JP2013524005A - 表面電荷を利用した被膜の自己組織化 - Google Patents
表面電荷を利用した被膜の自己組織化 Download PDFInfo
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- 238000000576 coating method Methods 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 claims abstract description 66
- 239000000463 material Substances 0.000 claims abstract description 64
- 239000011248 coating agent Substances 0.000 claims abstract description 50
- 239000000758 substrate Substances 0.000 claims abstract description 24
- 238000004070 electrodeposition Methods 0.000 claims abstract description 17
- 239000010949 copper Substances 0.000 claims description 61
- 229910017119 AlPO Inorganic materials 0.000 claims description 38
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 19
- 229910052802 copper Inorganic materials 0.000 claims description 19
- 238000000151 deposition Methods 0.000 claims description 16
- 230000008021 deposition Effects 0.000 claims description 13
- 239000012530 fluid Substances 0.000 claims description 8
- 230000000284 resting effect Effects 0.000 claims description 7
- 238000004891 communication Methods 0.000 claims description 6
- 238000001652 electrophoretic deposition Methods 0.000 claims description 6
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 3
- 239000000908 ammonium hydroxide Substances 0.000 claims description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N zinc oxide Inorganic materials [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 3
- 238000001338 self-assembly Methods 0.000 abstract description 19
- 239000007772 electrode material Substances 0.000 abstract description 12
- 239000007787 solid Substances 0.000 abstract description 9
- 239000007784 solid electrolyte Substances 0.000 abstract description 8
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- 239000000243 solution Substances 0.000 description 53
- 239000010408 film Substances 0.000 description 27
- 229910052698 phosphorus Inorganic materials 0.000 description 13
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 12
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 12
- 239000011574 phosphorus Substances 0.000 description 12
- 239000003792 electrolyte Substances 0.000 description 11
- 229910052782 aluminium Inorganic materials 0.000 description 10
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 9
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical group [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 8
- 229910001416 lithium ion Inorganic materials 0.000 description 8
- 238000005259 measurement Methods 0.000 description 8
- 238000001228 spectrum Methods 0.000 description 8
- 230000008569 process Effects 0.000 description 7
- 239000003115 supporting electrolyte Substances 0.000 description 7
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 5
- 230000008901 benefit Effects 0.000 description 5
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 4
- 229910021607 Silver chloride Inorganic materials 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000000724 energy-dispersive X-ray spectrum Methods 0.000 description 4
- 230000014759 maintenance of location Effects 0.000 description 4
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910013684 LiClO 4 Inorganic materials 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 238000002484 cyclic voltammetry Methods 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 2
- 229910016201 LiMn1.42Ni0.42Co0.16O4 Inorganic materials 0.000 description 2
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 229910052787 antimony Inorganic materials 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000000970 chrono-amperometry Methods 0.000 description 2
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 2
- 239000008151 electrolyte solution Substances 0.000 description 2
- 229940021013 electrolyte solution Drugs 0.000 description 2
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 2
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000001103 potassium chloride Substances 0.000 description 2
- 235000011164 potassium chloride Nutrition 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 229910052596 spinel Inorganic materials 0.000 description 2
- 239000011029 spinel Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- XNDZQQSKSQTQQD-UHFFFAOYSA-N 3-methylcyclohex-2-en-1-ol Chemical compound CC1=CC(O)CCC1 XNDZQQSKSQTQQD-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 description 1
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 239000002001 electrolyte material Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
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- 230000001788 irregular Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011244 liquid electrolyte Substances 0.000 description 1
- MHCFAGZWMAWTNR-UHFFFAOYSA-M lithium perchlorate Chemical compound [Li+].[O-]Cl(=O)(=O)=O MHCFAGZWMAWTNR-UHFFFAOYSA-M 0.000 description 1
- 229910001486 lithium perchlorate Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 235000019837 monoammonium phosphate Nutrition 0.000 description 1
- 239000006012 monoammonium phosphate Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
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- 230000004044 response Effects 0.000 description 1
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- 238000000926 separation method Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- -1 sodium saturated calomel Chemical class 0.000 description 1
- 230000005641 tunneling Effects 0.000 description 1
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Abstract
【選択図】図1
Description
本願は、2010年3月26日に出願されたAmy L.Prietoらによる「等電点決定装置および電池製造における使用(isoelectric Determination Apparatus and Use In The Fabrication Of Batteries」に関する米国仮特許出願第61/318,068号の利益を主張する。この仮特許出願の全内容は、それが開示しかつ教示するすべてに関して、参照によって本願に明確に組み込まれる。
J.M.MosbyおよびA.L.Prieto著「リチウムイオン電池のアノードに対するCu2Sbの直接堆積(Direct Deposition of Cu2Sb for Lithium−ion Battery Anodes)」、J.Am.Chem.Soc.誌、2008年、130、10656−10661に従って、電着法を用いて、直径約5cmの銅の円形ディスク上にCu2Sbを堆積した。ディスクにはステンレス鋼のシャフトを連結し、本発明の図1の装置10の中に組み込んだ。Cu2Sbの等電pHを、支持電解質としての1mM KCLと、基準電極としてのAg/AgClと、約750rpmの回転速度とを用いて決定した。溶液のpHは、pHを低下させるために希塩酸を添加するか、pHを高めるに希釈水酸化アンモニウムを添加することで制御した。溶液のpH調整には他の試薬を用いてもよい。Cu2Sbの等電pHは約7.5であると決定された(本明細書の図2)。
ここで、被膜厚さを増大するための、上記の自己組織化手順と電着法との組み合わせについて、AlPO4で被膜されたCu2Sb基板を1例として取り上げて述べる。
Claims (22)
- 材料の等電pHを決定するための装置において、
選択されたpHを有する溶液を包含するのに適合した第1チャンバであって、
軸心と第1面と前記材料が配備される反対側の第2面とを有する円形ディスクと、
前記ディスクの第1面に取り付けられるシャフトと、
前記ディスクの第2面の近傍および前記軸心の近傍に配備される第1基準電極と、
前記第1チャンバにおけるオリフィスにおいて前記第1チャンバの壁面に固着される中空のチューブと、
を含む第1チャンバと、
前記チューブを介して前記第1チャンバに流体連絡される第2チャンバであって第2基準電極を含む第2チャンバと、
前記シャフトを選択された速度で回転する手段と、
前記第1基準電極および前記第2基準電極間の電位差を測定する手段と、
を組み合わせて含むことを特徴とする装置。 - 請求項1に記載の装置において、前記溶液のpHを測定する手段をさらに含むことを特徴とする装置。
- 請求項1に記載の装置において、前記材料が前記ディスクの第2面の上に堆積されることを特徴とする装置。
- 材料の等電pHを決定するための方法において、
回転軸心を有すると共に第1チャンバ内において選択されたpH値を有する溶液内に配備される円形ディスクの1つの面に前記材料を固着するステップと、
前記ディスクを選択された速度で回転するステップと、
前記ディスクの軸心および前記材料の両者の近傍に配備される第1基準電極、および、チューブを介して前記第1チャンバに流体連絡される第2チャンバ内に配備される第2基準電極の間の電位差を測定するステップと、
前記電位差が前記第1基準電極および前記第2基準電極間の休止時電位差に近似的に等しくなるように前記溶液のpHを調整するステップと、
前記電位差が前記休止時電位差に近似的に等しい場合の前記溶液のpHを測定するステップと、
を含むことを特徴とする方法。 - 請求項4に記載の方法において、前記材料がCu2Sbを含むことを特徴とする方法。
- 請求項5に記載の方法において、前記Cu2Sbを円形ディスクの1つの面に固着する前記ステップが堆積法によって行われることを特徴とする方法。
- 請求項6に記載の方法において、前記堆積法が電着法を含むことを特徴とする方法。
- 請求項5に記載の方法において、前記ディスクが約750rpmで回転されることを特徴とする方法。
- 請求項4に記載の方法において、前記溶液がKCl水溶液を含むことを特徴とする方法。
- 請求項4に記載の方法において、前記溶液のpHを調整する前記ステップが、前記溶液のpHを低下させるには塩酸を、前記溶液のpHを高めるには水酸化アンモニウムを用いて行われることを特徴とする方法。
- 被膜材料を基板上に堆積するための方法において、
前記基板の等電pHを決定するステップと、
前記被膜材料の等電pHを決定するステップと、
前記基板の等電pHおよび前記被膜材料の等電pHの間のpHを有する前記被膜材料の溶液を調製するステップと、
前記基板を、前記溶液の中に、前記基板上に前記被膜材料が自己組織化するのに十分な時間浸漬するステップと、
を含むことを特徴とする方法。 - 請求項11に記載の方法において、前記溶液のpHが、近似的に、前記基板の等電pHと前記被膜材料の等電pHとの平均であることを特徴とする方法。
- 請求項11に記載の方法において、前記基板がCu2Sbを含むことを特徴とする方法。
- 請求項11に記載の方法において、前記被膜材料がAlPO4、Al2O3、ZnOおよびBi2O3から選択されることを特徴とする方法。
- 請求項11に記載の方法において、前記基板上の被膜材料の厚さを増大するステップをさらに含むことを特徴とする方法。
- 請求項15に記載の方法において、前記被膜材料の厚さを増大する前記ステップが、前記自己組織化された被膜材料の上に付加的な被膜材料を電気堆積することを含むことを特徴とする方法。
- 請求項16に記載の方法において、前記電着法が電気泳動堆積法を含むことを特徴とする方法。
- 請求項17に記載の方法において、前記基板がCu2Sbを含むことを特徴とする方法。
- 請求項18に記載の方法において、前記Cu2Sbが銅の集電体の上に電気メッキされることを特徴とする方法。
- 請求項15に記載の方法において、前記被膜材料がAlPO4、Al2O3、ZnOおよびBi2O3から選択されることを特徴とする方法。
- 請求項17に記載の方法において、前記基板がCu2Sbを含み、前記自己組織化被膜がAlPO4を含み、かつ、前記Cu2Sb基板上のAlPO4の自己組織化被膜の上へのAlPO4の電気泳動堆積が、開路電位に対して正の電圧における自己組織化被着によって行われることを特徴とする方法。
- 請求項21に記載の方法において、前記電気泳動堆積用の前記被膜材料の溶液が、前記被膜材料の前記自己組織化用に用いた溶液と同じであることを特徴とする方法。
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