JP5947297B2 - 炭素素材を用いた高効率放熱塗料組成物 - Google Patents
炭素素材を用いた高効率放熱塗料組成物 Download PDFInfo
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- JP5947297B2 JP5947297B2 JP2013523098A JP2013523098A JP5947297B2 JP 5947297 B2 JP5947297 B2 JP 5947297B2 JP 2013523098 A JP2013523098 A JP 2013523098A JP 2013523098 A JP2013523098 A JP 2013523098A JP 5947297 B2 JP5947297 B2 JP 5947297B2
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- 238000000926 separation method Methods 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 125000003011 styrenyl group Chemical group [H]\C(*)=C(/[H])C1=C([H])C([H])=C([H])C([H])=C1[H] 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- FRGPKMWIYVTFIQ-UHFFFAOYSA-N triethoxy(3-isocyanatopropyl)silane Chemical compound CCO[Si](OCC)(OCC)CCCN=C=O FRGPKMWIYVTFIQ-UHFFFAOYSA-N 0.000 description 1
- JXUKBNICSRJFAP-UHFFFAOYSA-N triethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCOCC1CO1 JXUKBNICSRJFAP-UHFFFAOYSA-N 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
- ZVWKZXLXHLZXLS-UHFFFAOYSA-N zirconium nitride Chemical compound [Zr]#N ZVWKZXLXHLZXLS-UHFFFAOYSA-N 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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Description
本発明の表面改質した炭素素材を含む分散液は、表面改質した炭素素材とアクリル系樹脂共重合体高分子とを用いた分散性が向上した水系または溶剤系の分散液であり、第1放熱塗料組成物は、前記表面改質した炭素素材を含む分散液と耐熱性添加剤である金属酸化物とを含む水系または溶剤系の分散液であり、第2放熱塗料組成物は、前記第1放熱塗料組成物に基材であるアルミニウム放熱板などとの接着性を向上させるために、粘着性向上エマルションが含まれた水系または溶剤系の分散液である。また、第3放熱塗料組成物は、前記第1放熱塗料組成物に絶縁性を付与するために、絶縁性添加剤をさらに含んだ水系または溶剤系の分散液である。また、第4放熱塗料組成物は、前記第2放熱塗料組成物に絶縁性を付与するために、絶縁性添加剤をさらに含んだ水系または溶剤系の分散液である。
本発明の第1放熱塗料組成物は、表面改質した炭素素材を含む分散液80〜99重量%と、耐熱性添加剤1〜20重量%とを含む。前記耐熱性添加剤の含量が1重量%未満で用いられる場合は、耐熱性が十分に増加しないために放熱性の向上効果が微弱であり、20重量%を超過して用いられる場合は、炭素素材の熱伝導性および熱放射率の効果が低下する。
第2放熱塗料組成物は、表面改質した炭素素材を含む分散液80〜95重量%と、耐熱性添加剤1〜15重量%と、粘着性向上エマルション1〜10重量%とを混合して用いる。前記粘着性向上エマルションの場合、1重量%未満で含む場合は、付着力が向上する効果が微弱であり、10重量%を超過する場合は、むしろ放熱効果が低下するので好ましくない。
本発明の第3放熱組成物は、前記第1放熱塗料組成物100重量部に対し、前記絶縁性添加剤を50〜150重量部で含む。
1)付着性評価
テープテスト(JIS D0202)方法によって測定した。放熱塗料がコーティングされたアルミニウム放熱板に横、縦1mm間隔で碁盤模様の目をカッティングし、セロハンテープを接着してから剥がれた時に発生する離脱現象を観測する。M6は正方形セルが全部剥がれたものであり、M5<M4<M3<M2<M1まで次第に強い付着性を評価する。例えば、M3は、直線に沿って剥がれることが認められ、正方形セルの正方形塗膜が50%以上剥がれたものがあってはならないレベルであり、M2は、コーナー部の破れが全体に現れ、直線に沿った剥がれはなく、正方形セルの正方形塗膜が50%以上剥がれたものがあってはならないレベルである。
Heating roll test方法によって測定した(図2参照)。下段のゴムロールと上段の金属ヒーティングロールとからなり、この二つを同時にローリングしつつ、上段のヒーティングロールに20〜350℃まで10℃間隔で温度を上げる。放熱塗料がコーティングされたコーティング面をヒーティングロールの面に向かうようにし、二つのロールの間を通過する時にヒーティングロール面にコーティング部分が転写されるか否かを確認する。この方法によってコーティング面の状態とヒーティングロールに転写されることで耐熱性を評価する。
表面抵抗測定方法(JIS K7194、ASTM D257)によって測定した。試料は5x8cmの大きさに切断し、9部分に区画を分けて測定する。探針が4個である4端子法を利用して10〜1000voltの電圧を印加した後、最大限に接触抵抗を排除することによって試料固有の表面抵抗を求めることができる。絶縁性は105Ω/sq以上の表面抵抗を示すことで評価した。
表面改質した炭素素材を含む分散液の製造
炭素ナノチューブ(CNT)15gを蒸留水985gと循環ポンプで混合し、前処理槽においてCNT水溶液を準備した。前記CNT溶液を高圧注入ポンプを介して30g/min流速で予熱槽に投入される前、これと共に252atmで圧縮された気相状態の酸素は、熱交換器の前端において0.8g/minの流速でCNT溶液と混合され、前記混合液は、熱交換器を介して200℃に予熱された予熱槽に投入した。前記予熱された混合液は、210℃および250atmの亜臨界水状態の表面改質反応器に注入して表面改質し、前記表面改質した生成物は再び熱交換器に移送して100℃に1次冷却した後、再び冷却装置を介して約25℃の温度に冷却した後、連続的に表面改質された14.3gのCNTを得た。
耐熱性添加剤の製造
前記製造例1で製造された分散液90重量%と耐熱性金属酸化物として酸化亜鉛を含むアルカリ水溶性樹脂エマルション10重量%とを用いて、耐熱性添加剤を製造した。
粘着性向上エマルションの製造
水54.9重量%、27%アンモニア水0.2重量%、固形分としてアクリル系樹脂(重量平均分子量15,000)44.9重量%を混合して製造した。
絶縁性添加剤の製造
テトラプロピルジルコネート(100ml)とエチルアセトアセテート(100ml)を混合した後、硝酸溶液(17ml)を後添して、ジルコニアゾルを製造した。
第1放熱塗料組成物1の製造
前記製造例1で製造した第1放熱塗料組成物80重量%と製造例2で製造した耐熱性添加剤20重量%とを混合して、第1放熱塗料組成物1を製造した。
第1放熱塗料組成物2の製造
前記製造例1で製造した第1放熱塗料組成物90重量%と製造例2で製造した耐熱性添加剤10重量%とを混合して、第1放熱塗料組成物2を製造した。
第1放熱塗料組成物3の製造
前記製造例1で製造した第1放熱塗料組成物99重量%と製造例2で製造した耐熱性添加剤1重量%とを混合して、第1放熱塗料組成物3を製造した。
第2放熱塗料組成物1の製造
前記製造例1で製造した第1放熱塗料組成物80重量%と製造例2で製造した耐熱性添加剤10重量%および製造例3で製造した粘着性向上エマルション10重量%を混合して、第2放熱塗料組成物1を製造した。
第2放熱塗料組成物2の製造
前記製造例1で製造した第1放熱塗料組成物85重量%と製造例2で製造した耐熱性添加剤10重量%および製造例3で製造した粘着性向上エマルション5重量%を混合して、第2放熱塗料組成物2を製造した。
第2放熱塗料組成物3の製造
前記製造例1で製造した第1放熱塗料組成物84重量%と製造例2で製造した耐熱性添加剤15重量%および製造例3で製造した粘着性向上エマルション1重量%を混合して、第2放熱塗料組成物1を製造した。
第3放熱塗料組成物の製造
前記実施例1〜3で製造された放熱塗料組成物100重量部に対し、製造例4で製造された絶縁性添加剤を80重量部添加して、第3放熱塗料組成物を製造した。
第4放熱塗料組成物の製造
前記実施例4〜6で製造された放熱塗料組成物100重量部に対し、製造例4で製造された絶縁性添加剤を80重量部添加して、第4放熱塗料組成物を製造した。
前記製造例2で製造された耐熱性添加剤70重量%と粘着性向上エマルション30重量%とを混合して用いた。製造された放熱塗料組成物の物性を測定して、下記表2に示す。
前記製造例1で製造した分散液90重量%と製造例3で製造した粘着性向上エマルション10重量%とを混合して用いた。製造された放熱塗料組成物の物性を測定して、下記表2に示す。
放熱テスト:LEDランプに適用
前記実施例1〜12および比較例1〜3で製造された放熱塗料組成物の物性を測定して、下記表2に示す。
放熱テスト:ヒットシンクに適用
半導体およびディスプレイに用いられるCPUのLid(放熱のためのプレート(plate)形状のアルミニウムおよび合金のヒットシンク(heat sink))に、実施例4および実施例7で製造された放熱塗料組成物をコーティングした後、放熱性能を確認した。
その結果は下記表3に示す。
放熱テスト:発熱体に適用
発熱素子の全部分に実施例4および実施例7で製造された放熱塗料組成物をコーティングした後、放熱性能を確認した。
その結果は下記表4に示す。
放熱テスト:コンデンサに適用
冷蔵庫コンデンサ(condenser)の外部に実施例4および実施例7で製造された放熱塗料組成物をコーティングした後、放熱性能を確認した。試験条件は、ファンを設置せずに測定した。
その結果は下記表5に示す。
20 層間熱伝導接着層
30 放熱塗料がコーティングされたアルミニウム放熱板
40 LEDランプ
50 ゴムロール
60 ヒーティング金属ロール
70 放熱塗料コーティング層
80 アルミニウム基材
Claims (3)
- 酸素を供給源とし、表面改質した炭素素材0.1〜10重量%、スチレン/アクリル系水溶性樹脂0.04〜50重量%、アンモニア水、アミン系化合物、無機アルカリ溶液若しくはこれらの混合物0.005〜15重量%および溶媒25〜99.855重量%を含む分散液80〜95重量%と、
酸化亜鉛0.1〜20重量%、および水と、アンモニア水、アミン系化合物、無機アルカリ溶液若しくはこれらの混合物と、スチレン/アクリル系水溶性樹脂とを含み、固形分含量が40〜50重量%であるアルカリ水溶性樹脂エマルション80〜99.9重量%とを含む耐熱性添加剤1〜20重量%と、
アクリル系樹脂を含む粘着性向上エマルション1〜10重量%とを含み、
前記表面改質した炭素素材は、単一壁炭素ナノチューブ、二重壁炭素ナノチューブ、薄い多重壁炭素ナノチューブ、多重壁炭素ナノチューブ、束型炭素ナノチューブ、グラファイト、グラファイトオキシド、グラフェン、グラフェンオキシド、カーボンブラック、炭素繊維、炭素ナノ繊維から選択されるいずれか一つまたは二つ以上の混合物である、放熱塗料組成物。 - 前記分散液と耐熱性添加剤および粘着性向上エマルションの混合物100重量部に対し、オルガノメタルゾル、ポリエステル−ポリウレタン共重合体、ポリウレタン−エポキシ共重合体、ポリエステル−ポリウレタン−シリコン共重合体、およびポリエステル−エポキシ共重合体からなる群から選択されるいずれか一つまたは二つ以上の混合物である絶縁性添加剤50〜150重量部をさらに含む、請求項1に記載の放熱塗料組成物。
- 前記放熱塗料組成物は、LEDランプ、電子チップ、熱交換器、半導体装置、コンデンサ、蒸発器、ヒータ、ディスプレイ装置、モニター、ボイラー配管、通信装置、エンジン、モータ、バッテリー、ハウジング材料、電極材料または繊維製造の用途として用いられる、請求項1または2に記載の放熱塗料組成物。
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EP2602291A4 (en) | 2014-07-23 |
EP2602291A2 (en) | 2013-06-12 |
EP2602291B1 (en) | 2016-07-27 |
CN103097470B (zh) | 2015-10-14 |
US20130200300A1 (en) | 2013-08-08 |
WO2012018242A3 (ko) | 2012-05-10 |
KR101270932B1 (ko) | 2013-06-11 |
CN103097470A (zh) | 2013-05-08 |
KR20120013914A (ko) | 2012-02-15 |
US9624379B2 (en) | 2017-04-18 |
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