CN101805574A - Sintered type conductive adhesive adopting silver filling with surfaces subjected to activating treatment and preparation method thereof - Google Patents

Sintered type conductive adhesive adopting silver filling with surfaces subjected to activating treatment and preparation method thereof Download PDF

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Publication number
CN101805574A
CN101805574A CN 201010121877 CN201010121877A CN101805574A CN 101805574 A CN101805574 A CN 101805574A CN 201010121877 CN201010121877 CN 201010121877 CN 201010121877 A CN201010121877 A CN 201010121877A CN 101805574 A CN101805574 A CN 101805574A
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silver
conductive resin
nano
acid
activation
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肖斐
张中鲜
陈项艳
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Fudan University
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Fudan University
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Abstract

The invention relates to a sintered type conductive adhesive adopting silver filling with surfaces subjected to activating treatment and a preparation method thereof, belonging to the technical field of micro-electronics package interconnected materials. The surfaces of nano silver are subjected to activating treatment by adopting organic diacid which can remove micro oxide layers on the surfaces of the nano silver and is attracted on the surfaces of the nano sliver for preventing the further oxidation and agglomeration, and the organic diacid can be desorbed in the curing process of the conductive adhesive to promote the sintering among nano silver particles, thereby greatly increasing the conductivity of the conductive adhesive. The nano silver subjected to activating treatment and micro silver are mixed to be filled into matrix resin formed by epoxy resin, an anhydride curing agent, an active diluents and a curing accelerator, thereby being prepared into the sintered type conductive adhesive. The inductive adhesive has the characteristics of high electrical conductivity, simple process, convenient use, good repeatability, complete compatibility with the traditional inductive adhesive process, and the like, and has wide application potential and practicality value in the field of electronic packaging and the like.

Description

Sintered type conductive resin of the silver fillers of employing surface activation process and preparation method thereof
Technical field
The invention belongs to microelectronics Packaging interconnection material technical field, be specifically related to a kind of nanometer silver surface treatment method and with the high conductivity sintered type conductive resin of its preparation, and the preparation method of this conductive resin.
Background technology
Along with the miniaturization and the high performance of modern micro-electronic device, the electronics package technique also develops towards the direction of microminiaturization, densification, high integration, thereby resolving power, the strength of joint of semiconductor packages connection material are had higher requirement.Simultaneously, along with the raising of people's environmental consciousness, low, the eco-friendly connection material of research and development energy consumption has caused people's great attention.As a kind of lead-free interconnection material, conductive resin is low with its solidification value, resolving power is high, thermomechanical property good, technology is simple and with advantages such as the material wettability is good, become the ideal substitute of traditional wiping solder and solder.
The nano material that is in the nanoscale scope on one dimension, two dimension or the three-dimensional shows the unusual characteristic that is different from macro object or single isolated atom usually, has special physics, chemistry and mechanical property.Nano metal particles has the character of a lot of uniquenesses, and wherein one of the most noticeable feature is that its sintering temperature is lower than the metal scale fusing point widely, utilizes this specific character of nano metal can form the metal sinter of arbitrary shape at a lower temperature.Because its excellent electrical and thermal conductivity performance, add stable in properties, oxidation slowly and its oxide compound also have electroconductibility, argent becomes the most widely used conductive resin filler.Present commercially available conductive resin filler is mainly based on micro-silver powder (sheet), and the problem of existence comprises shortcomings such as unsettled contact resistance, low current density, low shock strength, and having restricted silver is the high-end applications of conductive resin.Relative nano-powder, nano silver wire has increased the one dimension size, more helps the contact between nanoparticle, can prepare the conductive resin of high conductance under the condition of low loading level.As publication number be CN 1948414A patent report adopt nano wire and nanoparticle as the ultraviolet light polymerization conductive resin of conductive filler material preparation, in loading level 56%, just can obtain 1.2 * 10 -4The high conductivity of Ω cm.Consider that from the angle that improves loading level nanometer is mixed filling with micron particle can improve filler content in the conductive resin, reduces resistivity.Publication number is that the patent of CN 101215450A adopts homemade corynebacterium nano-silver powder and commercially available micron silver mixing silver powder to prepare conductive resin as conductive filler material, improved conductivity, mechanical property and the ageing resistance of conductive resin, the total loading level of silver powder is that the volume specific resistance of 60% o'clock conductive resin reaches 2.0 * 10 -4Ω cm.If make nano-Ag particles (as the matrix resin solidification value) sintering and the conductive network that form to connect at a lower temperature in the conductive resin, not only can eliminate the contact resistance between nano silver particles, increase substantially the specific conductivity of conductive resin, and can improve the shock resistance of conductive resin.
Because the surfactivity of nano-metal particle is very high; so exist easy oxidation, easily form aggregate and in organism, be difficult to problems such as dispersion; therefore in the various preparation methods of nano metal; tend to use organism such as lipid acid, polyvinylpyrrolidone to protect its surface; prevent its oxidation and reunion; but the existence of these surface organic matters can hinder the formation of contact, sintering and the conductive network of nano metal in the conductive resin solidification process, is unfavorable for reducing the resistivity of conductive resin.Therefore, carry out suitable surface treatment for nano metal and adopt suitable technology to make that its sintering in organism is the key of preparation high conductivity conductive resin.
The present invention protects and activation treatment nanometer silver with organic dibasic acid; diprotic acid not only can be removed the zone of oxidation of nanometer silver surface trace; and can be adsorbed on the surface and prevent its further oxidation and reunion; and in the conductive resin solidification process desorption; produce the sintering between new life, activating surface promotion nano silver particles, thereby increased the specific conductivity of conductive resin greatly.Present method technology is simple, easy to use, good reproducibility, compatible fully with existing conductive resin technology, has broad application prospects in fields such as microelectronics Packaging.
Summary of the invention
The object of the present invention is to provide a kind of method of nano-Ag particles surface activation process, and adopt the high conductivity sintered type conductive resin of this surface-treated nanometer silver preparation and the preparation method of this conductive resin.
The method of the nanometer silver surface activation process that the present invention proposes, its step is as follows: at first prepare certain density organic dibasic acid solution as surface activation process reagent, organic acid concentration is 0.1-4mol/L, solvent can be conventional organic solvents such as ethanol, Virahol, organic dibasic acid can be propanedioic acid, Succinic Acid, pentanedioic acid, hexanodioic acid or senior diprotic acid etc., place surface activation process reagent ultrasonic or stirred 10-60 minute nanometer silver, the mol ratio of nanometer silver and surface activation process reagent is 1: 0.5-2; The supernatant liquid that inclines with a small amount of solvent drip washing nanometer silver, is removed unnecessary surface activation process agent.The nanometer silver here comprises nano-silver powder and/or nano-silver thread.
With above-mentioned same method micron silver is carried out surface activation process.
The invention allows for a kind of sintered type conductive resin that mixes the filling preparation with nanometer silver and micron silver through above-mentioned surface activation process, its prescription weight share meter is as follows: 100 parts of Resins, epoxy, 10~15 parts of epoxy active diluents, 80~100 parts of anhydride curing agents and curing catalyst constitute matrix resin for 0.2~2 part, and the ratio of the mixed fillers of nanometer silver that matrix resin and surface activation process are crossed and micron silver is 1: 2.5-4; In the mixed fillers, the mass ratio of nanometer silver and micron silver is 0.2~1: 1.The concrete preparation method of this conductive resin is as follows: by above-mentioned conductive resin prescription, Resins, epoxy, epoxy active diluent and anhydride curing agent are mixed, add the mixed fillers of surface treated nanometer silver and micron silver then and mix, add curing catalyst at last, continue to be stirred to mixing of materials and evenly get final product.
The present invention gives the using method of surface treating nano silver sintered type conductive resin: described conductive resin is directly filmed in glass, silicon chip, printed circuit board or other dielectric surface, place under the 150-250 ℃ of temperature and reacted 0.5-1 hour, can make its completely solidified, realize the sintering between the nano-Ag particles simultaneously.And sintering degree and Nano silver grain size, solidification value are relevant, and nano-particles size is more little, and sintering at low temperatures is obvious more.
Nanometer silver surface treatment that the present invention provides and sintered type conductive resin preparation method, technology is simple, easy to use, good reproducibility, has broad application prospects in fields such as Electronic Packaging.
Description of drawings
Fig. 1 is thermogravimetric analysis (TGA) curve of nano-silver thread after pentanedioic acid is handled.
Fig. 2 is the stereoscan photograph before nano-silver thread sintered type conductive resin solidifies.
Fig. 3 is the stereoscan photograph after nano-silver thread sintered type conductive resin solidifies.
Embodiment
The invention is further illustrated by the following examples.
Embodiment 1 is an activation treatment nano-silver powder and micron preparation of silver strip conductive resin not: the ratio that according to mass ratio is 1: 0.15: 0.9 mixes bisphenol A type epoxy resin (Dow-332), epoxy active diluent and solidifying agent 4-methylhexahydrophthalic anhydride, makes the matrix resin of conductive resin; Nano-silver powder (diameter is about 50-60nm) and micron silver strip (diameter is about 6-9 μ m) that mass ratio is about 1: 3 mix as conductive filler material; According to 1: 4 ratio of mass ratio matrix resin and silver fillers are mixed then; At last, the 1-cyano ethyl-2-ethyl-4-methylimidazole (2E4MZ-CN) that adds matrix resin consumption 1% is made catalyzer, mixes.Conductive resin is coated on the sheet glass of cleaning, the thickness of conductive resin is by the Kapton Tape control that is attached to the sheet glass two ends, put into 200 ℃ of baking ovens then and solidify after 1 hour, make the conductive coating sample 1 of thick 0.1mm, wide 10mm, long 25.4mm, resistivity is 2.3 * 10 -4Ω cm.
The preparation of embodiment 2 Ethanol Treatment nano-silver powders and micron silver strip conductive resin: it is centrifugal with it after 30 minutes that mass ratio is about in the ethanolic soln that 1: 3 nano-silver powder (diameter is about 50-60nm) and micron silver strip (diameter is about 6-9 μ m) join certain volume supersound process, incline behind the supernatant liquid, nano-silver powder and micron silver strip were placed the vacuum drying oven drying at room temperature 1 hour.The ratio that according to mass ratio is 1: 0.15: 0.9 mixes bisphenol A type epoxy resin (Dow-332), epoxy active diluent and solidifying agent 4-methylhexahydrophthalic anhydride, makes the matrix resin of conductive resin; And then according to 1: 4 mixed matrix resin of mass ratio and surface-treated nano-silver powder and micron silver strip filler; At last, the 1-cyano ethyl-2-ethyl-4-methylimidazole (2E4MZ-CN) that adds matrix resin consumption 1% is made catalyzer, mixes.Conductive resin is coated on the sheet glass of cleaning, the thickness of conductive resin is by the Kapton Tape control that is attached to the sheet glass two ends, put into 200 ℃ of baking ovens then and solidify after 1 hour, make the conductive coating sample 2 of thick 0.1mm, wide 10mm, long 25.4mm, resistivity is 1.6 * 10 -4Ω cm.
The preparation of embodiment 3 nano-silver powder sintered type conductive resins: the nano-silver powder (diameter is about 50-60nm) and the micron silver strip (diameter is about 6-9 μ m) that mass ratio are about 1: 3 join in the pentane two acid alcohol solution of 0.5mol/L of certain volume, the mol ratio of silver and pentanedioic acid is 1: 1, supersound process is centrifugal with it after 30 minutes, incline behind the supernatant liquid, nano-silver powder and micron silver strip were placed the vacuum drying oven drying at room temperature 1 hour.The ratio that according to mass ratio is 1: 0.15: 0.9 mixes bisphenol A type epoxy resin (Dow-332), epoxy active diluent and solidifying agent 4-methylhexahydrophthalic anhydride, makes the matrix resin of conductive resin; And then according to 1: 4 mixed matrix resin of mass ratio and surface-treated nano-silver powder and micron silver strip filler; At last, the 1-cyano ethyl-2-ethyl-4-methylimidazole (2E4MZ-CN) that adds matrix resin consumption 1% is made catalyzer, mixes.Conductive resin is coated on the sheet glass of cleaning, the thickness of conductive resin is by the Kapton Tape control that is attached to the sheet glass two ends, put into 200 ℃ of baking ovens then and solidify after 1 hour, make the conductive coating sample 3 of thick 0.1mm, wide 10mm, long 25.4mm, resistivity is 4.2 * 10 -5Ω cm.
The preparation of embodiment 4 nano-silver powder sintered type conductive resins: the nano-silver powder (diameter is about 50-60nm) and the micron silver strip (diameter is about 6-9 μ m) that mass ratio are about 2: 3 join in the hexanodioic acid ethanolic soln of 0.4mol/L of certain volume, the mol ratio of silver and pentanedioic acid is 1: 1, supersound process is centrifugal with it after 30 minutes, incline behind the supernatant liquid, nano-silver powder and micron silver strip were placed the vacuum drying oven drying at room temperature 1 hour.The ratio that according to mass ratio is 1: 0.85 mixes bisphenol A type epoxy resin (Dow-332) and solidifying agent 4-methylhexahydrophthalic anhydride, makes the matrix resin of conductive resin; And then according to 1: 4 mixed matrix resin of mass ratio and surface-treated nano-silver powder and micron silver strip filler; At last, the 1-cyano ethyl-2-ethyl-4-methylimidazole (2E4MZ-CN) that adds matrix resin consumption 1% is made catalyzer, mixes.Conductive resin is coated on the sheet glass of cleaning, the thickness of conductive resin is by the Kapton Tape control that is attached to the sheet glass two ends, put into 200 ℃ of baking ovens then and solidify after 1 hour, make the conductive coating sample 4 of thick 0.1mm, wide 10mm, long 25.4mm, resistivity is 7.0 * 10 -5Ω cm.
The preparation of embodiment 5 nano-silver thread sintered type conductive resins: mass ratio is about 2: 3 nano-silver thread, and (diameter is about 50-60nm, length is about 2-3 μ m) and micron silver strip (diameter is about 6-9 μ m) join in the pentane two acid alcohol solution of 0.5mol/L of certain volume, the mol ratio of silver and pentanedioic acid is 1: 1, supersound process is centrifugal with it after 30 minutes, incline behind the supernatant liquid, nano-silver thread and micron silver strip were placed the vacuum drying oven drying at room temperature 1 hour.The ratio that according to mass ratio is 1: 0.15: 0.9 mixes bisphenol A type epoxy resin (Dow-332), epoxy active diluent and solidifying agent 4-methylhexahydrophthalic anhydride, makes the matrix resin of conductive resin; And then according to 1: 3 mixed matrix resin of mass ratio and surface-treated nano-silver thread and micron silver strip filler; At last, the 1-cyano ethyl-2-ethyl-4-methylimidazole (2E4MZ-CN) that adds matrix resin consumption 1% is made catalyzer, mixes.Conductive resin is coated on the sheet glass of cleaning, the thickness of conductive resin is by the Kapton Tape control that is attached to the sheet glass two ends, then respectively at after solidifying 1 hour in 200 and 300 ℃ of baking ovens, make the conductive coating sample 5 and 6 of thick 0.1mm, wide 10mm, long 25.4mm, resistivity is respectively 8.3 * 10 -5With 6.4 * 10 -5Ω cm.
The preparation of embodiment 6 nano-silver thread sintered type conductive resins: mass ratio is about 2: 3 nano-silver thread, and (diameter is about 50-60nm, length is about 2-3 μ m) and micron silver strip (diameter is about 6-9 μ m) join in the pentane two acid alcohol solution of 0.5mol/L of certain volume, the mol ratio of silver and pentanedioic acid is 1: 1, supersound process is centrifugal with it after 30 minutes, incline behind the supernatant liquid, nano-silver thread and micron silver strip were placed the vacuum drying oven drying at room temperature 1 hour.The ratio that according to mass ratio is 1: 0.15: 0.9 mixes bisphenol A type epoxy resin (Dow-332), epoxy active diluent and solidifying agent 4-methylhexahydrophthalic anhydride, makes the matrix resin of conductive resin; And then according to 1: 3 mixed matrix resin of mass ratio and surface-treated nano-silver thread and micron silver strip filler; At last, the acetylacetone cobalt (Co (acac) that adds matrix resin consumption 1% 2) make catalyzer, mix.Conductive resin is coated on the sheet glass of cleaning, the thickness of conductive resin is by the Kapton Tape control that is attached to the sheet glass two ends, putting into 150,200,250,300 ℃ of baking ovens then respectively solidified after 1 hour, make the conductive coating sample 7-10 of thick 0.1mm, wide 10mm, long 25.4mm, it is 6.5 * 10 that resistivity is respectively -5, 7.1 * 10 -5, 4.5 * 10 -5, 1.3 * 10 -5Ω cm.
The resistance of all samples is by the test of the Shanghai Qian Feng SB100A/2 of Electron equipment Co., Ltd type four point probe conductor/semiconductor resistivity tester, and the sample resistivity values summarized is in table 1.By sample resistivity value in the table 1 as can be seen, tangible sintering has taken place in surface active nano-silver conductive glue in solidification process, thereby has reduced the contact resistance between the conductive resin filler, has improved the conductivity of conductive resin greatly.
The resistivity of conductive resin sample among table 1 embodiment

Claims (3)

1. sintered type conductive resin is characterized in that the moiety weight share meter of this conductive resin is as follows:
Matrix resin 1,
Silver fillers 2.5~4,
Wherein, the component of matrix resin weight share meter is:
Resins, epoxy 100,
Reactive thinner 10~15,
Anhydride curing agent 80~100,
Curing catalyst 0.2~2;
Silver fillers is made up of nanometer silver and micron silver through surface activation process, and the mass ratio of nanometer silver and micron silver is 0.2~1: 1;
The step of described surface activation process is as follows:
With organic dibasic acid solution as the surface activation process agent, organic dibasic acid is propanedioic acid, Succinic Acid, pentanedioic acid, hexanodioic acid or senior diprotic acid, the organic dibasic acid strength of solution is 0.1-4mol/L, nanometer silver or micron silver are 1: 0.5~2 with the mol ratio of surface activation process agent, and nanometer silver or micron silver are ultrasonic or stirred 10-60 minute in the surface activation process agent.
2. the preparation method of a sintered type conductive resin as claimed in claim 1, it is characterized in that concrete steps are as follows: Resins, epoxy, reactive thinner and anhydride curing agent are mixed by compositing formula, add the mixed fillers of surface treated nanometer silver and micron silver then and mix, add curing catalyst at last, it is even to continue to be stirred to mixing of materials.
3. the using method of a sintered type conductive resin as claimed in claim 1, it is characterized in that concrete steps are as follows: described conductive resin is directly filmed in glass, silicon chip, printed circuit board or other dielectric surface, place under the 150-250 ℃ of temperature and reacted 0.5-1 hour, can make its completely solidified, realize the sintering between the nano-Ag particles simultaneously.
CN 201010121877 2010-03-11 2010-03-11 Sintered type conductive adhesive adopting silver filling with surfaces subjected to activating treatment and preparation method thereof Pending CN101805574A (en)

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CN102174306A (en) * 2011-01-26 2011-09-07 烟台德邦电子材料有限公司 Conductive adhesive for LED (light emitting diode) packaging and preparation method of conductive adhesive
CN102373029A (en) * 2010-08-26 2012-03-14 上海亿金纳米科技有限公司 Preparation method of rapid curing of flexible conductive adhesive under room temperature
CN102443370A (en) * 2010-10-15 2012-05-09 深圳市道尔科技有限公司 Low-halogen high-conductivity single-ingredient conductive gum
CN102655030A (en) * 2011-03-02 2012-09-05 韩国电子通信研究院 Conductive composition, silicon solar cell including the same, and manufacturing method thereof
CN102676102A (en) * 2011-03-16 2012-09-19 上海富信新能源科技有限公司 Silver nanowire doped conductive silver colloid and preparation method thereof
CN102990056A (en) * 2012-10-15 2013-03-27 宁波广博纳米新材料股份有限公司 Surface processing method of submicron silver powder
CN104968746A (en) * 2012-12-27 2015-10-07 学校法人关西大学 Thermally-conductive, electrically-conductive adhesive composition
CN105618734A (en) * 2016-01-12 2016-06-01 昆明理工大学 Method for surface modification of flaky silver powder
CN105733470A (en) * 2014-12-11 2016-07-06 中国科学院苏州纳米技术与纳米仿生研究所 Modified conductive filling material, preparation method thereof and application
CN104751940B (en) * 2013-12-30 2017-04-12 财团法人工业技术研究院 Transparent conductive film composite and transparent conductive film
CN106833428A (en) * 2017-01-10 2017-06-13 金陵科技学院 A kind of conducting resinl suitable for flexible electrode bonding
CN108165209A (en) * 2018-01-31 2018-06-15 深圳名飞远科技有限公司 Low form power battery based on conducting resinl, the conducting resinl preparation method and application
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CN102373029A (en) * 2010-08-26 2012-03-14 上海亿金纳米科技有限公司 Preparation method of rapid curing of flexible conductive adhesive under room temperature
CN102443370A (en) * 2010-10-15 2012-05-09 深圳市道尔科技有限公司 Low-halogen high-conductivity single-ingredient conductive gum
CN102174306A (en) * 2011-01-26 2011-09-07 烟台德邦电子材料有限公司 Conductive adhesive for LED (light emitting diode) packaging and preparation method of conductive adhesive
CN102174306B (en) * 2011-01-26 2013-09-04 烟台德邦科技有限公司 Conductive adhesive for LED (light emitting diode) packaging and preparation method of conductive adhesive
CN102655030A (en) * 2011-03-02 2012-09-05 韩国电子通信研究院 Conductive composition, silicon solar cell including the same, and manufacturing method thereof
CN102655030B (en) * 2011-03-02 2015-07-15 韩国电子通信研究院 Conductive composition, silicon solar cell including the same, and manufacturing method thereof
CN102676102A (en) * 2011-03-16 2012-09-19 上海富信新能源科技有限公司 Silver nanowire doped conductive silver colloid and preparation method thereof
CN102676102B (en) * 2011-03-16 2014-03-12 上海富信新能源科技有限公司 Silver nanowire doped conductive silver colloid and preparation method thereof
CN102990056A (en) * 2012-10-15 2013-03-27 宁波广博纳米新材料股份有限公司 Surface processing method of submicron silver powder
CN104968746A (en) * 2012-12-27 2015-10-07 学校法人关西大学 Thermally-conductive, electrically-conductive adhesive composition
CN104751940B (en) * 2013-12-30 2017-04-12 财团法人工业技术研究院 Transparent conductive film composite and transparent conductive film
CN105733470A (en) * 2014-12-11 2016-07-06 中国科学院苏州纳米技术与纳米仿生研究所 Modified conductive filling material, preparation method thereof and application
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CN106833428A (en) * 2017-01-10 2017-06-13 金陵科技学院 A kind of conducting resinl suitable for flexible electrode bonding
CN108165209A (en) * 2018-01-31 2018-06-15 深圳名飞远科技有限公司 Low form power battery based on conducting resinl, the conducting resinl preparation method and application
CN108165209B (en) * 2018-01-31 2018-11-27 深圳名飞远科技有限公司 Low form power battery, the conducting resinl preparation method and application based on conducting resinl
CN109247003A (en) * 2018-04-12 2019-01-18 庆鼎精密电子(淮安)有限公司 Electromagnetic shielding film and preparation method thereof
CN109637693A (en) * 2018-12-17 2019-04-16 中国计量大学 A kind of conductive silver paste and preparation method thereof based on from the silver-colored frame of sintering

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