JP2006527154A - セラミックデバイス用のセラミックグリーンシートの製造方法 - Google Patents
セラミックデバイス用のセラミックグリーンシートの製造方法 Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 42
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 13
- 239000011230 binding agent Substances 0.000 claims abstract description 37
- 239000002270 dispersing agent Substances 0.000 claims abstract description 20
- 239000006185 dispersion Substances 0.000 claims abstract description 19
- 239000011877 solvent mixture Substances 0.000 claims abstract description 13
- 239000004014 plasticizer Substances 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 10
- 229920001577 copolymer Polymers 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 28
- 230000008569 process Effects 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- 239000002904 solvent Substances 0.000 claims description 7
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- 150000002148 esters Chemical class 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- ZFOZVQLOBQUTQQ-UHFFFAOYSA-N Tributyl citrate Chemical group CCCCOC(=O)CC(O)(C(=O)OCCCC)CC(=O)OCCCC ZFOZVQLOBQUTQQ-UHFFFAOYSA-N 0.000 claims description 4
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims description 4
- 150000004715 keto acids Chemical class 0.000 claims description 4
- 229920000642 polymer Polymers 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 4
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 3
- 150000007524 organic acids Chemical class 0.000 claims description 3
- GGLYDWDAMKQIJZ-UHFFFAOYSA-N 3,6,9-trioxodecanoic acid Chemical compound CC(=O)CCC(=O)CCC(=O)CC(O)=O GGLYDWDAMKQIJZ-UHFFFAOYSA-N 0.000 claims description 2
- WUQQVFQGWWMQLD-UHFFFAOYSA-N 3,6-dioxoheptanoic acid Chemical compound CC(=O)CCC(=O)CC(O)=O WUQQVFQGWWMQLD-UHFFFAOYSA-N 0.000 claims description 2
- KJTZGGMVRFZKOA-UHFFFAOYSA-N 6-(7-methyloctoxy)-6-oxohexanoic acid Chemical compound CC(C)CCCCCCOC(=O)CCCCC(O)=O KJTZGGMVRFZKOA-UHFFFAOYSA-N 0.000 claims description 2
- QZCLKYGREBVARF-UHFFFAOYSA-N Acetyl tributyl citrate Chemical compound CCCCOC(=O)CC(C(=O)OCCCC)(OC(C)=O)CC(=O)OCCCC QZCLKYGREBVARF-UHFFFAOYSA-N 0.000 claims description 2
- DOOTYTYQINUNNV-UHFFFAOYSA-N Triethyl citrate Chemical compound CCOC(=O)CC(O)(C(=O)OCC)CC(=O)OCC DOOTYTYQINUNNV-UHFFFAOYSA-N 0.000 claims description 2
- 239000001361 adipic acid Substances 0.000 claims description 2
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- 150000001298 alcohols Chemical class 0.000 claims description 2
- 150000002576 ketones Chemical class 0.000 claims description 2
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- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 claims description 2
- 239000001069 triethyl citrate Substances 0.000 claims description 2
- VMYFZRTXGLUXMZ-UHFFFAOYSA-N triethyl citrate Natural products CCOC(=O)C(O)(C(=O)OCC)C(=O)OCC VMYFZRTXGLUXMZ-UHFFFAOYSA-N 0.000 claims description 2
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- VMXHKWISKOTVHH-UHFFFAOYSA-N 3,6,9-trioxoundecanedioic acid Chemical compound OC(=O)CC(=O)CCC(=O)CCC(=O)CC(O)=O VMXHKWISKOTVHH-UHFFFAOYSA-N 0.000 claims 1
- 235000005985 organic acids Nutrition 0.000 claims 1
- 238000005979 thermal decomposition reaction Methods 0.000 claims 1
- 239000007788 liquid Substances 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 13
- 239000002002 slurry Substances 0.000 description 12
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- 229910052451 lead zirconate titanate Inorganic materials 0.000 description 10
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- 239000010949 copper Substances 0.000 description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 8
- 230000008901 benefit Effects 0.000 description 8
- 238000009472 formulation Methods 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 5
- 230000009471 action Effects 0.000 description 4
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- 238000005303 weighing Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
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- 230000015556 catabolic process Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
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- 239000001301 oxygen Substances 0.000 description 2
- 229920000058 polyacrylate Polymers 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920005479 Lucite® Polymers 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical group ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 150000008280 chlorinated hydrocarbons Chemical class 0.000 description 1
- 150000001879 copper Chemical class 0.000 description 1
- 239000007857 degradation product Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000007606 doctor blade method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 235000021323 fish oil Nutrition 0.000 description 1
- 229910000743 fusible alloy Inorganic materials 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 238000002372 labelling Methods 0.000 description 1
- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000006082 mold release agent Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012454 non-polar solvent Substances 0.000 description 1
- 239000006259 organic additive Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 150000003014 phosphoric acid esters Chemical class 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000193 polymethacrylate Polymers 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 229920003009 polyurethane dispersion Polymers 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000002296 pyrolytic carbon Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000000518 rheometry Methods 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
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- C04B35/49—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates containing also titanium oxides or titanates
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Abstract
Description
セラミック生産技術における重点は、未焼成品を製造する新規の方法を開発することにある。このための例は、セラミック射出成形、ゲルキャスティング又はニアネットシェープ技術である。全てのプロセスは、大量の有機助剤、例えば結合剤、離型剤又は安定剤の使用を必要とし、これらは焼結プロセスの前又はその間に未焼成品から除去しなければならない。この結合剤除去プロセスは一方で時間がかかりかつコストがかかり、他方ではこのプロセスは部分的に健康を害する分解生成物を生じることにより環境汚染を引き起こす。
セラミックグリーンシートの本発明による製造方法は、先行技術と比較して、セラミック多層デバイスは、はるかに時間を節約し、より低い温度で、従ってはるかに低コストで結合剤除去することができるという利点を有する。
アクリラートメタクリラートコポリマーをベースとするキャスティングスラリー用の改善された配合物は、セラミック多層デバイス用の、殊に圧電多層アクチュエータ用のセラミックグリーンシートの製造のために用いられ、未焼成のセラミック多層デバイスから熱により、時間が節約された、簡単でかつ完全に結合剤除去が可能であり、その際、結合剤除去する最高温度は350℃を上回らない。PZTセラミックとの関連で、結合剤の完全な分解はこの温度で完了する。このことは、アクリラート結合剤に関するPZT表面の触媒作用にある。この場合、100ppmよりも低い残留炭素含有量が得られる。この分解メカニズムは、主に解重合である。この場合、炭素鎖(backbone)の構造が攻撃されるため、主にモノマーが形成され、除去される。この場合に、ほとんど熱分解炭素の形成は生じない。
1) 分散剤溶液の製造
この分散剤溶液は、分散剤と、スラリーの全溶剤割合に対して約50質量%の割合の溶剤混合物との秤量及び均質化によって製造される。
結合剤溶液は、有利に70:20:10の割合の溶剤混合物、結合剤及び可塑剤の秤量及び均質化により製造される。一般に、溶剤の割合は、60〜80質量%の範囲内にあり、結合剤と可塑剤との比率は55:45〜75:25質量%の範囲内にある。
結合剤溶液の濃度に依存して70:30〜90:10質量%の割合での、有利に85:15質量%の割合でのセラミック粉末、殊にPZT粉末と、工程1において製造された分散剤溶液との秤量、均質化及びZrO2粉砕媒体を用いて振動ミル又はリングギャップミル(Ringspaltmuehle)中での0.1〜10時間、有利に3時間の期間にわたるデアグロメレーションにより、第1の分散液(前スラリー)を製造した。
工程3で製造された第1の分散液(前スラリー)と第2の工程からの結合剤溶液とを70:30〜90:10質量%、有利に80:20質量%の割合で秤量し、均質化し、ZrO2粉砕媒体を用いて振動ミル又はリングギャップミル中で、0.1〜5時間、有利に1時間の期間にわたりデアグロメレーションした。
真空ポンプを用いて、工程4で製造されたキャスティングスラリー(第2の分散液)から空気及び易揮発性溶剤成分を同時に除去し、通常のシートキャスティング装置に関するキャスティングのための粘度を、有利に公知のドクターブレード法により調節した。この場合、攪拌機を用いてスラリーを運動させかつ室温に温度調節しながら撹拌容器を排気する。この粘度は6.8l/Sの剪断速度で、1500〜4000mPas、有利に2000mPasの値に調節された。
Claims (16)
- 次の工程:
a) 1種又は数種の分散剤を溶剤混合物中で有機酸と組み合わせて均質化することによる分散剤溶液の製造;
b) 工程a)からの溶剤混合物と、結合剤としての1種又は数種のアクリラートメタクリラートコポリマーと、1種又は数種の可塑剤との均質化による結合剤溶液の製造;
c) セラミック粉末と分散剤溶液との均質化及び引き続くデアグロメレーションによる第1の分散液の製造;
d) 第1の分散液と結合剤溶液との均質化による第2の分散液の製造;及び
e) 第2の分散液からの空気及び易揮発性溶剤成分の除去
を特徴とする、セラミックデバイス、特に多層デバイス用のセラミックグリーンシートの製造方法。 - 分散剤として、酸基を有するポリマー分散剤を使用することを特徴とする、請求項1記載の方法。
- 有機酸としてオキソ酸を使用することを特徴とする、請求項1又は2記載の方法。
- オキソ酸は、3,6−ジオキソヘプタン酸、3,6,9−トリオキソデカン酸、3,6,9−トリオキソウンデカン二酸及びポリグリコール二酸からなるグループから選択されることを特徴とする、請求項3記載の方法。
- 溶剤混合物は、アルコール、エステル及びケトンからなるグループから選択され、その際、前記溶剤混合物は少なくとも1種のアルコールを含有することを特徴とする、請求項1から4までのいずれか1項記載の方法。
- 溶剤混合物は、エタノール、イソプロパノール、n−プロパノール、n−ブタノール、酢酸エチル、酢酸ブチル、1−メトキシ−2−プロピルアセタート及びメチルエチルケトンからなるグループから選択されることを特徴とする、請求項5記載の方法。
- 結合剤ポリマーの熱分解を解重合によって行うことを特徴とする、請求項1から6までのいずれか1項記載の方法。
- 可塑剤が、エステルベースの、フタラート不含の可塑剤であることを特徴とする、請求項1から7までのいずれか1項記載の方法。
- 可塑剤がクエン酸又はアジピン酸のエステルであることを特徴とする、請求項8記載の方法。
- 可塑剤が、トリブチルシトラート、トリエチルシトラート、アセチルトリブチルシトラート、ビス−2−エチルヘキシルアジパート及びイソノニルアジパートからなるグループから選択されることを特徴とする、請求項8又は9記載の方法。
- セラミック粉末がPZT粉末であることを特徴とする、請求項1から10までのいずれか1項記載の方法。
- セラミック粉末と分散剤溶液とを、70:30〜90:10の比率で、有利に85:15の比率で均質化することを特徴とする、請求項10又は11記載の方法。
- 第1の分散液と結合剤溶液とを、70:30〜90:10の比率で、有利に80:20の比率で均質化することを特徴とする、請求項1から12までのいずれか1項記載の方法。
- 第2の分散液から空気の除去と易揮発性溶剤成分の除去とを同時に真空ポンプを用いて行うことを特徴とする、請求項1から13までのいずれか1項記載の方法。
- 結合剤と可塑剤との比率が55:45〜75:25の範囲内、有利に67:33にあることを特徴とする、請求項1から14までのいずれか1項記載の方法。
- 圧電多層アクチュエータの製造のための、請求項1から15までのいずれか1項記載のセラミックグリーンシートの使用。
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DE10326040A DE10326040A1 (de) | 2003-06-10 | 2003-06-10 | Verfahren zur Herstellung von keramischen Grünfolien für keramische Bauteile |
PCT/DE2004/000777 WO2004110954A1 (de) | 2003-06-10 | 2004-04-14 | Verfahren zur herstellung von keramischen grünfolien für keramische bauteile |
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KR20120027158A (ko) * | 2009-03-31 | 2012-03-21 | 세키스이가가쿠 고교가부시키가이샤 | 슬러리 조성물의 제조 방법 |
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EP1881024A1 (en) * | 2006-07-18 | 2008-01-23 | Nederlandse Organisatie voor toegepast- natuurwetenschappelijk onderzoek TNO | Use of a plasticizer in an electroactive polymer composition |
CN112142480B (zh) * | 2020-09-22 | 2022-06-21 | 中国振华(集团)新云电子元器件有限责任公司(国营第四三二六厂) | 一种湿法工艺多层片式瓷介电容器的瓷浆及其制备方法 |
DE102022114964A1 (de) | 2022-06-14 | 2023-12-14 | Technische Universität Darmstadt Körperschaft des öffentlichen Rechts | Verfahren zur Herstellung eines Kondensatorelements mit einer dielektrischen keramischen Folie, Schlicker zur Herstellung einer dielektrischen keramischen Folie und Kondensatorelement mit einer dielektrischen keramischen Folie |
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- 2004-04-14 JP JP2006515648A patent/JP2006527154A/ja active Pending
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JPS61146753A (ja) * | 1984-12-20 | 1986-07-04 | 株式会社東芝 | 回路基板用グリ−ンシ−トの製造方法 |
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JPH0826832A (ja) * | 1994-05-09 | 1996-01-30 | Fuji Elelctrochem Co Ltd | セラミックスグリーンシート用スラリーの製造方法 |
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KR101696947B1 (ko) * | 2009-03-31 | 2017-02-01 | 세키스이가가쿠 고교가부시키가이샤 | 슬러리 조성물의 제조 방법 |
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