JP2006188411A - 窒化ホウ素の製造方法 - Google Patents
窒化ホウ素の製造方法 Download PDFInfo
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- JP2006188411A JP2006188411A JP2005339765A JP2005339765A JP2006188411A JP 2006188411 A JP2006188411 A JP 2006188411A JP 2005339765 A JP2005339765 A JP 2005339765A JP 2005339765 A JP2005339765 A JP 2005339765A JP 2006188411 A JP2006188411 A JP 2006188411A
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- lithium
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- boron nitride
- oxide
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Abstract
【解決手段】 六方晶窒化ホウ素化合物の製造方法であって、当該方法が、酸素含有ホウ素化合物を窒素含有源と、ドーパントとして用いられる1種以上の化合物の存在下1000℃以上の処理温度で、1時間以上反応させて六方晶窒化ホウ素化合物を形成する工程を含み、上記ドーパントが上記処理温度よりも気化温度の低い金属ホウ酸塩を形成する金属化合物である方法。
【選択図】 なし
Description
窒化ホウ素の製造方法では、一般に、ホウ素源と窒素源とを出発原料として使用し、これらを反応させてホウ素原子と窒素原子が共存する化合物を形成する。本発明は高純度窒化ホウ素の製造方法であって、高温での反応において、酸素含有ホウ素化合物及び有機窒素含有化合物の出発原料にドーパントを混合する方法に関する。反応中にドーパント金属から形成される金属ホウ酸塩が気化するので、浸出や洗浄によって除去する必要がない。
本発明のhBN製造方法は、後述の処理工程を含む回分法又は連続法のいずれとしても実施できる。
最初の工程では、ドーパントを含む出発原料をブレンダーのような適当な装置で乾燥状態で互いに混合又はブレンドする。
本発明の一実施形態では、混合/ブレンド工程後に、出発原料を約100〜400℃の温度で0.5〜15時間乾燥して反応体中の水分を駆逐し、原料間に多孔性を生じさせ、ナゲット、チャンク又はペレットの形態の集合体を形成する。
一実施形態では、混合/ブレンド工程後又は乾燥工程後に、ローラーミル、クロスビーターミル、ローリングディスクなどの慣用装置を用いて、出発原料を粗粉砕又は破砕して、後で緻密化できる小粒とする。一実施形態では、粗粉砕材料を1個当たり10mg〜10gの重量の小粒に破砕する。別の実施形態では、材料を1個当たり約0.2gの重量の小粒に破砕する。
一実施形態では、混合/ブレンド工程後に、混合前駆体を乾燥、粉砕し、当技術分野で周知の方法、例えば、特にタブレット形成、ブリケット形成、押出、ピル形成及び圧縮成形によって緻密化する。この工程で、粉砕混合物を緻密化して、1個当たり0.1g〜200gの重量のペレットにする。一実施形態では、ペレットの平均重量は10g程度である。第二の実施形態では、粉砕混合物を平均重量約2gのペレットに緻密化する。
次の工程では、ペレットを反応室内にて窒素雰囲気中で焼成する。反応室を室温から20〜1200℃/時の速度で1200〜2300℃の高温まで加熱する。その後プロセス温度を約1〜30時間保持し、この間窒素パージを非酸化性雰囲気を持続するのに十分な速度で維持する。
最後に、焼成ペレットの反応生成物を適宜適温に冷却した後、ジェットミルプロセスで粉砕して寸法0.1〜60μmのプレートレットの形態の高純度窒化ホウ素生成物とする。一実施形態では、反応生成物を微粉砕して平均粒径1〜5μmの粉末とする。各粒子はこのような寸法ではなく、緩く結合した微細サブミクロン微結晶の集塊であるので、上記粒径は呼称寸法である。
上述の通り、本発明の方法の窒化ホウ素生成物は十分高純度であるので、酸洗浄/浸出は不要である。しかし、本発明の一実施形態では、卓越した純度の窒化ホウ素生成物を得るための任意工程として、生成物を洗浄処理に付してもよい。一実施形態では、最終BN生成物をメタノールや1%硝酸水溶液のような溶剤で洗浄して、微細な白色高純度結晶性窒化ホウ素粉末を得る。
本発明の高純度窒化ホウ素粉末は、例えば複合材料、ポリマー、グリース、流体などの熱制御用途のための充填剤として用いることができる。窒化ホウ素粉末は、ホットプレス用途、或いは六方晶窒化ホウ素を立方晶窒化ホウ素(cBN)に変換する際の前駆体供給原料として使用することもできる。別の実施形態では、本材料を六方晶窒化ホウ素ペーストの調製に使用する。本明細書において、ペーストとは半固形標品である。この方法では、窒化ホウ素スラリーを形成し、スラリーを適当な条件下で処理して、約60〜約80重量%の固体六方晶窒化ホウ素を含有する窒化ホウ素ペーストを生成する。
メラミン及びホウ酸を23:27の重量比で含有する4つの試料を製造した。例1はメラミンとホウ酸しか含んでおらず、実施例2はほかに1.5重量%の硝酸リチウムを含んでおり、実施例3は3.0重量%の硝酸リチウムを含んでおり、実施例4は5.0重量%の硝酸リチウムを含んでいる。これらの試料すべてを275℃で一晩乾燥する。次に乾燥材料をプレスして円筒形ピルとし、窒素中500℃/時の速度で室温から1800℃に焼成し、3時間保持する。4つの例で製造したピルを、分析のために秤量し、ボールミルで粉砕する。試料パッドを作製し、熱伝導率を測定する。
Claims (26)
- 六方晶窒化ホウ素化合物の製造方法であって、当該方法が、
酸素含有ホウ素化合物を窒素含有源と、ドーパントとして用いられる1種以上の化合物の存在下1000℃以上の処理温度で、1時間以上反応させて六方晶窒化ホウ素化合物を形成する工程を含み、
上記ドーパントが、上記処理温度よりも気化温度の低い金属ホウ酸塩を形成する金属化合物である、方法。 - 六方晶窒化ホウ素化合物の熱伝導度が1.5W/mK以上である、請求項1記載の方法。
- 六方晶窒化ホウ素化合物の熱伝導度が3W/mK以上である、請求項1記載の方法。
- 六方晶窒化ホウ素化合物の熱伝導度が5W/mK以上である、請求項1記載の方法。
- 酸素含有ホウ素化合物を窒素含有源とドーパントの存在下1000〜2300℃の範囲の処理温度で反応させる、請求項1記載の方法。
- 前記処理温度が1500℃以上である、請求項5記載の方法。
- 前記処理温度が1800℃以上である、請求項6記載の方法。
- 酸素含有ホウ素化合物を窒素含有源とドーパントの存在下1000〜2300℃の範囲の処理温度で72時間以内の期間反応させる、請求項5記載の方法。
- 前記反応を30時間以内の期間実施する、請求項8記載の方法。
- 前記反応を12時間以内の期間実施する、請求項9記載の方法。
- 前記反応を6時間以内の期間実施する、請求項10記載の方法。
- 前記ドーパントが、バリウム化合物、セシウム化合物、カリウム化合物、ストロンチウム化合物、ルビジウム化合物、硝酸リチウム、酸化リチウム、アセチルアセトナトリチウム、リチウムシクロペンタジエナイド、ジリチウムフタロシアニン、二リチウム塩、酢酸リチウム、アセチルアセトナトリチウム、リチウムアミド、リチウムビス(トリメチルシリル)アミド、テトラヒドリドホウ酸リチウム、炭酸リチウム、リチウムジメチルアミド、水素化リチウム、水酸化リチウム、メタホウ酸リチウム、モリブデン酸リチウム、ニオブ酸リチウム、過塩素酸リチウム、過酸化リチウム、テトラホウ酸リチウム、ホウ水素化リチウム、トリエチルヒドリドホウ酸リチウム、シュウ酸リチウム及びこれらの混合物からなる群から選択される、請求項1記載の方法。
- 前記ドーパントが、酸化バリウム、硝酸バリウム、酸化セシウム、硝酸セシウム、水酸化カリウム、酸化ストロンチウム、硝酸ストロンチウム、酸化ルビジウム、窒化ルビジウム、硝酸リチウム、酸化リチウム、アセチルアセトナトリチウム、リチウムシクロペンタジエナイド、ジリチウムフタロシアニン、二リチウム塩、酢酸リチウム、アセチルアセトナトリチウム、リチウムアミド、リチウムビス(トリメチルシリル)アミド、テトラヒドリドホウ酸リチウム、炭酸リチウム、リチウムジメチルアミド、水素化リチウム、水酸化リチウム、メタホウ酸リチウム、モリブデン酸リチウム、ニオブ酸リチウム、過塩素酸リチウム、過酸化リチウム、テトラホウ酸リチウム、ホウ水素化リチウム、トリエチルヒドリドホウ酸リチウム、シュウ酸リチウム及びこれらの混合物からなる群から選択される、請求項12記載の方法。
- 前記ドーパントが酸素含有ホウ素化合物と窒素含有源の総重量の1重量%以上の量で存在する、請求項12記載の方法。
- 前記ドーパントが、酸化バリウム、酸化セシウム、水酸化カリウム、酸化ストロンチウム、酸化ルビジウム、硝酸リチウム及びこれらの混合物からなる群から選択される、請求項12記載の方法。
- 前記ドーパントが硝酸リチウムであり、ドーパントの存在量が酸素含有ホウ素化合物と窒素含有源の総重量の1重量%以上である、請求項13記載の方法。
- 前記ドーパントが硝酸リチウムであり、ドーパントの存在量が酸素含有ホウ素化合物と窒素含有源の総重量の2重量%以上である、請求項16記載の方法。
- 前記ドーパントが、硝酸リチウム、酸化リチウム、アセチルアセトナトリチウム、リチウムシクロペンタジエナイド、ジリチウムフタロシアニン、二リチウム塩、酢酸リチウム、アセチルアセトナトリチウム、リチウムアミド、リチウムビス(トリメチルシリル)アミド、テトラヒドリドホウ酸リチウム、炭酸リチウム、リチウムジメチルアミド、水素化リチウム、水酸化リチウム、メタホウ酸リチウム、モリブデン酸リチウム、ニオブ酸リチウム、過塩素酸リチウム、過酸化リチウム、テトラホウ酸リチウム、ホウ水素化リチウム、トリエチルヒドリドホウ酸リチウム、シュウ酸リチウム及びこれらの混合物から選択される、請求項13記載の方法。
- 前記ドーパントが、硝酸リチウム、酸化リチウム、炭酸リチウム、水素化リチウム、水酸化リチウム、メタホウ酸リチウム、過酸化リチウム、テトラホウ酸リチウム、ホウ水素化リチウム及びこれらの混合物から選択される、請求項18記載の方法。
- 前記ドーパントが硝酸リチウムである、請求項19記載の方法。
- 当該方法が連続法である、請求項1記載の方法。
- 請求項1記載の方法で製造した六方晶窒化ホウ素化合物。
- 請求項1記載の方法で製造した六方晶窒化ホウ素化合物を含有する物品。
- 六方晶窒化ホウ素化合物の製造方法であって、当該方法が、
(a)酸素含有ホウ素化合物、窒素含有源及びドーパントの混合物であって、ドーパントが酸素含有ホウ素化合物と窒素含有源の総重量の1重量%以上の量で存在する混合物を形成し、
(b)上記混合物を200℃以上の温度に0.5時間以上加熱して混合物中の水分を除去し、
(c)混合物を1200℃以上の処理温度に1時間以上付して六方晶窒化ホウ素化合物を形成する工程を含み、
前記ドーパントが上記処理温度よりも気化温度の低い金属ホウ酸塩を形成する金属化合物である、方法。 - 形成された生成物が99%以上の窒化ホウ素の純度を有する、請求項24記載の方法。
- 本質的に工程(a)及び(c)のみからなる、請求項24記載の六方晶窒化ホウ素化合物の製造方法。
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- 2005-11-23 DE DE602005027169T patent/DE602005027169D1/de active Active
- 2005-11-25 JP JP2005339765A patent/JP2006188411A/ja active Pending
- 2005-11-28 TW TW094141734A patent/TW200630295A/zh unknown
- 2005-11-29 KR KR1020050114671A patent/KR101285424B1/ko active IP Right Grant
- 2005-11-30 CN CNA2005101363840A patent/CN1799992A/zh active Pending
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2020179662A1 (ja) | 2019-03-01 | 2020-09-10 | 株式会社トクヤマ | 六方晶窒化ホウ素粉末、樹脂組成物、樹脂シートおよび六方晶窒化ホウ素粉末の製造方法 |
KR20210132639A (ko) | 2019-03-01 | 2021-11-04 | 가부시끼가이샤 도꾸야마 | 육방정 질화붕소 분말, 수지 조성물, 수지 시트 및 육방정 질화붕소 분말의 제조 방법 |
Also Published As
Publication number | Publication date |
---|---|
EP1676812A3 (en) | 2006-10-25 |
US7341702B2 (en) | 2008-03-11 |
KR20060092997A (ko) | 2006-08-23 |
KR101285424B1 (ko) | 2013-07-12 |
TW200630295A (en) | 2006-09-01 |
CN1799992A (zh) | 2006-07-12 |
EP1676812B1 (en) | 2011-03-30 |
EP1676812A2 (en) | 2006-07-05 |
DE602005027169D1 (de) | 2011-05-12 |
US20060140838A1 (en) | 2006-06-29 |
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