CN103192092A - Method for manufacturing silver nanowire - Google Patents
Method for manufacturing silver nanowire Download PDFInfo
- Publication number
- CN103192092A CN103192092A CN2013101521571A CN201310152157A CN103192092A CN 103192092 A CN103192092 A CN 103192092A CN 2013101521571 A CN2013101521571 A CN 2013101521571A CN 201310152157 A CN201310152157 A CN 201310152157A CN 103192092 A CN103192092 A CN 103192092A
- Authority
- CN
- China
- Prior art keywords
- silver
- acid
- manufacture method
- wire
- nano silver
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 238000000034 method Methods 0.000 title claims abstract description 55
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 34
- 239000002042 Silver nanowire Substances 0.000 title abstract 5
- 239000000243 solution Substances 0.000 claims abstract description 34
- 229910052709 silver Inorganic materials 0.000 claims abstract description 28
- 239000004332 silver Substances 0.000 claims abstract description 28
- -1 silver ions Chemical class 0.000 claims abstract description 24
- 239000003223 protective agent Substances 0.000 claims abstract description 22
- 239000002243 precursor Substances 0.000 claims abstract description 21
- 239000000654 additive Substances 0.000 claims abstract description 20
- 230000000996 additive effect Effects 0.000 claims abstract description 20
- 150000001875 compounds Chemical class 0.000 claims abstract description 19
- 239000011259 mixed solution Substances 0.000 claims abstract description 19
- 150000003839 salts Chemical class 0.000 claims abstract description 10
- 150000004820 halides Chemical class 0.000 claims abstract description 7
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 42
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 claims description 26
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 26
- 150000002148 esters Chemical class 0.000 claims description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- 235000011187 glycerol Nutrition 0.000 claims description 21
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 21
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 21
- 238000002347 injection Methods 0.000 claims description 15
- 239000007924 injection Substances 0.000 claims description 15
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 13
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 claims description 12
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 12
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 12
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 claims description 12
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 12
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 11
- 150000005846 sugar alcohols Polymers 0.000 claims description 11
- 239000002904 solvent Substances 0.000 claims description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 9
- 150000002170 ethers Chemical class 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 239000011734 sodium Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 7
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 claims description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 6
- SVTBMSDMJJWYQN-UHFFFAOYSA-N 2-methylpentane-2,4-diol Chemical compound CC(O)CC(C)(C)O SVTBMSDMJJWYQN-UHFFFAOYSA-N 0.000 claims description 6
- 101710134784 Agnoprotein Proteins 0.000 claims description 6
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims description 6
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 6
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 claims description 6
- 241001274216 Naso Species 0.000 claims description 6
- 241001311547 Patina Species 0.000 claims description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 6
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 6
- 229910021612 Silver iodide Inorganic materials 0.000 claims description 6
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 6
- DGEZNRSVGBDHLK-UHFFFAOYSA-N [1,10]phenanthroline Chemical group C1=CN=C2C3=NC=CC=C3C=CC2=C1 DGEZNRSVGBDHLK-UHFFFAOYSA-N 0.000 claims description 6
- LDHQCZJRKDOVOX-NSCUHMNNSA-N crotonic acid Chemical compound C\C=C\C(O)=O LDHQCZJRKDOVOX-NSCUHMNNSA-N 0.000 claims description 6
- XLLIQLLCWZCATF-UHFFFAOYSA-N ethylene glycol monomethyl ether acetate Natural products COCCOC(C)=O XLLIQLLCWZCATF-UHFFFAOYSA-N 0.000 claims description 6
- 239000001530 fumaric acid Substances 0.000 claims description 6
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 claims description 6
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 6
- 239000011976 maleic acid Substances 0.000 claims description 6
- 239000000178 monomer Substances 0.000 claims description 6
- 150000002825 nitriles Chemical class 0.000 claims description 6
- ZWRUINPWMLAQRD-UHFFFAOYSA-N nonan-1-ol Chemical compound CCCCCCCCCO ZWRUINPWMLAQRD-UHFFFAOYSA-N 0.000 claims description 6
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 6
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 6
- ADZWSOLPGZMUMY-UHFFFAOYSA-M silver bromide Chemical compound [Ag]Br ADZWSOLPGZMUMY-UHFFFAOYSA-M 0.000 claims description 6
- LFAGQMCIGQNPJG-UHFFFAOYSA-N silver cyanide Chemical compound [Ag+].N#[C-] LFAGQMCIGQNPJG-UHFFFAOYSA-N 0.000 claims description 6
- REYHXKZHIMGNSE-UHFFFAOYSA-M silver monofluoride Chemical compound [F-].[Ag+] REYHXKZHIMGNSE-UHFFFAOYSA-M 0.000 claims description 6
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 claims description 6
- 229910001494 silver tetrafluoroborate Inorganic materials 0.000 claims description 6
- RHUVFRWZKMEWNS-UHFFFAOYSA-M silver thiocyanate Chemical compound [Ag+].[S-]C#N RHUVFRWZKMEWNS-UHFFFAOYSA-M 0.000 claims description 6
- 239000011780 sodium chloride Substances 0.000 claims description 6
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 6
- HNEGQIOMVPPMNR-IHWYPQMZSA-N citraconic acid Chemical compound OC(=O)C(/C)=C\C(O)=O HNEGQIOMVPPMNR-IHWYPQMZSA-N 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- LZDKZFUFMNSQCJ-UHFFFAOYSA-N 1,2-diethoxyethane Chemical compound CCOCCOCC LZDKZFUFMNSQCJ-UHFFFAOYSA-N 0.000 claims description 3
- ZXSQEZNORDWBGZ-UHFFFAOYSA-N 1,3-dihydropyrrolo[2,3-b]pyridin-2-one Chemical compound C1=CN=C2NC(=O)CC2=C1 ZXSQEZNORDWBGZ-UHFFFAOYSA-N 0.000 claims description 3
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 3
- 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 claims description 3
- OQXSRALAOPBHPM-UHFFFAOYSA-N 2-hydroxypropanoic acid;silver Chemical compound [Ag].CC(O)C(O)=O OQXSRALAOPBHPM-UHFFFAOYSA-N 0.000 claims description 3
- LSRPLKNLQGMCNR-UHFFFAOYSA-N 2-methyl-6-sulfohex-2-enoic acid Chemical compound OC(=O)C(C)=CCCCS(O)(=O)=O LSRPLKNLQGMCNR-UHFFFAOYSA-N 0.000 claims description 3
- BRYKBDMLJJLFAB-UHFFFAOYSA-N 4-methylbenzenesulfonic acid;silver Chemical compound [Ag].CC1=CC=C(S(O)(=O)=O)C=C1 BRYKBDMLJJLFAB-UHFFFAOYSA-N 0.000 claims description 3
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N Butyraldehyde Chemical compound CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 claims description 3
- HKFZNXOQLIDTCS-UHFFFAOYSA-M C(CC)(=O)[O-].[Ag+].[F] Chemical compound C(CC)(=O)[O-].[Ag+].[F] HKFZNXOQLIDTCS-UHFFFAOYSA-M 0.000 claims description 3
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 claims description 3
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 claims description 3
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 3
- 108010010803 Gelatin Proteins 0.000 claims description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- LSDPWZHWYPCBBB-UHFFFAOYSA-N Methanethiol Chemical compound SC LSDPWZHWYPCBBB-UHFFFAOYSA-N 0.000 claims description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical class CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 3
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 claims description 3
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 claims description 3
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 claims description 3
- YNPNZTXNASCQKK-UHFFFAOYSA-N Phenanthrene Natural products C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 claims description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical class CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 3
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 3
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 3
- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 claims description 3
- 150000008065 acid anhydrides Chemical class 0.000 claims description 3
- 150000001298 alcohols Chemical class 0.000 claims description 3
- 229940037003 alum Drugs 0.000 claims description 3
- CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical compound CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 0.000 claims description 3
- 239000003153 chemical reaction reagent Substances 0.000 claims description 3
- PDXRQENMIVHKPI-UHFFFAOYSA-N cyclohexane-1,1-diol Chemical compound OC1(O)CCCCC1 PDXRQENMIVHKPI-UHFFFAOYSA-N 0.000 claims description 3
- IWQOYCSYXWODEB-UHFFFAOYSA-N decanoic acid;silver Chemical compound [Ag].CCCCCCCCCC(O)=O IWQOYCSYXWODEB-UHFFFAOYSA-N 0.000 claims description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 3
- KZNICNPSHKQLFF-UHFFFAOYSA-N dihydromaleimide Natural products O=C1CCC(=O)N1 KZNICNPSHKQLFF-UHFFFAOYSA-N 0.000 claims description 3
- FANSKVBLGRZAQA-UHFFFAOYSA-M dipotassium;sulfanide Chemical compound [SH-].[K+].[K+] FANSKVBLGRZAQA-UHFFFAOYSA-M 0.000 claims description 3
- JRBPAEWTRLWTQC-UHFFFAOYSA-N dodecylamine Chemical compound CCCCCCCCCCCCN JRBPAEWTRLWTQC-UHFFFAOYSA-N 0.000 claims description 3
- UPUANNBILBRCST-UHFFFAOYSA-N ethanol;ethene Chemical compound C=C.CCO UPUANNBILBRCST-UHFFFAOYSA-N 0.000 claims description 3
- 239000008273 gelatin Substances 0.000 claims description 3
- 229920000159 gelatin Polymers 0.000 claims description 3
- 235000019322 gelatine Nutrition 0.000 claims description 3
- 235000011852 gelatine desserts Nutrition 0.000 claims description 3
- 239000000174 gluconic acid Substances 0.000 claims description 3
- 235000012208 gluconic acid Nutrition 0.000 claims description 3
- 229940051250 hexylene glycol Drugs 0.000 claims description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 3
- 229920000609 methyl cellulose Polymers 0.000 claims description 3
- 239000001923 methylcellulose Substances 0.000 claims description 3
- 238000005453 pelletization Methods 0.000 claims description 3
- UWJJYHHHVWZFEP-UHFFFAOYSA-N pentane-1,1-diol Chemical compound CCCCC(O)O UWJJYHHHVWZFEP-UHFFFAOYSA-N 0.000 claims description 3
- 229920000642 polymer Polymers 0.000 claims description 3
- 229940072033 potash Drugs 0.000 claims description 3
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 3
- 235000015320 potassium carbonate Nutrition 0.000 claims description 3
- 239000001103 potassium chloride Substances 0.000 claims description 3
- 235000011164 potassium chloride Nutrition 0.000 claims description 3
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 3
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 3
- BHZRJJOHZFYXTO-UHFFFAOYSA-L potassium sulfite Chemical compound [K+].[K+].[O-]S([O-])=O BHZRJJOHZFYXTO-UHFFFAOYSA-L 0.000 claims description 3
- 235000011151 potassium sulphates Nutrition 0.000 claims description 3
- 235000019252 potassium sulphite Nutrition 0.000 claims description 3
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 3
- ULWHHBHJGPPBCO-UHFFFAOYSA-N propane-1,1-diol Chemical class CCC(O)O ULWHHBHJGPPBCO-UHFFFAOYSA-N 0.000 claims description 3
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 3
- 235000013772 propylene glycol Nutrition 0.000 claims description 3
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 claims description 3
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 3
- MCJGNVYPOGVAJF-UHFFFAOYSA-N quinolin-8-ol Chemical compound C1=CN=C2C(O)=CC=CC2=C1 MCJGNVYPOGVAJF-UHFFFAOYSA-N 0.000 claims description 3
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 claims description 3
- 229940071536 silver acetate Drugs 0.000 claims description 3
- XQLMNMQWVCXIKR-UHFFFAOYSA-M silver bromate Chemical compound [Ag+].[O-]Br(=O)=O XQLMNMQWVCXIKR-UHFFFAOYSA-M 0.000 claims description 3
- LKZMBDSASOBTPN-UHFFFAOYSA-L silver carbonate Substances [Ag].[O-]C([O-])=O LKZMBDSASOBTPN-UHFFFAOYSA-L 0.000 claims description 3
- 229910001958 silver carbonate Inorganic materials 0.000 claims description 3
- SDLBJIZEEMKQKY-UHFFFAOYSA-M silver chlorate Chemical compound [Ag+].[O-]Cl(=O)=O SDLBJIZEEMKQKY-UHFFFAOYSA-M 0.000 claims description 3
- 229940071575 silver citrate Drugs 0.000 claims description 3
- 229940098221 silver cyanide Drugs 0.000 claims description 3
- 229940096017 silver fluoride Drugs 0.000 claims description 3
- 229940045105 silver iodide Drugs 0.000 claims description 3
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 3
- KKKDGYXNGYJJRX-UHFFFAOYSA-M silver nitrite Chemical compound [Ag+].[O-]N=O KKKDGYXNGYJJRX-UHFFFAOYSA-M 0.000 claims description 3
- 229910001923 silver oxide Inorganic materials 0.000 claims description 3
- FJOLTQXXWSRAIX-UHFFFAOYSA-K silver phosphate Chemical compound [Ag+].[Ag+].[Ag+].[O-]P([O-])([O-])=O FJOLTQXXWSRAIX-UHFFFAOYSA-K 0.000 claims description 3
- YPNVIBVEFVRZPJ-UHFFFAOYSA-L silver sulfate Chemical compound [Ag+].[Ag+].[O-]S([O-])(=O)=O YPNVIBVEFVRZPJ-UHFFFAOYSA-L 0.000 claims description 3
- WYCFMBAHFPUBDS-UHFFFAOYSA-L silver sulfite Chemical compound [Ag+].[Ag+].[O-]S([O-])=O WYCFMBAHFPUBDS-UHFFFAOYSA-L 0.000 claims description 3
- ZYXPMOIHQRKWGT-UHFFFAOYSA-N silver;2,2,2-trifluoroacetic acid Chemical compound [Ag].OC(=O)C(F)(F)F ZYXPMOIHQRKWGT-UHFFFAOYSA-N 0.000 claims description 3
- DOQQTKLDEQSKIE-UHFFFAOYSA-N silver;isocyanate Chemical compound [Ag+].[N-]=C=O DOQQTKLDEQSKIE-UHFFFAOYSA-N 0.000 claims description 3
- CYLMOXYXYHNGHZ-UHFFFAOYSA-M silver;propanoate Chemical compound [Ag+].CCC([O-])=O CYLMOXYXYHNGHZ-UHFFFAOYSA-M 0.000 claims description 3
- FSJWWSXPIWGYKC-UHFFFAOYSA-M silver;silver;sulfanide Chemical compound [SH-].[Ag].[Ag+] FSJWWSXPIWGYKC-UHFFFAOYSA-M 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- FVAUCKIRQBBSSJ-UHFFFAOYSA-M sodium iodide Chemical compound [Na+].[I-] FVAUCKIRQBBSSJ-UHFFFAOYSA-M 0.000 claims description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 3
- 235000011152 sodium sulphate Nutrition 0.000 claims description 3
- 235000010265 sodium sulphite Nutrition 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 229960002317 succinimide Drugs 0.000 claims description 3
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 claims description 3
- QUTYHQJYVDNJJA-UHFFFAOYSA-K trisilver;2-hydroxypropane-1,2,3-tricarboxylate Chemical compound [Ag+].[Ag+].[Ag+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O QUTYHQJYVDNJJA-UHFFFAOYSA-K 0.000 claims description 3
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 3
- NLVXSWCKKBEXTG-UHFFFAOYSA-N vinylsulfonic acid Chemical compound OS(=O)(=O)C=C NLVXSWCKKBEXTG-UHFFFAOYSA-N 0.000 claims description 3
- 229940111121 antirheumatic drug quinolines Drugs 0.000 claims description 2
- 238000012423 maintenance Methods 0.000 claims description 2
- 150000003248 quinolines Chemical class 0.000 claims description 2
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 229940100890 silver compound Drugs 0.000 abstract 1
- 150000003379 silver compounds Chemical class 0.000 abstract 1
- 238000009826 distribution Methods 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- GNWBLLYJQXKPIP-ZOGIJGBBSA-N (1s,3as,3bs,5ar,9ar,9bs,11as)-n,n-diethyl-6,9a,11a-trimethyl-7-oxo-2,3,3a,3b,4,5,5a,8,9,9b,10,11-dodecahydro-1h-indeno[5,4-f]quinoline-1-carboxamide Chemical compound CN([C@@H]1CC2)C(=O)CC[C@]1(C)[C@@H]1[C@@H]2[C@@H]2CC[C@H](C(=O)N(CC)CC)[C@@]2(C)CC1 GNWBLLYJQXKPIP-ZOGIJGBBSA-N 0.000 description 1
- DPBJAVGHACCNRL-UHFFFAOYSA-N 2-(dimethylamino)ethyl prop-2-enoate Chemical compound CN(C)CCOC(=O)C=C DPBJAVGHACCNRL-UHFFFAOYSA-N 0.000 description 1
- GHUXAYLZEGLXDA-UHFFFAOYSA-N 8-azido-5-ethyl-6-phenylphenanthridin-5-ium-3-amine;bromide Chemical compound [Br-].C12=CC(N=[N+]=[N-])=CC=C2C2=CC=C(N)C=C2[N+](CC)=C1C1=CC=CC=C1 GHUXAYLZEGLXDA-UHFFFAOYSA-N 0.000 description 1
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- ZTWTYVWXUKTLCP-UHFFFAOYSA-L ethenyl-dioxido-oxo-$l^{5}-phosphane Chemical compound [O-]P([O-])(=O)C=C ZTWTYVWXUKTLCP-UHFFFAOYSA-L 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- MRNHPUHPBOKKQT-UHFFFAOYSA-N indium;tin;hydrate Chemical compound O.[In].[Sn] MRNHPUHPBOKKQT-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 1
- 230000002572 peristaltic effect Effects 0.000 description 1
- 150000004040 pyrrolidinones Chemical class 0.000 description 1
- LISFMEBWQUVKPJ-UHFFFAOYSA-N quinolin-2-ol Chemical class C1=CC=C2NC(=O)C=CC2=C1 LISFMEBWQUVKPJ-UHFFFAOYSA-N 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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Abstract
The invention discloses a method for manfuacturing a silver nanowire, and the method comprises the following steps of: (a) providing a mixed solution, wherein the mixed solution at least contains a protective agent and an additive, and the additive is a halide or a compound capable of generating an insoluble salt with silver ions; (b) providing a silver precursor solution containing silver compounds, and adding the precursor solution in the mixed solution at least in twice; and (c) separating to obtain the silver nanowire. The method for manufacturing a silver nanowire has the beneficial effects that the protective agent is adopted at first, and then the silver precursor solution is added at least in twice rather than one time, the silver nanowire with high wire diameter ratio and suitability for production in a large scale can be obtained.
Description
Technical field
The present invention relates to a kind of manufacture method of nano silver wire, belong to Metallic Functional Materials, technical field of nano material.
Background technology
Nano silver wire has optical clear and high conductivity in the visible-range, can be used for preparing transparent conductive film, is used for industries such as touch-screen, Organic Light Emitting Diode (OLED) and solar cell.Also can be used as simultaneously electrocondution slurry, be used for printed circuit etc.
Nano silver wire was more and more paid close attention to by people in the last few years owing to its high conductivity and potential application widely.The preparation method of nano silver wire is also varied, for example hydro-thermal method, polyalcohol method or template etc.Yet, take all factors into consideration operability, cost and the productive rate etc. of experiment, the polyalcohol method is because it is simple to operate, productive rate is high and with low cost, and paid close attention to by increasing people and developed.But existing polyalcohol fado adopts the polyalcohol that silver salt and protective agent is injected simultaneously high temperature, and gained nano silver wire line footpath is thick, line length is short, distribution is wide in range, and is difficult to mass production, can not satisfy real needs.
Therefore, be necessary the manufacture method of existing nano silver wire is improved, to overcome above technical problem.
Summary of the invention
The object of the present invention is to provide a kind of have high line directly than the manufacture method of nano silver wire.
Realize above-mentioned purpose for solving, the present invention adopts following technical scheme: a kind of manufacture method of nano silver wire, it comprises the steps:
(a). mixed solution is provided, contains a kind of protective agent and a kind of additive in this mixed solution at least, described additive is halide and/or the compound that can form property salt hard to tolerate with silver ion;
(b). the silver-colored precursor solution that contains the patina thing is provided, and should will divide at least twice to join in the described mixed solution by the silver precursor solution;
(c). separate obtaining described nano silver wire.
As further improved technical scheme of the present invention: in step (a), described protective agent is:
The polyvinylpyrrolidone of various molecular weight (PVP, (C
6H
9NO) n), the derivative of polyvinylpyrrolidone, polyvinyl alcohol (PVA, (C
2H
4O) n), PEO (PEO, (CH
2CH
2O) lauryl sodium sulfate (C n),
12H
25SO
4Na), lauryl amine (C
12H
27N), octadecylamine (CH
3(CH
2)
16CH
2NH
2), hexadecyltrimethylammonium chloride (CTAC, C
16H
33(CH
3)
3NCl), softex kw (CTAB, C
16H
33(CH
3)
3NBr), gelatin, methylcellulose, the ninth of the ten Heavenly Stems two mercaptan, succinimide mercaptans; Perhaps
Contain sulfydryl or amino protective agent; Perhaps
By the polymer that following one or several monomers form, described monomer comprises:
Acrylic acid (C
3H
4O
2), butenoic acid (C
4H
6O
2), maleic acid (C
4H
4O
4), methyl-maleic acid, fumaric acid and its esters;
Contain aforesaid propylene acid (C
3H
4O
2), butenoic acid (C
4H
6O
2), maleic acid (C
4H
4O
4), ester class, amide-type, acid anhydrides, the nitrile of methyl-maleic acid, fumaric acid and salts substances thereof;
Acrylic sulfonic acid, vinyl sulfonic acid, metering system sulfonic acid, 3-sulfopropyl methacrylic acid and the ester class, amide-type, the nitrile that contain phosphonate radical;
N-ethernamine class;
Ethene acetal, ethene butyral, ethene ethanol and ethers thereof, ester class.
As further improved technical scheme of the present invention: in step (a), described halide includes but not limited to sodium chloride (NaCl), potassium chloride (KCl), sodium bromide (NaBr), KBr (KBr), sodium iodide (NaI), KI (KI), softex kw (CTAB, C
16H
33(CH
3)
3NBr), hexadecyltrimethylammonium chloride (CTAC, C
16H
33(CH
3)
3NCl).
As further improved technical scheme of the present invention: in step (a), describedly can include but not limited to sodium sulphate (NaSO with the compound that silver ion forms property salt hard to tolerate
4), potassium sulfate (KSO
4), sodium sulfite (NaSO
3), potassium sulfite (KSO
3), sodium carbonate (NaCO
3), potash (KCO
3), sodium phosphate (Na
3PO
4), potassium phosphate (K
3PO
4), vulcanized sodium (Na
2S), potassium sulfide (K
2S).
As further improved technical scheme of the present invention: in step (b), described patina thing is silver nitrate (AgNO
3), silver nitrite (AgNO
2), silver oxide (AgO), silver carbonate (AgCO
3), silver acetate (CH
3COOAg), toillen's reagent ([Ag(NH
3)
2] OH), silver cyanide (AgCN), silver sulfate (Ag
2SO
4), silver sulfide (Ag
2S), trifluoroacetic acid silver (C
2F
3O
2Ag), silver thiocyanate (AgSCN), silver chlorate (AgCl), silver bromide (AgBr), silver sulfite (Ag
2SO
3), silver iodide (AgI), silver orthophosphate (Ag
3PO
4), silver fluoride (AgF), silver tetrafluoroborate (AgBF
4), pelletization silver (Ag
3N), silver propionate (C
3H
5O
2Ag), actol (C
3H
5AgO
3), capric acid silver, carboxylic first silver, silver citrate (C
6H
5Ag
3O
7), gluconic acid silver, silver cyanate (AgOCN), silver bromate (AgBrO
3), hyptafluorobutyric acid silver (CF
3CF
2CF
2CO
2Ag), acetylacetone,2,4-pentanedione silver ([CH
3COCH=C (O-) CH
3] Ag), five fluorine silver propionate (C
2F
5CO
2Ag), inclined to one side alum acid silver (AgVO
3), hexafluoroarsenate silver (AgAsF
6), hexafluorophosphoric acid silver (AgPF
6), p-methyl benzenesulfonic acid silver (CH
3C
6H
4SO
3Ag), silver tetrafluoroborate (AgBF
4), complex compound Ag (I) and the part NH of silver
3-, CN-, Cl-, S
2O
3-generation complex compound, Ag[II] generate complex compound, Ag[III with part Py (pyridine), an adjacent phenanthroline (0 one phen), 8 monohydroxy quinolines (oxin)] and part F-, IO
4-, TeO
66-generation complex compound.
As further improved technical scheme of the present invention: in step (b), be the mixture that contains ester class, ethers or the binary of two or more hydroxyls or polyalcohol or formed by described binary or polyalcohol or ester class in order to the solvent that dissolves described silver-colored presoma, again or by the mixture of above-mentioned solvent and other solvent composition; Described alcohols, ethers and ester class include but not limited to methyl alcohol (CH
3OH), ethanol (C
2H
5OH), propyl alcohol (C
3H
7OH), butanols (C
4H
9OH), amylalcohol (C
5H
11OH), hexanol (C
6H
13OH), enanthol (C
7H
15OH), octanol (C
8H
17OH), nonyl alcohol (C
9H
19OH), ethylene glycol (CH
2OHCH
2OH), propane diols (CH
2OHCH
2CH
2OH, CH
2OHCH
2OHCH
3), glycerine (CH
2OHCHOHCH
2OH), butanediol (C
4H
10O
2), pentanediol (C
5H
12O
2), hexylene glycol (C
6H
14O
2), cyclohexanediol (C
6H
10O
2), glycol dimethyl ether (C
4H
10O
2), ethylene glycol diethyl ether (C
6H
14O
2), diethylene glycol ether (C
6H
14O
3), 1,2-propane diols carbonic ester (C
4H
6O
3), propylene glycol methyl ether acetate (C
6H
12O
3), butyl glycol ether acetic acid esters (C
8H
16O
3), ethylene glycol monomethyl ether acetate (C
5H
10O
3).
As further improved technical scheme of the present invention: in step (a) forms the process of described mixed solution, comprise the step that adds described protective agent and heating for dissolving and the step that adds described additive.
As further improved technical scheme of the present invention: be to divide at least twice to join in the described mixed solution described silver-colored precursor solution with the injection rate of 0.05ml/min ~ 10ml/min in step (b), and for the first time the injection rate of silver-colored precursor solution greater than the injection rate of silver-colored precursor solution for the second time.
As further improved technical scheme of the present invention: the reaction temperature in the step (b) is 60 ℃ ~ 250 ℃.
As further improved technical scheme of the present invention: in step (a), described protective agent is polyvinylpyrrolidone (PVP, (C
6H
9NO) n), and with this protective agent heating for dissolving in glycerine; Described additive is hexadecyltrimethylammonium chloride (CTAC, C
16H
33(CH
3)
3NCl), and with this additive be dissolved in the glycerine; In step (b), described silver-colored precursor solution is for to be dissolved in resultant liquor argenti nitratis ophthalmicus in the glycerine with silver nitrate.
As further improved technical scheme of the present invention: in step (a), form in the process of described additive described hexadecyltrimethylammonium chloride (CTAC, C
16H
33(CH
3)
3NCl) be dissolved in that the concentration of gained solution behind the glycerine is interval to be 0.1mM ~ 200mM;
In step (b), form in the process of described liquor argenti nitratis ophthalmicus, described silver nitrate is dissolved in that the concentration of gained solution behind the glycerine is interval to be 0.01M ~ 1M;
In step (a), form in described protectant process described polyvinylpyrrolidone (PVP, (C
6H
9NO) n) addition and described silver nitrate addition maintenance mass ratio interval is 0.5 ~ 10.
As further improved technical scheme of the present invention: in step (c), the solution that step (b) is obtained carries out centrifugal motion with certain speed, adds ethanol then and disperses, repeats this centrifugal and disperse process.
As further improved technical scheme of the present invention: in step (c), after process centrifugal and that disperse finishes, obtain described nano silver wire in water or the ethanol thereby the gained nano silver wire is scattered in.
Compared with prior art, the present invention is by dividing at least twice injection silver presoma (not being disposable injection), therefore not only can access high line directly than nano silver wire and also be fit to preparation in enormous quantities.
Description of drawings
Fig. 1 is the schematic flow sheet of the manufacture method of nano silver wire of the present invention.
Fig. 2 is first microgram that adopts the resulting nano silver wire of manufacture method of nano silver wire of the present invention.
Fig. 3 is second microgram that adopts the resulting nano silver wire of manufacture method of nano silver wire of the present invention.
Fig. 4 is the 3rd microgram that adopts the resulting nano silver wire of manufacture method of nano silver wire of the present invention.
Fig. 5 is the line length distribution map that adopts the resulting nano silver wire of manufacture method of nano silver wire of the present invention.
Fig. 6 is the footpath grain distribution map that adopts the resulting nano silver wire of manufacture method of nano silver wire of the present invention.
The specific embodiment
Please join shown in Figure 1ly, the present invention has disclosed a kind of manufacture method of nano silver wire, and it comprises the steps:
(a). mixed solution is provided, contains a kind of protective agent and a kind of additive in this mixed solution at least, described additive is halide and/or the compound that can form property salt hard to tolerate with silver ion;
(b). the silver-colored precursor solution that contains the patina thing is provided, and should will divide at least twice to join in the described mixed solution by the silver precursor solution;
(c). separate obtaining described nano silver wire.
Particularly, in step (a), described protective agent includes but not limited to:
The polyvinylpyrrolidone of various molecular weight (PVP, (C
6H
9NO) n), the derivative of polyvinylpyrrolidone, polyvinyl alcohol (PVA, (C
2H
4O) n), PEO (PEO, (CH
2CH
2O) lauryl sodium sulfate (C n),
12H
25SO
4Na), lauryl amine (C
12H
27N), octadecylamine (CH
3(CH
2)
16CH
2NH
2), hexadecyltrimethylammonium chloride (CTAC, C
16H
33(CH
3)
3NCl), softex kw (CTAB, C
16H
33(CH
3)
3NBr), gelatin, methylcellulose, the ninth of the ten Heavenly Stems two mercaptan, succinimide mercaptans; Perhaps
Contain the protective agent of sulfydryl or amino etc.; Perhaps
By the polymer that following one or several monomers form, described monomer comprises:
Acrylic acid (C
3H
4O
2), butenoic acid (C
4H
6O
2), maleic acid (C
4H
4O
4), methyl-maleic acid, fumaric acid and its esters etc.;
Contain aforesaid propylene acid (C
3H
4O
2), butenoic acid (C
4H
6O
2), maleic acid (C
4H
4O
4), ester class of methyl-maleic acid, fumaric acid and salts substances thereof, amide-type, acid anhydrides, nitrile etc., as methyl acrylate, ethyl acrylate, methyl methacrylate, EMA, dimethylaminoethyl acrylate, DMAA etc.;
Acrylic sulfonic acid, vinyl sulfonic acid, metering system sulfonic acid, 3-sulfopropyl methacrylic acid and contain ester class, amide-type, nitrile of phosphonate radical etc. are as vinyl phosphonate, acrylic phosphonic acids etc.;
N-ethernamine classes etc. are as N-ethernamine pyrrolidones, N-ethene caprolactam etc.;
Ethene acetal, ethene butyral, ethene ethanol and ethers, ester class etc.
In step (a), described halide includes but not limited to sodium chloride (NaCl), potassium chloride (KCl), sodium bromide (NaBr), KBr (KBr), sodium iodide (NaI), KI (KI), softex kw (CTAB, C
16H
33(CH
3)
3NBr), hexadecyltrimethylammonium chloride (CTAC, C
16H
33(CH
3)
3NCl) etc.
In step (a), describedly can include but not limited to sodium sulphate (NaSO with the compound that silver ion forms property salt hard to tolerate
4), potassium sulfate (KSO
4), sodium sulfite (NaSO
3), potassium sulfite (KSO
3), sodium carbonate (NaCO
3), potash (KCO
3), sodium phosphate (Na
3PO
4), potassium phosphate (K
3PO
4), vulcanized sodium (Na
2S), potassium sulfide (K
2S) etc.
In step (b), described patina thing includes but not limited to silver nitrate (AgNO
3), silver nitrite (AgNO
2), silver oxide (AgO), silver carbonate (AgCO
3), silver acetate (CH
3COOAg), toillen's reagent ([Ag(NH
3)
2] OH), silver cyanide (AgCN), silver sulfate (Ag
2SO
4), silver sulfide (Ag
2S), trifluoroacetic acid silver (C
2F
3O
2Ag), silver thiocyanate (AgSCN), silver chlorate (AgCl), silver bromide (AgBr), silver sulfite (Ag
2SO
3), silver iodide (AgI), silver orthophosphate (Ag
3PO
4), silver fluoride (AgF), silver tetrafluoroborate (AgBF
4), pelletization silver (Ag
3N), silver propionate (C
3H
5O
2Ag), actol (C
3H
5AgO
3), capric acid silver, carboxylic first silver, silver citrate (C
6H
5Ag
3O
7), gluconic acid silver, silver cyanate (AgOCN), silver bromate (AgBrO
3), hyptafluorobutyric acid silver (CF
3CF
2CF
2CO
2Ag), acetylacetone,2,4-pentanedione silver ([CH
3COCH=C (O-) CH
3] Ag), five fluorine silver propionate (C
2F
5CO
2Ag), inclined to one side alum acid silver (AgVO
3), hexafluoroarsenate silver (AgAsF
6), hexafluorophosphoric acid silver (AgPF
6), p-methyl benzenesulfonic acid silver (CH
3C
6H
4SO
3Ag), silver tetrafluoroborate (AgBF
4), complex compound Ag (I) and the part NH of silver
3-, CN-, Cl-, S
2O
3-wait to generate complex compound, Ag[II] generate complex compound, Ag[III with part Py (pyridine), an adjacent phenanthroline (0 one phen), 8 monohydroxy quinolines (oxin) etc.] and part F-, IO
4-, TeO
66-etc. the minority part generate complex compound etc.
In step (b), the mixture that includes but not limited to contain ester class, ethers or the binary of two or more hydroxyls or polyalcohol etc. or be made up of described binary or polyalcohol or ester class in order to the solvent that dissolves described silver-colored presoma is again or by the mixture of above-mentioned solvent and other solvent composition; Described alcohols, ethers and ester class include but not limited to methyl alcohol (CH
3OH), ethanol (C
2H
5OH), propyl alcohol (C
3H
7OH), butanols (C
4H
9OH), amylalcohol (C
5H
11OH), hexanol (C
6H
13OH), enanthol (C
7H
15OH), octanol (C
8H
17OH), nonyl alcohol (C
9H
19OH), ethylene glycol (CH
2OHCH
2OH), propane diols (CH
2OHCH
2CH
2OH, CH
2OHCH
2OHCH
3), glycerine (CH
2OHCHOHCH
2OH), butanediol (C
4H
10O
2), pentanediol (C
5H
12O
2), hexylene glycol (C
6H
14O
2), cyclohexanediol (C
6H
10O
2), glycol dimethyl ether (C
4H
10O
2), ethylene glycol diethyl ether (C
6H
14O
2), diethylene glycol ether (C
6H
14O
3), 1,2-propane diols carbonic ester (C
4H
6O
3), propylene glycol methyl ether acetate (C
6H
12O
3), butyl glycol ether acetic acid esters (C
8H
16O
3), ethylene glycol monomethyl ether acetate (C
5H
10O
3) etc.
The process that forms described mixed solution in step (a) comprises the step that adds described protective agent and heating for dissolving and the step that adds described additive.
Be to divide at least twice to join in the described mixed solution described silver-colored precursor solution with the injection rate of 0.05ml/min ~ 10ml/min in step (b), and for the first time the injection rate (for example 2ml/min) of silver-colored precursor solution greater than the injection rate (for example 0.4ml/min) of silver-colored precursor solution for the second time.
Reaction temperature in the step (b) is 60 ℃ ~ 250 ℃.
Preferably, in step (a), described protective agent is polyvinylpyrrolidone ((C
6H
9NO) n is hereinafter to be referred as " PVP "), and with this protective agent heating for dissolving in glycerine; Described additive is hexadecyltrimethylammonium chloride (C
16H
33(CH
3)
3NCl is hereinafter to be referred as " CTAC "), and this additive is dissolved in the glycerine; In step (b), described silver-colored precursor solution is for to be dissolved in resultant liquor argenti nitratis ophthalmicus in the glycerine with silver nitrate.
In step (a), form in the process of described additive, described CTAC is dissolved in that the concentration of gained solution behind the glycerine is interval to be 0.1mM ~ 200mM; The implication of M is molar concentration, and namely mol/L is together following.For example can be with 0.32mg ~ 0.64g CTAC powder dissolution in 10ml glycerine.
In step (b), form in the process of described liquor argenti nitratis ophthalmicus, described silver nitrate is dissolved in that the concentration of gained solution behind the glycerine is interval to be 0.01M ~ 1M.For example can be with in 0.06115g ~ 6.115g silver nitrate powder dissolution 36ml glycerine.
In step (a), form in described protectant process, it is 0.5 ~ 10 that described PVP addition and described silver nitrate addition keep the mass ratio interval.
In step (c), the solution that step (b) is obtained carries out centrifugal motion with certain speed, adds ethanol then and disperses, repeats this centrifugal and disperse process.
In step (c), after process centrifugal and that disperse finishes, obtain described nano silver wire thereby the gained nano silver wire is scattered in water or ethanol or other solvent.
Below just the manufacture method of nano silver wire of the present invention illustrate, wherein the concentration of used liquor argenti nitratis ophthalmicus is 1M, the concentration of CTAC solution is 50mM.
Particularly, to the container that contains 50ml glycerine (for example comprise in the step (a), three mouthfuls of round-bottomed flasks) add 5.1g PVP in, be heated to 150 ℃ of stirring and dissolving, add 0.5ml CTAC solution then, finally obtain described mixed solution (that is, polyhydric alcohol solutions), and implementation step (b) after waiting for 2 minutes.
Comprise in the step (b) with injection speed (for example 2ml/min) slowly, the 18ml liquor argenti nitratis ophthalmicus is injected above-mentioned three mouthfuls of round-bottomed flasks, when question response becomes canescence, again the 12ml liquor argenti nitratis ophthalmicus is injected above-mentioned three mouthfuls of round-bottomed flasks with injection speed (for example 0.4ml/min) slowly, finish reaction after 3 hours.
Comprise the solution that to obtain in the step (b) in the step (c) with 2000 rev/mins speed centrifugal 20 minutes, add ethanol then and disperse again, repeat this centrifugal and process of disperseing three times, then the gained nano silver wire is scattered in the liquid such as water or ethanol.Preferably, in the above-mentioned steps (a) ~ (c), can adopt equipment such as magnetic agitation heating jacket, peristaltic pump as required.
Please join Fig. 2 to shown in Figure 6, by the resulting nano silver wire of the manufacture method of nano silver wire of the present invention, the statistics line length is 35.4 microns, and particle diameter is 39.8 nanometers, and the line of most nano silver wires is directly than greater than 1000.By the resulting nano silver wire of the manufacture method of nano silver wire of the present invention, the line of most nano silver wires footpath is less than 50 nanometers, and line length is greater than 15 microns, and productive rate is not less than 50%, is fit to prepared in batches.
Utilize the prepared conductive film of the resulting nano silver wire of manufacture method of the present invention, have the transmitance height, characteristics such as sheet resistance is little, and also than tin indium oxide (ITO) film, with low cost, pliability is good, can be used for replacing ito thin film.
Compared to prior art, the present invention adopts earlier with protective agent, the silver-colored presoma that reinjects, and divide at least twice injection (not being disposable injection), therefore not only can access high line directly than nano silver wire and also be fit to preparation in enormous quantities.
Need to prove: above embodiment only be used for explanation the present invention and and unrestricted technical scheme described in the invention, although this specification has been described in detail the present invention with reference to the above embodiments, but, those of ordinary skill in the art is to be understood that, the person of ordinary skill in the field still can make amendment or is equal to replacement the present invention, and all do not break away from technical scheme and the improvement thereof of the spirit and scope of the present invention, all should be encompassed in the claim scope of the present invention.
Claims (13)
1. the manufacture method of a nano silver wire, it is characterized in that: this manufacture method comprises the steps:
(a). mixed solution is provided, contains a kind of protective agent and a kind of additive in this mixed solution at least, described additive is halide and/or the compound that can form property salt hard to tolerate with silver ion;
(b). the silver-colored precursor solution that contains the patina thing is provided, and should will divide at least twice to join in the described mixed solution by the silver precursor solution;
(c). separate obtaining described nano silver wire.
2. the manufacture method of nano silver wire as claimed in claim 1, it is characterized in that: in step (a), described protective agent is:
The polyvinylpyrrolidone of various molecular weight (PVP, (C
6H
9NO) n), the derivative of polyvinylpyrrolidone, polyvinyl alcohol (PVA, (C
2H
4O) n), PEO (PEO, (CH
2CH
2O) lauryl sodium sulfate (C n),
12H
25SO
4Na), lauryl amine (C
12H
27N), octadecylamine (CH
3(CH
2)
16CH
2NH
2), hexadecyltrimethylammonium chloride (CTAC, C
16H
33(CH
3)
3NCl), softex kw (CTAB, C
16H
33(CH
3)
3NBr), gelatin, methylcellulose, the ninth of the ten Heavenly Stems two mercaptan, succinimide mercaptans; Perhaps
Contain sulfydryl or amino protective agent; Perhaps
By the polymer that following one or several monomers form, described monomer comprises:
Acrylic acid (C
3H
4O
2), butenoic acid (C
4H
6O
2), maleic acid (C
4H
4O
4), methyl-maleic acid, fumaric acid and its esters;
Contain aforesaid propylene acid (C
3H
4O
2), butenoic acid (C
4H
6O
2), maleic acid (C
4H
4O
4), ester class, amide-type, acid anhydrides, the nitrile of methyl-maleic acid, fumaric acid and salts substances thereof;
Acrylic sulfonic acid, vinyl sulfonic acid, metering system sulfonic acid, 3-sulfopropyl methacrylic acid and the ester class, amide-type, the nitrile that contain phosphonate radical;
N-ethernamine class;
Ethene acetal, ethene butyral, ethene ethanol and ethers thereof, ester class.
3. the manufacture method of nano silver wire as claimed in claim 1, it is characterized in that: in step (a), described halide includes but not limited to sodium chloride (NaCl), potassium chloride (KCl), sodium bromide (NaBr), KBr (KBr), sodium iodide (NaI), KI (KI), softex kw (CTAB, C
16H
33(CH
3)
3NBr), hexadecyltrimethylammonium chloride (CTAC, C
16H
33(CH
3)
3NCl).
4. the manufacture method of nano silver wire as claimed in claim 1 is characterized in that: in step (a), describedly can include but not limited to sodium sulphate (NaSO with the compound that silver ion forms property salt hard to tolerate
4), potassium sulfate (KSO
4), sodium sulfite (NaSO
3), potassium sulfite (KSO
3), sodium carbonate (NaCO
3), potash (KCO
3), sodium phosphate (Na
3PO
4), potassium phosphate (K
3PO
4), vulcanized sodium (Na
2S), potassium sulfide (K
2S).
5. the manufacture method of nano silver wire as claimed in claim 1, it is characterized in that: in step (b), described patina thing is silver nitrate (AgNO
3), silver nitrite (AgNO
2), silver oxide (AgO), silver carbonate (AgCO
3), silver acetate (CH
3COOAg), toillen's reagent ([Ag(NH
3)
2] OH), silver cyanide (AgCN), silver sulfate (Ag
2SO
4), silver sulfide (Ag
2S), trifluoroacetic acid silver (C
2F
3O
2Ag), silver thiocyanate (AgSCN), silver chlorate (AgCl), silver bromide (AgBr), silver sulfite (Ag
2SO
3), silver iodide (AgI), silver orthophosphate (Ag
3PO
4), silver fluoride (AgF), silver tetrafluoroborate (AgBF
4), pelletization silver (Ag
3N), silver propionate (C
3H
5O
2Ag), actol (C
3H
5AgO
3), capric acid silver, carboxylic first silver, silver citrate (C
6H
5Ag
3O
7), gluconic acid silver, silver cyanate (AgOCN), silver bromate (AgBrO
3), hyptafluorobutyric acid silver (CF
3CF
2CF
2CO
2Ag), acetylacetone,2,4-pentanedione silver ([CH
3COCH=C (O-) CH
3] Ag), five fluorine silver propionate (C
2F
5CO
2Ag), inclined to one side alum acid silver (AgVO
3), hexafluoroarsenate silver (AgAsF
6), hexafluorophosphoric acid silver (AgPF
6), p-methyl benzenesulfonic acid silver (CH
3C
6H
4SO
3Ag), silver tetrafluoroborate (AgBF
4), complex compound Ag (I) and the part NH of silver
3-, CN-, Cl-, S
2O
3-generation complex compound, Ag[II] generate complex compound, Ag[III with part Py (pyridine), an adjacent phenanthroline (0 one phen), 8 monohydroxy quinolines (oxin)] and part F-, IO
4-, TeO
66-generation complex compound.
6. the manufacture method of nano silver wire as claimed in claim 5, it is characterized in that: in step (b), be the mixture that contains ester class, ethers or the binary of two or more hydroxyls or polyalcohol or formed by described binary or polyalcohol or ester class in order to the solvent that dissolves described silver-colored presoma, again or by the mixture of above-mentioned solvent and other solvent composition; Described alcohols, ethers and ester class include but not limited to methyl alcohol (CH
3OH), ethanol (C
2H
5OH), propyl alcohol (C
3H
7OH), butanols (C
4H
9OH), amylalcohol (C
5H
11OH), hexanol (C
6H
13OH), enanthol (C
7H
15OH), octanol (C
8H
17OH), nonyl alcohol (C
9H
19OH), ethylene glycol (CH
2OHCH
2OH), propane diols (CH
2OHCH
2CH
2OH, CH
2OHCH
2OHCH
3), glycerine (CH
2OHCHOHCH
2OH), butanediol (C
4H
10O
2), pentanediol (C
5H
12O
2), hexylene glycol (C
6H
14O
2), cyclohexanediol (C
6H
10O
2), glycol dimethyl ether (C
4H
10O
2), ethylene glycol diethyl ether (C
6H
14O
2), diethylene glycol ether (C
6H
14O
3), 1,2-propane diols carbonic ester (C
4H
6O
3), propylene glycol methyl ether acetate (C
6H
12O
3), butyl glycol ether acetic acid esters (C
8H
16O
3), ethylene glycol monomethyl ether acetate (C
5H
10O
3).
7. as the manufacture method of any described nano silver wire in the claim 1 to 6, it is characterized in that: in step (a) forms the process of described mixed solution, comprise the step that adds described protective agent and heating for dissolving and the step that adds described additive.
8. as the manufacture method of any described nano silver wire in the claim 1 to 6, it is characterized in that: be to divide at least twice to join in the described mixed solution described silver-colored precursor solution with the injection rate of 0.05ml/min ~ 10ml/min in step (b), and for the first time the injection rate of silver-colored precursor solution greater than the injection rate of silver-colored precursor solution for the second time.
9. as the manufacture method of any described nano silver wire in the claim 1 to 6, it is characterized in that: the reaction temperature in the step (b) is 60 ℃ ~ 250 ℃.
10. as the manufacture method of any described nano silver wire in the claim 1 to 6, it is characterized in that: in step (a), described protective agent is polyvinylpyrrolidone (PVP, (C
6H
9NO) n), and with this protective agent heating for dissolving in glycerine; Described additive is hexadecyltrimethylammonium chloride (CTAC, C
16H
33(CH
3)
3NCl), and with this additive be dissolved in the glycerine; In step (b), described silver-colored precursor solution is for to be dissolved in resultant liquor argenti nitratis ophthalmicus in the glycerine with silver nitrate.
11. the manufacture method of nano silver wire as claimed in claim 10 is characterized in that: in step (a), form in the process of described additive described hexadecyltrimethylammonium chloride (CTAC, C
16H
33(CH
3)
3NCl) be dissolved in that the concentration of gained solution behind the glycerine is interval to be 0.1mM ~ 200mM;
In step (b), form in the process of described liquor argenti nitratis ophthalmicus, described silver nitrate is dissolved in that the concentration of gained solution behind the glycerine is interval to be 0.01M ~ 1M;
In step (a), form in described protectant process described polyvinylpyrrolidone (PVP, (C
6H
9NO) n) addition and described silver nitrate addition maintenance mass ratio interval is 0.5 ~ 10.
12. the manufacture method as any described nano silver wire in the claim 1 to 6, it is characterized in that: in step (c), the solution that step (b) is obtained carries out centrifugal motion with certain speed, adds ethanol then and disperses, repeats this centrifugal and disperse process.
13. the manufacture method of nano silver wire as claimed in claim 12 is characterized in that: in step (c), after process centrifugal and that disperse finishes, obtain described nano silver wire in water or the ethanol thereby the gained nano silver wire is scattered in.
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|---|---|---|---|
| CN201310152157.1A CN103192092B (en) | 2013-04-27 | 2013-04-27 | The manufacture method of nano silver wire |
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