JPWO2015163249A1 - 多孔質板状フィラー、その製造方法、及び断熱膜 - Google Patents
多孔質板状フィラー、その製造方法、及び断熱膜 Download PDFInfo
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- JPWO2015163249A1 JPWO2015163249A1 JP2016514900A JP2016514900A JPWO2015163249A1 JP WO2015163249 A1 JPWO2015163249 A1 JP WO2015163249A1 JP 2016514900 A JP2016514900 A JP 2016514900A JP 2016514900 A JP2016514900 A JP 2016514900A JP WO2015163249 A1 JPWO2015163249 A1 JP WO2015163249A1
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- filler
- porous plate
- shape
- plate
- heat insulating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/22—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed
- B32B5/30—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being formed of particles, e.g. chips, granules, powder
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- B23K26/00—Working by laser beam, e.g. welding, cutting or boring
- B23K26/02—Positioning or observing the workpiece, e.g. with respect to the point of impact; Aligning, aiming or focusing the laser beam
- B23K26/06—Shaping the laser beam, e.g. by masks or multi-focusing
- B23K26/062—Shaping the laser beam, e.g. by masks or multi-focusing by direct control of the laser beam
- B23K26/0622—Shaping the laser beam, e.g. by masks or multi-focusing by direct control of the laser beam by shaping pulses
- B23K26/0624—Shaping the laser beam, e.g. by masks or multi-focusing by direct control of the laser beam by shaping pulses using ultrashort pulses, i.e. pulses of 1ns or less
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- B23K26/00—Working by laser beam, e.g. welding, cutting or boring
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- B23K26/00—Working by laser beam, e.g. welding, cutting or boring
- B23K26/36—Removing material
- B23K26/38—Removing material by boring or cutting
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- B23K26/00—Working by laser beam, e.g. welding, cutting or boring
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- B23K26/40—Removing material taking account of the properties of the material involved
- B23K26/402—Removing material taking account of the properties of the material involved involving non-metallic material, e.g. isolators
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- B26—HAND CUTTING TOOLS; CUTTING; SEVERING
- B26D—CUTTING; DETAILS COMMON TO MACHINES FOR PERFORATING, PUNCHING, CUTTING-OUT, STAMPING-OUT OR SEVERING
- B26D3/00—Cutting work characterised by the nature of the cut made; Apparatus therefor
- B26D3/08—Making a superficial cut in the surface of the work without removal of material, e.g. scoring, incising
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Abstract
Description
図1に示すように、本発明の多孔質板状フィラー1は、アスペクト比が3以上の板状で、その板の面形状が円形、オーバル、および角丸多角形のいずれかであり、その最小長が0.1〜50μmである。図1は本発明の多孔質板状フィラー1のうち、面形状が円を示すものである。また、図2は本発明の多孔質板状フィラー1の面形状がオーバルを示すものである。更に図3は本発明の多孔質板状フィラー1の面形状が角丸多角形である角丸四角形を示すものである。
気孔率(%)={1−(見かけ粒子密度/真密度)}×100
この式において、「見かけ粒子密度」は、水銀を用いた液浸法により測定する。また、「真密度」は、多孔質板状フィラーを十分に粉砕した後、ピクノメータ法で測定する。
熱伝導率(W/(m・K))=熱拡散率×比熱×密度
この式において、「熱拡散率」は、光交流法により測定する。また、「比熱」は、DSC法により測定する。「密度」は、水銀ポロシメーターで測定する。
熱容量(kJ/(m3・K))=比熱×密度(見かけ粒子密度)
この式において、「比熱」は、DSC法により測定する。また、「密度(見かけ粒子密度)」は、水銀を用いた液浸法により測定する。本明細書において、熱容量は、一般的には容積比熱と呼ばれる単位体積当たりで議論することとするため、単位はkJ/(m3・K)である。
次に、本発明の多孔質板状フィラー1の製造方法について説明する。
レーザー加工機を用いた製造方法1について説明する。製造方法1は、多孔質板状フィラーの1成分を含む材料から形成されたグリーンシート32を、焼成前または焼成後に、10ピコ秒以下のパルス幅でレーザー照射できるレーザー加工機35を用いて加工して、所定の面形状の多孔質板状フィラー1を形成する方法である。多孔質板状フィラー1の成分を含むグリーンシート32を形成する方法としては、プレス成形、鋳込み成形、押出成形、射出成形、テープ成形、ドクターブレード法等が挙げられ、何れの方法であってもよい。以下、製造しようとする多孔質板状フィラー1の成分がセラミックスであり、ドクターブレード法によりグリーンシート32を形成する場合を例として説明する。
本発明の多孔質板状フィラー1の製造方法2は、多孔質板状フィラー1の成分を含む材料から調整された粘度100〜10000cpsのスラリー38を滴下又は吐出し、断面形状がアーチ形、楕円形、および少なくとも一部の角が丸まった四角形のいずれかである多孔質板状フィラー1を形成する方法である。また、スラリー38を滴下又は吐出する方法としては、インクジェット式スポッター装置37を用いることが好ましい。このような方法を用いると、図7Aのような多孔質板状フィラー1の断面が、少なくとも一部の角が丸まった四角形になりやすく、図7B、図7Cのように、中央部が凹んだ形状になることもある。
本発明の多孔質板状フィラー1の製造方法3は、多孔質板状フィラー1の成分を含む材料から調整された粘度100〜10000cpsのスラリー38を所定の形状を有する付着部41に付着させ、付着部41を基板面42に押し当てることにより、付着部41に付着したスラリー38を基板面42に付着させ、断面形状がアーチ形、楕円形、および少なくとも一部の角が丸まった四角形のいずれかである多孔質板状フィラー1を形成する方法である。
次に、本発明の断熱膜3について説明する。本発明の断熱膜3は、本発明の多孔質板状フィラー1を含むものである。具体的には、図12に示すように、本発明の断熱膜3は、本発明の多孔質板状フィラー1が、多孔質板状フィラー1を結合するためのマトリックス3mに分散して配置されたものである。マトリックス3mとは、多孔質板状フィラー1の周囲やこれらの粒子間に存在する成分であり、これらの粒子間を結合する成分である。
イットリア部分安定化ジルコニア粉末に、造孔材としてのカーボンブラックと、バインダーとしてのポリビニルブチラール樹脂(PVB)と、可塑剤としてのフタル酸ジオクチル(DOP)と、溶媒としてのキシレン及び1−ブタノールとを加え、ボールミルにて30時間混合し、グリーンシート成形用スラリーを調製した。このスラリーに真空脱泡処理又は溶媒(キシレン及び1−ブタノール)を加え、粘度を4000cpsに調整した後、ドクターブレード装置によって焼成後の厚さが5μm(設計値)となるようにグリーンシート32を形成した。このグリーンシート32にレーザー加工機35を使用して板の面形状が円形になるように加工した。レーザー加工機35には、10ピコ秒以下のパルス幅でレーザーを照射できるものを用い、周波数は200MPa、出力は2.5Wで加工した。こうして成形したグリーンシート集合体を600℃で5時間加熱して脱脂した後、1100℃で2時間加熱して焼成し、板の面形状が円形で、断面形状が角丸四角形の焼成体を得た。焼成体である多孔質板状フィラー集合体(多孔質板状フィラーの粉末)から、多孔質板状フィラー1(粒子)を任意に20個選んで、最小長の平均値と、最大長の平均値を計測し、その平均値からアスペクト比の平均値を計測し、それらの値を表1に示した。なお、これらの多孔質板状フィラー1の熱伝導率は0.2W/(m・K)、熱容量は900kJ/(m3・K)、平均気孔径は150nm、気孔率は65%であった。
焼成後の厚みが10μm(設計値)となるようにグリーンシートを形成した。他は実施例1と同じである。図13は、実施例2で得られた多孔質板状フィラー1の電子顕微鏡写真であり、図13の電子顕微鏡写真に、矢印で示した部分の長さが、多孔質板状フィラー1の最大長L1である。
焼成後の厚みが25μm(設計値)となるようにグリーンシートを形成した。他は実施例1と同じである。
実施例1と同様にして、スラリー38を調製した。このスラリー38に真空脱泡処理又は溶媒(キシレン及び1−ブタノール)を加え、粘度を1000cpsに調整した。その後、インクジェット式スポッター装置37によって、焼成後の最小長が8μm、最大長L1が60μmになるようにスラリー38を滴下し成形した。滴下によりできた成形体33を実施例1と同様にして、脱脂及び焼成し、板の面形状が円形で、断面形状がアーチ形の焼成体を得た。実施例1と同様にして、多孔質板状フィラー1の最小長の平均値と、最大長の平均値を計測し、その平均値からアスペクト比の平均値を計測し、それらの値を表1に示した。更に、図14の電子顕微鏡写真に、矢印で示した部分の長さが、多孔質板状フィラー1の最大長L1である。なお、これらの多孔質板状フィラー1の熱伝導率、熱容量、平均気孔径及び気孔率の値は、実施例1におけるそれらの値と同一であった。また、得られた多孔質板状フィラー集合体を用い、実施例1と同様にして、断熱膜3を形成した。こうして形成された断熱膜3の熱伝導率を計測し、その値を表2に示した。
実施例1と同様にして、スラリー38を調製した。このスラリー38に真空脱泡処理又は溶媒(キシレン及び1−ブタノール)を加え、粘度を2000cpsに調整した。その後、ニードル式ディスペンサ装置39によって、焼成後の最小長が9μm、最大長が60μmになるようにスラリー38を塗布した。塗布によりできた成形体33を実施例1と同様にして、脱脂及び焼成し、板の面形状が円形で、断面形状がアーチ形の焼成体を得た。実施例1と同様にして、多孔質板状フィラー1の最小長の平均値と、最大長の平均値を計測し、その平均値からアスペクト比の平均値を計測し、それらの値を表1に示した。更に、図15の電子顕微鏡写真に、矢印で示した部分の長さが、多孔質板状フィラー1の最大長L1である。なお、これらの多孔質板状フィラー1の熱伝導率、熱容量、平均気孔径及び気孔率の値は、実施例1におけるそれらの値と同一であった。また、得られた多孔質板状フィラー集合体を用い、実施例1と同様にして、断熱膜3を形成した。こうして形成された断熱膜3の熱伝導率を計測し、その値を表2に示した。
実施例5と同様にして、スラリー38を調整し、ニードル式ディスペンサ装置39によって塗布した。ニードル40の付着部41の形状を変更することで、多孔質板状フィラー1の形状を変更することができた。実施例6〜9の多孔質板状フィラー1の面形状を表1に示した。これらの成形体33を実施例1と同様にして、脱脂及び焼成をし、板の面形状が表1の焼成体を得た。実施例1と同様にして、多孔質板状フィラー1の最小長の平均値と、最大長の平均値を計測し、その平均値からアスペクト比の平均値を計測し、それらの値を表1に示した。更に、図16〜図19の電子顕微鏡写真に、矢印で示した部分の長さが、多孔質板状フィラー1の最大長L1である。なお、これらの多孔質板状フィラー1の熱伝導率、熱容量、平均気孔径及び気孔率の値は、実施例1におけるそれらの値と同一であった。また、得られた多孔質板状フィラー集合体を用い、実施例1と同様にして、断熱膜3を形成した。こうして形成された断熱膜3の熱伝導率を計測し、その値を表2に示した。
実施例1と同様にして、グリーンシート32を形成した。このグリーンシート32を600℃で5時間加熱して脱脂した後、1100℃で2時間加熱して焼成し、シート状焼成体を得た。このシート状焼成体を、目開き75μmのふるいの金網上に置き、ゴムヘラを押し付けて粉砕した。その後、目開きがそれぞれ40μmと63μmのふるいを使用して分級した。実施例1と同様にして、多孔質板状フィラー1の最小長の平均値と、最大長の平均値を計測し、その平均値からアスペクト比の平均値を計測し、それらの値を表1に示した。更に、得られた多孔質板状フィラー集合体の電子顕微鏡写真を図20及び図21に示した。図21の電子顕微鏡写真に、矢印で示した部分の長さが、多孔質板状フィラー1の最大長L1である。これらの多孔質板状フィラー1の熱伝導率は0.2W/(m・K)、熱容量は900kJ/(m3・K)、平均気孔径は150nm、気孔率は65%であった。また、得られた多孔質板状フィラー集合体を用い、実施例1と同様にして、断熱膜3を形成した。こうして形成された断熱膜3の熱伝導率を計測し、その値を表2に示した。
Claims (16)
- アスペクト比が3以上の板状で、その板の面形状が円形、オーバル、および角丸多角形のいずれかであり、その最小長が0.1〜50μmである多孔質板状フィラー。
- 前記面形状における前記角丸多角形の弧の半径Rは、前記最小長以上である請求項1に記載の多孔質板状フィラー。
- 断面形状が、アーチ形、楕円形、および少なくとも一部の角が丸まった四角形のいずれかである請求項1または2に記載の多孔質板状フィラー。
- 前記断面形状における少なくとも一部の角が丸まった四角形の弧の半径Rは、前記最小長の1/5以上である請求項3に記載の多孔質板状フィラー。
- 平均気孔径が10〜500nmである気孔を有する請求項1〜4のいずれか1項に記載の多孔質板状フィラー。
- 熱伝導率が、1W/(m・K)以下である請求項1〜5のいずれか1項に記載の多孔質板状フィラー。
- 熱容量が、10〜3000kJ/(m3・K)以下である請求項1〜6のいずれか1項に記載の多孔質板状フィラー。
- 請求項1〜7のいずれか1項に記載の多孔質板状フィラーを製造する方法であって、前記多孔質板状フィラーの成分を含む材料から形成されたグリーンシートを、焼成前または焼成後に、10ピコ秒以下のパルス幅でレーザー照射可能なレーザー加工機を用いて加工して、所定の面形状の前記多孔質板状フィラーを形成する多孔質板状フィラーの製造方法。
- 請求項1〜7のいずれか1項に記載の多孔質板状フィラーを製造する方法であって、前記多孔質板状フィラーの成分を含む材料から調整された粘度100〜10000cpsのスラリーを滴下又は吐出し、断面形状が、アーチ形、楕円形、および少なくとも一部の角が丸まった四角形のいずれかである前記多孔質板状フィラーを形成する多孔質板状フィラーの製造方法。
- インクジェット式スポッター装置を用いて、前記スラリーを滴下又は吐出する請求項9に記載の多孔質板状フィラーの製造方法。
- 請求項1〜7のいずれか1項に記載の多孔質板状フィラーを製造する方法であって、前記多孔質板状フィラーの成分を含む材料から調整された粘度100〜10000cpsのスラリーを所定の形状を有する付着部に付着させ、前記付着部を基板面に押し当てることにより、前記付着部に付着した前記スラリーを前記基板面に付着させて、断面形状が、アーチ形、楕円形、および少なくとも一部の角が丸まった四角形のいずれかである前記多孔質板状フィラーを形成する多孔質板状フィラーの製造方法。
- ニードル式ディスペンサ装置を用いて前記スラリーを前記基板面に付着させる請求項11に記載の多孔質板状フィラーの製造方法。
- 請求項1〜7のいずれか1項に記載の多孔質板状フィラーを含む断熱膜。
- 前記多孔質板状フィラーが層状に配置されている請求項13に記載の断熱膜。
- 厚さが、1μm〜5mmである請求項13または14に記載の断熱膜。
- 熱伝導率が、1W/(m・K)以下である請求項13〜15のいずれか1項に記載の断熱膜。
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Application Number | Priority Date | Filing Date | Title |
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