JP6956599B2 - 金属ナノワイヤ転写用の金属ナノワイヤ付支持基材及び透明導電フィルムの製造方法 - Google Patents
金属ナノワイヤ転写用の金属ナノワイヤ付支持基材及び透明導電フィルムの製造方法 Download PDFInfo
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- JP6956599B2 JP6956599B2 JP2017217245A JP2017217245A JP6956599B2 JP 6956599 B2 JP6956599 B2 JP 6956599B2 JP 2017217245 A JP2017217245 A JP 2017217245A JP 2017217245 A JP2017217245 A JP 2017217245A JP 6956599 B2 JP6956599 B2 JP 6956599B2
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- metal nanowires
- metal
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- film
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- 239000002184 metal Substances 0.000 title claims description 190
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- 238000012546 transfer Methods 0.000 title claims description 16
- 238000000034 method Methods 0.000 title description 43
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- 239000002042 Silver nanowire Substances 0.000 description 65
- 239000002585 base Substances 0.000 description 59
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- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- XCOHAFVJQZPUKF-UHFFFAOYSA-M octyltrimethylammonium bromide Chemical compound [Br-].CCCCCCCC[N+](C)(C)C XCOHAFVJQZPUKF-UHFFFAOYSA-M 0.000 description 1
- 229910052762 osmium Inorganic materials 0.000 description 1
- SYQBFIAQOQZEGI-UHFFFAOYSA-N osmium atom Chemical compound [Os] SYQBFIAQOQZEGI-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000006174 pH buffer Substances 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
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- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920002312 polyamide-imide Polymers 0.000 description 1
- 229920006393 polyether sulfone Polymers 0.000 description 1
- 239000011112 polyethylene naphthalate Substances 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 229920006324 polyoxymethylene Polymers 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 235000009518 sodium iodide Nutrition 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 description 1
- JRMUNVKIHCOMHV-UHFFFAOYSA-M tetrabutylammonium bromide Chemical compound [Br-].CCCC[N+](CCCC)(CCCC)CCCC JRMUNVKIHCOMHV-UHFFFAOYSA-M 0.000 description 1
- HWCKGOZZJDHMNC-UHFFFAOYSA-M tetraethylammonium bromide Chemical compound [Br-].CC[N+](CC)(CC)CC HWCKGOZZJDHMNC-UHFFFAOYSA-M 0.000 description 1
- YMBCJWGVCUEGHA-UHFFFAOYSA-M tetraethylammonium chloride Chemical compound [Cl-].CC[N+](CC)(CC)CC YMBCJWGVCUEGHA-UHFFFAOYSA-M 0.000 description 1
- DDFYFBUWEBINLX-UHFFFAOYSA-M tetramethylammonium bromide Chemical compound [Br-].C[N+](C)(C)C DDFYFBUWEBINLX-UHFFFAOYSA-M 0.000 description 1
- BGQMOFGZRJUORO-UHFFFAOYSA-M tetrapropylammonium bromide Chemical compound [Br-].CCC[N+](CCC)(CCC)CCC BGQMOFGZRJUORO-UHFFFAOYSA-M 0.000 description 1
- FBEVECUEMUUFKM-UHFFFAOYSA-M tetrapropylazanium;chloride Chemical compound [Cl-].CCC[N+](CCC)(CCC)CCC FBEVECUEMUUFKM-UHFFFAOYSA-M 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- PDSVZUAJOIQXRK-UHFFFAOYSA-N trimethyl(octadecyl)azanium Chemical compound CCCCCCCCCCCCCCCCCC[N+](C)(C)C PDSVZUAJOIQXRK-UHFFFAOYSA-N 0.000 description 1
- AQZSPJRLCJSOED-UHFFFAOYSA-M trimethyl(octyl)azanium;chloride Chemical compound [Cl-].CCCCCCCC[N+](C)(C)C AQZSPJRLCJSOED-UHFFFAOYSA-M 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
Images
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- Laminated Bodies (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
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Description
銀ナノワイヤは、硝酸銀、ハロゲン化四級アンモニウム塩、ポリビニルピロリドン、プロピレングリコールを用いた公知のポリオール法により合成した。
上記銀ナノワイヤ合成液からセラミックろ過膜を用いた公知のクロスフロー法によってメタノールを溶剤として精製した。クロスフローによって精製された銀ナノワイヤメタノール分散液を濃縮し、0.2質量%に調整した。銀ナノワイヤ合成液同様に求めたこの銀ナノワイヤ精製液中の銀ナノワイヤの平均径は32nm、平均長さは22μm、不純物微粒子の質量は0.003質量%であった。クロスフローろ過精製時に銀ナノワイヤの一部が破砕したため、銀ナノワイヤ精製液中の銀ナノワイヤの平均長さは、銀ナノワイヤ合成液中の銀ナノワイヤの平均長さより短くなった。
上記金属ナノワイヤの合成により得られた銀ナノワイヤ合成液(クロスフローろ過精製前)を用いて以下の製造工程により透明導電フィルムを製造した。メンブランタイプのろ過器として、柴田科学社製47mm用メンブレンフィルター装置(フィルターホルダー ガラスフィルターベースタイプ)を用いた。また、セルロース系多孔質フィルムは、47mmφ 孔径0.8μm(カタログ値)のセルロースアセテートタイプのろ材(形式:C080A047A、アドバンテック社製)を用いた。使用する前にろ材を水30mlに5分間浸した後、フィルターベース上部にセット、ファネルをクランプではさんだ。
表1に記載のプレス温度、プレス圧力、プレス時間に変更した以外は実施例1同様の操作により透明導電フィルムを作製し、その評価を行った。結果を表1に示す。
上記銀ナノワイヤ精製液を用いた以外は実施例1と同様の操作により透明導電フィルムを得た。評価結果を表1に示す。
ろ材を孔径が3μm(カタログ値)のセルロースアセテートタイプ(形式:C300A047A、アドバンテック社製)、透明フィルム基材をシクロオレフィンポリマーフィルム(日本ゼオン社製 ZF−14 厚み50μm)に変更した以外は実施例1と同様の操作により透明導電フィルムを得た。結果を表1に示す。
上記銀ナノワイヤ合成液をメタノールで100倍(質量)に希釈し、実施例1で用いたPETフィルムのハードコート層上に塗布、乾燥して表面観察を行った。
ろ材を孔径が1μm(カタログ値)の親水性PTFEタイプ(形式:H100A047A、アドバンテック社製)に変更した以外は実施例5同様の操作により透明導電フィルムの作製を試みた。顕微鏡観察を行った結果、ほとんど銀ナノワイヤの転写はできなかった(目視で観察したPETフィルム上へ転写できた銀ナノワイヤは0%)。
ろ材を孔径が0.8μm(カタログ値)のポリカーボネートタイプ(形式:K080A047A、アドバンテック社製)に変更した以外は実施例5同様の操作により透明導電フィルムの作製を試みたが、目視で観察したPETフィルム上へ転写できた銀ナノワイヤは約20%程度であった。
Claims (5)
- 金属ナノワイヤがセルロース系多孔質フィルム上に堆積されていることを特徴とする金属ナノワイヤ転写用の金属ナノワイヤ付支持基材。
- 前記セルロース系多孔質フィルムの平均孔径が0.01〜10μmである請求項1に記載の金属ナノワイヤ付支持基材。
- 透明フィルム基材上に金属ナノワイヤが堆積した透明導電フィルムの製造方法であって、金属ナノワイヤを含有する分散液を、セルロース系多孔質フィルムを通してろ過して金属ナノワイヤを堆積させ、金属ナノワイヤ付支持基材を準備する工程と、前記金属ナノワイヤ付支持基材に堆積した金属ナノワイヤを透明フィルム基材上へ転写する工程と、を含む透明導電フィルムの製造方法。
- 前記金属ナノワイヤを含有する分散液が、金属ナノワイヤを合成した反応液を水および有機溶剤の少なくとも一種からなる液体により希釈された分散液である請求項3に記載の透明導電フィルムの製造方法。
- 前記転写する工程が前記金属ナノワイヤ付支持基材上に堆積された金属ナノワイヤと前記透明フィルム基材との加圧を含む、請求項3又は4に記載の透明導電フィルムの製造方法。
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