CN104178053A - Graphene composite conductive adhesive - Google Patents
Graphene composite conductive adhesive Download PDFInfo
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- CN104178053A CN104178053A CN201310202478.8A CN201310202478A CN104178053A CN 104178053 A CN104178053 A CN 104178053A CN 201310202478 A CN201310202478 A CN 201310202478A CN 104178053 A CN104178053 A CN 104178053A
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- graphene
- graphene composite
- conducting glue
- composite conducting
- ether
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Abstract
The invention provides a graphene composite conductive adhesive which is characterized by comprising the following components by the mass percentage: 30-65% of a conductive filler, 1-50% of grapheme, 1-20% of resin, 0.1-5% of an additive, and 10-67% of a main solvent. With combination of the graphene advantage of high thermal conductivity and the nano metal advantage of low melting point, the sintering temperature of the conductive adhesive can be allowed to be lower, and thus energy and costs are saved; with super large specific surface area of the graphene, nano particles can be uniformly dispersed between graphene sheet layers, the problems of graphene agglomeration and nano particle settlement in the conductive adhesive are avoided, and the conductive property and bonding strength of the conductive adhesive are improved. The conductive adhesive is simple in preparation process and suitable for mass production.
Description
Technical field
The present invention relates to a kind of conductive resin, particularly a kind of Graphene composite conducting glue, belongs to electron device package and manufactures field.
Background technology
Graphene is to conduct electricity at present and heat conductivility best material, resistivity approximately 10
-6Ω cm, lower than copper or silver, be the current material of resistivity minimum in the world; Thermal conductivity is up to 3000W/mK, and higher than carbon nanotube and diamond, under normal temperature, its electronic mobility exceedes 15000cm
2/ Vs, again than CNT (carbon nano-tube) or silicon wafer height.Because its resistivity is extremely low, the speed of electronic migration is exceedingly fast, and is therefore expected to can be used to develop thinner, conduction speed electronic component of new generation or transistor faster.
Along with the development of semiconductor integrated circuit package industry, the selection of electronic package material is most important.Conductive resin is a kind of specific function assembly glue that contains conductive filler material, and the conduction that can realize between plain conductor and base material connects, and perfect physical adhesion, is the critical material in electron device package manufacturing technology.Conductive resin without Lead contamination, ultra fine-pitch connect, the feature such as technique is simple, all meet the requirement of semiconductor integrated circuit functionalization, miniaturization, high-performance and health.The at present also following problem of ubiquity of conductive resin, as high in solidification value, conduction, heat conductivility are poor etc. limits its development.
The Electronic Performance of Graphene excellence, the specific surface area of super large and lower production cost, be suitable for the high quality filler of high performance polymer composite material.Graphene composite conducting glue, utilizes the low-melting advantage of Graphene high thermal conductivity and nano metal, can make conductive resin sintering temperature lower, realizes excellent conductivity.
Summary of the invention
The object of the invention is to make up above-mentioned the deficiencies in the prior art, a kind of Graphene composite conducting glue is provided, compound by Graphene and micron order metallic particles or nanometer grade gold metal particles, realize conduction and the interior better transmission of heat conduction two-dimensions plane between metallic particles, shorten greatly the pathway between metallic particles, improved conduction and the heat conductivility of conductive resin; Conductive resin of the present invention has lower sintering temperature, save energy and cost, and also preparation technology is simple, is applicable to scale operation.
The present invention realizes in the following way, a kind of Graphene composite conducting glue, is characterized in that: be made up of following component and mass percent: conductive filler material 30～65%, Graphene 1～50%, resin 1～20%, additive 0.1～5%, main body solvent 10～67%.Above-mentioned each constituent mass percentage composition sum is 100%.
Described conductive filler material can be micron order metallic particles, nanometer grade gold metal particles or micro-nano composite metal particles composition.
It is the shapes such as spherical, sheet, disk, triangle that the particle shape of described conductive filler material can be, but not limited to.
Described metallic particles can be but be not limited to gold and silver, copper, aluminum metal particle.
Described micron metal grain diameter scope is 0.1 μ m～10 μ m, and nano-metal particle particle size range is 1nm～100nm.
Described Graphene is selected from the grapheme material that in chemical Vapor deposition process, mechanically peel method, chemical stripping method, chemical synthesis prepared by any method.
Described resin includes but not limited to it is one or both in polyester, polyacrylic, vinyl chloride-vinyl acetate resin, urethane, epoxy resin.
Described additive is flow agent, pH value conditioning agent, tensio-active agent.
Described Graphene composite conducting glue, is characterized in that: described flow agent is the one in polyacrylic ester, cellaburate, polymethyl siloxane.
Described Graphene composite conducting glue, is characterized in that: described pH value conditioning agent is the one in ammoniacal liquor, sodium hydroxide, trolamine, sodium phosphate and azanol.
Described Graphene composite conducting glue, is characterized in that: described tensio-active agent is the one in lipid acid, fatty acid ester, Sodium dodecylbenzene sulfonate, sodium lauryl sulphate, polyoxyethylene alkylamide, polysiloxane, polysorbate and Sodium perfluorooctanoate.
Described main body solvent includes but not limited to ethanol, ethylene glycol, Virahol, glycol ether, triglycol, ethylene glycol monomethyl ether, ethylene glycol ethyl ether, butyl glycol ether, ethylene glycol phenyl ether, ethylene glycol benzyl oxide, , diethylene glycol methyl ether, diethylene glycol ethyl ether, butyl carbitol, triglycol methyl ether, Pyranton, methyl-sulphoxide, N-Methyl pyrrolidone, N,N-DIMETHYLACETAMIDE, Trivalin SF acetic ester, oleum lini, high-boiling point kerosene, tridecanol, tung oil, common gummy oil, tetradecyl alcohol, tetramethylolmethane, soybean oil, rosinol, virtue camphor tree Terpineol 350, dioctyl phthalate (DOP), vinyl acetic monomer, N-BUTYL ACETATE, pimelinketone, bicyclohexyl, hexanaphthene, propyl carbinol, butanone, deionized water, hydroxyethyl-pyrrolidone, dimethyl phthalate, oxyethane, Sorbitol Powder, plam oil, one or more in spearmint oil.
The present invention compared with prior art tool has the following advantages:
1, the present invention, in conjunction with the low-melting advantage of Graphene high thermal conductivity and nano metal, can make the sintering temperature of conductive resin lower, save energy and cost.
2, the specific surface area of Graphene super large, can make nano particle be dispersed in graphene film interlayer, has avoided reunion and the settlement issues of nano particle in conductive resin of Graphene, has improved electroconductibility and the cohesive strength of conductive resin.
Embodiment
Below in conjunction with specific embodiment, the present invention will be described in detail.
The experimental technique using in following embodiment if no special instructions, is ordinary method.
Material, reagent etc. used in following embodiment, if no special instructions, all can obtain from commercial channels.
Embodiment 1:
The compound micro-silver powder of Graphene is prepared conductive resin, accurately takes 2g polymethyl acrylic acid, joins in 9g Trivalin SF acetic ester, in planetary power mixer, stirs 2h; The flake silver powder and the 1g graphene powder Morsh-P2 (Ningbo Mo Xi science and technology) that are 2 μ m by 10g particle diameter add in above-mentioned solution successively, ultrasonic 30 minutes, add the trolamine of 0.1g flow agent, 0.1g Sodium dodecylbenzene sulfonate and 0.05g, continue to stir 1h, obtain Graphene composite conducting glue; Using RTS-9 four point probe tester to survey under 150 DEG C of conditions of this conductive resin sheet resistance after sintering 3min is 11.2m Ω/.
Embodiment 2
Graphene composite micro-nano rice silver powder is prepared conductive resin, accurately takes 2g vibrin, joins in 10g ethylene glycol phenyl ether, in planetary power mixer, stirs 2h; Be that the flake silver powder of 2 μ m and the nano-silver powder of 1g particle diameter 50nm and 1.5g graphene powder Morsh-P2 (Ningbo Mo Xi science and technology) add in above-mentioned solution successively by 9g particle diameter, ultrasonic 30 minutes, add 30% the ammonia soln of 0.1g flow agent, 0.2g Sodium dodecylbenzene sulfonate and 0.1g, continue to stir 1.5h, obtain Graphene composite conducting glue; Using RTS-9 four point probe tester to survey under 150 DEG C of conditions of this conductive resin sheet resistance after sintering 3min is 2.6m Ω/.
Embodiment 3
The compound micro-silver powder of Graphene is prepared conductive resin, accurately takes 3.5g polymethyl acrylic acid, joins in 15g Trivalin SF acetic ester, in planetary power mixer, stirs 2h; The flake copper and the 1.5g import CVD copper base single-layer graphene (Nanjing Xian Feng nano material) that are 2 μ m by 10g particle diameter add in above-mentioned solution successively, ultrasonic 30 minutes, add the trolamine of 0.15g flow agent, 0.3g Sodium dodecylbenzene sulfonate and 0.1g, continue to stir 1h, obtain Graphene composite conducting glue; Using RTS-9 four point probe tester to survey under 150 DEG C of conditions of this conductive resin sheet resistance after sintering 3min is 3.4m Ω/.
Embodiment 4
The compound micro-silver powder of Graphene is prepared conductive resin, accurately takes 2.5g vinyl chloride-vinyl acetate resin, joins in 12g Trivalin SF acetic ester, in planetary power mixer, stirs 2h; The ball shape silver powder and the 1g CVD copper base single-layer graphene (Nanjing Xian Feng nano material) that are 3 μ m by 10g particle diameter add in above-mentioned solution successively, ultrasonic 30 minutes, add the trolamine of 0.1g flow agent, 0.1g Sodium dodecylbenzene sulfonate and 0.05g, continue to stir 1h, obtain Graphene composite conducting glue; Using RTS-9 four point probe tester to survey under 150 DEG C of conditions of this conductive resin sheet resistance after sintering 3min is 3.2m Ω/.
Embodiment 5
Graphene composite micro-nano rice silver powder is prepared conductive resin, accurately takes 2.5g vibrin, joins in 13g ethylene glycol phenyl ether, in planetary power mixer, stirs 2h; Be that the ball aluminum powder of 3 μ m and the nano-silver powder of 1g particle diameter 50nm and 2.0g graphene powder SX-I (Changzhou No.6 Element Material Technology Co., Ltd.) add in above-mentioned solution successively by 12g particle diameter, ultrasonic 30 minutes, add 30% the ammonia soln of 0.1g flow agent, 0.3g Sodium dodecylbenzene sulfonate and 0.1g, continue to stir 1.5h, obtain Graphene composite conducting glue; Using RTS-9 four point probe tester to survey under 150 DEG C of conditions of this conductive resin sheet resistance after sintering 3min is 6.5m Ω/.
Embodiment 6
Graphene composite micro-nano rice silver powder is prepared conductive resin, accurately takes 2.5g polymethacrylate resin, joins in 12g butyl carbitol, in planetary power mixer, stirs 2h; Be that the ball shape silver powder of 5 μ m and the nano-silver powder of 0.5g particle diameter 30nm and 1.5g CVD copper base single-layer graphene (Nanjing Xian Feng nano material) add in above-mentioned solution successively by 8g particle diameter, ultrasonic 30 minutes, add the trolamine of 0.1g flow agent, 0.25g Sodium dodecylbenzene sulfonate and 0.1g, continue to stir 1h, obtain Graphene composite conducting glue; Using RTS-9 four point probe tester to survey under 150 DEG C of conditions of this conductive resin sheet resistance after sintering 3min is 5.3m Ω/.
Embodiment 7
Graphene composite micro-nano rice silver powder is prepared conductive resin, accurately takes 1.5g vibrin, joins in 12g ethylene glycol phenyl ether, in planetary power mixer, stirs 2h; Be that the spherical copper powder of 3 μ m and the nano-silver powder of 1g particle diameter 50nm and 2.0g multi-layer graphene microplate JCG-4 (lucky storehouse nanometer) add in above-mentioned solution successively by 7g particle diameter, ultrasonic 30 minutes, add 30% the ammonia soln of 0.1g flow agent, 0.3g Sodium dodecylbenzene sulfonate and 0.1g, continue to stir 1.5h, obtain Graphene composite conducting glue; Using RTS-9 four point probe tester to survey under 150 DEG C of conditions of this conductive resin sheet resistance after sintering 3min is 9.7m Ω/.
Embodiment 8
Graphene composite micro-nano rice silver powder is prepared conductive resin, accurately takes 2.5g vibrin, joins in 13g ethylene glycol phenyl ether, in planetary power mixer, stirs 2h; Be that the trilateral silver powder of 3 μ m and the nano-silver powder of 1g particle diameter 100nm and 2.0g graphene powder graphene powder SX-II (Changzhou No.6 Element Material Technology Co., Ltd.) add in above-mentioned solution successively by 10g particle diameter, ultrasonic 30 minutes, add 30% the ammonia soln of 0.1g flow agent, 0.3g Sodium dodecylbenzene sulfonate and 0.1g, continue to stir 1.5h, obtain Graphene composite conducting glue; Using RTS-9 four point probe tester to survey under 150 DEG C of conditions of this conductive resin sheet resistance after sintering 3min is 4.8m Ω/.
Claims (9)
1. a Graphene composite conducting glue, is characterized in that: be made up of following component and percentage composition: conductive filler material 30～65%, Graphene 1～50%, resin 1～20%, additive 0.1～5%, main body solvent 10～67%.Above-mentioned each constituent mass percentage composition sum is 100%.
2. Graphene composite conducting glue according to claim 1, is characterized in that: described conductive filler material can be micron order metallic particles, nanometer grade gold metal particles or micro-nano composite metal particles.
It is the shapes such as spherical, sheet, disk, triangle that the particle shape of described conductive filler material can be, but not limited to.
Described metallic particles can be but be not limited to gold and silver, copper, aluminum metal particle.
Described micron metal grain diameter scope is 0.1 μ m～10 μ m; Nano-metal particle particle size range is 1nm～100nm.
3. Graphene composite conducting glue according to claim 1, is characterized in that: described Graphene can be the grapheme material that in chemical Vapor deposition process, mechanically peel method, chemical stripping method, chemical synthesis prepared by any method.
4. Graphene composite conducting glue according to claim 1, is characterized in that: described resin includes but not limited to it is one or both in polyester, polyacrylic, vinyl chloride-vinyl acetate resin, urethane, epoxy resin.
5. Graphene composite conducting glue according to claim 1, is characterized in that: described additive comprises flow agent, pH value conditioning agent, tensio-active agent.
6. Graphene composite conducting glue according to claim 5, is characterized in that: described flow agent is the one in polyacrylic ester, cellaburate, polymethyl siloxane.
7. Graphene composite conducting glue according to claim 5, is characterized in that: described pH value conditioning agent is the one in ammoniacal liquor, sodium hydroxide, trolamine, sodium phosphate and azanol.
8. Graphene composite conducting glue according to claim 5, is characterized in that: described tensio-active agent is the one in lipid acid, fatty acid ester, Sodium dodecylbenzene sulfonate, sodium lauryl sulphate, polyoxyethylene alkylamide, polysiloxane, polysorbate and Sodium perfluorooctanoate.
9. according to the Graphene composite conducting glue described in claim 1-8 any one, it is characterized in that: described main body solvent includes but not limited to ethanol, ethylene glycol, Virahol, glycol ether, triglycol, ethylene glycol monomethyl ether, ethylene glycol ethyl ether, butyl glycol ether, ethylene glycol phenyl ether, ethylene glycol benzyl oxide, , diethylene glycol methyl ether, diethylene glycol ethyl ether, butyl carbitol, triglycol methyl ether, Pyranton, methyl-sulphoxide, N-Methyl pyrrolidone, N,N-DIMETHYLACETAMIDE, Trivalin SF acetic ester, oleum lini, high-boiling point kerosene, tridecanol, tung oil, common gummy oil, tetradecyl alcohol, tetramethylolmethane, soybean oil, rosinol, virtue camphor tree Terpineol 350, dioctyl phthalate (DOP), vinyl acetic monomer, N-BUTYL ACETATE, pimelinketone, bicyclohexyl, hexanaphthene, propyl carbinol, butanone, deionized water, hydroxyethyl-pyrrolidone, dimethyl phthalate, oxyethane, Sorbitol Powder, plam oil, one or more in spearmint oil.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201310202478.8A CN104178053A (en) | 2013-05-28 | 2013-05-28 | Graphene composite conductive adhesive |
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| CN201310202478.8A CN104178053A (en) | 2013-05-28 | 2013-05-28 | Graphene composite conductive adhesive |
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| CN104178053A true CN104178053A (en) | 2014-12-03 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106450326A (en) * | 2016-09-28 | 2017-02-22 | 成都新柯力化工科技有限公司 | Highly-dispersed graphene conductive powder and application thereof in lithium battery |
| CN106753025A (en) * | 2016-12-16 | 2017-05-31 | 吴中区穹窿山天仲高分子材料技术研究所 | A kind of graphene composite conductive glue |
| CN108779363A (en) * | 2016-03-29 | 2018-11-09 | 拓自达电线株式会社 | Conductive coating paint and used the conductive coating paint barrier enclosure body manufacturing method |
| CN108877990A (en) * | 2018-05-24 | 2018-11-23 | 江苏时瑞电子科技有限公司 | A kind of graphene nano conductive silver slurry and preparation method thereof |
| CN112031039A (en) * | 2020-08-28 | 2020-12-04 | 顾聪颖 | Pure titanium implosion expansion electrode for concrete electroosmosis waterproofing and use method |
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| CN102254584A (en) * | 2011-05-12 | 2011-11-23 | 中国科学院宁波材料技术与工程研究所 | General electronic paste based on graphene filler |
| CN102746808A (en) * | 2012-07-27 | 2012-10-24 | 清华大学深圳研究生院 | High-conductivity graphene conducting resin and preparation method thereof |
| CN102925100A (en) * | 2012-11-28 | 2013-02-13 | 上海材料研究所 | High-thermal conductivity conductive silver adhesive and preparation method thereof |
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2013
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Patent Citations (3)
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| CN102254584A (en) * | 2011-05-12 | 2011-11-23 | 中国科学院宁波材料技术与工程研究所 | General electronic paste based on graphene filler |
| CN102746808A (en) * | 2012-07-27 | 2012-10-24 | 清华大学深圳研究生院 | High-conductivity graphene conducting resin and preparation method thereof |
| CN102925100A (en) * | 2012-11-28 | 2013-02-13 | 上海材料研究所 | High-thermal conductivity conductive silver adhesive and preparation method thereof |
Non-Patent Citations (1)
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| 黄万抚: "《矿物材料及其加工工艺》", 31 January 2012, 冶金工业出版社 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108779363A (en) * | 2016-03-29 | 2018-11-09 | 拓自达电线株式会社 | Conductive coating paint and used the conductive coating paint barrier enclosure body manufacturing method |
| CN106450326A (en) * | 2016-09-28 | 2017-02-22 | 成都新柯力化工科技有限公司 | Highly-dispersed graphene conductive powder and application thereof in lithium battery |
| CN106450326B (en) * | 2016-09-28 | 2019-05-03 | 成都新柯力化工科技有限公司 | A kind of high dispersive graphene conductive powder and its application in lithium battery |
| CN106753025A (en) * | 2016-12-16 | 2017-05-31 | 吴中区穹窿山天仲高分子材料技术研究所 | A kind of graphene composite conductive glue |
| CN108877990A (en) * | 2018-05-24 | 2018-11-23 | 江苏时瑞电子科技有限公司 | A kind of graphene nano conductive silver slurry and preparation method thereof |
| CN112031039A (en) * | 2020-08-28 | 2020-12-04 | 顾聪颖 | Pure titanium implosion expansion electrode for concrete electroosmosis waterproofing and use method |
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Application publication date: 20141203 |