CN101555393B - High-temperature resistant one-component isotropic conductive adhesive and preparation method thereof - Google Patents
High-temperature resistant one-component isotropic conductive adhesive and preparation method thereof Download PDFInfo
- Publication number
- CN101555393B CN101555393B CN2009100292511A CN200910029251A CN101555393B CN 101555393 B CN101555393 B CN 101555393B CN 2009100292511 A CN2009100292511 A CN 2009100292511A CN 200910029251 A CN200910029251 A CN 200910029251A CN 101555393 B CN101555393 B CN 101555393B
- Authority
- CN
- China
- Prior art keywords
- conductive adhesive
- epoxy resin
- temperature resistant
- isotropic conductive
- component
- 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
Images
Abstract
The invention provides a high-temperature resistant one-component isotropic conductive adhesive and a preparation method thereof. The one-component isotropic conductive adhesive capable of resisting the high temperature of 180 DEG C for a long time is prepared by adding silver nano-wire as the conductive filler to an epoxy resin matrix and adding core-shell structure toughening epoxy resin and poly-functional epoxy resin as modifiers. The conductive adhesive comprises the following components by the mass percentage: 10% to 15% of matrix epoxy resin, 62% to 65% of silver nano-wire, 3.5% to 5.5%of poly-functional epoxy resin, 6% to 10% of core-shell structure toughening epoxy resin, 0.4% to 0.6% of gas-phase silicon dioxide, 0.6% to 1.0% of toughening diluting agent, 0.3% to 0.4% of couplin g agent, 9% to 15% of curing agent and 0.1% to 0.2% of curing accelerator. The invention has the advantages of simple preparation method, good controllability, high material availability and mild preparation condition.
Description
Technical field
The invention belongs to the microelectronic packaging material preparing technical field, particularly a kind of high-temperature resistant one-component isotropic conductive adhesive and preparation method thereof.
Background technology
The Pb/Sn scolder is a connection material basic on the printed-wiring board (PWB), and what use always among the SMT (Surface Mount Technology) also is this material.Along with electronic product develops to miniaturization, portability, improving constantly of device integrated level presses for the connection material and the method for development of new.From early 1990s till now, the I/O number on the IC develops into 1500 from 500, expects 2005 and will reach 3800, will reach 4600 by 2008, will reach 8000 in 2010.High I/O density requirements connects material and has very high linear resolution.The Pb/Sn scolder can only be applied in the connection of the following pitch of 0.65mm, can not satisfy the needs of technology.Temperature is higher than 400 ℃ in the Pb/Sn connection technology, and the thermal stresses of generation also can damage device and substrate.In addition, Pb is deleterious heavy metal element, and many countries are to the plumbous clearly regulation that proposes of used in electronic industry: Japan and Europe require respectively to stop plumbous use calendar year 2001 and 2004.Under this pressure, developing unleaded connection material has become inevitable.With Pb/Sn alloy phase ratio, what use in the conductive resin is the metal-powder conduction, and the linear resolution of connection is improved a lot, and more can adapt to high I/O density.The coating process of conductive resin is simple, and solidification value is low, can increase work efficiency effectively.Because the conductive resin matrix is a macromolecular material, can be used on the flexible base, board, adapt to the requirement of miniaturization of electronic products, lightness.In the tackiness agent interconnection technique international conference in first electron production that hold Berlin in 1994 (InternationalConference on Adhesive Joining Technology inElectronics Manufacturing), just pointed out that conductive resin replaces the inexorable trend of Sn-Pb alloy.
Substitute as the Sn/Pb scolder, conductive resin has also shown some shortcomings of self in the application of reality, good inadequately as resistivity instability, mechanical property, these defectives progressively have been studied personnel and have captured, employing nano silver wire or silver-colored nanometer rod compound silver nanometer particle have all been introduced as conductive filler material as national patent CN1948414 and CN101215450 etc., can reduce the content of conductive filler material in conductive resin, improve mechanical strength.Because the existence of bat wool can strengthen the stability of conductive network, make the ageing-resistant performance of conductive resin be improved simultaneously.
But because the IC that installs on a pcb board on the present microelectronics Packaging industry is a lot, it is excessive to cause the regional area heat release occurring in the process of the actual use of client, the phenomenon of destroying the bonded part exists, this mainly is because existing bad causing of conductive resin ubiquity resistance to elevated temperatures, the resistance to extreme temperature of general conductive resin cohesive force can occur after envrionment temperature surpasses 100 ℃ and sharply descend about 100 ℃.Develop for this reason a kind of be suitable for that present microelectronics Packaging uses have good heat resistance can conductive resin be very essential.Enter the colloidal pitch system by introducing polyfunctional epoxy resin among the present invention, improved the cross-linking density of resin after the curing, improved the colloidal heat resisting temperature.The introducing of nucleocapsid structure toughened resin simultaneously makes conductive resin not lose good impact resistance again.
Summary of the invention
Purpose of the present invention provides a kind of easy, method of single component isotropic conductive adhesive cheaply, to overcome the shortcoming of conventional conductive glue resistance to elevated temperatures difference.
A kind of high-temperature resistant one-component isotropic conductive adhesive, it is characterized in that: component is calculated by percentage to the quality, substrate ring epoxy resins 10～15%, nano silver wire 62～65%, polyfunctional epoxy resin 3.5～5.5%, nucleocapsid structure epoxy resin toughened 6～10%, aerosil 0.4～0.6%, toughness thinner 0.6～1.0%, coupling agent 0.3～0.4%, solidifying agent 9～15%, curing catalyst 0.1～0.2%.
In the above-mentioned isotropic conductive adhesive, the substrate ring epoxy resins is E51, E44, EPON828 or EPON826 resin.
In the above-mentioned isotropic conductive adhesive, polyfunctional epoxy resin is four-functional group or trifunctional Resins, epoxy, as AG-80, AG-90 etc.
In the above-mentioned isotropic conductive adhesive, nucleocapsid structure is epoxy resin toughened to be soft nuclear hard-shell type, as the Japanese Kaneka product MX125 of company, MX153, MX157 or MX135.
In the above-mentioned isotropic conductive adhesive, coupling agent is KH550, KH560 or phenyltrimethoxysila,e.
In the above-mentioned isotropic conductive adhesive, aerosil is TS-720 or RD907.
In the above-mentioned isotropic conductive adhesive, the toughness thinner is NC513 or dibutyl phthalate.
In the above-mentioned isotropic conductive adhesive, solidifying agent is methyl tetrahydro phthalic anhydride or methyl hexahydrophthalic anhydride.
In the above-mentioned isotropic conductive adhesive, curing catalyst is 2-ethyl-4-methylimidazole or Methylimidazole.
In the above-mentioned isotropic conductive adhesive, nano silver wire is according to the disclosed preparation method's preparation of Chinese patent CN101310899.
Above-mentioned property conductive resin preparation method is as follows: at first Resins, epoxy, epoxy resin toughened, coupling agent, polyfunctional epoxy resin, aerosil, toughness thinner are mixed in proportion, mixing for the first time in the high-speed mixer that band vacuumizes then, then in proportion to wherein adding dry good nano silver wire, in high-speed mixer, carry out the mixing second time once more, mix the back and take out to wherein adding solidifying agent and curing catalyst; In high-speed mixer, carry out taking out behind the mixing for the third time, be encapsulated in the special-purpose sebific duct.Use is that colloid is extruded from sebific duct, and directly being coated in needs the agglutinating position to get final product, and condition of cure is 170 ℃, 30min.Condition of storage is-20～-40 ℃ at ordinary times, and the storage time was above 8 months.
Among the above-mentioned preparation method, the first time, the working conditions with the mixing high-speed mixer second time was: 2000 rev/mins of rate processing 3min; The working conditions of mixing high-speed mixer is for the third time: 2000 rev/mins of speed are mixed 30s.
The beneficial effect that the present invention has is:
1, this preparation method is simple, and controllability is good, and starting material are easy to get, and preparation condition is not harsh.
2, the conductive resin that makes of this preparation method can be-20 ℃～250 ℃ uses, and the viscosity of glue is between 100～500mPa.s under the room temperature, and Tg is 210～230 ℃.Reach 22MPa in aluminium-aluminium surface shear intensity under the room temperature, the T type stripping strength on aluminium-aluminium surface reaches 5.1N/mm, can also reach 17MPa in 180 ℃ of following aluminium-aluminium surface shear intensity, and the shelf lives was greater than 8 months.High energy surface to metal, pottery, glass and polymkeric substance all has advantages of good caking property.
3, adopt nano silver wire as conductive filler material in this conductive resin, the filling of conductive filler material significantly reduces, and conductive resin has very high mechanical property.By introducing polyfunctional epoxy resin colloidal dispersion is carried out modification, improve the heat resistance of conductive resin greatly.The introducing of nucleocapsid structure epoxy toughening agent makes the still in store good toughness of conductive resin.
Description of drawings
Fig. 1 is the room temperature shearing resistance test result according to the high-temperature resistant one-component isotropic conductive adhesive of embodiment 1 preparation
Fig. 2 is the room temperature T type peel strength test result according to the high-temperature resistant one-component isotropic conductive adhesive of embodiment 1 preparation
Fig. 3 is 180 ℃ of shearing resistance test results according to the high-temperature resistant one-component isotropic conductive adhesive of embodiment 1 preparation
Embodiment
Embodiment 1:
The composition and the mass percent of conductive resin are as follows: epoxy resin ON828 10.6%; Nano silver wire 65%; AG-80 4.5%; MX125 7%; TS-720 0.6%; NC513 0.7%; Phenyltrimethoxysila,e 0.4%; Methyl tetrahydro phthalic anhydride 11%; 2-ethyl-4-methyl-imidazoles 0.2%.
Preparation technology and process are as follows:
At first epoxy resin ON828, the epoxy resin toughened MX125 of nucleocapsid, phenyltrimethoxysila,e, polyfunctional epoxy resin AG-80, aerosil TS-720, toughness thinner NC513 are mixed, then in the high-speed mixer that band vacuumizes with 2000 rev/mins of rate processing 3min, then in proportion to wherein adding dry good nano silver wire, in 2000 rev/mins mixing machine, handle 3min once more, mix the back and take out to wherein adding solidifying agent methyl tetrahydro phthalic anhydride and curing catalyst 2-ethyl-4-methyl-imidazoles.After mixing 30s under 2000 rev/mins of speed, take out, be encapsulated in the special-purpose sebific duct.Condition of cure is 170 ℃, 30min.The shearing resistance test is carried out according to GB7124-1986; T type peel strength test carries out according to GB2791-1981.
Fig. 1 is the room temperature shearing resistance test result according to the high-temperature resistant one-component isotropic conductive adhesive of embodiment 1 preparation, the shearing resistance of this conductive resin on the aluminium flake base material reaches 22MPa as can be seen from Figure 1, shearing resistance on the copper sheet base material also can surpass 20MPa, and experiment is repeated fine.
Fig. 2 is the room temperature T type peel strength test result according to the high-temperature resistant one-component isotropic conductive adhesive of embodiment 1 preparation.The average T type peeling force of this conductive resin on aluminium flake surpasses 120N as can be seen from Figure 2, and corresponding T type stripping strength surpasses 5N/mm.
Fig. 3 is 180 ℃ of shearing resistance test results according to the high-temperature resistant one-component isotropic conductive adhesive of embodiment 1 preparation, as can be seen from Figure 3 in hot environment, this conductive resin also presents extraordinary shearing resistance, average shear strength on the aluminium flake base material reaches 17MPa, and shear strength reaches more than the 16MPa on the copper sheet base material.
A kind of preparation method of high-temperature resistant one-component isotropic conductive adhesive, its preparation technology and process are as follows with the mass percent of embodiment 1 each component:
Each embodiment all can prepare the high-temperature resistant one-component isotropic conductive adhesive product, and over-all properties has characteristics and effect described in the content of the present invention, can satisfy the bonding of different substrate materials structural part.
Claims (8)
1. high-temperature resistant one-component isotropic conductive adhesive, it is characterized in that: component is calculated by percentage to the quality, substrate ring epoxy resins 10～15%, nano silver wire 62～65%, polyfunctional epoxy resin 3.5～5.5%, nucleocapsid structure epoxy resin toughened 6～10%, aerosil 0.4～0.6%, toughness thinner 0.6～1.0%, coupling agent 0.3～0.4%, solidifying agent 9～15%, curing catalyst 0.1～0.2%; Described substrate ring epoxy resins is E51, E44, EPON828 or EPON826 resin, and described toughness thinner is NC513 or dibutyl phthalate.
2. a kind of high-temperature resistant one-component isotropic conductive adhesive as claimed in claim 1 is characterized in that: polyfunctional epoxy resin is four-functional group or trifunctional Resins, epoxy.
3. a kind of high-temperature resistant one-component isotropic conductive adhesive as claimed in claim 1 is characterized in that: nucleocapsid structure is epoxy resin toughened to be soft nuclear hard-shell type.
4. a kind of high-temperature resistant one-component isotropic conductive adhesive as claimed in claim 1 is characterized in that: coupling agent is KH550, KH560 or phenyltrimethoxysila,e.
5. a kind of high-temperature resistant one-component isotropic conductive adhesive as claimed in claim 1 is characterized in that: aerosil is TS-720 or RD907; Solidifying agent is methyl tetrahydro phthalic anhydride or methyl hexahydrophthalic anhydride; Curing catalyst is 2-ethyl-4-methylimidazole or Methylimidazole.
6. the preparation method of a kind of high-temperature resistant one-component isotropic conductive adhesive as claimed in claim 1 is as follows: at first Resins, epoxy, epoxy resin toughened, coupling agent, polyfunctional epoxy resin, aerosil, toughness thinner are mixed in proportion, mixing for the first time in the high-speed mixer that band vacuumizes then, then in proportion to wherein adding dry good nano silver wire, in high-speed mixer, carry out the mixing second time once more, mix the back and take out to wherein adding solidifying agent and curing catalyst; Promptly make isotropic conductive adhesive after in high-speed mixer, carrying out for the third time taking out behind the mixing.
7. the preparation method of a kind of high-temperature resistant one-component isotropic conductive adhesive as claimed in claim 6 is characterized in that: for the first time and for the second time the working conditions of mixing high-speed mixer is: 2000 rev/mins of rate processing 3min; The working conditions of mixing high-speed mixer is for the third time: 2000 rev/mins of speed are mixed 30s.
8. the using method of a kind of high-temperature resistant one-component isotropic conductive adhesive as claimed in claim 1 is: be coated in directly during use that to need agglutinating position, condition of cure be 170 ℃, 30min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100292511A CN101555393B (en) | 2009-04-03 | 2009-04-03 | High-temperature resistant one-component isotropic conductive adhesive and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100292511A CN101555393B (en) | 2009-04-03 | 2009-04-03 | High-temperature resistant one-component isotropic conductive adhesive and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101555393A CN101555393A (en) | 2009-10-14 |
| CN101555393B true CN101555393B (en) | 2011-08-24 |
Family
ID=41173682
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009100292511A Expired - Fee Related CN101555393B (en) | 2009-04-03 | 2009-04-03 | High-temperature resistant one-component isotropic conductive adhesive and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101555393B (en) |
Families Citing this family (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101805574A (en) * | 2010-03-11 | 2010-08-18 | 复旦大学 | Sintered type conductive adhesive adopting silver filling with surfaces subjected to activating treatment and preparation method thereof |
| CN102093833B (en) * | 2010-12-06 | 2013-09-18 | 常州合润新材料科技有限公司 | Method for preparing silver conductive adhesive by in situ synthesis |
| CN102002336A (en) * | 2010-12-09 | 2011-04-06 | 中国电器科学研究院 | Solvent-free high-performance conductive adhesive |
| CN102086364A (en) * | 2010-12-16 | 2011-06-08 | 广东风华高新科技股份有限公司 | Conductive silver paste for microelectronic packaging and preparation method thereof |
| CN102127384B (en) * | 2010-12-27 | 2014-01-01 | 广东风华高新科技股份有限公司 | Impact and light decay-resistant die attach insulation paste and preparation method thereof |
| CN102079958B (en) * | 2011-02-09 | 2013-11-13 | 常州合润新材料科技有限公司 | Diamond-filled isotropical high-performance heat-conductive adhesive and preparation method thereof |
| CN102108264B (en) * | 2011-03-08 | 2013-05-08 | 常州大学 | Single-component epoxy structure adhesive tape and preparation method thereof |
| CN102161871A (en) * | 2011-03-09 | 2011-08-24 | 烟台德邦电子材料有限公司 | Heat-conductive insulated adhesive tape for large-power light-emitting diode (LED) and preparation method thereof |
| CN102382606B (en) * | 2011-09-19 | 2013-10-30 | 常州合润新材料科技有限公司 | Graphene filling isotropic high-performance conducting adhesive and preparation method thereof |
| CN102719211A (en) * | 2011-12-06 | 2012-10-10 | 常州大学 | Silver nanowire-filled self-repairing conducting resin and preparation method thereof |
| CN102585744B (en) * | 2012-02-21 | 2013-12-04 | 绵阳艾萨斯电子材料有限公司 | Adhesive composition and preparation method and application thereof in silk-screen printing |
| CN103450833A (en) * | 2013-08-05 | 2013-12-18 | 天津静达保光汽车零部件有限公司 | Automotive body structure adhesive and manufacturing method thereof |
| CN104332215A (en) * | 2014-10-30 | 2015-02-04 | 中国建材国际工程集团有限公司 | Preparation method for low specific resistance transparent conducting film |
| CN104804691B (en) * | 2015-05-04 | 2018-01-30 | 上海都伟光伏科技有限公司 | A kind of epoxy adhesive of room curing and high temperature resistant high tenacity and preparation method thereof |
| CN104974470B (en) * | 2015-07-14 | 2017-12-05 | 江苏兆鋆新材料股份有限公司 | A kind of high heat-resisting, high strength epoxy resin composite preparation method |
| CN109906246B (en) | 2016-11-02 | 2021-06-15 | 株式会社百奥尼 | Epoxy paste composition comprising silver-coated copper nanowires of core-shell structure and conductive film comprising the same |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1948414A (en) * | 2006-11-13 | 2007-04-18 | 浙江理工大学 | Method of preparing high performance conductive glue |
-
2009
- 2009-04-03 CN CN2009100292511A patent/CN101555393B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1948414A (en) * | 2006-11-13 | 2007-04-18 | 浙江理工大学 | Method of preparing high performance conductive glue |
Non-Patent Citations (4)
| Title |
|---|
| JP特开2004-339325A 2004.12.02 |
| JP特开2007-51272A 2007.03.01 |
| 何影翠.导电胶的研究与发展.《化学与黏合》.2008,第30卷(第1期),第47-51页. * |
| 吴海平 等.填充银纳米线各向同性导电胶的性能.《复合材料学报》.2006,第23卷(第5期),第24-28页. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101555393A (en) | 2009-10-14 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101555393B (en) | High-temperature resistant one-component isotropic conductive adhesive and preparation method thereof | |
| WO2020220395A1 (en) | Low-temperature conductive silver paste for hit solar cell and preparation method therefor | |
| CN104449455B (en) | A kind of intermediate temperature setting type high-performance conductive silver paste and its preparation method and application | |
| CN113012844B (en) | HJT low-temperature silver paste capable of being rapidly cured and sintered and preparation method thereof | |
| CN101029212A (en) | Epoxy-resin anisotropic conductive glue | |
| CN107207935A (en) | Thermal conductivity conductive adhesive composition | |
| JP2010258006A (en) | Solar cell module and method of manufacturing the same | |
| KR20110089812A (en) | Anisotropic electroconductive film | |
| CN104650789B (en) | A kind of anisotropy conductiving glue and method for packing | |
| JP6247059B2 (en) | Conductive adhesive, solar cell module, and method for manufacturing solar cell module | |
| CN106433509A (en) | Conductive silver adhesive and preparation method and application thereof | |
| CN114276766A (en) | Nano-silver sintered conductive adhesive for microelectronic packaging and preparation method thereof | |
| CN109273136A (en) | A kind of solderable conductive silver paste and preparation method thereof that can be low-temperature fast-curing | |
| CN107189103B (en) | A kind of conductive filler, preparation method and the usage | |
| CN102311713A (en) | Nanometer conductive adhesive | |
| CN111243778B (en) | Low-temperature conductive silver adhesive for screen printing and preparation method thereof | |
| CN101054500A (en) | Method for preparing composite nano-gold conducting resin | |
| CN114805750A (en) | Bisphenol A-novolac epoxy resin, conductive adhesive for main-gate-free battery component prepared from bisphenol A-novolac epoxy resin and application of conductive adhesive | |
| CN114023487A (en) | HJT photovoltaic silver paste and preparation method thereof | |
| JP6092754B2 (en) | Conductive epoxy resin composition, solar cell using the composition, and method for producing the solar cell | |
| JP5692347B2 (en) | Conductive adhesive | |
| CN105802561A (en) | High-waterproof-performance and high-acid-and-alkali-resistance conductive silver adhesive | |
| CN110033877A (en) | A kind of silver base conductive slurry and preparation method thereof and the application in encapsulation chip interconnection | |
| CN113817426B (en) | Conductive adhesive applied to large-size chip bonding and preparation method thereof | |
| CN112435773B (en) | Low-temperature conductive nano slurry for heterojunction solar cell and preparation method thereof |
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 | ||
| C56 | Change in the name or address of the patentee | ||
| CP02 | Change in the address of a patent holder |
Address after: Gehu Lake Road Wujin District 213164 Jiangsu city of Changzhou province No. 1 Patentee after: Jiangsu Polytechnic University Address before: 213016 Baiyun District, Changzhou, Jiangsu Patentee before: Jiangsu Polytechnic University |
|
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20110824 Termination date: 20150403 |
|
| EXPY | Termination of patent right or utility model |