JP6750798B2 - 銀ナノワイヤーベースの透明導電性フィルム形成用のヨウ化物添加剤入り短鎖フッ素系界面活性剤 - Google Patents
銀ナノワイヤーベースの透明導電性フィルム形成用のヨウ化物添加剤入り短鎖フッ素系界面活性剤 Download PDFInfo
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- JP6750798B2 JP6750798B2 JP2019010670A JP2019010670A JP6750798B2 JP 6750798 B2 JP6750798 B2 JP 6750798B2 JP 2019010670 A JP2019010670 A JP 2019010670A JP 2019010670 A JP2019010670 A JP 2019010670A JP 6750798 B2 JP6750798 B2 JP 6750798B2
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- ink
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims description 36
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 title claims description 34
- 239000002042 Silver nanowire Substances 0.000 title claims description 29
- 239000004094 surface-active agent Substances 0.000 title claims description 24
- 239000000654 additive Substances 0.000 title claims description 12
- 230000000996 additive effect Effects 0.000 title claims description 9
- 239000000203 mixture Substances 0.000 claims description 47
- 238000009472 formulation Methods 0.000 claims description 41
- 239000008199 coating composition Substances 0.000 claims description 33
- 229910052709 silver Inorganic materials 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- -1 -OH Chemical group 0.000 claims description 22
- 239000004332 silver Substances 0.000 claims description 21
- 239000012535 impurity Substances 0.000 claims description 19
- 239000000126 substance Substances 0.000 claims description 13
- 239000002086 nanomaterial Substances 0.000 claims description 12
- 125000001153 fluoro group Chemical group F* 0.000 claims description 11
- 229910052739 hydrogen Inorganic materials 0.000 claims description 11
- 239000001257 hydrogen Substances 0.000 claims description 9
- 239000004034 viscosity adjusting agent Substances 0.000 claims description 8
- 239000002270 dispersing agent Substances 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims description 5
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 4
- 239000006184 cosolvent Substances 0.000 claims description 4
- 229910052731 fluorine Inorganic materials 0.000 claims description 4
- 239000011737 fluorine Substances 0.000 claims description 4
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 4
- XMBWDFGMSWQBCA-UHFFFAOYSA-M iodide Chemical compound [I-] XMBWDFGMSWQBCA-UHFFFAOYSA-M 0.000 claims description 2
- 229940006461 iodide ion Drugs 0.000 claims description 2
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- HSZCZNFXUDYRKD-UHFFFAOYSA-M lithium iodide Chemical compound [Li+].[I-] HSZCZNFXUDYRKD-UHFFFAOYSA-M 0.000 description 19
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- 238000002834 transmittance Methods 0.000 description 4
- JKFYKCYQEWQPTM-UHFFFAOYSA-N 2-azaniumyl-2-(4-fluorophenyl)acetate Chemical compound OC(=O)C(N)C1=CC=C(F)C=C1 JKFYKCYQEWQPTM-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
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- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 2
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- 229920002274 Nalgene Polymers 0.000 description 1
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- NNLVGZFZQQXQNW-ADJNRHBOSA-N [(2r,3r,4s,5r,6s)-4,5-diacetyloxy-3-[(2s,3r,4s,5r,6r)-3,4,5-triacetyloxy-6-(acetyloxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6s)-4,5,6-triacetyloxy-2-(acetyloxymethyl)oxan-3-yl]oxyoxan-2-yl]methyl acetate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](OC(C)=O)[C@H]1OC(C)=O)O[C@H]1[C@@H]([C@@H](OC(C)=O)[C@H](OC(C)=O)[C@@H](COC(C)=O)O1)OC(C)=O)COC(=O)C)[C@@H]1[C@@H](COC(C)=O)O[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@H]1OC(C)=O NNLVGZFZQQXQNW-ADJNRHBOSA-N 0.000 description 1
- 150000001241 acetals Chemical class 0.000 description 1
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- 125000000524 functional group Chemical group 0.000 description 1
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- 125000001183 hydrocarbyl group Chemical group 0.000 description 1
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- LZKLAOYSENRNKR-LNTINUHCSA-N iron;(z)-4-oxoniumylidenepent-2-en-2-olate Chemical compound [Fe].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O LZKLAOYSENRNKR-LNTINUHCSA-N 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
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- FVAUCKIRQBBSSJ-UHFFFAOYSA-M sodium iodide Chemical compound [Na+].[I-] FVAUCKIRQBBSSJ-UHFFFAOYSA-M 0.000 description 1
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- ISXSCDLOGDJUNJ-UHFFFAOYSA-N tert-butyl prop-2-enoate Chemical compound CC(C)(C)OC(=O)C=C ISXSCDLOGDJUNJ-UHFFFAOYSA-N 0.000 description 1
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- H—ELECTRICITY
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- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
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- Inorganic Chemistry (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
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Description
(1)化学式(I):
で表される短鎖フッ素系界面活性剤と、
(2)前記短鎖フッ素系界面活性剤の略3質量%未満の量の、化学式(II)で表される不純物と、
(3)前記短鎖フッ素系界面活性剤の略0.5−2.5%の量のヨウ化物を与えるヨウ化物添加剤と、を備える、精製された界面活性剤配合物であって、
mは0,1,2,3,4または5であり;
nは1,2,3または4であり;
Xは−O−;−S−;または直接結合であり;
Yは水素、−OH、またはフルオロであり;
Zは−CH3,−CH2F,−CHF2または−CF3であり;
M+はLi+,Na+,K+,H+またはNH4 +であり;かつ、
それぞれR1,R2,R3,R4およびR5は、同じまたは異なる、独立したフルオロまたは水素を示す、精製された界面活性剤配合物を提供する。
(1)化学式(I):
で表される短鎖フッ素系界面活性剤と、
(2)前記短鎖フッ素系界面活性剤の略3質量%未満の量の、化学式(II)で表され
(3)前記短鎖フッ素系界面活性剤の略0.5−2.5%の量のヨウ化物を与えるヨウ化物添加剤と、を備える、精製された界面活性剤配合物であって、
mは0,1,2,3,4,または5であり;
nは1,2,3,または4であり;
Xは−O−;−S−;または直接結合であり;
Yは水素、−OHまたはフルオロであり;
Zは−CH3,−CH2F,−CHF2または−CF3であり;
M+はLi+,Na+,K+,H+またはNH4 +であり;かつ、
それぞれR1,R2,R3,R4およびR5は、同じまたは異なる、独立したフルオロまたは水素を示す、精製された界面活性剤配合物を指向する。
(1)a.複数の銀ナノワイヤーと;
b.粘度調整剤と;
c.任意の分散剤と;
d.水を含む液体キャリアと;
を含むナノワイヤー配合物を含む第1の容器と、
(2)上述の、精製された界面活性剤配合物を含む第2の容器と、
を備える銀ナノワイヤーコーティング用の2パートのキットであって、
そのうち、
ナノワイヤー含有配合物は1質量%の前記銀ナノワイヤーに対して0.005−0.02質量%の銀イオンを備え;
前記精製された界面活性剤配合物は、前記ナノワイヤー含有配合物における銀イオンに対して略等モル量のヨウ化物イオンを備える、2パートのキットを開示する。
[短鎖フッ素系界面活性剤の精製]
特定のフッ素系界面活性剤内に存在する不純物は、コーティング性能への悪い影響をもちうる。市販の短鎖フッ素系界面活性剤(Hexafor612N)内の知られている不純物の一つは、未反応の3−メルカプトプロピオン酸(3-mercaptopropionic acid)で、これは銀ナノワイヤーを不動態化する可能性があり、それゆえワイヤーとワイヤーの接触を低下させることでネットワークを非伝導性にする。流入する原料を精製することは、ナノワイヤーネットワーク生成に否定的に作用する全ての成分が、最終コーティング組成物を配合するより前に除かれることを確実にすることができる。これはまた、全てのコーティング成分の、ロット毎の一貫性についての信頼性を確かにするものでもある。
[ヨウ化物添加剤付きの精製されたフッ素系界面活性剤配合物]
0.1341kgの99.995%ヨウ化リチウム(Aldrich, St Louis MO)は、実施例1における、精製された25%のHexafor612Nが50%IPA/25%H2O中にある溶液に加えられ、140rpmで30分撹拌された。結果物のフッ素系界面活性剤配合物は4500ppmのLiIを含む。
[精製された25%のHexafor612Nと4500ppmのLiIを含むインク1配合物]
0.735kgのインク濃縮物は0.136%の銀(Ag)と0.28%のMethocell 311 バインダ(Dow Chemical, Midland Ml)と、175ppmのFS-3100(Dupont Wilmington, DE)とを含み、初めに1.264kgの脱イオン水を加えて希釈された。希釈溶液は500rpmで5分混合された。
[未精製の25%のHexafor612Nと4500ppmのLiIを含むインク2配合物]
0.735kgのインク濃縮物は0.136%の銀(Ag)と0.28%のMethocell 311 バインダ(Dow Chemical, Midland Ml)と、175ppmのFS-3100(Dupont Wilmington, DE)とを含み、初めに1.264kgの脱イオン水を加えて希釈された。希釈溶液は500rpmで5分混合された。
[インク1およびインク2から形成した導電性フィルムの比較結果]
インク1とインク2は、PETフィルム(たとえば、MELINEX-454またはTORAY U483)上に、スロットダイ・ロールツーロールコーティング方式によって別々に塗布された。それぞれのインクはコーティング前に−28“Hgで30分脱気された。それぞれのインクは、それから15ml/分の流量で塗布され、40℃、60℃、そして90℃でそれぞれ1分乾燥させられた。乾燥後、試料は2MPaの圧力で薄層化された。
示された通り、未精製のHexafor612Nを含むインク2から生成したフィルムは、不動態化させる不純物のために非導電性のフィルムとなった。対照的に、インク1は、配合前にHexafor612Nを精製したことのみがインク2と異なっていたが、十分なシート抵抗とヘイズ特性をもった導電性ネットワークを形成した。
[コーティング欠陥の減少]
本実施例は、短鎖フッ素系界面活性剤によって、欠陥レベルがZONYL(登録商標)FSAに比べて著しく減少したことを示す。
FSAに比べ、ナノワイヤーインクの気泡欠陥に関してかなり低い傾向をもつ。加えて、精製済みHexafor612Nもまた、粒子欠陥レベルを下げる。
[ヨウ化物添加剤の安定化効果]
この例は、ヨウ化物のようなアニオンが最終コーティング組成物に付加するとき、銀カチオンにヨウ化物イオンが結合し得るために、結果物の導電性フィルムが信頼性の向上を示すことを実証する。信頼性試験の条件は85℃、乾燥、周囲の室内照明および蛍光である。
[Ag+]含有量:1%の銀に対して0.014%のAg+
コーティング組成物中の[Ag]は0.05%の銀、従って[Ag+]含有量は0.014%×0.05%Ag/1%Ag=0.0007%
Ag+モル=[Ag+]/Ag分子量(M.W.)=0.0007%/108=6.5×10−8
[I−]=0.000353/25%×0.004500=6.354×10−6
I−モル=[I−]/I分子量=6.354×10−6/127=5×10−8
Ag+/I−モル比=6.5×10−8/5×10−8=1.3/1
Claims (16)
- 導電性ナノ構造体および、精製された界面活性剤配合物を含有するコーティング組成物であって、
前記精製された界面活性剤配合物は
(1)化学式(I):
で表される短鎖フッ素系界面活性剤と、
(2)前記短鎖フッ素系界面活性剤の3質量%未満の量の、化学式(II)で表される不純物と、
(3)前記短鎖フッ素系界面活性剤の0.5−2.5質量%の量のヨウ化物を与えるヨウ化物添加剤と、を備え、ここで、
mは0,1,2,3,4または5であり;
nは1,2,3または4であり;
Xは−O−;−S−;または直接結合であり;
Yは水素、−OH、またはフルオロであり;
Zは−CH3,−CH2F,−CHF2または−CF3であり;
M+はLi+,Na+,K+,H+またはNH4 +であり;かつ、
それぞれR1,R2,R3,R4およびR5は、同じまたは異なる、独立したフルオロまたは水素を示す、
コーティング組成物。 - 化学式(I)の前記短鎖フッ素系界面活性剤が6個以下のフルオロベアリング炭素を有する、
請求項1に記載のコーティング組成物。 - Xが直接結合である、
請求項1または2に記載のコーティング組成物。 - Yが−OHである、
請求項1に記載のコーティング組成物。 - Zが−CF3である、
請求項1に記載のコーティング組成物。 - nが2である、
請求項1に記載のコーティング組成物。 - 化学式(II)の不純物が前記フッ素系界面活性剤の0.4質量%よりも少ない、
請求項1に記載のコーティング組成物。 - 前記精製されたフッ素系界面活性剤配合物中のヨウ化物が前記フッ素系界面活性剤の0.6−2.4質量%である、
請求項1に記載のコーティング組成物。 - 前記導電性ナノ構造体は、銀ナノワイヤーを含む、
請求項1に記載のコーティング組成物。 - 粘度調整剤をさらに含み、
前記銀ナノワイヤーと前記粘度調整剤の比は、0.00626から5である、
請求項9に記載のコーティング組成物。 - 前記コーティング組成物は、1質量%の前記銀ナノワイヤーに対して0.005−0.02質量%の銀イオンを備える、
請求項9に記載のコーティング組成物。 - 精製された界面活性剤配合物は、銀イオンに対して略等モル量のヨウ化物イオンを備える、
請求項11に記載のコーティング組成物。 - 銀ナノワイヤーは、30nm以下の直径および、5μm以上より長い、
請求項9に記載のコーティング組成物。 - 分散剤をさらに含む、
請求項1に記載のコーティング組成物。 - 液体キャリアをさらに含む、
請求項1に記載のコーティング組成物。 - 前記液体キャリアは、水または、水混和性共溶媒を含む、
請求項15に記載のコーティング組成物。
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