CN114743717A - Silver powder composed of three-dimensional granular crystal and two-dimensional flaky crystal and preparation method thereof - Google Patents
Silver powder composed of three-dimensional granular crystal and two-dimensional flaky crystal and preparation method thereof Download PDFInfo
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- CN114743717A CN114743717A CN202210399670.XA CN202210399670A CN114743717A CN 114743717 A CN114743717 A CN 114743717A CN 202210399670 A CN202210399670 A CN 202210399670A CN 114743717 A CN114743717 A CN 114743717A
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- silver
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- silver powder
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 136
- 239000013078 crystal Substances 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 229910052709 silver Inorganic materials 0.000 claims abstract description 79
- 239000004332 silver Substances 0.000 claims abstract description 79
- 238000006243 chemical reaction Methods 0.000 claims abstract description 33
- -1 silver ions Chemical class 0.000 claims description 30
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical class [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims description 29
- 239000002245 particle Substances 0.000 claims description 29
- 239000003638 chemical reducing agent Substances 0.000 claims description 26
- 239000002904 solvent Substances 0.000 claims description 22
- 239000000843 powder Substances 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- 239000002270 dispersing agent Substances 0.000 claims description 12
- 239000011521 glass Substances 0.000 claims description 12
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 12
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 11
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical group [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 9
- 239000011248 coating agent Substances 0.000 claims description 8
- 238000000576 coating method Methods 0.000 claims description 8
- 239000012074 organic phase Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000006722 reduction reaction Methods 0.000 claims description 7
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 6
- 125000003172 aldehyde group Chemical group 0.000 claims description 6
- 150000001299 aldehydes Chemical group 0.000 claims description 6
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 6
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 5
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 5
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 4
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 4
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- 108010010803 Gelatin Proteins 0.000 claims description 4
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 4
- 239000005642 Oleic acid Substances 0.000 claims description 4
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 4
- 230000008859 change Effects 0.000 claims description 4
- 229920000159 gelatin Polymers 0.000 claims description 4
- 239000008273 gelatin Substances 0.000 claims description 4
- 235000019322 gelatine Nutrition 0.000 claims description 4
- 235000011852 gelatine desserts Nutrition 0.000 claims description 4
- 239000008103 glucose Substances 0.000 claims description 4
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 229920000084 Gum arabic Polymers 0.000 claims description 3
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical class CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 3
- 229920002845 Poly(methacrylic acid) Polymers 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- 229920000388 Polyphosphate Polymers 0.000 claims description 3
- 241000978776 Senegalia senegal Species 0.000 claims description 3
- 229920002125 Sokalan® Polymers 0.000 claims description 3
- 239000000205 acacia gum Substances 0.000 claims description 3
- 235000010489 acacia gum Nutrition 0.000 claims description 3
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 claims description 3
- 239000011668 ascorbic acid Substances 0.000 claims description 3
- 235000010323 ascorbic acid Nutrition 0.000 claims description 3
- 229960005070 ascorbic acid Drugs 0.000 claims description 3
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 3
- 239000003990 capacitor Substances 0.000 claims description 3
- 229920001577 copolymer Polymers 0.000 claims description 3
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 3
- 239000004584 polyacrylic acid Substances 0.000 claims description 3
- 229920005646 polycarboxylate Polymers 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 239000001205 polyphosphate Substances 0.000 claims description 3
- 235000011176 polyphosphates Nutrition 0.000 claims description 3
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 claims description 3
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 3
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 3
- 229940048086 sodium pyrophosphate Drugs 0.000 claims description 3
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 3
- 235000019818 tetrasodium diphosphate Nutrition 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims description 2
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 150000003863 ammonium salts Chemical class 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 claims description 2
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 239000010408 film Substances 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- YPNVIBVEFVRZPJ-UHFFFAOYSA-L silver sulfate Chemical compound [Ag+].[Ag+].[O-]S([O-])(=O)=O YPNVIBVEFVRZPJ-UHFFFAOYSA-L 0.000 claims description 2
- 229910000367 silver sulfate Inorganic materials 0.000 claims description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical class [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 claims description 2
- 150000003467 sulfuric acid derivatives Chemical class 0.000 claims description 2
- 229910001428 transition metal ion Inorganic materials 0.000 claims description 2
- 239000010409 thin film Substances 0.000 claims 1
- 239000012535 impurity Substances 0.000 abstract description 6
- 238000005245 sintering Methods 0.000 abstract description 5
- 238000000034 method Methods 0.000 description 12
- 230000008569 process Effects 0.000 description 8
- 238000002156 mixing Methods 0.000 description 7
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000013081 microcrystal Substances 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 239000012634 fragment Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000009864 tensile test Methods 0.000 description 2
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 2
- VXQBJTKSVGFQOL-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethyl acetate Chemical compound CCCCOCCOCCOC(C)=O VXQBJTKSVGFQOL-UHFFFAOYSA-N 0.000 description 1
- 239000001856 Ethyl cellulose Substances 0.000 description 1
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- GHPGOEFPKIHBNM-UHFFFAOYSA-N antimony(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Sb+3].[Sb+3] GHPGOEFPKIHBNM-UHFFFAOYSA-N 0.000 description 1
- 239000004359 castor oil Substances 0.000 description 1
- 235000019438 castor oil Nutrition 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 235000019325 ethyl cellulose Nutrition 0.000 description 1
- 229920001249 ethyl cellulose Polymers 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
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- 239000000463 material Substances 0.000 description 1
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- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 229910000160 potassium phosphate Inorganic materials 0.000 description 1
- 235000011009 potassium phosphates Nutrition 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000001488 sodium phosphate Substances 0.000 description 1
- 229910000162 sodium phosphate Inorganic materials 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
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- H—ELECTRICITY
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- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/14—Conductive material dispersed in non-conductive inorganic material
- H01B1/16—Conductive material dispersed in non-conductive inorganic material the conductive material comprising metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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- H—ELECTRICITY
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- H01C—RESISTORS
- H01C10/00—Adjustable resistors
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- H—ELECTRICITY
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- H01C—RESISTORS
- H01C7/00—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material
- H01C7/02—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material having positive temperature coefficient
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- H01C7/00—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material
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- H01C—RESISTORS
- H01C7/00—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material
- H01C7/10—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material voltage responsive, i.e. varistors
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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
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/005—Electrodes
- H01G4/008—Selection of materials
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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
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/30—Stacked capacitors
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
- H01H13/00—Switches having rectilinearly-movable operating part or parts adapted for pushing or pulling in one direction only, e.g. push-button switch
- H01H13/70—Switches having rectilinearly-movable operating part or parts adapted for pushing or pulling in one direction only, e.g. push-button switch having a plurality of operating members associated with different sets of contacts, e.g. keyboard
- H01H13/702—Switches having rectilinearly-movable operating part or parts adapted for pushing or pulling in one direction only, e.g. push-button switch having a plurality of operating members associated with different sets of contacts, e.g. keyboard with contacts carried by or formed from layers in a multilayer structure, e.g. membrane switches
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- H01L31/02—Details
- H01L31/0224—Electrodes
- H01L31/022408—Electrodes for devices characterised by at least one potential jump barrier or surface barrier
- H01L31/022425—Electrodes for devices characterised by at least one potential jump barrier or surface barrier for solar cells
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- H01P—WAVEGUIDES; RESONATORS, LINES, OR OTHER DEVICES OF THE WAVEGUIDE TYPE
- H01P1/00—Auxiliary devices
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/0277—Bendability or stretchability details
- H05K1/0283—Stretchable printed circuits
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The application discloses silver powder consisting of three-dimensional granular crystals and two-dimensional flaky crystals and a preparation method thereof. The silver powder composed of the three-dimensional granular crystals and the two-dimensional flaky crystals is generated by one-time reaction in the same reaction system. The silver powder is generated by one-time reaction of the three-dimensional granular crystal and the two-dimensional flaky crystal, and the surface state of the silver powder is close to that of the three-dimensional granular crystal and the two-dimensional flaky crystal, so that the problem that the purity of mixed silver powder is insufficient due to the introduction of impurities in the preparation process of silver powder with different forms is avoided. The silver paste prepared from the silver powder can be better suitable for precision printing, and has the advantages of high strength and high conductivity after sintering.
Description
Technical Field
The application relates to the technical field of silver powder, in particular to silver powder consisting of three-dimensional granular crystals and two-dimensional flaky crystals and a preparation method thereof.
Background
Silver paste is made by mixing silver powder, glass frit and organic phase, and is widely used as an internal electrode of a capacitor, a conductor of a circuit board, a solar cell or a circuit of a display panel substrate. When silver paste is used, it is usually printed on a substrate to form a predetermined pattern; then, the silver powder is sintered at a high temperature to remove the organic solvent, thereby sintering the silver powder into an integrally formed electrode.
In order to meet the growing use requirements, the conductive paste needs to be more suitable for the precision of the printed patterns. Therefore, the silver powder is required to achieve narrow particle size distribution, approximate surface state, no phase separation in slurry and good dispersion in organic phase.
Therefore, researches propose that silver powders with different forms can be considered to be mixed for use so as to improve the requirements of high conductivity, densification and high adhesion of the silver paste. However, the mixing of silver powders with different forms requires that silver powders with different forms are respectively prepared and then the silver powders with various forms are mixed according to the proportion; the mode has higher requirements on the process and needs to be prepared respectively for multiple times; moreover, the silver powder with different forms has larger surface state difference due to the batch-to-batch difference of the preparation process. In addition, the silver powders with different forms are respectively prepared and then mixed, the uniformity is poor, and impurities are introduced in the preparation and mixing processes, so that the performance of the silver paste is influenced.
In a word, the existing process and method for mixing silver powder with different forms have many defects and shortcomings, so that the performance of the prepared silver paste cannot meet the expectation. Therefore, how to prepare mixed silver powder with better performance is a problem to be solved urgently.
Disclosure of Invention
The application aims to provide silver powder consisting of improved three-dimensional granular crystals and two-dimensional flaky crystals and a preparation method thereof.
The following technical scheme is adopted in the application:
one aspect of the application discloses silver powder consisting of three-dimensional granular crystals and two-dimensional flaky crystals, wherein the three-dimensional granular crystals and the two-dimensional flaky crystals are generated by one-time reaction in the same reaction system.
It should be noted that in the mixed silver powder of the present application, the three-dimensional particle crystal and the two-dimensional flaky crystal are generated by one-time reaction in the same reaction system, and the surface states are close to each other, so that the purity deficiency of the mixed silver powder caused by introducing impurities into silver powders of different forms in the preparation process is avoided. The silver paste prepared from the mixed silver powder can be better suitable for precision printing, and has the advantages of high strength, high conductivity and the like after sintering.
In one implementation of the present application, the three-dimensional particle crystals in the silver powder account for at least 60% of the total weight of the silver powder, and the balance is two-dimensional plate-like crystals.
It should be noted that, the silver paste prepared from the silver powder can ensure good printing performance by mixing at least 60% of three-dimensional particle crystals and not more than 40% of two-dimensional flaky crystals.
In one implementation of the present application, the size of the three-dimensional particle crystals is 0.3-1.5 μm, and the size of the two-dimensional plate crystals is less than 10 μm in length, 5-6 μm in width, and 200 nm in thickness.
The other side of this application discloses a silver thick liquid of silver powder of this application.
It should be noted that the silver paste of the present application has good printing performance due to the adoption of the silver powder of the present application; also, after sintering, the sintered ceramic has advantages of high strength, high conductivity, and the like.
This application one side again discloses the application of the silver thick liquid of this application in the internal electrode of laminated capacitor, LTCC, solar cell, 5G wave filter, plasma display panel, touch panel, PET are the membrane switch of substrate, flexible circuit board, piezo-resistor and thermistor, piezoceramics or carbon film potentiometre.
The application also discloses a solar cell silver paste which is composed of 45-55 parts by weight of silver powder, 40-50 parts by weight of organic phase and 2-7 parts by weight of glass powder.
The silver paste for the solar cell has the advantages that due to the adoption of the silver powder, the leveling property and the stability are better, the printing performance is better, and the silver paste is better suitable for precision printing. It can be understood that the key of the solar cell silver paste is that the silver powder is adopted, and the organic phase and the glass powder can refer to the existing solar cell silver paste, and are not specifically limited here.
The application further discloses a solar cell adopting the solar cell silver paste.
It should be noted that, the solar cell of the present application, because of the use of the solar cell silver paste of the present application, has better product consistency and stability, and solves the problem of printing yield reduction caused by poor stability of the silver paste.
The application further discloses a preparation method of the silver powder, which comprises the following steps:
controlling the solution of silver ions or silver ion complexes at the reaction temperature;
stirring the solution of silver ions or silver ion complexes in an inert gas environment, adding a reducing agent into the solution for reduction reaction, and keeping the temperature change in the whole reaction process to be less than 5 ℃; and, the solvent of the solution of silver ions or silver ion complexes is incompatible with the solvent of the reducing agent;
after the reduction reaction is finished, adding a surface coating solution into the reaction system for surface coating to obtain a solution containing silver particles;
and washing the obtained solution containing the silver particles by pure water, drying after washing to obtain dry powder, and crushing the dry powder to obtain the silver powder.
In the process of producing silver powder by reduction with a reducing agent, the present invention produces silver particles of different forms by making a solvent of a solution of silver ions or a silver ion complex incompatible with a solvent of the reducing agent and by producing a two-phase interface with the incompatible solvents when mixing the two; the three-dimensional particle crystal and the two-dimensional flaky crystal are simultaneously generated by one-time reaction in one reaction system.
In one implementation of the application, the source of silver ions is silver nitrate or silver sulfate.
In one implementation of the application, the silver ion complex is a complex of silver ions with at least one of ammonia, ammonium salts, sulfites, sulfates, amines, and transition metal ions.
In one embodiment of the application, the solvent in the solution of silver ions or silver ion complexes is water, and the concentration of silver ions is 0.1 to 10mol/L, preferably 0.1 to 5mol/L, and more preferably 0.5 to 2 mol/L.
It should be noted that too high concentration of silver ions may cause explosive nucleation of silver particles, resulting in serious particle agglomeration; too low silver ion concentration results in low economy and is not suitable for industrial production.
In one implementation of the application, the reducing agent is a solution of a substance containing an aldehyde group or a hydroxyl group.
In one embodiment of the application, the substance containing an aldehyde group or a hydroxyl group is at least one of glucose, formaldehyde, acetaldehyde, ascorbic acid, ethylene glycol and glycerol.
In one implementation of the application, the solvent of the solution of the aldehyde or hydroxyl containing substance is a water-immiscible solvent.
Preferably, the solvent of the solution of the aldehyde or hydroxyl containing substance is cyclohexane.
In one embodiment of the present application, the concentration of the aldehyde group-or hydroxyl group-containing substance in the solution is 10 to 30%, preferably 15 to 20%.
In one embodiment of the application, the reducing agent is added in an amount of 1 to 10 times equivalent, preferably 3 to 8 times, and more preferably 5 to 7 times the silver ion content.
The reaction time is directly affected by the amount of the reducing agent, and if the amount of the reducing agent is too small, the reaction time becomes too long, and if the amount of the reducing agent is too high, the reaction heat is instantaneously released, which is not favorable for temperature control.
In one embodiment of the application, the reaction temperature is 5 to 55 ℃, preferably 35 to 50 ℃, more preferably 40 to 45 ℃.
It should be noted that the reaction temperature is mainly used to control the progress of the reduction reaction and the size of primary crystallites; the reaction temperature is too low, so that the nucleation rate is too low, primary microcrystal particles grow up easily, the primary silver microcrystal particles meeting the requirements cannot be prepared, and the method is not suitable for printing fine patterns; if the reaction temperature is too high, the primary microcrystal particles are too small and the particle size distribution is not uniform, which is not beneficial to the preparation of silver paste.
In order to control the reaction temperature, the temperature of the reducing solution may be lowered, the rate of addition of the reducing solution may be controlled, the rate of addition of cold water may be controlled, or the temperature rise due to the reaction heat may be suppressed by means of external circulating water cooling or the like.
In one embodiment of the application, the reducing agent is added to the solution of silver ions or silver ion complexes at a temperature of 3 to 15 ℃ lower than the temperature of the solution of silver ions or silver ion complexes, preferably 5 to 10 ℃ lower than the temperature of the solution of silver ions or silver ion complexes.
In one implementation of the application, the surface coating solution is an ethanol solution containing 25-30% oleic acid.
In one embodiment, the method further comprises adding a dispersant to the solution of silver ions or silver ion complexes, or adding the dispersant while stirring the reducing agent, in order to prevent agglomeration of silver particles.
In one implementation of the application, the dispersant is at least one of gum arabic, gelatin, PVP, polyethylene glycol, polyacrylic acid, polycarboxylate, poly (meth) acrylic acid derivative, maleic anhydride copolymer, polyphosphate, sodium pyrophosphate, sodium tripolyphosphate, sodium hexametaphosphate.
In one implementation of the application, the dispersant is PVP.
Preferably, the molecular weight of PVP is between 3000-100000, preferably 3000-10000, more preferably 5000-8000.
The beneficial effect of this application lies in:
the silver powder is generated by one-time reaction of the three-dimensional granular crystal and the two-dimensional flaky crystal, and the surface state of the silver powder is close to that of the three-dimensional granular crystal and the two-dimensional flaky crystal, so that the problem that the purity of mixed silver powder is insufficient due to the introduction of impurities in the preparation process of silver powder with different forms is avoided. The silver paste prepared from the silver powder can be better suitable for precision printing, and has the advantages of high strength and high conductivity after sintering.
Drawings
FIG. 1 is an SEM image of a silver powder prepared in examples of the present application;
FIG. 2 is an SEM image of another silver powder prepared in examples of the present application;
FIG. 3 is an SEM photograph of a silver powder as a comparative experiment in examples of the present application;
FIG. 4 is an SEM photograph of another silver powder as a comparative experiment in examples of the present application.
Detailed Description
At present, mixed silver powder with different forms, such as mixed silver powder of spherical silver powder and flake silver powder, is prepared, and generally, the spherical silver powder and the flake silver powder are separately prepared, and then are mixed and ball-milled to prepare the mixed silver powder. The whole process is complex and is easy to introduce impurities; as the spherical silver powder and the flake silver powder are respectively prepared by different methods, the surface states of the spherical silver powder and the flake silver powder are greatly different, and the performance of the silver paste is influenced.
The research of the application finds that in the process of preparing the silver powder by reducing the silver ions by using the reducing agent, if the solvent of the reducing agent is incompatible with the solvent of the silver ions, the incompatible solvents are used for manufacturing two-phase interfaces, three-dimensional particle crystals and two-dimensional flaky crystals can be simultaneously generated in a reaction system, and mixed silver powder with different forms can be obtained. Because a reaction system is generated simultaneously, the surface states of the three-dimensional granular crystal and the two-dimensional flaky crystal are close, impurities are prevented from being generated respectively and then mixed, and the performance of the silver paste is improved.
The present application is described in further detail below with reference to specific embodiments and the attached drawings. The following examples are intended to be illustrative of the present application only and should not be construed as limiting the present application.
Example 1
685g of silver nitrate is dissolved in 8654g of distilled water, 84g of potassium phosphate is added after dissolution, 37g of PVP k30 is then added, silver ion complex solution is obtained after even stirring, the prepared solution is poured into a double-layer glass beaker, and water with the temperature of 35 ℃ is introduced into the interlayer of the beaker for heat preservation.
Under the conditions of stirring at 2000r/min and introducing argon gas for 1L/min, a cyclohexane solution of glucose with the mass fraction of 25% is adopted as a reducing solution, the reducing solution with the silver ion content of 4 times equivalent is added into the solution at the speed of 1 equivalent/min, and the temperature change in the process is kept to be less than 5 ℃.
After the addition, stirring was carried out for 10min, and then 20g of an ethanol solution containing 30% oleic acid was added to carry out surface coating, to obtain a solution containing silver particles.
The above slurry was washed with pure water until the conductivity of the solution after precipitation was more than 0.2ms, centrifuged, and then put into an oven to dry at 50 ℃ for 24 hours to obtain a dry powder, which was then pulverized to obtain the silver powder of this example.
The silver powder of this example was observed by SEM and the results are shown in FIG. 1. The results of FIG. 1 show that the silver powder of this example contains both three-dimensional granular crystals and two-dimensional plate-like crystals, and in which the proportion of the three-dimensional granular crystals was about 95% and the proportion of the two-dimensional plate-like crystals was about 5%.
Example 2
352g of silver nitrate is dissolved in 3514g of distilled water, 152g of sodium phosphate is added after the silver nitrate is dissolved, 23g of gelatin is added, silver ion complex solution is obtained after the mixture is stirred uniformly, the prepared solution is poured into a double-layer glass beaker, and 40 ℃ water is introduced into an interlayer of the beaker for heat preservation.
Under the conditions of stirring at 3000r/min and introducing argon gas for 1.3L/min, adopting a cyclohexane solution containing acetaldehyde with the mass fraction of ethyl acetate being 10% as a reducing solution, adding 1.7g of ethyl acetate and the reducing solution with the content of 4 times equivalent of silver ions into the solution at the speed of 1 equivalent/min, and keeping the temperature change in the process to be less than 5 ℃.
After the addition, the mixture was stirred for 10min, and then 10g of an ethanol solution containing 25% oleic acid was added to carry out surface coating, to obtain a solution containing silver particles.
The above slurry was washed with pure water until the conductivity of the solution after precipitation was more than 0.2ms, centrifuged, and then put into an oven to be dried at 50 ℃ for 24 hours to obtain a dried powder, which was then pulverized to obtain the silver powder of this example.
The silver powder of this example was observed by SEM and the results are shown in FIG. 2. The results of FIG. 2 show that the silver powder of this example contains both three-dimensional granular crystals and two-dimensional plate-like crystals, and in which the proportion of the three-dimensional granular crystals is about 70% and the proportion of the two-dimensional plate-like crystals is about 30%.
Comparative test
In this example, the commercially available silver powders were observed by SEM and the results are shown in FIGS. 3 and 4, respectively. FIG. 3 is an SEM image of imported silver powder DOWA-4A8F, and FIG. 4 is an SEM image of Seaman noble metal Co., Ltd., Severe, Seaman, in the case of domestic silver powder. The results of FIGS. 3 and 4 show that the imported silver powder, DOWA-4A8F, and the domestic silver powder both consist of three-dimensional granular crystals and that no mixture of three-dimensional granular crystals and two-dimensional plate-like crystals is found.
Example 3
In addition to the above examples 1 and 2, this example was further tested for the effect of the silver ion concentration on the reaction and silver powder. The results show that the particle size distribution of the silver powder can be adjusted by adjusting the concentration of silver ions, and the concentration of silver ions is generally controlled to be 0.1-10mol/L, preferably 0.1-5mol/L or 0.5-2mol/L, at which a mixed silver powder having a three-dimensional particle crystal size of 0.3-1.5 μm, a two-dimensional plate crystal size of 10 μm or less, a width of 5-6 μm, and a thickness of 200-500nm can be prepared by combining other conditions.
Further to this example, different reducing agents were tested. The results show that the reducing agent can be a solution of a substance containing an aldehyde group or a hydroxyl group, such as a cyclohexane solution of glucose, formaldehyde, acetaldehyde, ascorbic acid, ethylene glycol or glycerol.
In this example, the reaction temperature was further tested in addition to example 1. The result shows that the silver powder meeting the requirement can be prepared at the reaction temperature of 5-55 ℃; the preferred reaction temperature is 35-50 deg.C, more preferably 40-45 deg.C.
In this example, further, different dispersants were tested on the basis of example 1. The results show that the dispersant can be gum arabic, gelatin, PVP, polyethylene glycol, polyacrylic acid, polycarboxylate, poly (meth) acrylic acid derivative, maleic anhydride copolymer, polyphosphate, sodium pyrophosphate, sodium tripolyphosphate, or sodium hexametaphosphate; among them, PVP with a molecular weight of 3000-100000 is preferably used, PVP with a molecular weight of 3000-10000 is more preferably used, and PVP with a molecular weight of 5000-8000 is more preferably used.
In general, regardless of the silver ion concentration, reducing agent or dispersant, a silver powder containing both three-dimensional particle crystals and two-dimensional plate crystals can be produced by ensuring that the solvent for the silver ions is water and the solvent for the reducing agent is a solvent incompatible with water, such as cyclohexane. In addition, in the two solvents, the more water, the less cyclohexane and the larger proportion of three-dimensional particles in the generated silver powder; that is, the smaller the amount of the same reducing substance, the more cyclohexane, the more two-dimensional plate-like crystals in the silver powder produced. As for the silver ion concentration, the reaction temperature, the amount of the reducing agent, the use of the dispersing agent, etc., only the size of the three-dimensional particle crystals and the two-dimensional plate crystals is affected.
The application aspect of silver powder, for example:
1. the silver powder, the organic phase and the glass powder in example 1 were mixed in a mass ratio of 5:4:0.5 to prepare a silver paste. The silver paste is printed on the back of the solar cell and sintered to form a back silver electrode. And a tensile test is carried out, and the result shows that the bearable tensile force of the steel is 3.9N, so that the steel meets the use requirement.
2. The silver powder, the organic phase and the glass powder in example 2 are mixed according to the mass ratio of 5:4:0.5 to prepare the silver paste. The silver paste is printed on the back of the solar cell and sintered to form a back silver electrode. And a tensile test is carried out, and the result shows that the bearable tensile force of the steel is 4.7N, so that the steel meets the use requirement.
In the above experiments, the formulation of the organic phase was: 5 parts of ethyl cellulose, 5 parts of hydrogenated castor oil, 20 parts of alcohol ester twelve and 70 parts of diethylene glycol butyl ether acetate. Glass powder: ZnO and SiO2、Bi2O3、Sb2O3、Al2O3、B2O3Mixing the materials according to the mass ratio of 50:5:30:2:2:11, putting the mixture into a muffle furnace, preserving the temperature at 1100 ℃ for 1h, pouring the mixture into water to obtain glass fragments, adding alcohol, and grinding the glass fragments into powder with the size of 3 mu m, namely the glass powder in the embodiment.
The foregoing is a more detailed description of the present application in connection with specific embodiments thereof, and it is not intended that the present application be limited to the specific embodiments thereof. For those skilled in the art to which the present application pertains, several simple deductions or substitutions may be made without departing from the concept of the present application, and all should be considered as belonging to the protection scope of the present application.
Claims (10)
1. The silver powder consisting of the three-dimensional granular crystals and the two-dimensional flaky crystals is characterized in that: the three-dimensional particle crystal and the two-dimensional flaky crystal are generated by one-time reaction in the same reaction system.
2. The silver powder according to claim 1, characterized in that: the three-dimensional particle crystals in the silver powder account for at least 60% of the total weight of the silver powder, and the balance is two-dimensional flaky crystals.
3. The silver powder according to claim 1 or 2, characterized in that: the size of the three-dimensional particle crystal is 0.3-1.5 μm, and the size of the two-dimensional flaky crystal is less than 10 μm in length, 5-6 μm in width and 200-500nm in thickness.
4. A silver paste using the silver powder according to any one of claims 1 to 3.
5. Use of the silver paste according to claim 4 in internal electrodes of laminated capacitors, LTCC, solar cells, 5G filters, plasma display panels, touch panels, PET-based thin film switches, flexible circuit boards, piezoresistors and thermistors, piezoelectric ceramics or carbon film potentiometers.
6. The solar cell silver paste is characterized in that: 45 to 55 parts by weight of the silver powder according to any one of claims 1 to 3, 40 to 50 parts by weight of the organic phase and 2 to 7 parts by weight of the glass frit.
7. A solar cell using the solar cell silver paste of claim 6.
8. The method for producing a silver powder according to any one of claims 1 to 3, characterized in that: comprises the following steps of (a) carrying out,
controlling the solution of silver ions or silver ion complexes at the reaction temperature;
stirring the solution of silver ions or silver ion complexes in an inert gas environment, adding a reducing agent into the solution for reduction reaction, and keeping the temperature change in the whole reaction process to be less than 5 ℃; and, the solvent of the solution of silver ions or silver ion complexes is incompatible with the solvent of the reducing agent;
after the reduction reaction is finished, adding a surface coating solution into the reaction system for surface coating to obtain a solution containing silver particles;
and washing the obtained solution containing the silver particles by pure water, drying after washing is finished to obtain dry powder, and crushing the dry powder to obtain the silver powder.
9. The production method according to claim 8, characterized in that: the silver ion source is silver nitrate or silver sulfate;
preferably, the silver ion complex is a complex of silver ions and at least one of ammonia, ammonium salts, sulfites, sulfates, amines and transition metal ions;
preferably, the solvent in the solution of silver ions or silver ion complexes is water, and the concentration of silver ions is 0.1-10mol/L, preferably 0.1-5mol/L, and more preferably 0.5-2 mol/L.
10. The production method according to claim 8 or 9, characterized in that: the reducing agent is a solution of a substance containing aldehyde groups or hydroxyl groups;
preferably, the substance containing aldehyde group or hydroxyl group is at least one of glucose, formaldehyde, acetaldehyde, ascorbic acid, ethylene glycol and glycerol;
preferably, the solvent of the solution of the substance containing aldehyde group or hydroxyl group is a solvent which is incompatible with water;
preferably, the solvent of the solution of the aldehyde group-or hydroxyl group-containing substance is cyclohexane;
preferably, in the solution of the substance containing aldehyde or hydroxyl, the concentration of the substance containing aldehyde or hydroxyl is 10-30%, preferably 15-20%;
preferably, the addition amount of the reducing agent is 1 to 10 times equivalent of the silver ion content, preferably 3 to 8 times, and more preferably 5 to 7 times;
preferably, the reaction temperature is 5-55 ℃, preferably 35-50 ℃, and more preferably 40-45 ℃;
preferably, before the reducing agent is added into the solution of the silver ions or the silver ion complexes, the temperature of the reducing agent is controlled to be 3-15 ℃ lower than the temperature of the solution of the silver ions or the silver ion complexes, and preferably 5-10 ℃ lower than the temperature of the solution of the silver ions or the silver ion complexes;
preferably, the surface coating solution is an ethanol solution containing 25-30% of oleic acid;
preferably, the preparation method further comprises adding a dispersing agent into the solution of the silver ions or the silver ion complex, or adding the dispersing agent while stirring and adding the reducing agent;
preferably, the dispersant is at least one of gum arabic, gelatin, PVP, polyethylene glycol, polyacrylic acid, polycarboxylate, poly (meth) acrylic acid derivative, maleic anhydride copolymer, polyphosphate, sodium pyrophosphate, sodium tripolyphosphate and sodium hexametaphosphate;
preferably, the dispersant is PVP;
preferably, the molecular weight of PVP is between 3000-100000, preferably 3000-10000, more preferably 5000-8000.
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Cited By (1)
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