JP6606097B2 - 三次元基板のコンフォーマルコーティング - Google Patents
三次元基板のコンフォーマルコーティング Download PDFInfo
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- JP6606097B2 JP6606097B2 JP2016561002A JP2016561002A JP6606097B2 JP 6606097 B2 JP6606097 B2 JP 6606097B2 JP 2016561002 A JP2016561002 A JP 2016561002A JP 2016561002 A JP2016561002 A JP 2016561002A JP 6606097 B2 JP6606097 B2 JP 6606097B2
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Images
Classifications
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/04—Processes of manufacture in general
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- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
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- B05D3/04—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to gases
- B05D3/0433—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to gases the gas being a reactive gas
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
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- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1254—Sol or sol-gel processing
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1291—Process of deposition of the inorganic material by heating of the substrate
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
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Description
・短絡、熱暴走および熱爆発の危険性が低下する。
・ケーシングが小さくなること、分離膜が不要になることにより、軽量化、小型化される。
・乾燥しており、それゆえ電極材料が劣化しにくくなることから、各充電/放電に伴う性能の安定性が増す。
・動作温度の幅が広がる。
表面に凹凸を有する基板の上にコンフォーマルコーティングを形成する方法であって、
(a)前記基板の温度を140℃以上275℃以下に調整するステップと、
(b)前記基板の上に、ゾル−ゲル(または溶液−ゲル)前駆体を含む水溶液をコーティングするステップと、
を含む方法に関する。
a.カソード層
b.電解質層
c.アノード層
これらの層のうち少なくとも1つ(好ましくは、カソード層とアノード層のうち少なくとも1つ)は、ゾル−ゲル前駆体を含む水溶液を前記基板の上にコーティングすることにより、基板の上に形成される。前記基板は、140℃以上275℃以下(好ましくは140℃以上220℃以下)の温度に調整される。
少なくとも1つの金属酸化物ゾル−ゲル前駆体であって、少なくとも、
・Li、Na、K、Mg、Ca、Sr、Ba、Sc、Y、La、Ti、Zr、Hf、V、Nb、Ta、Cr、Mo、W、Mn、Fe、Ru、Co、Ni、Cu、Zn、Al、Ga、In、Sn、Pb、Bi、Ce、Pr、Nd、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、YbおよびLuから成り、好ましくは、Li、Mg、La、Ti、Zr、Ta、Cr、Mo、W、Mn、Fe、Ni、Zn、Al、Ga、In、Bi、NdおよびLuから成り、より好ましくはLi、La、Ti、W、FeおよびLuから成る群から選択された金属と、
・クエン酸塩、グリコール酸塩、リンゴ酸塩、乳酸塩、酒石酸塩、酢酸塩およびシュウ酸塩から成り、好ましくは、クエン酸塩、グリコール酸塩および乳酸塩から成る群から選択された、少なくとも1つのアニオンと、
を含む金属カルボン酸錯体であるゾル−ゲル前駆体と、
水混和性を有し且つ水の表面張力を低下させるのに適した溶媒であって、前記溶媒と水との体積比は、水と前記溶媒との混合物の表面張力が、25℃で40mN/m未満、好ましくは35mN/m未満、より好ましくは30mN/m未満となるように調整された溶媒
とを含む水溶液に関する。
開始物質として、液体のTi(IV)イソプロポキシド(Ti(OiPr)4、Acros organics社、98%以上)を用いた。0.73mol/lの溶液が得られるように、適量のTi(IV)イソプロポキシドを10倍の体積の水に追加した。すぐに加水分解と濃縮が生じ、白色沈殿が生成した。沈殿は濾過して水で洗い流した。加水分解の生成物は、不溶性物質となるのを避けるため、迅速に処理した。次のステップでは、クエン酸(CA、C6H8O7、Sigma−Aldrich社、99%)と過酸化水素(H2O2、安定化されている、Acros社、35%p.a水溶液)を、Ti4+:CA:H2O2のモル比が1:2:1.2となるように、生成したばかりの濡れた沈殿に加えた。次に、混合物を80℃で攪拌した。短い時間の後に、赤紫色の透明な溶液(pHは約1)が生成した。溶液を室温まで冷却し、第3ステップで、アンモニア(NH3、Merck社、32%水溶液、EP(extra pure))を溶液に滴下し、pHを上昇させた(pH電極(WTW社のSentix 81 electrodeを備えたinoLab 740)を用いて測定した)。このとき、激しくガスが発生し、溶液の温度が上昇した。溶液を再び室温まで冷却し、pHを正確に7とした。第3ステップ中、溶液の色は赤紫色(burgendy)(pH=1)から黄橙色(pH=7)に変化した。最終のステップで、前駆体をH2Oで希釈し、これに併せてエタノールを追加し、Ti4+濃度を0.05Mとし、エタノールと水との体積比を0.9:1とした。
シリコンのマイクロピラーが、表面積の大きい3D基板として用いられている。Siマイクロピラーは、薄膜バッテリにおいて基板として用いられることに鑑みて、TiNの薄い層(約20nm)でコーティングした。この層は、最終のバッテリスタックにおける集電体として用いられるだけでなく、Li用のブロック層としても機能する。図1は、(実施例1の水溶液を用いてコンフォーマルコーティングを行う前の)20nmのTiNコーティングを有するSiマイクロピラーのSEM写真を示しており、図1(A)は45°傾斜した方向から撮影したピラーの写真を、図1(B)はピラーの写真を、図1(C)はピラーの下部を撮影した写真を、図1(D)はピラーの上部を撮影した写真を示す。図1のSEM写真からわかるように、ピラーの直径は、約1.85μm以上約2.85μm以下である(測定対象としたピラーに沿った高さに応じて変わる)。ピラーの高さは約50μmであり、互いに5μm(ピラー間距離)を隔てて配置されている。シリコンピラーのアスペクト比は17以上27以下であると見積もられる。この値は、計算に用いた直径に応じて変わる。ピラーの長さで直径を平均化すると、アスペクト比は約22である。シリコンマイクロピラーを含む基板をUV/O3プロセスで洗浄した。超音波コーティングシステム(ExactaCoat(商標))内で180℃に調整された基板の上に、実施例1の溶液をスプレー塗布することにより、ピラーの上に前駆体を堆積させた。ノズルには、AccuMist社製の超音波スプレーノズル(precision ultrasonic spray nozzle)を用いた。Ti前駆体を用いて、シリコンピラーのコンフォーマル被覆を行うことができた。得られるゲルを、堆積後のピラーのSEM写真で示している(図2)。図2は、20nmのTiNでコーティングされたSiマイクロピラーのSEM写真を示しており、TiNはTi配位錯体から成るゲルで覆われている。図2(A)は45°傾斜した方向から撮影したピラーの写真を、図2(B)はピラーの下部を撮影した写真を、図1(D)はピラーの上部を撮影した写真を示す。より薄いTiO2層も準備したところ、より優れたコンフォーマリティを示したが、SEM写真で区別するのはさらに困難であった。
まず、単金属Ti(IV)のイオン溶液とLi(I)のイオン溶液を別々に準備した。
実施例1の水溶液の代わりに実施例3の水溶液を用いる点、ホットプレートの上でピラーの(ゲルの分解のための)更なる熱処理を行う点を除いて、実施例2を繰り返した。熱処理は、まず260℃で2分間、次に470℃で2分間行った。TiNでコーティングされたSiマイクロピラーの上で、最適な前駆体をスプレー塗布すると、ピラーが完全に前駆体で覆われる。これは、図5に示すSEM写真において見ることができる。ゲルの形成が明らかに視認される。図5は、20nmのTiNでコーティングされ、Li、Ti配位錯体から成るゲルで被覆されたSiマイクロピラーのSEM写真を示している。ゲルは、実施例3の溶液をTiNの上でスプレー塗布することにより得られる。図5(A)は、45度傾斜した方向から撮影したピラーの写真である。図5(B)は、ピラーの上部を撮影した写真である。図5(C)は、ピラーの下部を撮影した写真である。
まず、単金属のLi(I)のイオン溶液、La(III)のイオン溶液およびTi(IV)のイオン溶液を別々に準備した。
実施例1の水溶液の代わりに実施例5の水溶液を利用する点、基板の温度を180℃でなく200℃に調整する点、ホットプレートの上でピラーをさらに熱処理する点を除いて、実施例2を繰り返した。熱処理は、まず180℃で2分間、次に300℃で2分間、次に600℃で2分間、最後に700℃で60分間(加熱炉内で)行った。TiNでコーティングされたSiマイクロピラーの上での最適な前駆体をスプレー塗布し、その後にアニールして前駆体を分解し、Li/La/Ti酸化物を形成することにより、ピラーが完全に被覆される。これは、図6に示すSEM写真で見ることができる。図6では、完全なコーティングが見られる。図6は、20nmのTiNでコーティングされ、Li3xLa(2/3)−xTiO3(x=0.117)で被覆されたSiマイクロピラーのSEM写真を示している。Li3xLa(2/3)−xTiO3(x=0.117)は、実施例5の溶液をTiNの上でスプレー塗布することにより得られる。図6(A)はピラーの全体写真であり、図6(B)はピラーの下部、図6(C)はピラーの中央部を示し、図6(D)はピラーの上部を示す。さらに、結晶性コーティングを達成できることがわかった。
まず、単金属のLi(I)のイオン溶液、La(III)のイオン溶液およびTi(IV)のイオン溶液を別々に準備した。
実施例1の水溶液の代わりに実施例7の水溶液を利用する点、基板の温度を180℃でなく200℃に調整する点、ホットプレートの上でピラーをさらに熱処理する点を除いて、実施例2を繰り返した。熱処理は、まず180℃で2分間、次に300℃で2分間、次に600℃で2分間、最後に700℃で60分間(加熱炉内で)行った。TiNでコーティングされたSiマイクロピラーの上での最適な前駆体をスプレー塗布し、その後にホットプレートの上でアニールして前駆体を分解し、Li/W酸化物を形成することにより、ピラーが完全に被覆される。これは、図7に示すSEM写真で見ることができる。図7では、完全なコーティングが見られる。図7は、20nmのTiNでコーティングされ、前記酸化物で被覆されたSiマイクロピラーのSEM写真を示している。前記酸化物は、実施例7の溶液をTiNの上でスプレー塗布することにより得られる。図7(A)はピラーの全体写真であり、図7(B)はピラーの下部、図7(C)はピラーの中央部を示し、図7(D)はピラーの上部を示す。
まず、単金属のLu(III)のイオン溶液およびFe(III)のイオン溶液を別々に準備した。
実施例1の水溶液の代わりに実施例9の水溶液を利用する点、基板の温度を180℃でなく200℃に調整する点、ホットプレートの上でピラーをさらに熱処理する点を除いて、実施例2を繰り返した。熱処理は、まず320℃で2分間、次に510℃で2分間、次に800℃で60分間(加熱炉内で)、または1000℃で60分間(加熱炉内で)行った。800℃では純粋な六方相(hexagonal phase)が得られ、1000℃では純粋な斜方晶相が得られた。TiNでコーティングされたSiマイクロピラーの上での最適な前駆体をスプレー塗布し、その後にホットプレートの上でアニールして前駆体を分解し、Lu/Fe酸化物を形成することにより、ピラーが完全に被覆される。これは、図8に示すSEM写真で見ることができる。図8では、完全なコーティングが見られる。図8は、20nmのTiNでコーティングされ、前記酸化物で被覆されたSiマイクロピラーのSEM写真を示している。前記酸化物は、実施例9の溶液をTiNの上でスプレー塗布することにより得られる。図8(A)はピラーの全体写真であり、図8(B)はピラーの下部、図8(C)はピラーの中央部を示し、図8(D)はピラーの上部を示す。更なる熱処理により、堆積層が結晶化した。同じ実験を平坦なSi3N4表面で繰り返し、LuFeO3膜の結晶化を容易に調べることができた。これにより、アニール温度に応じて、相純粋な六方晶LuFeO3および相純粋な斜方晶LuFeO3の両方を得られることがわかった。
Claims (9)
- 表面に凹凸を有する基板の上にコンフォーマルコーティングを形成する方法であって、
(a)前記基板の温度を140℃以上275℃以下に調整するステップと、
(b)前記基板の上に、ゾル−ゲル前駆体を含む水溶液をコーティングするステップと、
を含む方法。 - 前記水溶液は、水混和性を有し且つ水の表面張力を低下させるのに適した溶媒をさらに含み、
前記溶媒と水との体積比は、水と前記溶媒との混合物の表面張力が、25℃で40mN/m未満となるように調整する、
請求項1に記載の方法。 - ステップ(b)の後に、前記水溶液がコーティングされた基板をアニールするステップ(c)をさらに含む、
請求項1または2に記載の方法。 - 前記凹凸は、1つまたは複数の要素から構成され、
前記要素の少なくとも1つのアスペクト比は、10以上である、
請求項1から3のいずれか1項に記載の方法。 - 前記凹凸を構成する少なくとも1つの要素は、ピラー形状またはトレンチ形状を有する、
請求項1から4のいずれか1項に記載の方法。 - 前記水溶液をコーティングするステップは、スプレー塗布により実施する、
請求項1から5のいずれか1項に記載の方法。 - 前記スプレー塗布は、超音波ノズルを用いて実施する、
請求項6に記載の方法。 - ステップ(b)の前に、紫外線照射を照射しつつオゾンガスを用いて前記基板を洗浄するステップをさらに含む、
請求項1から7のいずれか1項に記載の方法。 - バッテリ、キャパシタ、触媒、太陽電池またはセンサを製造する方法であって、
請求項1から8のいずれか1項に記載の方法に従って、表面に凹凸を有する基板の上にコンフォーマル層を形成するステップを含む、
方法。
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EP14169181.6A EP2947178A1 (en) | 2014-05-21 | 2014-05-21 | Conformal coating on three-dimensional substrates |
PCT/EP2015/061133 WO2015177221A1 (en) | 2014-05-21 | 2015-05-20 | Conformal coating on three-dimensional substrates |
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EP (2) | EP2947178A1 (ja) |
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US5238877A (en) | 1992-04-30 | 1993-08-24 | The United States Of America As Represented By The Secretary Of The Navy | Conformal method of fabricating an optical waveguide on a semiconductor substrate |
FR2693558B1 (fr) * | 1992-07-09 | 1994-08-19 | Commissariat Energie Atomique | Procédé de fabrication de couches minces présentant des propriétés optiques. |
JPH0769645A (ja) * | 1993-08-27 | 1995-03-14 | Murata Mfg Co Ltd | 鉛含有複合酸化物の製造方法 |
US6770257B1 (en) * | 1999-02-04 | 2004-08-03 | Kawasaki Jukogyo Kabushiki Kaisha | Processes for producing anatase titanium oxide and titanium oxide coating material |
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JP4543617B2 (ja) * | 2002-04-22 | 2010-09-15 | セイコーエプソン株式会社 | アクティブマトリクス基板の製造方法、電気光学装置の製造方法、電子機器の製造方法、アクティブマトリクス基板の製造装置、電気光学装置の製造装置、及び電気機器の製造装置 |
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US10644302B2 (en) | 2020-05-05 |
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JP2017523023A (ja) | 2017-08-17 |
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