない。従って、水スラリーを使用する
鋳込成形やデープ成形が利用できず、成形方法を限定せ
ざるを得ない問題がある。a) When molding and sintering aluminum nitride powder to create an aluminum nitride sintered body, water cannot be used as a molding medium. Therefore, casting molding or deep molding using water slurry cannot be used, and there is a problem that the molding method must be limited.
加えて、成形媒体として水を使用することができないの
で、従来は成形媒体として水の代りに有機溶剤が使用さ
れてきたが、有機溶剤使用のためにコスト高になり、爆
発の危険性もある。In addition, since water cannot be used as a molding medium, conventionally organic solvents have been used instead of water as a molding medium, but the use of organic solvents increases costs and poses a risk of explosion. .
仮に成形媒体として水を使用したとしても、窒化アルミ
ニウム粉末中の酸素含量が水との反応によって増大する
ため所望の熱伝導度を有する焼結体が得られない。Even if water were used as a molding medium, the oxygen content in the aluminum nitride powder would increase due to the reaction with water, making it impossible to obtain a sintered body with the desired thermal conductivity.
ｂ）窒化アルミニウムは人気中の水分によっても加水分
解が進行するため、保管状況が悪ければ、貯蔵・取扱い
中にアンモニア臭が発生する他、酸素含量が増大する。b) Hydrolysis of aluminum nitride progresses due to moisture, so if storage conditions are poor, an ammonia odor will be generated during storage and handling, and the oxygen content will increase.
従って、窒化アルミニウム粉末をフィラーとして使用し
た場合にはフィラーの品質が経時的に著しく変化する恐
れがある。Therefore, when aluminum nitride powder is used as a filler, the quality of the filler may change significantly over time.
上記した問題を解消すべく、窒化アルミニウムを約６０
０〜８００℃で加熱して表面に酸化アルミの皮膜を形成
することにより窒化アルミニウムの耐水性を改善する方
法が提案されているが、この方法でも窒化アルミニウム
の耐水性を長期間安定に維持することができない。In order to solve the above problems, approximately 60% of aluminum nitride
A method has been proposed to improve the water resistance of aluminum nitride by heating it at 0 to 800°C to form an aluminum oxide film on the surface, but this method also maintains the water resistance of aluminum nitride stably for a long period of time. I can't.
本発明の目的は、長期間に亘り安定な耐水性を有づる窒
化アルミニウム粉末を提供することにある。An object of the present invention is to provide aluminum nitride powder that has stable water resistance over a long period of time.
本発明の他の目的は、窒化アルミニウム焼結体の製造原
料として及びＩＣ用封止材や樹脂混線材用フィラーどし
て適当に使用され得る耐水性に優れた窒化アルミニウム
粉末を提供することにある。Another object of the present invention is to provide aluminum nitride powder with excellent water resistance, which can be suitably used as a raw material for producing aluminum nitride sintered bodies, and as a filler for IC sealing materials and resin hybrid wire materials. be.
本発明の目的は、耐水性の優れた窒化アルミニウム粉末
を得るための表面処理方法を提供することにある。An object of the present invention is to provide a surface treatment method for obtaining aluminum nitride powder with excellent water resistance.
題 を解決するだめの手段
今回、窒化アルミニウム粉末に特定量の有機リン酸化合
物を添加して処理した後加熱処理して得られた窒化アル
ミニウム粉末が優れた耐水性をイ１することが知見され
た。As a means to solve the problem, it has now been discovered that aluminum nitride powder obtained by adding a specific amount of an organic phosphoric acid compound to aluminum nitride powder, followed by heat treatment, has excellent water resistance. Ta.
従って、本発明により提供される耐水性の優れた窒化ア
ルミニウム粉末は、窒化アルミニウム粉末に対して窒化
アルミニウム粉末１００重量部当り０．１〜１０重量部
の有機リン酸化合物を添枦して処理した後、約１５０〜
８００℃の温度で加熱処理することにより表面処理され
ていることを特徴とするものである。Therefore, the aluminum nitride powder with excellent water resistance provided by the present invention is obtained by adding 0.1 to 10 parts by weight of an organic phosphoric acid compound per 100 parts by weight of the aluminum nitride powder to the aluminum nitride powder. After, about 150~
It is characterized by being surface-treated by heat treatment at a temperature of 800°C.
本発明の耐水性の優れた窒化アルミニウム粉末を得るた
めには、まず窒化アルミニウム粉末を溶剤に分散させ、
攪拌下の分散液に有機リン酸化合物を滴下して所定量の
有機リン酸化合物を窒化アルミニウムと反応させる。窒
化アルミニウムと有機リン酸化合物とを反応させる温度
は特に限定されないが、通常室温〜８０℃の範囲で選択
され、好ましくは４０〜６０℃である。In order to obtain the aluminum nitride powder of the present invention with excellent water resistance, first, the aluminum nitride powder is dispersed in a solvent,
An organic phosphoric acid compound is added dropwise to the dispersion under stirring to cause a predetermined amount of the organic phosphoric acid compound to react with aluminum nitride. The temperature at which aluminum nitride and the organic phosphoric acid compound are reacted is not particularly limited, but is usually selected in the range of room temperature to 80°C, preferably 40 to 60°C.
また、窒化アルミニウム粉末を有機リン酸化合物の共存
下室温で乾式混合後約１５０〜８００℃の温度で加熱処
理することにより、本発明の耐水性の優れた窒化アルミ
ニウム粉末を得ることができる。Further, the aluminum nitride powder of the present invention having excellent water resistance can be obtained by dry mixing the aluminum nitride powder at room temperature in the presence of an organic phosphoric acid compound and then heat-treating the powder at a temperature of about 150 to 800°C.
有機リン酸化合物で処理される窒化アルミニウム粉末は
特に限定されず、粉末アルミニウムを窒素中で加熱する
直接窒化法、アルミナと炭素の混合物を窒素中で加熱す
るアルミブ還元法等の方法で製造した窒化アルミニウム
粉末であり得る。通常、平均粒径が約０．１μｓ〜約１
ｍの窒化アルミニウム粉末を使用する。The aluminum nitride powder treated with an organic phosphoric acid compound is not particularly limited, and includes nitriding produced by methods such as a direct nitriding method in which powdered aluminum is heated in nitrogen, and an aluminum reduction method in which a mixture of alumina and carbon is heated in nitrogen. It can be aluminum powder. Usually, the average particle size is about 0.1 μs to about 1
m aluminum nitride powder is used.
有機リン酸化合物としては、
（ＲＯ） Ｐ（０）叶又はＲＯＰ（０）（叶）２ ［
式中、Ｒは炭素数１〜１８のアルキル、アルケニル若し
くはアリール基である］で表わされる酸性リン酸エステ
ル類、例えばメチルアシッドボスフェート、エチルアシ
ッドホスフェート、ブヂルアシッドボスフエート、２−
エチルヘキシルアシッドホスフェート。As an organic phosphate compound, (RO) P(0) Kano or ROP(0) (Kano)2 [
Acidic phosphoric acid esters represented by the formula, R is an alkyl, alkenyl or aryl group having 1 to 18 carbon atoms, such as methyl acid bosphate, ethyl acid bosphate, butyl acid bosphate, 2-
Ethylhexyl acid phosphate.
ラウリルアシッドホスフェート、パルミチルアシッドホ
スフェート、ステアリルアシッドボスフェート、オレイ
ルアシッドホスフェート、フェニルアシッドホスフェー
ト、ノニルフェニルアシッドホスフェ−１・等；
ピロリン酸又はポリリン酸のモノ−若しくはジアルキル
、アルケニル又はアリールエステル類、例えばジー２−
エチルへキシルビロホスノエート等；ボスホン酸類及び
そのエステル類、例えばメチレンホスボン酸、アミノメ
チレンボスホン酸、 １−ブチルニトリロビスメチレン
ホスホン酸、ｎ−ブチルニトリロビスメチレンホスホン
酸、ニトリロトリスメチレンホスホン酸、エチレンジア
ミンテトラメチレンボスホン酸、１−ヒドロキシエチリ
デン１１−ジホスホン酸、ブチルハイドロジエンホスフ
ァイト、２−エチルへキシルハイドロジエンホスファイ
１〜．ラウリルハイドロジエンホスファイト。lauryl acid phosphate, palmityl acid phosphate, stearyl acid bosphate, oleyl acid phosphate, phenyl acid phosphate, nonylphenyl acid phosphate, etc.; mono- or dialkyl, alkenyl or aryl esters of pyrophosphoric acid or polyphosphoric acid, e.g. G2-
Ethylhexyl bilophosnoate, etc.; bosphonic acids and their esters, such as methylenephosboxic acid, aminomethylenebosphonic acid, 1-butylnitrilobismethylenephosphonic acid, n-butylnitrilobismethylenephosphonic acid, nitrilotrismethylenephosphonic acid acid, ethylenediaminetetramethylenebosphonic acid, 1-hydroxyethylidene 11-diphosphonic acid, butylhydrodiene phosphite, 2-ethylhexylhydrodiene phosphite 1-. Lauryl hydrogen phosphite.
ジブデルヒドロキシメチルホスボネート等；及びこれら
の混合物が例示される。Dibdelhydroxymethyl phosphonate, etc.; and mixtures thereof are exemplified.
有機リン酸化合物としてアルカリ金属塩を使用すること
は避けるべきである。何故ならば、該金属塩は溶剤に不
溶であり且つ金属が残留する問題が生ずるからである。The use of alkali metal salts as organophosphate compounds should be avoided. This is because the metal salt is insoluble in the solvent and there is a problem that the metal remains.
有機リン酸化合物の量は重要であり、窒化アルミニウム
粉末１００重量部に対して０．１重石部未満では所期の
効果が得られず、一方１０重量部を越えるときには窒化
アルミニウム粉末中の酸素含量が増大するので好ましく
ない。好ましくは、有機リン酸化合物を窒化アルミニウ
ム粉末１００重量部に対して０．２〜３重量部使用する
。The amount of organic phosphoric acid compound is important; if it is less than 0.1 parts by weight per 100 parts by weight of aluminum nitride powder, the desired effect will not be obtained, while if it exceeds 10 parts by weight, the oxygen content in the aluminum nitride powder will decrease. is undesirable because it increases Preferably, the organic phosphoric acid compound is used in an amount of 0.2 to 3 parts by weight per 100 parts by weight of aluminum nitride powder.
窒化アルミニウム粉末を分散ざ眩る溶剤としては、低沸
点溶剤が好ましく、エタノール、イソプロピルアルコー
ル、ブタノール等の炭素数１〜４の低級アルコールを使
用するか、又は前記低級アルコールと混和性のある中低
級アルカン（例えばｎ−ヘキサン、ｎ−オクタン又はｎ
−デカン）又はアセトンを併用してもよい。溶剤をドラ
イにする必要はないが、溶剤中に水を混入させることは
避けるべきである。As the solvent for dispersing the aluminum nitride powder, a low boiling point solvent is preferable, and a lower alcohol having 1 to 4 carbon atoms such as ethanol, isopropyl alcohol, butanol is used, or a medium-lower alcohol that is miscible with the lower alcohol is used. Alkanes (e.g. n-hexane, n-octane or n-
-decane) or acetone may be used in combination. Although it is not necessary for the solvent to be dry, mixing water into the solvent should be avoided.
前記した溶剤は、窒化アルミニウム粉末の分散溶剤と同
時に有機リン酸化合物の溶剤としても作用する。従って
、有機リン酸化合物を滴下させる際有機リン酸化合物を
窒化アルミニウム粉末を分散させたと同一の溶剤に溶解
させた状態で滴下させることが好ましい。The above-described solvent acts both as a dispersion solvent for the aluminum nitride powder and as a solvent for the organic phosphoric acid compound. Therefore, when dropping the organic phosphoric acid compound, it is preferable that the organic phosphoric acid compound is dissolved in the same solvent in which the aluminum nitride powder is dispersed.
本発明において目的とする耐水性の優れた窒化アルミニ
ウム粉末を得るためには、上記した如く窒化アルミニウ
ム粉末に特定量の有機リン酸化合物を添加して処理した
後更に加熱処理しなければならない。この加熱処理によ
り、有機リン酸化合物は熱分解され、窒化アルミニウム
粉末の表面に親水性の皮膜が形成される。加熱処理温度
は約１５０〜８００℃であり、好ましくは約３５０〜６
００℃である。加熱処理温度が１５０℃未満では有機リ
ン酸化合物の熱分解が不十分であり、一方８００℃を越
えるとぎには窒化アルミニウム粉末の酸化や凝集が生じ
易くなるので好ましくない。加熱処理雰囲気は通常大気
、真空もしくは不活性ガス雰囲気である。加熱処理時間
は有機リン酸化合物の種類や加熱処理温度に応じて約３
０分〜２４時間の範囲から選択される。In order to obtain the aluminum nitride powder with excellent water resistance, which is the object of the present invention, it is necessary to add a specific amount of an organic phosphoric acid compound to the aluminum nitride powder and then heat it. By this heat treatment, the organic phosphoric acid compound is thermally decomposed and a hydrophilic film is formed on the surface of the aluminum nitride powder. The heat treatment temperature is about 150-800°C, preferably about 350-600°C.
It is 00℃. If the heat treatment temperature is less than 150°C, thermal decomposition of the organic phosphoric acid compound will be insufficient, while if it exceeds 800°C, oxidation and agglomeration of the aluminum nitride powder will easily occur, which is not preferred. The heat treatment atmosphere is usually air, vacuum, or an inert gas atmosphere. The heat treatment time depends on the type of organic phosphoric acid compound and the heat treatment temperature.
Selected from the range of 0 minutes to 24 hours.
実施例 以下、本発明の非限定的実施例を示す。Example Below, non-limiting examples of the invention are presented.
友直璽ユ
容量１ρの容器にイソプロピルアルコール／ｎ−ヘキサ
ン（１：１）２５０＠９を導入後、窒化アルミニウム粉
末（平均粒径４．３μｓ、酸素含量０．６６％）１００
ｇを添加し、攪拌して窒化アルミニウム分散液を作成し
た。容器を湯浴上で振動させることにより、分散液を攪
拌しながら約６０℃に加温した。After introducing isopropyl alcohol/n-hexane (1:1) 250@9 into a container with a capacity of 1ρ, aluminum nitride powder (average particle size 4.3 μs, oxygen content 0.66%) 100
g was added and stirred to prepare an aluminum nitride dispersion. The dispersion was heated to about 60° C. with stirring by shaking the container on a hot water bath.
次いでブチルアシッドホスフェート３ｇをイソプロピル
アルコール／ｎ−ヘキサン（１：１）５０−に溶解させ
たものを滴下し、ゆるやかに反応させた。Next, a solution of 3 g of butyl acid phosphate dissolved in 50 parts of isopropyl alcohol/n-hexane (1:1) was added dropwise to cause a gentle reaction.
反応中に水分が系内に入らないように乾燥不活性気体を
容器に小流量で流し続けた。Dry inert gas was kept flowing through the vessel at a small flow rate to prevent moisture from entering the system during the reaction.
十分に反応させた後、大気中、５００℃で５時間加熱処
理した。After sufficient reaction, heat treatment was performed at 500° C. in the air for 5 hours.
ブチルアシッドホスフェートに代えて他の有機リン酸化
合物或いはイソプロピルアルコール又はｎ−ヘキサンに
可溶性の各種表面処理剤を使用する以外は上記と同様に
処理して、表面処理した窒化アルミニウム粉末を得た。Surface-treated aluminum nitride powder was obtained in the same manner as described above, except that other organic phosphoric acid compounds or various surface treatment agents soluble in isopropyl alcohol or n-hexane were used in place of butyl acid phosphate.
但し、有機リン酸化合物以外の表面処理剤を使用したと
きには加熱処理を行なわなかった。However, when a surface treatment agent other than an organic phosphoric acid compound was used, no heat treatment was performed.
こうして表面処理した窒化アルミニウム粉末の耐水性を
次のようにして試験した。The water resistance of the aluminum nitride powder thus surface-treated was tested as follows.
窒化アルミニウム粉末４．１ｇを８０℃に加熱した純水
（ｐＨ＃５．６） ５４ｇに添加し、攪拌混合して窒化
アルミニウム分散液を作成し、窒化アルミニウム分散液
の経時的ｐＨ（８０℃）変化をｐＨ試験紙を用いて調べ
た。4.1 g of aluminum nitride powder was added to 54 g of pure water (pH #5.6) heated to 80°C, stirred and mixed to create an aluminum nitride dispersion, and the pH of the aluminum nitride dispersion over time (80°C) Changes were examined using pH test paper.
結果を以下の表に示す。The results are shown in the table below.
表から明らかな通り、有機リン酸化合物で処理後加熱処
理した窒化アルミニウム粉末の場合には分散液を作成し
てから少なくとも２時間後でもｐＨの変化が全く乃至殆
んど認められないが、それ以外の表面処理剤で処理した
窒化アルミニウム粉末の場合には分散液を作成してから
１０〜３０分後にｐｌ＋は９．６以上に達し、アンモニ
ア臭も検知された。As is clear from the table, in the case of aluminum nitride powder that has been treated with an organic phosphoric acid compound and then heat-treated, no or almost no change in pH is observed even at least 2 hours after the dispersion is prepared; In the case of aluminum nitride powder treated with other surface treatment agents, pl+ reached 9.6 or more 10 to 30 minutes after the dispersion was prepared, and an ammonia odor was also detected.
なお、ブチルアシッドホスフェートで処理するが後続の
加熱処理を行なわなかった場合には分散液を作成してか
ら３０分後のｐＨが既に９．６以上に達し、またβ（３
，４−エポキシシクロヘキシル）エヂルトリメトキシシ
ランで処理後本発明と同様に大気中、５００℃で５時間
加熱処理したとしても水溶液を作成してから １時間後
にｐＨが９．６以上に達した。このことから、本発明に
おいて有機リン酸化合物による処理と加熱処理との組合
せが非常に重要であることが明らかである。In addition, in the case of treatment with butyl acid phosphate but no subsequent heat treatment, the pH already reached 9.6 or higher 30 minutes after preparing the dispersion, and β(3
, 4-epoxycyclohexyl) ethyltrimethoxysilane, and then heat-treated in the air at 500° C. for 5 hours as in the present invention, the pH reached 9.6 or higher 1 hour after the aqueous solution was prepared. From this, it is clear that the combination of treatment with an organic phosphoric acid compound and heat treatment is very important in the present invention.
実施例２
容量１ｐのエバポレータ用フラスコにイソプロピルアル
コール２００ｄを導入後、窒化アルミニウム粉末（平均
粒径１．１μｓ、酸素含量１．３９％）１００びを添加
し、攪拌して窒化アルミニウム分散液を作成した。次い
でブチルアシッドホスフェ−１−０，５ｇをイソプロピ
ルアルコール５０Ｉｄに溶解したものを添加し、フラス
コを湯浴上で回転させることにより、分散液を攪拌しな
がら約６０℃の加温下でゆるやかに反応させた。Example 2 After introducing 200 d of isopropyl alcohol into an evaporator flask with a capacity of 1 p, 100 d of aluminum nitride powder (average particle size 1.1 μs, oxygen content 1.39%) was added and stirred to create an aluminum nitride dispersion. did. Next, 0.5 g of butyl acid phosphate 1-1 dissolved in 50 Id of isopropyl alcohol was added, and the flask was rotated on a hot water bath to gently stir the dispersion while heating to about 60°C. Made it react.
十分反応させた後、ｐＨ試験紙でｐｌ＋ ４．５以上に
なっているのを確認し、真空ポンプによってイソプロピ
ルアルコールを揮発させた。十分に揮発させた後、大気
中４５０℃で１時間加熱処押した。After sufficient reaction, it was confirmed with a pH test paper that pl+ was 4.5 or higher, and the isopropyl alcohol was evaporated using a vacuum pump. After sufficient volatilization, the mixture was heated in the air at 450° C. for 1 hour.
こうして得られた窒化アルミニウム粉末の耐水性を実施
例１の方法に従って試験したところ、分散液を作成して
から１２時間後にｐＨは９．６以上に達し、未処理の窒
化アルミニウム粉末の場合には上記の如くして得られた
窒化アルミニウムの耐水性を別の方法で試験すべく、窒
化アルミニウム粉末の加熱処理直後及び４０℃の水に５
時間浸漬させた後の酸素含量の変化を■堀場製作所製セ
ラミック中酸素窒素分析計ＥＨＧＡ−２８００を用いて
測定した。加熱直後の窒化アルミニウム粉末の酸素含量
は１．７７％であり、４０℃の水に５時間浸漬させた後
の酸素含量は１，７４％であり、ブチルアシッドホスフ
ェートで表面処理後加熱処理された窒化アルミニウム粉
末を４０℃の水に浸漬させても酸素含量の変化は認めら
れなかった。一方、未処理の窒化アルミニウム粉末を同
一条件で水に浸漬させたところ、酸素含量は２０．４％
に増大した。When the water resistance of the aluminum nitride powder thus obtained was tested according to the method of Example 1, the pH reached 9.6 or higher 12 hours after preparing the dispersion, and in the case of untreated aluminum nitride powder, In order to test the water resistance of the aluminum nitride obtained as described above using another method, aluminum nitride powder was immersed in water at 40°C immediately after heat treatment and
Changes in oxygen content after immersion for a time were measured using a ceramic oxygen nitrogen analyzer EHGA-2800 manufactured by Horiba, Ltd. The oxygen content of the aluminum nitride powder immediately after heating is 1.77%, and the oxygen content after being immersed in 40 °C water for 5 hours is 1.74%, and the aluminum nitride powder is heated after surface treatment with butyl acid phosphate. No change in oxygen content was observed even when aluminum nitride powder was immersed in water at 40°C. On the other hand, when untreated aluminum nitride powder was immersed in water under the same conditions, the oxygen content was 20.4%.
It increased to
上記の表面処理後加熱処理した窒化アルミニウム粉末に
焼結助剤として５％の酸化イツトリウム、水溶性アクリ
ルバインダー（中央理化工業■製、ＥＳＺ−１３１１、
固型分４２％）を固型分として３％、解膠剤として１％
のアクリル系オリゴマーのアンモニウム塩（アロンＡ−
６１１４＞及び適量の水をボールミル中で１時間半混合
し、混合物を真空脱泡して固型分７０％の水スラリーを
調製した。得られたスラリーをドクターブレード法を用
いてシート状に成形し、４８時間乾燥して厚さ０．８膿
の窒化アルミニウムグリーンシートを得た。ついで、得
られたシートを脱脂して、１８５０℃で３時間常圧焼結
した板は、レーザーフラッシュ法熱定数測定装＠（理学
電機■製、ＬＦ／ＴＣＨ−８５１０）で測定したところ
、窒化アルミニウム粉末中の酸素含量がかなり多いにも
かかわらず、高い熱伝導率（１５４Ｗ／ｍに）を示した
。この値は未処理の窒化アルミニウム粉末を同一条件下
で焼結した板の熱伝導率（１４７Ｗ／ｍＫ）とほぼ同じ
値であり、処理被膜の熱伝導率への影響が小さいことが
確認された。After the above surface treatment, heat-treated aluminum nitride powder was added with 5% yttrium oxide as a sintering aid, water-soluble acrylic binder (manufactured by Chuo Rika Kogyo ■, ESZ-1311,
Solid content: 42%), 3% as solid content, 1% as deflocculant
Ammonium salt of acrylic oligomer (Aron A-
6114> and an appropriate amount of water were mixed in a ball mill for 1.5 hours, and the mixture was vacuum defoamed to prepare a water slurry with a solids content of 70%. The obtained slurry was formed into a sheet using a doctor blade method and dried for 48 hours to obtain an aluminum nitride green sheet with a thickness of 0.8 mm. Next, the obtained sheet was degreased and sintered at 1850°C for 3 hours under normal pressure.The plate was measured with a laser flash method thermal constant measurement device @ (manufactured by Rigaku Denki ■, LF/TCH-8510), and it was found that nitridation was detected. Despite the fairly high oxygen content in the aluminum powder, it showed high thermal conductivity (up to 154 W/m). This value is almost the same as the thermal conductivity (147 W/mK) of a plate made of untreated aluminum nitride powder sintered under the same conditions, confirming that the effect of the treated film on the thermal conductivity is small. .
なお、焼結板のＰ含量を調べるため、少量の焼結板を濃
塩酸中で加圧加熱分解させ、溶出液を１ＣＰ （Ｉｎｄ
ｕｃｔｉｖｅ Ｃｏｕｐｌｅｄ Ｐｌａｓｍａ 、高周
波誘導結合）発光分析したところ、Ｐ含量は殆んど無い
（５０ｐｐｍ以下）ことが判明した。In order to investigate the P content of the sintered plate, a small amount of the sintered plate was decomposed under pressure and heat in concentrated hydrochloric acid, and the eluate was 1CP (Ind
As a result of optical emission analysis (active coupled plasma, high frequency inductive coupling), it was found that there was almost no P content (less than 50 ppm).
実施例３
容量２ｆｌのアルミナ製ポットに１０＃φ高純度アルミ
ナボール３．７５に９ （８５容量％）を導入後、窒化
アルミニウム粉末（平均粒径４．３μｓ、酸素含量０．
６６％） ３９０ｇを添加し、次いでブチルアシッド
ホスフェート２ｇを添加し、中央化工機■製バッチ式振
動ミルで５時間粉砕し、粉砕によって細かくなった窒化
アルミニウム粉末を大気中４５０℃で１時間加熱処理し
た。Example 3 After introducing 10#φ high-purity alumina balls 3.75 to 9 (85% by volume) into an alumina pot with a capacity of 2 fl, aluminum nitride powder (average particle size 4.3 μs, oxygen content 0.75%) was introduced.
66%), then 2 g of butyl acid phosphate was added, and the mixture was ground for 5 hours in a batch-type vibration mill manufactured by Chuo Kakoki ■.The aluminum nitride powder made fine by the grinding was heat-treated at 450°C in the atmosphere for 1 hour. did.
こうして得られた窒化アルミニウム粉末（平均粒径１．
２ＩＪ！ＩＩ、酸素含量０．６６％）の耐水性を次のよ
うにして試験した。The aluminum nitride powder thus obtained (average particle size: 1.
2IJ! II, oxygen content 0.66%) was tested for water resistance as follows.
窒化アルミニウム粉末４．１ｇを４０℃に加熱した純水
（Ｆ）Ｈ！＝； ５．６） ５４ｇに添加し、攪拌混合
して窒化アルミニウム分散液を作成し、実施例１と同様
にして経時的ｐＨ（４０℃）変化をｐＨ試験紙を用いて
調べた。この結果ｐＨは９．６以上に達し、アンモニア
臭が検知されるまでに１２時間経過した。これに対して
、加熱処理を行なっていない窒化アルミニウム粉末の場
合は１．５時間後にｐＨが９．６以上に達し、アンモニ
ア臭も検知された。Pure water (F)H! in which 4.1 g of aluminum nitride powder was heated to 40°C. =; 5.6) was added to 54 g and stirred and mixed to prepare an aluminum nitride dispersion, and in the same manner as in Example 1, the change in pH (at 40° C.) over time was examined using pH test paper. As a result, the pH reached 9.6 or higher, and 12 hours passed before an ammonia odor was detected. On the other hand, in the case of aluminum nitride powder that had not been heat-treated, the pH reached 9.6 or higher after 1.5 hours, and an ammonia odor was also detected.
発明の効果
本発明の有機リン酸化合物で処理後加熱処理された窒化
アルミニウム粉末は優れた耐水性を有しているので、貯
蔵・取扱い中にアンモニアが発生したり、酸素含量が増
大する恐れはない。また、本発明の窒化アルミニウム粉
末は殆んど凝集することもないので、ＩＣ用封止材や樹
脂混線用フィラーとして好適に使用され得る。Effects of the Invention The aluminum nitride powder that has been heat-treated after being treated with the organophosphate compound of the present invention has excellent water resistance, so there is no possibility that ammonia will be generated or the oxygen content will increase during storage and handling. do not have. Furthermore, since the aluminum nitride powder of the present invention hardly aggregates, it can be suitably used as an IC sealing material or a filler for resin cross-wires.
本発明の窒化アルミニウム粉末は耐水性に優れているの
で焼結体を製造する際に成形媒体として水を使用するこ
とが可能であることに加えて、表面に親水性の皮膜が形
成されているので水分散性の点でも優れているので、窒
化アルミニウム焼結体を製造するとき各種成形方法を利
用できる。また、成形媒体として水を使用しても原料の
窒化アルミニウム粉末の酸素含量が増大することがない
ので、所望の熱伝導度を有する焼結体を製造することが
できる。従って、本発明の窒化アルミニウム粉末は窒化
アルミニウム焼結体の製造原料として好適である。The aluminum nitride powder of the present invention has excellent water resistance, so water can be used as a molding medium when producing a sintered body, and a hydrophilic film is formed on the surface. Therefore, it has excellent water dispersibility, so various molding methods can be used when producing aluminum nitride sintered bodies. Further, even if water is used as a molding medium, the oxygen content of the raw material aluminum nitride powder does not increase, so a sintered body having a desired thermal conductivity can be produced. Therefore, the aluminum nitride powder of the present invention is suitable as a raw material for producing aluminum nitride sintered bodies.
更に、本発明の窒化アルミニウム粉末は特別の製造工程
を必要としないので安価に得ることがで２、Furthermore, the aluminum nitride powder of the present invention does not require any special manufacturing process, so it can be obtained at low cost.
Claims (1)
ム粉末１００重量部当り０．１〜１０重量部の有機リン
酸化合物を添加して処理した後、約１５０〜８００℃の
温度で加熱処理することを特徴とする窒化アルミニウム
粉末の表面処理方法。(1) The aluminum nitride powder is treated by adding 0.1 to 10 parts by weight of an organic phosphoric acid compound per 100 parts by weight of the aluminum nitride powder, and then heat-treated at a temperature of about 150 to 800°C. A method for surface treatment of aluminum nitride powder.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1183886A JP2675149B2 (en) | 1988-08-01 | 1989-07-17 | Surface treatment method for aluminum nitride powder |
| US07/381,066 US4923689A (en) | 1988-08-01 | 1989-07-18 | Aluminum nitride power having improved water-resistance |
| DE3925338A DE3925338C2 (en) | 1988-08-01 | 1989-07-31 | Aluminum nitride powder with improved water resistance |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63-192266 | 1988-08-01 | ||
| JP19226688 | 1988-08-01 | ||
| JP1183886A JP2675149B2 (en) | 1988-08-01 | 1989-07-17 | Surface treatment method for aluminum nitride powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02141410A true JPH02141410A (en) | 1990-05-30 |
| JP2675149B2 JP2675149B2 (en) | 1997-11-12 |
Family
ID=26502159
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1183886A Expired - Lifetime JP2675149B2 (en) | 1988-08-01 | 1989-07-17 | Surface treatment method for aluminum nitride powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2675149B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012147999A1 (en) * | 2011-04-28 | 2012-11-01 | 株式会社トクヤマ | Method for producing water-resistant aluminum nitride |
| WO2015133037A1 (en) * | 2014-03-04 | 2015-09-11 | 日東電工株式会社 | Aluminum nitride powder, resin composition, and thermally conductive molded object |
-
1989
- 1989-07-17 JP JP1183886A patent/JP2675149B2/en not_active Expired - Lifetime
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012147999A1 (en) * | 2011-04-28 | 2012-11-01 | 株式会社トクヤマ | Method for producing water-resistant aluminum nitride |
| JPWO2012147999A1 (en) * | 2011-04-28 | 2014-07-28 | 株式会社トクヤマ | Method for producing water-resistant aluminum nitride |
| JP5965899B2 (en) * | 2011-04-28 | 2016-08-10 | 株式会社トクヤマ | Method for producing water-resistant aluminum nitride |
| WO2015133037A1 (en) * | 2014-03-04 | 2015-09-11 | 日東電工株式会社 | Aluminum nitride powder, resin composition, and thermally conductive molded object |
| JP2015166301A (en) * | 2014-03-04 | 2015-09-24 | 日東電工株式会社 | Aluminum nitride powder, resin composition, and thermally conductive molded object |
| KR20160129849A (en) | 2014-03-04 | 2016-11-09 | 닛토덴코 가부시키가이샤 | Aluminum nitride powder, resin composition, and thermally conductive molded object |
| US9663635B2 (en) | 2014-03-04 | 2017-05-30 | Nitto Denko Corporation | Aluminum nitride powder, resin composition, and thermally conductive molded object |
| EP3115337A4 (en) * | 2014-03-04 | 2017-08-09 | Nitto Denko Corporation | Aluminum nitride powder, resin composition, and thermally conductive molded object |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2675149B2 (en) | 1997-11-12 |
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