CN108997952A - Low temperature high adhesion force conductive silver paste - Google Patents

Low temperature high adhesion force conductive silver paste Download PDF

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Publication number
CN108997952A
CN108997952A CN201710420253.8A CN201710420253A CN108997952A CN 108997952 A CN108997952 A CN 108997952A CN 201710420253 A CN201710420253 A CN 201710420253A CN 108997952 A CN108997952 A CN 108997952A
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CN
China
Prior art keywords
parts
silver
low temperature
high adhesion
adhesion force
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.)
Pending
Application number
CN201710420253.8A
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Chinese (zh)
Inventor
叶旭东
胡曰康
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
SUZHOU A-TES ELECTRONIC TECHNOLOGY Co Ltd
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SUZHOU A-TES ELECTRONIC TECHNOLOGY Co Ltd
Priority date (The priority date 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 date listed.)
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Publication date
Application filed by SUZHOU A-TES ELECTRONIC TECHNOLOGY Co Ltd filed Critical SUZHOU A-TES ELECTRONIC TECHNOLOGY Co Ltd
Priority to CN201710420253.8A priority Critical patent/CN108997952A/en
Publication of CN108997952A publication Critical patent/CN108997952A/en
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J9/00Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
    • C09J9/02Electrically-conducting adhesives
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/06Non-macromolecular additives organic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/08Macromolecular additives
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J175/00Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
    • C09J175/04Polyurethanes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/014Additives containing two or more different additives of the same subgroup in C08K
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Conductive Materials (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The present invention discloses a kind of low temperature high adhesion force conductive silver paste, it is grouped as by the group of following parts by weight: conductive filler, polyurethane resin, glycerin ether epoxy resin, polyethers, rilanit special, dicyandiamide, hexahydrophthalic acid anhydride, N, N- dipropyl -1- propylamine, neopentyl glycol glycidol ether, gamma-aminopropyl-triethoxy-silane, defoaming agent, methyl second butanone, cyclohexanone;The conductive filler is silver powder and silver nanowires according to 100:(25 ~ 40) mixture that the ratios of parts by weight is mixed to form, the diameter of the silver powder is 2 ~ 8 μm, and the silver nanowires length is 20 ~ 200 μm, and diameter is 20 ~ 100nm.Low temperature high adhesion force conductive silver paste of the present invention at 15 DEG C of environment temperature or less can be reserved for 12 months, storage stability is good, under the conditions of 120 DEG C, 100 seconds can dry solidification, to improve production efficiency and yield.

Description

Low temperature high adhesion force conductive silver paste
Technical field
The present invention relates to conductive silver glue fields, and in particular to a kind of low temperature high adhesion force conductive silver paste.
Background technique
Conductive silver glue has been widely used in electronics industry, is mainly used for the viscous of the conductive body between unlike material It connects.Currently, in the market it is visible it is most of be using epoxy resin be that basic resin is aided with different types of amino resins as solidification The two-component system of agent, and the conductive silver glue formed using super fine silver powder as conducting medium, silver content is between 60 ~ 70%, cost Also higher, there is also two big defects for this kind of elargol, first is that needing stringent storage condition, stability is poor, and the shelf-life is short;Second is that solid It is high to change temperature, the time is long, and generally requiring 130 ~ 150 DEG C, 20 ~ 30 minutes or longer time could solidify, and is unfavorable for production effect The promotion of rate;Therefore, above-mentioned technical problem how to be overcome to become the direction that those of ordinary skill in the art make great efforts.
Summary of the invention
The object of the present invention is to provide a kind of low temperature high adhesion force conductive silver paste, which exists It can be reserved for 12 months at 15 DEG C of environment temperature or less, storage stability is good, under the conditions of 120 DEG C, can dry within 100 seconds solid Change, to improve production efficiency and yield.
In order to achieve the above objectives, the technical solution adopted by the present invention is that: a kind of low temperature high adhesion force conductive silver paste, by following The group of parts by weight is grouped as:
80 parts of conductive filler,
8 ~ 12 parts of polyurethane resin,
3 ~ 5 parts of glycerin ether epoxy resin,
6 ~ 9 parts of polyethers,
0.1 ~ 0.4 part of rilanit special,
0.6 ~ 1.5 part of dicyandiamide,
0.3 ~ 0.5 part of hexahydrophthalic acid anhydride,
0.1 ~ 0.25 part of propylamine of N, N- dipropyl -1-,
10 ~ 15 parts of neopentyl glycol glycidol ether,
0.5 ~ 1 part of gamma-aminopropyl-triethoxy-silane,
0.2 ~ 0.4 part of defoaming agent,
4 ~ 7 parts of methyl second butanone,
2 ~ 3 parts of cyclohexanone;
The conductive filler is silver powder and silver nanowires according to 100:(25 ~ 40) mixture that is mixed to form of the ratios of parts by weight, The diameter of the silver powder is 2 ~ 8 μm, and the silver nanowires length is 20 ~ 200 μm, and diameter is 20 ~ 100nm.
The further improved technical solution of above-mentioned technical proposal is as follows:
In above scheme, the defoaming agent is dodecyl sodium sulfate or 4,4- diaminodiphenylmethane.
Due to the application of the above technical scheme, compared with the prior art, the invention has the following advantages:
1. low temperature high adhesion force conductive silver paste of the present invention uses 8 ~ 12 parts of polyurethane resin, 3 ~ 5 parts of glycerin ether epoxy resin It is equipped with rilanit special, N, N- dipropyl -1- propylamine can be reserved for 12 months at 15 DEG C of environment temperature or less, storage stability It is good;Conductive filler is silver powder and silver nanowires according to 100:(25 ~ 40) mixture that is mixed to form of the ratios of parts by weight, the silver The diameter of powder is 2 ~ 8 μm, and the silver nanowires length is 20 ~ 200 μm, and diameter is 20 ~ 100nm, is improved between conductive filler Contact area, conductive channel can be more readily formed in conducting resinl, also by silver content be reduced to 50% hereinafter, conductive silver glue body Product resistivity is≤1.2 × 10-4Ω cm, thus the conductive effect that colloid can also be got well in the smaller situation of Ag doping amount.
2. low temperature high adhesion force conductive silver paste of the present invention, 10 ~ 15 parts of neopentyl glycol glycidol ether, 6 ~ 9 parts of polyethers, 0.6 ~ 1.5 part of dicyandiamide, 0.3 ~ 0.5 part of hexahydrophthalic acid anhydride, the dry solidification time is short, and elargol is in 90 DEG C of conditions when use Under, 9 minutes can dry solidification, under the conditions of 120 DEG C, 100 seconds can dry solidification, to improve production efficiency and good Rate.
Specific embodiment
Embodiment 1 ~ 4: a kind of low temperature high adhesion force conductive silver paste is grouped as by the group of following parts by weight, as shown in table 1:
Table 1
Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4
Conductive filler 80 parts 80 parts 80 parts 80 parts
Polyurethane resin 9 parts 12 parts 10 parts 8 parts
Glycerin ether epoxy resin 4 parts 3.8 part 3.5 part 5 parts
Polyethers 8 parts 6 parts 9 parts 8.5 part
Rilanit special 0.3 part 0.1 part 0.4 part 0.2 part
Dicyandiamide 0.9 part 1.2 part 0.6 part 1.4 part
Hexahydrophthalic acid anhydride 0.5 part 0.35 part 0.32 part 0.4 part
N, N- dipropyl -1- propylamine 0.12 part 0.2 part 0.18 part 0.15 part
Neopentyl glycol glycidol ether 13 parts 15 parts 12 parts 14 parts
Gamma-aminopropyl-triethoxy-silane 0.8 part 0.6 part 1 part 0.5 part
Defoaming agent 0.2 part 0.3 part 0.25 part 0.4 part
Methyl second butanone 5 parts 7 parts 6 parts 5.4 part
Cyclohexanone 2.2 part 2 parts 3 parts 2.8 part
Conductive filler is silver powder and the mixture that silver nanowires is mixed to form according to the ratio of 100:30 parts by weight in embodiment 1; Conductive filler is silver powder and the mixture that silver nanowires is mixed to form according to the ratio of 100:28 parts by weight in embodiment 2;Implement Conductive filler is silver powder and the mixture that silver nanowires is mixed to form according to the ratio of 100:32 parts by weight in example 3;In embodiment 4 Conductive filler is silver powder and the mixture that silver nanowires is mixed to form according to the ratio of 100:38 parts by weight;
The diameter of the silver powder is 2 ~ 8 μm, and the silver nanowires length is 20 ~ 200 μm, and diameter is 20 ~ 100nm.
The defoaming agent of Examples 1 and 2 is dodecyl sodium sulfate, and the defoaming agent of embodiment 3 and 4 is 4,4- diamino hexichol Methane.
A kind of preparation process of above-mentioned low temperature high adhesion force conductive silver paste, comprising the following steps:
Step 1: 8 ~ 12 parts of polyurethane resin, 3 ~ 5 parts of glycerin ether epoxy resin, N, 0.1 ~ 0.25 part of N- dipropyl -1- propylamine, 10 ~ 15 parts of neopentyl glycol glycidol ether, 0.2 ~ 0.4 part of defoaming agent, 4 ~ 7 parts of methyl second butanone, 2 ~ 3 parts of cyclohexanone, at 120 DEG C Mixture after carrying out pre-dispersed formation dispersion for 10 ~ 30 minutes is stirred at a temperature of ~ 150 DEG C;
Step 2: again by 6 ~ 9 parts of polyethers, 0.1 ~ 0.4 part of rilanit special, 0.6 ~ 1.5 part of dicyandiamide, hexahydrophthalic acid anhydride 0.3 ~ 0.5 part, 0.5 ~ 1 part of gamma-aminopropyl-triethoxy-silane is added mixture after the dispersion that step 1 obtains, to obtain base Body;
It is sufficiently stirred Step 3: 80 parts of addition step 2 of conductive filler are obtained in matrix, is then placed in three-roller and grinds, obtain The low temperature high adhesion force conductive silver paste is obtained, the conductive filler is silver powder and silver nanowires according to 100:(25 ~ 40) parts by weight The mixture that is mixed to form of ratio, the diameter of the silver powder is 2 ~ 8 μm, and the silver nanowires length is 20 ~ 200 μm, diameter For 20 ~ 100nm.
Mixture re-ultrasonic dispersion 10 ~ 30 minutes after the dispersion that above-mentioned steps one obtain.
The whipping temp of above-mentioned steps one is 130 DEG C.
When using above-mentioned low temperature high adhesion force conductive silver paste, 8 ~ 12 parts of polyurethane resin, glycerin ether epoxy resin 3 are used ~ 5 parts are equipped with rilanit special, N, and N- dipropyl -1- propylamine can be reserved for 12 months at 15 DEG C of environment temperature or less, and storage is steady It is qualitative good;Conductive filler is silver powder and silver nanowires according to 100:(25 ~ 40) mixture that is mixed to form of the ratios of parts by weight, institute The diameter for stating silver powder is 2 ~ 8 μm, and the silver nanowires length is 20 ~ 200 μm, and diameter is 20 ~ 100nm, improves conductive filler Between contact area, conductive channel can be more readily formed in conducting resinl, silver content is also reduced to 50% hereinafter, conductive silver glue Volume resistivity be≤1.2 × 10-4Ω cm, thus the conductive effect that colloid can also be got well in the smaller situation of Ag doping amount Fruit;Again, 10 ~ 15 parts of neopentyl glycol glycidol ether, 6 ~ 9 parts of polyethers, 0.6 ~ 1.5 part of dicyandiamide, hexahydrophthalic acid anhydride 0.3 ~ 0.5 part, the dry solidification time is short, when use elargol under the conditions of 90 DEG C, 9 minutes can dry solidification, in 120 DEG C of conditions Under, 100 seconds can dry solidification, to improve production efficiency and yield.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art Scholar cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all according to the present invention Equivalent change or modification made by Spirit Essence, should be covered by the protection scope of the present invention.

Claims (2)

1. a kind of low temperature high adhesion force conductive silver paste, it is characterised in that: be grouped as by the group of following parts by weight:
80 parts of conductive filler,
8 ~ 12 parts of polyurethane resin,
3 ~ 5 parts of glycerin ether epoxy resin,
6 ~ 9 parts of polyethers,
0.1 ~ 0.4 part of rilanit special,
0.6 ~ 1.5 part of dicyandiamide,
0.3 ~ 0.5 part of hexahydrophthalic acid anhydride,
0.1 ~ 0.25 part of propylamine of N, N- dipropyl -1-,
10 ~ 15 parts of neopentyl glycol glycidol ether,
0.5 ~ 1 part of gamma-aminopropyl-triethoxy-silane,
0.2 ~ 0.4 part of defoaming agent,
4 ~ 7 parts of methyl second butanone,
2 ~ 3 parts of cyclohexanone;
The conductive filler is silver powder and silver nanowires according to 100:(25 ~ 40) mixture that is mixed to form of the ratios of parts by weight, The diameter of the silver powder is 2 ~ 8 μm, and the silver nanowires length is 20 ~ 200 μm, and diameter is 20 ~ 100nm.
2. low temperature high adhesion force conductive silver paste according to claim 1, it is characterised in that: the defoaming agent is dodecyl Sodium sulfonate or 4,4- diaminodiphenylmethane.
CN201710420253.8A 2017-06-06 2017-06-06 Low temperature high adhesion force conductive silver paste Pending CN108997952A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710420253.8A CN108997952A (en) 2017-06-06 2017-06-06 Low temperature high adhesion force conductive silver paste

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710420253.8A CN108997952A (en) 2017-06-06 2017-06-06 Low temperature high adhesion force conductive silver paste

Publications (1)

Publication Number Publication Date
CN108997952A true CN108997952A (en) 2018-12-14

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CN201710420253.8A Pending CN108997952A (en) 2017-06-06 2017-06-06 Low temperature high adhesion force conductive silver paste

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102653659A (en) * 2012-04-26 2012-09-05 苏州艾达仕电子科技有限公司 Conductive coating material based on polyurethane dispersion body
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
CN105810294A (en) * 2016-06-01 2016-07-27 合肥微晶材料科技有限公司 Waterborne conductive silver paste and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN102653659A (en) * 2012-04-26 2012-09-05 苏州艾达仕电子科技有限公司 Conductive coating material based on polyurethane dispersion body
CN105810294A (en) * 2016-06-01 2016-07-27 合肥微晶材料科技有限公司 Waterborne conductive silver paste and preparation method thereof

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