CN102925099A - Modified copper powder conducting resin and preparation method thereof - Google Patents
Modified copper powder conducting resin and preparation method thereof Download PDFInfo
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- CN102925099A CN102925099A CN2012104326468A CN201210432646A CN102925099A CN 102925099 A CN102925099 A CN 102925099A CN 2012104326468 A CN2012104326468 A CN 2012104326468A CN 201210432646 A CN201210432646 A CN 201210432646A CN 102925099 A CN102925099 A CN 102925099A
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Abstract
The invention relates to the technical field of conducting resin and particularly relates to modified copper powder conducting resin and a preparation method thereof. An existing technology is modified. The conducting resin comprises, by weight, 2-8% of curing agent, 1.0-10.0% of diluting agent, 0.05-3.5% of accelerant, 0.01-1% of plasticizing agent, 15-45% of grapheme modified copper powder and the balance organic silicon resin, and the sum of all component weights is 100%. The grapheme modified copper powder and the organic silicon resin are added, and then compared with the prior art, the conducting resin has good electric conductivity, hydroscopic property and silver anti-migration. The material cost is reduced greatly. The conducting resin and the method have great market potential and are practical.
Description
Technical field
The present invention relates to the conductive resin technical field, is improvements over the prior art, is specifically related to a kind of modification cupric powder conductive adhesive and preparation method thereof.
Background technology
In the microelectronics Packaging industry, conductive resin is attracting the strong development interest of people as a kind of special adhesive that has electroconductibility concurrently.Compare with traditional scolder, conductive resin have connect temperature low, need not to clean, be applicable to the advantages such as meticulousr lead spacing and high density components assembling, be acknowledged as the connecting material in the Electronic Packaging of future generation.
Disclose a kind of sliver-powder conducting glue and preparation method thereof in CN 1939999 patents, described conductive resin is comprised of the component of following parts by weight: 10-20 part Resins, epoxy, 5-25 part anhydride curing agent, 1-10 part reactive thinner, 0.01-0.1 part curing catalyst, 5-85 part flake silver powder, the granular silver powder of 5-85 part.The silver powder price that this patent adopts is very expensive and have silver migration risk so that product reliability is received has a strong impact on.
A kind of fire resistant epoxy conducting adhesive and preparation method thereof is disclosed in the CN101148571 patent, the weight percent of this adhesive formulation is: A15%～17% A Hydrogenated Bisphenol A, 8%～9.5% Resins, epoxy TGDDM (N, N, N ', N '-four glycidyl group-4,4 '-diaminodiphenylmethane), 1.5%～2.5% solidifying agent, 1%～2% promotor, 27%～30% silver powder, 41%～44 silver-coated copper powder %.This patent adopts the part silver-coated copper powder as conductive filler material, although part has reduced material cost; But contain the silver powder of higher proportion.
Graphene has unique physics, chemistry and mechanical property by a kind of novel material that the carbon six-ring forms, and the application that is considered to it may make many fields have a revolutionary change.
Summary of the invention
A kind of modification cupric powder conductive adhesive that the objective of the invention is to avoid above-mentioned weak point of the prior art and provide and preparation method thereof.This Graphene modification cupric powder conductive adhesive has the performances such as better electroconductibility, water absorbability, the migration of anti-silver, and material cost greatly reduces.
Purpose of the present invention can realize by following measure:
Modification cupric powder conductive adhesive of the present invention and preparation method thereof, its ingredient weight percent (%) is: 2.0 ~ 8.0% solidifying agent, 1.0 ~ 10.0% thinners, 0.05 ~ 3.5% promotor, 0.01 ~ 1.0% softening agent, 15.0 ~ 45.0% Graphene modification copper powder, all the other are silicone resin, each composition weight sum is 100%.
Described solidifying agent is one or more in glyoxal ethyline, 2-ethyl imidazol(e), titanic acid ester, methyl tributanoximo silane, tetraethoxy, methyl silicate, Trimethoxy silane, imidazoles, diethylenetriamine, the triethylene tetramine.Its Main Function is that its Main Function is the cross-linking system that forms tridimensional network, improves the mechanical property of product.
Described thinner is one or more in dimethyl succinate, Methyl glutarate, dimethyl adipate, methylal〔Su〕, tripropylene glycol butyl ether, dibutyl ethylene glycol ether, Virahol, the mixed propyl alcohol.Its Main Function is low-viscosity, and is easy to use and improve work-ing life.
Described promotor is ethylene thiourea, 2, one or more in the 2-dithio-bis-benzothiazole.Its Main Function is to accelerate curing reaction.
Described softening agent be in adipic acid ester, azelate, sebate, triethyl citrate, acetyl triethyl citrate, hexanodioic acid propanediol polyester, the sebacic acid propanediol polyester one or more.Its Main Function is the impact resistance that improves product.
The Main Function of described Graphene modification copper powder is as conductive filler material, improves conductivity, anti-silver-colored migration performance and reduces product cost etc.The preparation method of described Graphene modification copper powder comprises: mechanical ball milling, centrifugal mixer, little parcel, ultrasonic atomizatio, centrifugal atomizing etc.
The Main Function of described silicone resin is the body material as tackiness agent, except the required cohesive strength of product is provided, also effectively improves the water absorbability of product.
The preparation method of modification cupric powder conductive adhesive of the present invention, comprise the steps: that (1) is successively with silicone resin, 2 ~ 8% solidifying agent, 1.0 ~ 10.0% thinners, 0.05 ~ 3.5% promotor and 0.01 ~ 1% softening agent, add successively in the vacuum planetary mixer, be stirred to evenly, wherein vacuum tightness is that 0.065 ~ 0.099MPa, rotating speed are 25r/min ± 5 r/min; (2) add 15 ~ 45% Graphene modification copper powders again, be stirred to evenly, wherein vacuum tightness is that 0.065 ~ 0.099 MPa, rotating speed are 20r/min ± 5r/min; Namely get modification cupric powder conductive adhesive of the present invention.
The present invention has following advantage compared to existing technology: the one, the interpolation of Graphene modification copper powder, Effective Raise the performances such as the electroconductibility of product, the migration of anti-silver, and greatly reduce material cost; The 2nd, adopt silicone resin as the matrix of tackiness agent, effectively improved the water absorbability of product.The present invention is practical, has preferably prospects for commercial application.
Embodiment
Embodiment 1: silicone resin 81.84%
Diethylenetriamine 2.0%
Dimethyl succinate 1.0%
Ethylene thiourea 0.15%
Triethyl citrate 0.01%
Graphene modification copper powder 15.0%
By above-mentioned weight percentage, successively with silicone resin, diethylenetriamine, dimethyl succinate, ethylene thiourea and triethyl citrate, add successively that the rotating speed with 25r/min is stirred to evenly in the vacuum planetary mixer, add again Graphene modification copper powder, rotating speed with 20r/min is stirred to evenly, vacuum tightness is 0.075Mpa in the whole process, namely makes modification cupric powder conductive adhesive of the present invention.Adopt EDKSD-3 type volume specific resistance instrument to test behind 150 ℃ of curing 2.5h it, can get volume specific resistance is 1.3 * 10
-5Ω cm.
Embodiment 2: silicone resin 58.35%
Tetraethoxy 6.0%
Dimethyl succinate 3.0%
Dimethyl adipate 3.0%
2,2-dithio-bis-benzothiazole 1.25%
Hexanodioic acid propanediol polyester 0.4%
Graphene modification copper powder 28.0%
By above-mentioned weight percentage, successively with silicone resin, diethylenetriamine, dimethyl succinate, ethylene thiourea and triethyl citrate, add successively that the rotating speed with 25r/min is stirred to evenly in the vacuum planetary mixer, add again Graphene modification copper powder, rotating speed with 20r/min is stirred to evenly, vacuum tightness is 0.080Mpa in the whole process, namely makes modification cupric powder conductive adhesive of the present invention.Adopt EDKSD-3 type volume specific resistance instrument to test behind 150 ℃ of curing 2.5h it, can get volume specific resistance is 3.8 * 10
-5Ω cm.
Embodiment 3: silicone resin 32.5%
Methyl tributanoximo silane 8.0%
Dimethyl succinate 6.0%
Methylal〔Su〕 4.0%
2,2-dithio-bis-benzothiazole 3.5%
Sebate 1.0%
Graphene modification copper powder 45.0%
By above-mentioned weight percentage, successively with silicone resin, diethylenetriamine, dimethyl succinate, ethylene thiourea and triethyl citrate, add successively that the rotating speed with 25r/min is stirred to evenly in the vacuum planetary mixer, add again Graphene modification copper powder, rotating speed with 20r/min is stirred to evenly, vacuum tightness is 0.070Mpa in the whole process, namely makes modification cupric powder conductive adhesive of the present invention.Adopt EDKSD-3 type volume specific resistance instrument to test behind 150 ℃ of curing 2.5h it, can get volume specific resistance is 2.4 * 10
-5Ω cm.
Claims (6)
1. modification cupric powder conductive adhesive, its ingredient weight percent (%) is:
Solidifying agent 2.0 ~ 8.0%
Thinner 1.0 ~ 10.0%
Promotor 0.05 ~ 3.5%
Softening agent 0.01 ~ 1.0%
Graphene modification copper powder 15.0 ~ 45.0%
All the other are silicone resin, and each composition weight sum is 100%.
2. modification cupric powder conductive adhesive according to claim 1, it is characterized in that: described solidifying agent is one or more in glyoxal ethyline, 2-ethyl imidazol(e), titanic acid ester, methyl tributanoximo silane, tetraethoxy, methyl silicate, Trimethoxy silane, imidazoles, diethylenetriamine, the triethylene tetramine.
3. modification cupric powder conductive adhesive according to claim 1 is characterized in that: described thinner is one or more in dimethyl succinate, Methyl glutarate, dimethyl adipate, methylal〔Su〕, tripropylene glycol butyl ether, dibutyl ethylene glycol ether, Virahol, the mixed propyl alcohol.
4. modification cupric powder conductive adhesive according to claim 1, it is characterized in that: described promotor is ethylene thiourea, 2, one or more in the 2-dithio-bis-benzothiazole.
5. modification cupric powder conductive adhesive according to claim 1 is characterized in that: described softening agent be in adipic acid ester, azelate, sebate, triethyl citrate, acetyl triethyl citrate, hexanodioic acid propanediol polyester, the sebacic acid propanediol polyester one or more.
6. the preparation method of modification cupric powder conductive adhesive according to claim 1, it is characterized in that, comprise the steps: that (1) is successively with silicone resin, 2 ~ 8% solidifying agent, 1.0 ~ 10.0% thinners, 0.05 ~ 3.5% promotor and 0.01 ~ 1% softening agent, add successively in the vacuum planetary mixer, be stirred to evenly, wherein vacuum tightness is that 0.065 ~ 0.099MPa, rotating speed are 25r/min ± 5 r/min; (2) add 15 ~ 45% Graphene modification copper powders again, be stirred to evenly, wherein vacuum tightness is that 0.065 ~ 0.099 MPa, rotating speed are 20r/min ± 5r/min; Namely get modification cupric powder conductive adhesive of the present invention.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2012104326468A CN102925099A (en) | 2012-11-03 | 2012-11-03 | Modified copper powder conducting resin and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012104326468A CN102925099A (en) | 2012-11-03 | 2012-11-03 | Modified copper powder conducting resin and preparation method thereof |
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| CN102925099A true CN102925099A (en) | 2013-02-13 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103666354A (en) * | 2013-11-14 | 2014-03-26 | 昆山珍实复合材料有限公司 | Epoxy resin adhesive and preparation method thereof |
| CN104073188A (en) * | 2014-06-06 | 2014-10-01 | 苏州之诺新材料科技有限公司 | Acrylate conductive adhesive and preparation method thereof |
| CN109517177A (en) * | 2018-11-26 | 2019-03-26 | 衡阳思迈科科技有限公司 | The preparation method of the carboxy-modified conductive silver glue lotion of hydrocarbon |
| WO2019227559A1 (en) * | 2018-05-30 | 2019-12-05 | 江苏大学 | Solid conductive gel suitable for electrochemical system and preparation method therefor |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002086911A1 (en) * | 2001-04-23 | 2002-10-31 | Henkel Loctite Corporation | Conductive, silicone-based compositions with improved initial adhesion and reduced microvoiding |
| CN102436862A (en) * | 2011-09-08 | 2012-05-02 | 西北师范大学 | Graphene/nanometer copper electric conducting composite material and preparation thereof |
| CN102627833A (en) * | 2012-04-01 | 2012-08-08 | 浙江华正新材料股份有限公司 | Environment-friendly fire-resistant insulating material and manufacturing method thereof |
-
2012
- 2012-11-03 CN CN2012104326468A patent/CN102925099A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002086911A1 (en) * | 2001-04-23 | 2002-10-31 | Henkel Loctite Corporation | Conductive, silicone-based compositions with improved initial adhesion and reduced microvoiding |
| CN102436862A (en) * | 2011-09-08 | 2012-05-02 | 西北师范大学 | Graphene/nanometer copper electric conducting composite material and preparation thereof |
| CN102627833A (en) * | 2012-04-01 | 2012-08-08 | 浙江华正新材料股份有限公司 | Environment-friendly fire-resistant insulating material and manufacturing method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103666354A (en) * | 2013-11-14 | 2014-03-26 | 昆山珍实复合材料有限公司 | Epoxy resin adhesive and preparation method thereof |
| CN104073188A (en) * | 2014-06-06 | 2014-10-01 | 苏州之诺新材料科技有限公司 | Acrylate conductive adhesive and preparation method thereof |
| WO2019227559A1 (en) * | 2018-05-30 | 2019-12-05 | 江苏大学 | Solid conductive gel suitable for electrochemical system and preparation method therefor |
| CN109517177A (en) * | 2018-11-26 | 2019-03-26 | 衡阳思迈科科技有限公司 | The preparation method of the carboxy-modified conductive silver glue lotion of hydrocarbon |
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Application publication date: 20130213 |