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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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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| CN102618107B (en) * | 2012-03-31 | 2014-10-08 | 深圳市贝特瑞纳米科技有限公司 | Conductive graphite cream and preparation method thereof |
| 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 high temperature resistant sensing conductive carbon paste 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 |
Citations (2)
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|---|---|---|---|---|
| CN101407628A (en) * | 2008-11-21 | 2009-04-15 | 天津市华林伟业科技发展有限公司 | Method for producing water-soluble PTC functional conductive carbon paste |
| 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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| JP2010062507A (en) * | 2008-09-05 | 2010-03-18 | Dynic Corp | Sheet for electrode material for electric double layer capacitor, electrode material for electric double layer capacitor, and method of manufacturing the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101407628A (en) * | 2008-11-21 | 2009-04-15 | 天津市华林伟业科技发展有限公司 | Method for producing water-soluble PTC functional conductive carbon paste |
| 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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| JP特开2010-062507A 2010.03.18 |
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