CN104263303B - Flexible conductive adhesive that a kind of direct coating is used and preparation method thereof - Google Patents
Flexible conductive adhesive that a kind of direct coating is used and preparation method thereof Download PDFInfo
- Publication number
- CN104263303B CN104263303B CN201410538834.8A CN201410538834A CN104263303B CN 104263303 B CN104263303 B CN 104263303B CN 201410538834 A CN201410538834 A CN 201410538834A CN 104263303 B CN104263303 B CN 104263303B
- Authority
- CN
- China
- Prior art keywords
- flexible
- conductive adhesive
- nano
- wire
- silver powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Abstract
Flexible conductive adhesive and a method for making that direct coating is used, it is made up of the flexible 1-dimention nano conductive material of 15-20wt% flexible epoxy, 3-8wt% curing agent, 0.1-0.5wt% promoter, 0.1-0.5wt% coupling agent, 65-80wt% silver powder and 0.2-10wt%; Flexible epoxy the has been grafting bisphenol A epoxide resin of soft section of ethylene-vinyl acetate copolymer and the mixture of aliphatic glycidyl ether epoxy resin; Curing agent is one or more in methylhexahydrophthalic anhydride, methyl tetrahydrophthalic anhydride, tetrabydrophthalic anhydride; Promoter is glyoxaline compound; Coupling agent is one or more in KH550, KH560 and KH570; Flexible 1-dimention nano conductive material is CNT or conducting metal nano wire; Have superior electrical conductivity energy and good pliability, after repeatedly bending, electric conductivity does not almost change, and can meet flexible electronic product demand.
Description
Technical field
The invention belongs to microelectronic packaging material and preparing technical field, what particularly a kind of direct coating was used is softProperty conducting resinl and preparation method thereof.
Background technology
As the substitute products of traditional Sn/Pb scolder, it is low that conducting resinl has bonding temp, high density, thin spaceConcatenation ability, well environmental-protecting performance, can connect from different substrates, and it is excellent that the simple and cost of bonding apparatus is low etc.Point, is therefore widely used.
In general, conducting resinl is by matrix and media assemblage. Matrix is mainly in the majority with epoxy resin. Epoxy resin toolHave good physics, chemical property, it has excellent adhesive strength to the surface of metal and nonmetallic materials, is situated betweenElectrical property is good, product size good stability, and hardness is high, to alkali and most of solvent-stable. In addition, commonly useFiller has gold, silver, copper, aluminium, nickel, graphite etc. Silver has good electric conductivity, is difficult for oxidized in air.Even and oxidized, silver oxide also has good electric conductivity. So silver is proper as conductive filler,And conducting resinl is in the market also main mainly with silver.
In recent years, along with scientific and technological progress, flexible electronic product has obtained fast development, and people often wishFlexible electronic product, such as flexible display screen, flexible general character antenna, thin film transistor (TFT), sensor array, electronicsSolar battery array, flexible energy storage facilities etc., can bend and be curled into complicated shape, or roll,So that convenient storage. This just has higher requirement to conductive connecting material. Matrix aspect, with traditional epoxyAlthough the conducting resinl that resin is matrix has many good qualities, its pliability should be not, easily cracking, more notCan bend curling. Surface side filler, Chinese invention patent application CN102653668, CN101503608, CN102191001With filler used in CN101781540 etc. be all flake silver powder. And conducting resinl is in the market also mainly with sheetShape silver powder is main. But, the conducting resinl that this class is filled with flake silver powder in the curling process of bending, original leadingElectric pathway is easy to destroyed, and its electric conductivity is significantly reduced. Therefore, can not meet flexible electronic productThe demand that compliant conductive is connected.
Summary of the invention
The object of this invention is to provide that a kind of to adopt flexible epoxy be resin, with micron flake silver powder with have flexible1-dimention nano conductive material, as conductive filler, has to prepare the conducting resinl that good flexible direct coating is used,Thereby can meet the demand of flexible electronic product.
Technical scheme of the present invention is as follows:
The flexible conductive adhesive that direct coating provided by the invention is used, it is by flexible epoxy, curing agent, promoter, idolConnection agent, silver powder and flexible 1-dimention nano conductive material composition; The mass percent proportioning of each component is:
Bisphenol A epoxide resin and the aliphatic of soft section of ethylene-vinyl acetate copolymer that described flexible epoxy has been graftingThe mixture of tetraglycidel ether epoxy resin; Wherein aliphatic glycidyl ether epoxy resin accounts for described mixture weight10-60wt%;
Described curing agent is methylhexahydrophthalic anhydride, methyl tetrahydrophthalic anhydride, tetrahydrochysene O-phthalicOne or more in acid anhydrides;
Described promoter is glyoxaline compound;
Described coupling agent is one or more in KH550, KH560 and KH570;
Described flexible 1-dimention nano conductive material is CNT or conducting metal nano wire.
Described silver powder is micron-stage sheet-like silver powder.
Described conducting metal nano wire is nanowires of gold, nano silver wire, copper nano-wire, Fe nanowire or aluminium nanometerLine.
Described glyoxaline compound is one or more in imidazoles or imidazole salts.
The preparation method of the flexible conductive adhesive that the direct coating that the present invention passes through is used, its preparation process is as follows:
2) first take each component by following percentage by weight proportioning:
2) flexible epoxy in above-mentioned component, curing agent, promoter and coupling agent are fully mixed, obtain baseBody;
3) the flexible 1-dimention nano conductive material in above-mentioned component is joined in matrix, fully mix; AfterwardsAdd again the silver powder in above-mentioned component, fully mix, obtain directly applying the flexible conductive adhesive using;
Bisphenol A epoxide resin and the aliphatic of soft section of ethylene-vinyl acetate copolymer that described flexible epoxy has been graftingThe mixture of tetraglycidel ether epoxy resin; Wherein aliphatic glycidyl ether epoxy resin accounts for described mixture weight10-60wt%;
Described curing agent is methylhexahydrophthalic anhydride, methyl tetrahydrophthalic anhydride, tetrahydrochysene O-phthalicOne or more in acid anhydrides;
Described promoter is glyoxaline compound;
Described coupling agent is one or more in KH550, KH560 and KH570;
Described flexible 1-dimention nano conductive material is CNT or conducting metal nano wire.
Described silver powder is micron-stage sheet-like silver powder.
Described conducting metal nano wire is nanowires of gold, nano silver wire, copper nano-wire, Fe nanowire or aluminium nanometerLine.
Described glyoxaline compound is one or more in imidazoles or imidazole salts.
The using method of the flexible conductive adhesive that direct coating prepared by the inventive method is used is: when use, directly applyOr being printed on the parts position that needs bonding, condition of cure is 150 DEG C, 2 hours.
Compared with existing conducting resinl, the flexible conductive adhesive that direct coating of the present invention is used not only has excellent conductionPerformance, but also there is good pliability, overcome the easily problem of cracking of conventional conductive glue, and through too muchAfter inferior bending, its electric conductivity does not almost change, and can meet the growth requirement of flexible electronic product.
Brief description of the drawings
Fig. 1 is that the flexible conductive adhesive prepared according to embodiment 1 and embodiment 2 and common epoxy are made matrix and sheetThe resistance to bending performance contrast of conducting resinl prepared by shape silver powder as filler;
Fig. 2 is that the flexible conductive adhesive prepared according to embodiment 3 and embodiment 4 and common epoxy are made matrix and sheetThe resistance to bending performance contrast of conducting resinl prepared by shape silver powder as filler.
Detailed description of the invention
Embodiment 1
1) first take following each component:
2) by 1) in TKM-828, the DER732, methylhexahydrophthalic anhydride, the 2-ethyl-4-methyl that takeImidazoles, KH560 fully mix, and obtain matrix;
3) ethanolic solution of nano silver wire is joined to 2) matrix in, fully mix, vacuumize 24 hours,To remove ethanol; Add again 1 afterwards) in the flake silver powder SF-0340 that takes, fully mix, obtain directlyApply the flexible conductive adhesive using.
In the nano silver wire ethanolic solution that the present embodiment uses, the length of nano silver wire is 15-60 μ m, and diameter is150-350nm, concentration is 0.05g/ml.
The flexible conductive adhesive of the present embodiment, at 150 DEG C, solidifies 2 hours, and resistivity is 6.65 × 10-5Ω·cm，Electric conductivity excellence; And as shown in Figure 1, the resistance to bending performance of this flexible conductive adhesive is made base than common epoxyThe conducting resinl that body and flake silver powder are prepared as filler is well a lot.
Embodiment 2
1) first take following each component:
2) by 1) in take TKM-828, DER732, methyl tetrahydrophthalic anhydride, Ni-imidazol complex,KH550 fully mixes, and obtains matrix;
3) ethanolic solution of copper nano-wire is joined to 2) matrix in, fully mix, vacuumize 24 hours,To remove ethanol; Add again 1 afterwards) in the flake silver powder SF-0340 that takes, fully mix, obtain directlyApply the flexible conductive adhesive using.
In the ethanolic solution of the copper nano-wire that the present embodiment uses, the length of copper nano-wire is 0.8-6 μ m, and diameter is100-200nm, concentration is 0.2g/ml.
The flexible conductive adhesive of the present embodiment, at 150 DEG C, solidifies 2 hours, and resistivity is 8.56 × 10-5Ω·cm，Electric conductivity excellence; And as shown in Figure 1, the resistance to bending performance of this flexible conductive adhesive is made base than common epoxyThe conducting resinl that body and flake silver powder are prepared as filler is well a lot.
Embodiment 3
1) first take following each component:
2) by 1) in the adjacent benzene two of TKM-828, DER732, methylhexahydrophthalic anhydride, methyl tetrahydrochysene that takesFormic anhydride, 2-ethyl-4-methylimidazole, 2-ethyl imidazol(e), KH570 fully mix, and obtain matrix;
3) ethanolic solution of nanowires of gold is joined to 2) matrix in, fully mix, vacuumize 24 hours,To remove ethanol; Add again 1 afterwards) in the flake silver powder SF-0340 that takes, fully mix, obtain directlyApply the flexible conductive adhesive using.
In the ethanolic solution of the nanowires of gold that the present embodiment uses, the length of nanowires of gold is 3-6 μ m, and diameter is 20-50Nm, concentration is 0.1g/ml.
The flexible conductive adhesive of the present embodiment, at 150 DEG C, solidifies 2 hours, and resistivity is 7.83 × 10-5Ω·cm，Electric conductivity excellence; And as shown in Figure 2, the resistance to bending performance of this flexible conductive adhesive is made base than common epoxyThe conducting resinl that body and flake silver powder are prepared as filler is well a lot.
Embodiment 4
1) first take following each component:
2) by 1) in TKM-828, the DER732, tetrabydrophthalic anhydride, the 1-butyl-3-methylimidazole that takeHexafluorophosphate, KH570, KH560 fully mix, and obtain matrix;
3) by 1) in the CNT that takes join 2) matrix in, fully mix; Add again 1 afterwards)In the flake silver powder SF-0340 that takes, fully mix, obtain directly applying the flexible conductive adhesive using.
The length of carbon nanotube that the present embodiment uses is 10-20 μ m, and diameter is 30-50nm.
The flexible conductive adhesive of the present embodiment, at 150 DEG C, solidifies 2 hours, and resistivity is 6.17 × 10-5Ω·cm，Electric conductivity excellence; And as shown in Figure 2, the resistance to bending performance of this flexible conductive adhesive is made base than common epoxyThe conducting resinl that body and flake silver powder are prepared as filler is well a lot.
Claims (6)
1. directly apply the flexible conductive adhesive using, its by flexible epoxy, curing agent, promoter, coupling agent,Silver powder and flexible 1-dimention nano conductive material composition; The mass percent proportioning of each component is:
Bisphenol A epoxide resin and the aliphatic of soft section of ethylene-vinyl acetate copolymer that described flexible epoxy has been graftingThe mixture of tetraglycidel ether epoxy resin; Wherein aliphatic glycidyl ether epoxy resin accounts for described mixture weight10-60wt%;
Described curing agent is methylhexahydrophthalic anhydride, methyl tetrahydrophthalic anhydride, tetrahydrochysene O-phthalicOne or more in acid anhydrides;
Described promoter is glyoxaline compound;
Described coupling agent is one or more in KH550, KH560 and KH570;
Described flexible 1-dimention nano conductive material is CNT or conducting metal nano wire;
Described silver powder is micron-stage sheet-like silver powder.
2. the flexible conductive adhesive using by direct coating claimed in claim 1, is characterized in that described conductionMetal nanometer line is nanowires of gold, nano silver wire, copper nano-wire, Fe nanowire or aluminium nano wire.
3. the flexible conductive adhesive using by direct coating claimed in claim 1, is characterized in that described imidazolesCompounds is one or more in imidazoles or imidazole salts.
4. a preparation method for the flexible conductive adhesive that direct coating claimed in claim 1 is used, its preparation processAs follows:
1) first take each component by following percentage by weight proportioning:
2) flexible epoxy in above-mentioned component, curing agent, promoter and coupling agent are fully mixed, obtain baseBody;
3) the flexible 1-dimention nano conductive material in above-mentioned component is joined in matrix, fully mix; AfterwardsAdd again the silver powder in above-mentioned component, fully mix, obtain directly applying the flexible conductive adhesive using;
Bisphenol A epoxide resin and the aliphatic of soft section of ethylene-vinyl acetate copolymer that described flexible epoxy has been graftingThe mixture of tetraglycidel ether epoxy resin; Wherein aliphatic glycidyl ether epoxy resin accounts for described mixture weight10-60wt%;
Described curing agent is methylhexahydrophthalic anhydride, methyl tetrahydrophthalic anhydride, tetrahydrochysene O-phthalicOne or more in acid anhydrides;
Described promoter is glyoxaline compound;
Described coupling agent is one or more in KH550, KH560 and KH570;
Described flexible 1-dimention nano conductive material is CNT or conducting metal nano wire;
Described silver powder is micron-stage sheet-like silver powder.
5. the preparation method of the flexible conductive adhesive using by direct coating claimed in claim 4, is characterized in that,Described conducting metal nano wire is nanowires of gold, nano silver wire, copper nano-wire, Fe nanowire or aluminium nano wire.
6. the preparation method of the flexible conductive adhesive using by direct coating claimed in claim 4, is characterized in that,Described glyoxaline compound is one or more in imidazoles or imidazole salts.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410538834.8A CN104263303B (en) | 2014-10-13 | 2014-10-13 | Flexible conductive adhesive that a kind of direct coating is used and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410538834.8A CN104263303B (en) | 2014-10-13 | 2014-10-13 | Flexible conductive adhesive that a kind of direct coating is used and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104263303A CN104263303A (en) | 2015-01-07 |
| CN104263303B true CN104263303B (en) | 2016-05-18 |
Family
ID=52154892
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410538834.8A Expired - Fee Related CN104263303B (en) | 2014-10-13 | 2014-10-13 | Flexible conductive adhesive that a kind of direct coating is used and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104263303B (en) |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10147512B2 (en) * | 2015-12-09 | 2018-12-04 | C3Nano Inc. | Methods for synthesizing silver nanoplates and noble metal coated silver nanoplates and their use in transparent films for control of light hue |
| CN105400477A (en) * | 2015-12-24 | 2016-03-16 | 常熟昊虞电子信息科技有限公司 | Conductive adhesive for high-power LED |
| CN105802531A (en) * | 2016-04-15 | 2016-07-27 | 安庆市晶科电子有限公司 | Electric-heating flame-retardant conductive silver adhesive for circuit board |
| CN107274967A (en) * | 2017-06-27 | 2017-10-20 | 西安工程大学 | A kind of warm therapy powdery electric slurry and preparation method thereof |
| CN107393626A (en) * | 2017-06-27 | 2017-11-24 | 西安工程大学 | A kind of hot method powdery electric slurry and preparation method thereof |
| CN110564327A (en) * | 2019-09-16 | 2019-12-13 | 常州斯威克光伏新材料有限公司 | Epoxy resin conductive adhesive film |
| CN111100591B (en) * | 2019-10-30 | 2022-02-01 | 南昌欧菲显示科技有限公司 | Conductive element and electronic device |
| CN113563837B (en) * | 2021-09-26 | 2022-03-08 | 西安宏星电子浆料科技股份有限公司 | HJT conductive silver colloid composition, preparation method thereof and HJT solar cell |
| US20230402968A1 (en) * | 2022-06-10 | 2023-12-14 | Maxeon Solar Pte. Ltd. | Soft spacers for shingled solar cell panels |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102191001A (en) * | 2011-03-28 | 2011-09-21 | 彩虹集团公司 | Epoxy conductive adhesive composition |
| CN102719210A (en) * | 2011-03-30 | 2012-10-10 | 中国科学院理化技术研究所 | Adhesive with insulating and heat-conducting properties used at ultralow temperature |
-
2014
- 2014-10-13 CN CN201410538834.8A patent/CN104263303B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102191001A (en) * | 2011-03-28 | 2011-09-21 | 彩虹集团公司 | Epoxy conductive adhesive composition |
| CN102719210A (en) * | 2011-03-30 | 2012-10-10 | 中国科学院理化技术研究所 | Adhesive with insulating and heat-conducting properties used at ultralow temperature |
Non-Patent Citations (1)
| Title |
|---|
| "银纳米线的制备及其在导电胶中的应用";段素萍;《哈尔滨工业大学硕士论文》;20131201;正文第51页第2段、第53页5.2.2部分、第55页倒数第1段、第57页倒数第1段、第59页倒数第2段 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104263303A (en) | 2015-01-07 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104263303B (en) | Flexible conductive adhesive that a kind of direct coating is used and preparation method thereof | |
| WO2018006503A1 (en) | Silver salt-doped conductive silver adhesive, and preparation method and use thereof | |
| WO2016008187A1 (en) | Method for preparing conductive adhesive and conductive adhesive | |
| CN106118539B (en) | A kind of conductive silver glue for adulterating silver nano-grain and preparation method and application | |
| CN101555393B (en) | High-temperature resistant one-component isotropic conductive adhesive and preparation method thereof | |
| CN107502257B (en) | Silver/graphene low-temperature curing conductive adhesive, conductive film, conductor and preparation method thereof | |
| CN102153976A (en) | Preparation method of graphene/nano silver epoxy conductive adhesive | |
| CN103059767A (en) | Conductive silver paste with high-temperature resistance and low sheet resistance and preparation method of conductive silver paste | |
| CN104021842A (en) | Graphene composite copper thick film conductive slurry and preparation method thereof | |
| CN103333632A (en) | Graphite conductive adhesive and preparation method thereof | |
| Chen et al. | Regulation of multidimensional silver nanostructures for high-performance composite conductive adhesives | |
| TW201217481A (en) | Anisotropic conductive adhesive film and curing agent | |
| CN103409083B (en) | Graphite carbon black conductive adhesive and preparation method thereof | |
| CN105111988A (en) | Flexible conductive silver adhesive | |
| CN104021841A (en) | Carbon nano tube composite copper thick membrane electroconduction slurry and preparation method thereof | |
| CN110066633A (en) | A kind of preparation method of low silver content conducting resinl | |
| CN107189103B (en) | A kind of conductive filler, preparation method and the usage | |
| Cao et al. | Carbon nanotubes with carbon blacks as cofillers to improve conductivity and stability | |
| CN111534154A (en) | Silver nanowire-silica sol modified composite conductive ink and preparation method thereof | |
| JP2009269976A (en) | Conductive resin composition | |
| CN102378482A (en) | Circuit board substrate and manufacturing method thereof | |
| CN113354855A (en) | Bendable electrothermal film device based on graphene and preparation method thereof | |
| TW201828307A (en) | Resistance material | |
| CN106710669B (en) | One kind can flexing metal grill method for preparing transparent conductive film and its product | |
| CN107446525A (en) | Paste heat-conducting glue containing conducting high polymers thing |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160518 Termination date: 20201013 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |