CN102329496B - High-conductivity carbon slurry and preparation method thereof - Google Patents
High-conductivity carbon slurry and preparation method thereof Download PDFInfo
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- CN102329496B CN102329496B CN201110180193A CN201110180193A CN102329496B CN 102329496 B CN102329496 B CN 102329496B CN 201110180193 A CN201110180193 A CN 201110180193A CN 201110180193 A CN201110180193 A CN 201110180193A CN 102329496 B CN102329496 B CN 102329496B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 115
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 113
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000002002 slurry Substances 0.000 title abstract description 9
- 238000007613 slurry method Methods 0.000 title description 2
- 239000011347 resin Substances 0.000 claims abstract description 43
- 229920005989 resin Polymers 0.000 claims abstract description 43
- 239000000203 mixture Substances 0.000 claims abstract description 26
- 239000002608 ionic liquid Substances 0.000 claims abstract description 23
- 239000002994 raw material Substances 0.000 claims abstract description 20
- 238000005303 weighing Methods 0.000 claims abstract description 18
- 239000002904 solvent Substances 0.000 claims abstract description 16
- 239000007822 coupling agent Substances 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 5
- -1 fluoro-alkyl alkylsulfonyl acid amides ions Chemical class 0.000 claims description 69
- 239000000428 dust Substances 0.000 claims description 19
- 150000002500 ions Chemical class 0.000 claims description 15
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- 239000006185 dispersion Substances 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims description 10
- 238000009835 boiling Methods 0.000 claims description 9
- 229920002803 thermoplastic polyurethane Polymers 0.000 claims description 7
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 7
- 229920002554 vinyl polymer Polymers 0.000 claims description 7
- 229920000570 polyether Polymers 0.000 claims description 6
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- 229910019142 PO4 Inorganic materials 0.000 claims description 4
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 4
- ZMZDMBWJUHKJPS-UHFFFAOYSA-M Thiocyanate anion Chemical compound [S-]C#N ZMZDMBWJUHKJPS-UHFFFAOYSA-M 0.000 claims description 4
- 229940063013 borate ion Drugs 0.000 claims description 4
- XHEDLZYGAQSNTR-UHFFFAOYSA-N ethene;hexanedioic acid Chemical group C=C.C=C.OC(=O)CCCCC(O)=O XHEDLZYGAQSNTR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- ZMZDMBWJUHKJPS-UHFFFAOYSA-N hydrogen thiocyanate Natural products SC#N ZMZDMBWJUHKJPS-UHFFFAOYSA-N 0.000 claims description 4
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims description 4
- 239000010452 phosphate Substances 0.000 claims description 4
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 4
- NQBXSWAWVZHKBZ-UHFFFAOYSA-N 2-butoxyethyl acetate Chemical compound CCCCOCCOC(C)=O NQBXSWAWVZHKBZ-UHFFFAOYSA-N 0.000 claims description 3
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical group O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 2
- 239000005864 Sulphur Substances 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 2
- 150000008051 alkyl sulfates Chemical class 0.000 claims description 2
- 125000003118 aryl group Chemical group 0.000 claims description 2
- 229910052801 chlorine Inorganic materials 0.000 claims description 2
- 229910052731 fluorine Inorganic materials 0.000 claims description 2
- 229910052736 halogen Inorganic materials 0.000 claims description 2
- 150000002367 halogens Chemical class 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-M perchlorate Inorganic materials [O-]Cl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-M 0.000 claims description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 2
- 125000005010 perfluoroalkyl group Chemical group 0.000 claims description 2
- 150000005837 radical ions Chemical class 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 5
- 239000010439 graphite Substances 0.000 abstract 2
- 229910002804 graphite Inorganic materials 0.000 abstract 2
- 239000002270 dispersing agent Substances 0.000 abstract 1
- 238000000227 grinding Methods 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 238000007581 slurry coating method Methods 0.000 abstract 1
- 238000007711 solidification Methods 0.000 abstract 1
- 230000008023 solidification Effects 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 description 13
- 238000000465 moulding Methods 0.000 description 12
- 230000000694 effects Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 230000002596 correlated effect Effects 0.000 description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- 238000009775 high-speed stirring Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000007792 addition Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- KAIPKTYOBMEXRR-UHFFFAOYSA-N 1-butyl-3-methyl-2h-imidazole Chemical compound CCCCN1CN(C)C=C1 KAIPKTYOBMEXRR-UHFFFAOYSA-N 0.000 description 1
- WLWHLUQQCLCFNE-UHFFFAOYSA-N 1-ethenyl-3-methyl-2h-imidazole Chemical compound CN1CN(C=C)C=C1 WLWHLUQQCLCFNE-UHFFFAOYSA-N 0.000 description 1
- AYMDKQQFUZHWGX-UHFFFAOYSA-N 1-ethyl-3-methyl-1,2-dihydroimidazol-1-ium;thiocyanate Chemical compound [S-]C#N.CC[NH+]1CN(C)C=C1 AYMDKQQFUZHWGX-UHFFFAOYSA-N 0.000 description 1
- AGRDPFQSSPSPDK-UHFFFAOYSA-N CN1CN(C=C1)CCCCCCCCCCCC.N#CS Chemical compound CN1CN(C=C1)CCCCCCCCCCCC.N#CS AGRDPFQSSPSPDK-UHFFFAOYSA-N 0.000 description 1
- FSYWHOOHZWIKRS-UHFFFAOYSA-N Cl(=O)(=O)(=O)O.C(=C)N1CN(C=C1)C Chemical compound Cl(=O)(=O)(=O)O.C(=C)N1CN(C=C1)C FSYWHOOHZWIKRS-UHFFFAOYSA-N 0.000 description 1
- RMLHVYNAGVXKKC-UHFFFAOYSA-N [SH2]=N.C(F)(F)F Chemical compound [SH2]=N.C(F)(F)F RMLHVYNAGVXKKC-UHFFFAOYSA-N 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000006184 cosolvent Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 229950004288 tosilate Drugs 0.000 description 1
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- Conductive Materials (AREA)
Abstract
The invention discloses high-conductivity carbon slurry and a preparation method thereof. The high-conductivity carbon slurry is prepared from the following raw materials in parts by weight: 3-15 parts of colloidal graphite, 0.5-8 parts of ionic liquid, 69-75 parts of resin carrier and 12-26 parts of carbon powder. The preparation method comprises the following steps of: 1) preparing the resin carrier: weighing solvent type resin A, solvent type resin B and a high-boiling-point solvent, stirring at the temperature of 80-95 DEG C for fully dissolving, then adding a coupling agent, and uniformly stirring; and 2) preparing the high-conductivity carbon slurry: sufficiently stirring and mixing the carbon powder, colloidal graphite, ionic liquid, dispersant and resin carrier to obtain a mixture, and grinding the mixture to form a homogenous phase. The invention provides a high-conductivity carbon slurry which has high electric conductivity, improved solidification efficiency of conductive carbon slurry coating and enlarged application range in high-grade electric instruments, and also provides a preparation method of the high-conductivity carbon slurry, which has simple process and low preparation cost.
Description
Technical field
The present invention relates to a kind of high conductivity carbon slurry and preparation method thereof.High conductivity carbon slurry can be widely used in film key, printed resistor, heat generating component, flexible circuitry, the joint line in communication goods, computer, portable type electronic product, consumer electronics, the network hardware, Medical Instruments, domestic electronic appliances and the electronicss such as space flight and national defence.
Background technology
Conductive carbon paste is that the carbon with the non-metal conductor material is that particulate is distributed in thermoplastic resin and the electrically conductive ink processed equably; Have good electrical conductivity, be widely used in communication goods (mobile telephone), computer, portable type electronic product, consumer electronics, the network hardware (server etc.), Medical Instruments, domestic electronic appliances and electronicss such as space flight and national defence.
Conductive carbon paste forms after being heating and curing and is coated with rete, is coated with the rete stable performance and is difficult for oxidation, acid-and base-resisting and solvent corrosion, can play the effect of protection and conduction.And be coated with strong adhesion, the antistripping of rete, combine well with metal, glass-cloth board and VC, PET and PC sheet material.Though existing conductive carbon paste is compared with conductive silver paste, have high cost performance, its resistance is lower than conductive silver paste, so effect is limited in utilization, in requiring the high conduction performance product, application is restricted.
Summary of the invention
The technical problem that the present invention will solve is; Can not satisfy the defective that high conductivity requires to the conductivity of conductive carbon paste in the prior art, provide a kind of and have high conduction performance, improved conductive carbon paste and apply the curing efficiency that uses, the high conductive carbon paste that enlarges conductive carbon paste range of application in high-end electronic equipment.
The technical problem that the present invention further will solve is, the preparation method of the high conductive carbon paste that a kind of technology is simple, cost of manufacture is low is provided.
The technical solution adopted for the present invention to solve the technical problems is: a kind of high conductive carbon paste comprises that the raw material of following parts by weight is processed: oildag 3～15, ionic liquid 0.5～8, resin carrier 69-75, carbon dust 12～26.
In the high conductive carbon paste, said ionic liquid is K
+A
-, wherein, K
+Be selected from following positively charged ion:
R
1-R
5Independent separately is H, halogen, C
1-C
8Alkyl, part hydrogen or all hydrogen by F, Cl, N (C
nF
(2n+1-x)H
x)
2, O (C
nF
(2n+1-x)H
x), SO
2(C
nF
(2n+1-x)H
x) or C
nF
(2n+1-x)H
xIn the substituted C of one or more groups
1-C
8Alkyl, 1＜n＜6 and 0＜x≤13;
A
-Be selected from halide-ions; Two fluoro-alkyl alkylsulfonyl acid amides ions; Perfluoroalkyl alkylsulfonyl acid amides ion; Two fluoro-alkyl alkylsulfonyl amide imide ions; Perfluoroalkyl alkylsulfonyl amide imide ion; The alkyl toluene sulfonate ion; Aryl toluenesulphonic acids radical ion; Perfluoroalkyl toluenesulphonic acids radical ion; Nitrate ion; Sulfate ion; The hydrosulphuric acid radical ion; Alkyl sulfate ion; The aromatic sulfuric acid radical ion; The polyether thiourea acid ion; The polyether sulphur acid ion; The perfluoroalkyl sulfate ion; Sulfonate ion; Alkyl sulfonate ion; The aryl sulfonic acid radical ion; The perfluoro alkyl sulfonic acid radical ion; Perfluoro aryl sulfonic acid radical ion; The alkyl carboxylic acid radical ion; The aryl carboxylic acid radical ion; The perfluoroalkyl carboxylic acid ion; Perchlorate or tetrachloro aluminate ion; The dicyanamide ion; Thiocyanate ion; Tricyano methyl ion; The isothiocyanic acid radical ion; The tetraphenyl borate ion; Tetrafluoro is for the phenyl-boron dihydroxide radical ion; Phenyl-pentafluoride ylboronic acid radical ion; Tetrafluoro is for borate ion; The hexafluoro-phosphate anion; Polyethers phosphate anion or phosphate anion.
In the high conductive carbon paste, said K
+Preferably certainly: 1,3-dialkylimidazolium positively charged ion, 1,3-dialkyl group pyridylium or 1,2,3-trialkyl glyoxaline cation.
In the high conductive carbon paste, said A
-Preferably certainly: dicyanamide ion, thiocyanate ion or isothiocyanic acid radical ion.
In the high conductive carbon paste, said resin carrier is preferably processed by the raw material of following parts by weight: urethane resin 12-15, vinyl resin 12-15, high boiling solvent 65-68, coupling agent 0.1-0.8.
In the high conductive carbon paste, said high boiling solvent is diethylene adipate, 2-Butoxyethyl acetate or 1, a kind of in the 4-GBL.
In the high conductive carbon paste, said coupling agent is silane coupling agent or titanate coupling agent.
In the high conductive carbon paste, said high conductive carbon paste also comprises the dispersion agent of 0.2-1 parts by weight.
In the high conductive carbon paste, said dispersion agent is talcum powder or ZX-I dispersion agent.
A kind of preparation method of above-mentioned high conductive carbon paste may further comprise the steps:
1), the preparation resin carrier: weighing urethane resin, vinyl resin, high boiling solvent, under 80-95 ℃, be stirred to fully dissolving, add then and make resin carrier after coupling agent stirs;
2), prepare high conductive carbon paste: with carbon dust, oildag, ionic liquid and resin carrier fully mix mixture, grind then and make mixture form even matter phase, promptly obtain high conductive carbon paste.
In the high conductive carbon paste of the present invention, except carbon dust, also introduce the ionic liquid of high conductivity effectively, make the conductivity of carbon slurry obtain very big improvement.This is because on microtexture, carbon dust provides long-range conduction, and ionic liquid provides the short range conduction.When both were used simultaneously, ionic liquid played the effect of " bridge joint " to the overlap joint of adjacent carbons powder particles, thereby made material have higher electroconductibility.Add in the ion liquid high conductive carbon paste, even reduce under the situation of carbon dust addition, the electroconductibility of material is constant even higher than originally.High conduction performance of the present invention is that conductive carbon paste is applied in the high-end product coating processing safety is provided, and can be used for substituting expensive conductive silver paste commonly used.
The introducing of intermediate ion liquid of the present invention makes that conductive carbon paste forms be coated with rete and matrix combine even more ideally, can not come off by peeling, and improved the curing efficiency that is coated with rete.This is because ionic liquid also serves as cosolvent in feed composition effect can not only keep feed composition characteristics separately, can also pass through differing mol combination each other, plays the mutual supplement with each other's advantages effect, the conducting coat layer that obtained performance is better.
The present invention has effectively improved the conductivity of conductive carbon paste; Improve conductive carbon paste and applied the curing efficiency that uses; For it provides reliable assurance in the utilization of high-end field, may be used in high-end film key, printed resistor, heat generating component, flexibility and the hybrid circuit.
Preparing method of the present invention, simple and reliable process, low cost of manufacture, preparing product quality are good.
Embodiment
Below in conjunction with several concrete embodiment; Further specify high conductive carbon paste provided by the present invention and preparation method thereof; And, explain through the advantage of the resulting high conductive carbon paste of preparation method provided by the present invention on conductivity, curing efficiency to the test of product The coating experiment.
The preparation of resin carrier:
(1) adopt the raw material of following parts by weight to process:
By above prescription weighing urethane resin, vinyl resin, high boiling solvent 2-Butoxyethyl acetate high-speed stirring 3 hours in 80 ℃ of water-baths; Make resin be dissolved in the solvent fully; Add coupling agent A150 then and stirred 30 minutes, evenly back tagged resin carrier A is for use.
(2) adopt the raw material of following parts by weight to process:
By above prescription weighing urethane resin, vinyl resin, high boiling solvent diethylene adipate high-speed stirring 5 hours in 85 ℃ of water-baths; Make resin be dissolved in the solvent fully; Add coupling agent A170 then and stirred 30 minutes, evenly back tagged resin carrier B is for use.
(3) adopt the raw material of following parts by weight to process:
By above prescription weighing urethane resin, vinyl resin, high boiling solvent diethylene adipate high-speed stirring 5 hours in 85 ℃ of water-baths, make resin be dissolved in fully in the solvent, add then coupling agent A170 stirred 30 minutes resin carrier C.
Embodiment 1: a kind of high conductive carbon paste comprises the raw material of following parts by weight:
Taking by weighing carbon dust, oildag, ionic liquid (1-ethyl-3-Methylimidazole thiocyanate-) and resin carrier A fully mixes; Use three-roll grinder to grind 5 times then according to per 10 minutes one kilogram speed; Make mixture form even matter phase, promptly obtain high conductive carbon paste.
High conductive carbon paste is coated on the insulcrete, and then 135 ℃ of moulding that are heating and curing, balance was tested resistance per square after 7 days under different humiture environment at last.
The comparative example 1: a kind of conductive carbon paste comprises the raw material of following parts by weight:
12.5 parts of carbon dusts (0.7 μ m)
15 parts of oildags (800 order)
75 parts of resin carrier A
Take by weighing carbon dust, oildag, resin carrier A by above proportioning and fully mix, use three-roll grinder to grind 5 times then, make mixture form even matter phase, promptly obtain correlated conductive carbon paste according to per 10 minutes one kilogram speed.
Correlated conductive carbon paste is coated on the insulcrete, and then 135 ℃ of moulding that are heating and curing, balance was tested resistance per square after 7 days under different humiture environment at last.
Embodiment 2: a kind of high conductive carbon paste comprises the raw material of following parts by weight:
Taking by weighing carbon dust, oildag, ionic liquid (1-butyl-3-Methylimidazole villaumite) and resin carrier by above proportioning fully mixes; Use three-roll grinder to grind 5 times then according to per 10 minutes one kilogram speed; Make mixture form even matter phase, promptly obtain high conductive carbon paste.
High conductive carbon paste is coated on the insulcrete, and then 135 ℃ of moulding that are heating and curing, balance was tested resistance per square after 7 days under different humiture environment at last.
The comparative example 2: a kind of conductive carbon paste comprises the raw material of following parts by weight:
29 parts of carbon dusts (0.7 μ m)
8 parts of oildags (800 order)
69 parts of resin carrier B
Take by weighing carbon dust, oildag and resin carrier B by above proportioning and fully mix, use three-roll grinder to grind 4 times then, make mixture form even matter phase, promptly obtain correlated conductive carbon paste according to per 10 minutes one kilogram speed.
Correlated conductive carbon paste is coated on the insulcrete, and then 135 ℃ of moulding that are heating and curing, balance was tested resistance per square after 7 days under different humiture environment at last.
Embodiment 3: a kind of high conductive carbon paste comprises the raw material of following parts by weight:
Take by weighing carbon dust, oildag, ionic liquid (1-dodecyl-3-Methylimidazole thiocyanate-), DA dispersion agent and resin carrier A, fully mix by above proportioning; Use three-roll grinder to grind 6 times then according to per 10 minutes one kilogram speed; Make mixture form even matter phase, promptly obtain high conductive carbon paste.
High conductive carbon paste is coated on the insulcrete, and then 135 ℃ of moulding that are heating and curing, balance was tested resistance per square after 7 days under different humiture environment at last.
Embodiment 4: a kind of high conductive carbon paste comprises the raw material of following parts by weight:
Taking by weighing carbon dust, oildag, ionic liquid (1-benzyl-3-methyl imidazolium tetrafluoroborate) DA dispersion agent and resin carrier A by above proportioning fully mixes; Use three-roll grinder to grind 6 times then according to per 10 minutes one kilogram speed; Make mixture form even matter phase, promptly obtain high conductive carbon paste.
High conductive carbon paste is coated on the insulcrete, and then 135 ℃ of moulding that are heating and curing, balance was tested resistance per square after 7 days under different humiture environment at last.
Embodiment 5: a kind of high conductive carbon paste comprises the raw material of following parts by weight:
Take by weighing carbon dust oildag ionic liquid (1-octyl group-3-picoline hexafluorophosphate salt) talcum powder and resin carrier A fully mixes by above proportioning; Use three-roll grinder to grind 4 times then according to per 10 minutes one kilogram speed; Make mixture form even matter phase, promptly obtain high conductive carbon paste.
High conductive carbon paste is coated on the insulcrete, and then 135 ℃ of moulding that are heating and curing, balance was tested resistance per square after 7 days under different humiture environment at last.
Embodiment 6: a kind of high conductive carbon paste comprises the raw material of following parts by weight:
Taking by weighing carbon dust, oildag, ionic liquid (1-ethyl-3-Methylimidazole isothiocyanate) and resin carrier B by above prescription fully mixes; Use three-roll grinder to grind 5 times then according to per 10 minutes one kilogram speed; Make mixture form even matter phase, promptly obtain high conductive carbon paste.
High conductive carbon paste is coated on the insulcrete, and then 135 ℃ of moulding that are heating and curing, balance was tested resistance per square after 7 days under different humiture environment at last.
Embodiment 7: a kind of high conductive carbon paste comprises the raw material of following parts by weight:
Taking by weighing carbon dust, oildag, ionic liquid (1-vinyl-3-Methylimidazole perchlorate), DA dispersion agent and resin carrier B by above prescription fully mixes; Use three-roll grinder to grind 5 times then according to per 10 minutes one kilogram speed; Make mixture form even matter phase, promptly obtain high conductive carbon paste.
High conductive carbon paste is coated on the insulcrete, and then 135 ℃ of moulding that are heating and curing, balance was tested resistance per square after 7 days under different humiture environment at last.
Embodiment 8: a kind of high conductive carbon paste comprises the raw material of following parts by weight:
Taking by weighing carbon dust, oildag, ionic liquid (the two fluoroform sulfimide salt of 1-allyl group-3-Methylimidazole), DA dispersion agent and resin carrier B by above proportioning fully mixes; Use three-roll grinder to grind 4 times then according to per 10 minutes one kilogram speed; Make mixture form even matter phase, promptly obtain high conductive carbon paste.
High conductive carbon paste is coated on the insulcrete, and then 135 ℃ of moulding that are heating and curing, balance was tested resistance per square after 7 days under different humiture environment at last.
Embodiment 9: a kind of high conductive carbon paste comprises the raw material of following parts by weight:
Take by weighing carbon dust, oildag, ionic liquid (1-ethyl-2 by above prescription; 3-methylimidazole dicyan amine salt), DA dispersion agent and resin carrier B fully mix; Use three-roll grinder to grind 6 times then according to per 10 minutes one kilogram speed; Make mixture form even matter phase, promptly obtain high conductive carbon paste.
High conductive carbon paste is coated on the insulcrete, and then 135 ℃ of moulding that are heating and curing, balance was tested resistance per square after 7 days under different humiture environment at last.
Embodiment 10: a kind of high conductive carbon paste comprises the raw material of following parts by weight:
Taking by weighing carbon dust, oildag, ionic liquid (1-vinyl-3-Methylimidazole tosilate), DA dispersion agent and resin carrier C by above prescription fully mixes; Use three-roll grinder to grind 5 times then according to per 10 minutes one kilogram speed; Make mixture form even matter phase, promptly obtain high conductive carbon paste.
High conductive carbon paste is coated on the insulcrete, and then 135 ℃ of moulding that are heating and curing, balance was tested resistance per square after 7 days under different humiture environment at last.
The test result of the foregoing description is recorded in table 1.
The electric property of table 1 oil film
Resistance per square is the resistance of certain thickness, unit surface material.
From last table, can find out: after only adding small amount of ionic liquid among the embodiment 1; The resistance per square of conductive carbon paste is with regard to decrease to some degree; After embodiment 2～10 intermediate ion liquid additions increased to a certain degree, the resistance per square of conductive carbon paste just had reduction significantly.
Claims (8)
1. a high conductive carbon paste is characterized in that, comprises that the raw material of following parts by weight is processed: oildag 3-15 part, ionic liquid 0.5-8 part, resin carrier 69-75 part, carbon dust 12-26 part;
Said ionic liquid is K
+A
-, wherein, K
+Be selected from following positively charged ion:
R
1-R
5Independent separately is H, halogen, C
1-C
8Alkyl, part hydrogen or all hydrogen by F, Cl, N (C
nF
(2n+1-x)H
x)
2, O (C
nF
(2n+1-x)H
x), SO
2(C
nF
(2n+1-x)H
x) or C
nF
(2n+1-x)H
xIn the substituted C of one or more groups
1-C
8Alkyl, 1<n<6 and 0<x<13;
A
-Be selected from halide-ions; Two fluoro-alkyl alkylsulfonyl acid amides ions; Perfluoroalkyl alkylsulfonyl acid amides ion; Two fluoro-alkyl alkylsulfonyl amide imide ions; Perfluoroalkyl alkylsulfonyl amide imide ion; The alkyl toluene sulfonate ion; Aryl toluenesulphonic acids radical ion; Perfluoroalkyl toluenesulphonic acids radical ion; Nitrate ion; Sulfate ion; The hydrosulphuric acid radical ion; Alkyl sulfate ion; The aromatic sulfuric acid radical ion; The polyether thiourea acid ion; The polyether sulphur acid ion; The perfluoroalkyl sulfate ion; Sulfonate ion; Alkyl sulfonate ion; The perfluoro alkyl sulfonic acid radical ion; Perfluoro aryl sulfonic acid radical ion; The alkyl carboxylic acid radical ion; The aryl carboxylic acid radical ion; The perfluoroalkyl carboxylic acid ion; Perchlorate or tetrachloro aluminate ion; The dicyanamide ion; Thiocyanate ion; Tricyano methyl ion; The isothiocyanic acid radical ion; The tetraphenyl borate ion; Tetrafluoro is for the phenyl-boron dihydroxide radical ion; Phenyl-pentafluoride ylboronic acid radical ion; Tetrafluoro is for borate ion; The hexafluoro-phosphate anion; Polyethers phosphate anion or phosphate anion;
Said resin carrier is processed by the raw material of following parts by weight: urethane resin 12-15 part, vinyl resin 12-15 part, high boiling solvent 65-68 part, coupling agent 0.1-0.8 part.
2. high conductive carbon paste according to claim 1 is characterized in that, said K
+Be selected from: 1,3-dialkylimidazolium positively charged ion, 1,3-dialkyl group pyridylium or 1,2,3-trialkyl glyoxaline cation.
3. high conductive carbon paste according to claim 1 is characterized in that, said A
-Be selected from: dicyanamide ion, thiocyanate ion or isothiocyanic acid radical ion.
4. high conductive carbon paste according to claim 1 is characterized in that, said high boiling solvent is diethylene adipate, 2-Butoxyethyl acetate or 1, a kind of in the 4-GBL.
5. high conductive carbon paste according to claim 1 is characterized in that, said coupling agent is silane coupling agent or titanate coupling agent.
6. according to any described high conductive carbon paste of claim 1-5, it is characterized in that said high conductive carbon paste also comprises the dispersion agent of 0.2-1 parts by weight.
7. high conductive carbon paste according to claim 6 is characterized in that, said dispersion agent is talcum powder or ZX-I dispersion agent.
8. the preparation method of any said high conductive carbon paste of claim 1-5 is characterized in that, may further comprise the steps:
1), the preparation resin carrier: weighing urethane resin, vinyl resin, high boiling solvent, under 80-95 ℃, be stirred to fully dissolving, add then and make resin carrier after coupling agent stirs;
2), prepare high conductive carbon paste: with carbon dust, oildag, ionic liquid and resin carrier fully mix mixture, grind then and make mixture form even matter phase, promptly obtain high conductive carbon paste.
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| CN104766951A (en) * | 2015-04-16 | 2015-07-08 | 田东 | Preparation method of liquid-cladding modified lithium ion battery negative pole piece |
| CN106952677A (en) * | 2017-03-28 | 2017-07-14 | 北京印刷学院 | A kind of conductive carbon paste for high temperature resistant sensing and preparation method thereof |
| CN108962607A (en) * | 2017-05-23 | 2018-12-07 | 中国振华集团云科电子有限公司 | A kind of impregnated graphite slurry and preparation method thereof |
| CN116313510B (en) * | 2023-05-12 | 2023-08-15 | 先禾新材料(苏州)有限公司 | Conductive carbon paste for high molecular tantalum capacitor and preparation method and application method thereof |
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| CN101935477A (en) * | 2010-09-27 | 2011-01-05 | 彩虹集团公司 | Low-temperature conductive carbon paste and preparation method thereof |
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