CN109135629A - A kind of preparation method of printed wiring board PPTC adhesive - Google Patents

A kind of preparation method of printed wiring board PPTC adhesive Download PDF

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Publication number
CN109135629A
CN109135629A CN201810721988.9A CN201810721988A CN109135629A CN 109135629 A CN109135629 A CN 109135629A CN 201810721988 A CN201810721988 A CN 201810721988A CN 109135629 A CN109135629 A CN 109135629A
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CN
China
Prior art keywords
parts
adhesive
pptc
wiring board
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.)
Withdrawn
Application number
CN201810721988.9A
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Chinese (zh)
Inventor
汪元元
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.)
New Mstar Technology Ltd In Hefei
Original Assignee
New Mstar Technology Ltd In Hefei
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Filing date
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Application filed by New Mstar Technology Ltd In Hefei filed Critical New Mstar Technology Ltd In Hefei
Priority to CN201810721988.9A priority Critical patent/CN109135629A/en
Publication of CN109135629A publication Critical patent/CN109135629A/en
Withdrawn legal-status Critical Current

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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
    • C09J133/00Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
    • C09J133/04Homopolymers or copolymers of esters
    • C09J133/06Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
    • C09J133/08Homopolymers or copolymers of acrylic acid esters
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10Esters
    • C08F220/12Esters of monohydric alcohols or phenols
    • C08F220/16Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
    • C08F220/18Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
    • 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
    • C09J11/04Non-macromolecular additives inorganic
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10Esters
    • C08F220/12Esters of monohydric alcohols or phenols
    • C08F220/16Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
    • C08F220/18Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
    • C08F220/1804C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The invention belongs to electronic materials and adhesive area, are related to a kind of preparation method of printed wiring board PPTC adhesive.Present invention process is simple, low in cost, and the PPTC adhesive curing time of preparation is short, for the conductive bond of the end electronic component I/O in the circuit board, and plays the role of excess-current excess-temperature protection.Wiring board area can be effectively saved, manufacturing cost and process cycle is reduced, device circuit reliability can be promoted.

Description

A kind of preparation method of printed wiring board PPTC adhesive
Technical field
The invention belongs to electronic materials and adhesive area, are related to a kind of preparation side of printed wiring board PPTC adhesive Method.
Background technique
The resistivity of positive temperature coefficient (PTC) material increases with the raising of temperature, and macromolecule is blended with conductive filler can Composite material (PPTC) obtained has lower room temperature resistivity, increases resistivity with temperature and increases and in some temperature spot electricity Resistance sharply increases, and resistance, which sharply increases, under current state realizes circuit shutdown, and can voluntarily restore low after troubleshooting Resistance state.In view of PPTC device is all to connect to play a protective role in circuit, using the medium of PTC current-limiting protection function as The cohesive body of connection and component pin and wiring board can effectively save wiring board area, reduce manufacturing cost, promote device Circuit reliability.
The adhesive solidification time often directly affects time and the reliability of SMT process flow, and the present invention develops one kind and is used for Conductive connection can rapid curing PPTC adhesive with overcurrent protection.
Summary of the invention
For prior art defect, the purpose of the present invention is to provide a kind of preparations of PPTC adhesive of printed wiring board Method, which comprises the steps of:
(1) cupric salt being dissolved into deionized water, sequentially adds alkali and complexing agent, stirring dissolves it sufficiently, Graphite oxide is added, is dispersed with stirring under ultrasonic environment, obtains uniform colloidal sol, be eventually adding reducing agent, stop after completely dissolution Stirring;After room temperature~70 DEG C isothermal reaction 6~8 hours, after obtained precipitating is used deionized water, ethanol washing, it is distributed to In butyl acrylate, powder and butyl acetate mass ratio 1: 2~1: 3;
(2) step (1) butyl acrylate dispersion liquid is divided into two parts, is separately added into functional component for preparing adhesive Component A and B component,
Each weight ratio of constituents of component A are as follows:
100 parts of butyl acrylate dispersion liquid
10-20 parts of methacrylic acid
20-30 parts of ABS
3-8 parts of isopropyl benzene hydroperoxide
0.1-0.5 parts of hydroquinone
Each weight ratio of constituents of B component are as follows:
100 parts of butyl acrylate dispersion liquid
10-20 parts of methacrylic acid
10-15 parts of nitrile rubber
1-5 parts of thiocarbamide
0.1-0.5 parts of hydroquinone
(3) two kinds of components of A, B are mixed in equal volume, at room temperature solidification bonding.
The cupric salt includes or mixtures thereof one of copper nitrate, copper acetate, cupric oxalate, cupric tartrate, concentration For 0.01mol/L~0.06mol/L;The sulfydryl complexing agent includes one of thioacetic acid, mercaptopropionic acid or combinations thereof, is added The mole for entering complexing agent is 1~3 times of copper atom mole in reaction system;The alkali concentration be 0.1mol/L~ 0.5mol/L。
0.5~1.5g/L of the graphite oxide concentration, the reducing agent be one of potassium borohydride, sodium borohydride or its Combination;The mole that reducing agent is added is 12~25 times of Cu atomic mol in reaction system.
The printed wiring board of preparation is bonded and is played for the input and/or output end of electronic component with PPTC adhesive and led Logical effect, when electric current is excessive or element over-temperature, resistance, which sharply increases, realizes circuit shutdown, can be self-healing after troubleshooting Conducting.
Present invention process is simple, low in cost, and the PPTC adhesive curing time of preparation is short, is used for the end electronic component I/O Conductive bond in the circuit board, and play the role of excess-current excess-temperature protection.Wiring board area can be effectively saved, system is reduced This and process cycle are caused, device circuit reliability can be promoted.
The contents of the present invention and feature have revealed that as above, however the present invention that describes of front only briefly or pertains only to this The specific part of invention, feature of the invention may be more than what content disclosed herein was related to.Therefore, protection model of the invention The revealed content of embodiment should be not limited to by enclosing, and should include the combination of all the elements embodied in different piece, with And it is various without departing substantially from replacement and modification of the invention, and covered by claims of the present invention.
Specific embodiment
Embodiment 1:
(1) 0.01mol/L copper nitrate is dissolved into deionized water, sequentially add 0.1mol/L sodium hydroxide and 0.03mol/L thioacetic acid, stirring dissolve it sufficiently, and 1.5g/L graphite oxide is added, is dispersed with stirring, obtains under ultrasonic environment To uniform colloidal sol, it is eventually adding 0.25mol/L sodium borohydride, stops stirring after completely dissolution;After room temperature isothermal reaction 8 hours, After obtained precipitating is used deionized water, ethanol washing, it is distributed in butyl acrylate, powder and butyl acetate mass ratio 1: 2;
(2) step (1) butyl acrylate dispersion liquid is divided into two parts, is separately added into functional component for preparing adhesive Component A and B component,
Each weight ratio of constituents of component A are as follows:
100 parts of butyl acrylate dispersion liquid
20 parts of methacrylic acid
30 parts of ABS
8 parts of isopropyl benzene hydroperoxide
0.5 part of hydroquinone
Each weight ratio of constituents of B component are as follows:
100 parts of butyl acrylate dispersion liquid
20 parts of methacrylic acid
15 parts of nitrile rubber
5 parts of thiocarbamide
0.5 part of hydroquinone
(3) two kinds of components of A, B are mixed in equal volume, at room temperature solidification bonding, tensile strength: 67MPa;Conductivity: 55Scm-1;PTC intensity: 3.1.
Embodiment 2:
(1) 0.06mol/L copper acetate is dissolved into deionized water, sequentially add 0.5mol/L potassium hydroxide and 0.06mol/L thioacetic acid, stirring dissolve it sufficiently, and 0.5g/L graphite oxide is added, is dispersed with stirring, obtains under ultrasonic environment To uniform colloidal sol, it is eventually adding 0.72mol/L potassium borohydride, stops stirring after completely dissolution;70 DEG C after isothermal reaction 6 hours, After obtained precipitating is used deionized water, ethanol washing, it is distributed in butyl acrylate, powder and butyl acetate mass ratio 1: 3;
(2) step (1) butyl acrylate dispersion liquid is divided into two parts, is separately added into functional component for preparing adhesive Component A and B component,
Each weight ratio of constituents of component A are as follows:
100 parts of butyl acrylate dispersion liquid
100 parts of methacrylic acid
20 parts of ABS
3 parts of isopropyl benzene hydroperoxide
0.1 part of hydroquinone
Each weight ratio of constituents of B component are as follows:
100 parts of butyl acrylate dispersion liquid
10 parts of methacrylic acid
10 parts of nitrile rubber
1 part of thiocarbamide
0.1 part of hydroquinone
(3) two kinds of components of A, B are mixed in equal volume, at room temperature solidification bonding, tensile strength: 59MPa;Conductivity: 51Scm-1;PTC intensity: 3.9.
Embodiment 3:
(1) 0.05mol/L cupric oxalate is dissolved into deionized water, sequentially add 0.4mol/L sodium hydroxide and 0.1mol/L thioacetic acid, stirring dissolve it sufficiently, and 1g/L graphite oxide is added, is dispersed with stirring, obtains under ultrasonic environment Uniform colloidal sol is eventually adding 0.8mol/L sodium borohydride, stops stirring after completely dissolution;50 DEG C after isothermal reaction 7 hours, will After the precipitating arrived is using deionized water, ethanol washing, it is distributed in butyl acrylate, powder and butyl acetate mass ratio 1: 3;
(2) step (1) butyl acrylate dispersion liquid is divided into two parts, is separately added into functional component for preparing adhesive Component A and B component,
Each weight ratio of constituents of component A are as follows:
100 parts of butyl acrylate dispersion liquid
15 parts of methacrylic acid
20 parts of ABS
5 parts of isopropyl benzene hydroperoxide
0.5 part of hydroquinone
Each weight ratio of constituents of B component are as follows:
100 parts of butyl acrylate dispersion liquid
15 parts of methacrylic acid
10 parts of nitrile rubber
3 parts of thiocarbamide
0.3 part of hydroquinone
(3) two kinds of components of A, B are mixed in equal volume, at room temperature solidification bonding, tensile strength: 51MPa;Conductivity: 62Scm-1;PTC intensity: 2.8.
Embodiment 4:
(1) 0.03mol/L cupric tartrate is dissolved into deionized water, sequentially add 0.3mol/L potassium hydroxide and 0.06mol/L thioacetic acid, stirring dissolve it sufficiently, and 1g/L graphite oxide is added, is dispersed with stirring, obtains under ultrasonic environment Uniform colloidal sol is eventually adding 0.5mol/L potassium borohydride, stops stirring after completely dissolution;After room temperature reaction 7 hours, by what is obtained After precipitating is using deionized water, ethanol washing, it is distributed in butyl acrylate, powder and butyl acetate mass ratio 1: 2;
(2) step (1) butyl acrylate dispersion liquid is divided into two parts, is separately added into functional component for preparing adhesive Component A and B component,
Each weight ratio of constituents of component A are as follows:
100 parts of butyl acrylate dispersion liquid
20 parts of methacrylic acid
30 parts of ABS
8 parts of isopropyl benzene hydroperoxide
0.5 part of hydroquinone
Each weight ratio of constituents of B component are as follows:
100 parts of butyl acrylate dispersion liquid
15 parts of methacrylic acid
10 parts of nitrile rubber
5 parts of thiocarbamide
0.4 part of hydroquinone
(3) two kinds of components of A, B are mixed in equal volume, at room temperature solidification bonding, tensile strength: 42MPa;Conductivity: 66Scm-1;PTC intensity: 3.6.

Claims (4)

1. a kind of printed wiring board preparation method of PPTC adhesive, which comprises the steps of:
(1) cupric salt is dissolved into deionized water, sequentially adds alkali and complexing agent, stirring dissolves it sufficiently, is added Graphite oxide is dispersed with stirring under ultrasonic environment, obtains uniform colloidal sol, be eventually adding reducing agent, stops stirring after completely dissolution; After room temperature~70 DEG C isothermal reaction 6~8 hours, after obtained precipitating is used deionized water, ethanol washing, it is distributed to acrylic acid In butyl ester, powder and butyl acetate mass ratio 1: 2~1: 3;
(2) step (1) butyl acrylate dispersion liquid is divided into two parts, be separately added into functional component for match preparing adhesive A Component and B component,
Each weight ratio of constituents of component A are as follows:
100 parts of butyl acrylate dispersion liquid
10-20 parts of methacrylic acid
20-30 parts of ABS
3-8 parts of isopropyl benzene hydroperoxide
0.1-0.5 parts of hydroquinone
Each weight ratio of constituents of B component are as follows:
100 parts of butyl acrylate dispersion liquid
10-20 parts of methacrylic acid
10-15 parts of nitrile rubber
1-5 parts of thiocarbamide
0.1-0.5 parts of hydroquinone
(3) two kinds of components of A, B are mixed in equal volume, at room temperature solidification bonding.
2. the preparation method of a kind of printed wiring board PPTC adhesive according to claim 1, which is characterized in that described two Valence mantoquita includes or mixtures thereof one of copper nitrate, copper acetate, cupric oxalate, cupric tartrate, concentration be 0.01mol/L~ 0.06mol/L;The sulfydryl complexing agent includes one of thioacetic acid, mercaptopropionic acid or combinations thereof, and rubbing for complexing agent is added Your amount is 1~3 times of copper atom mole in reaction system;The alkali concentration is 0.1mol/L~0.5mol/L.
3. the preparation method of a kind of printed wiring board PPTC adhesive according to claim 1, which is characterized in that the oxygen 0.5~1.5g/L of graphite concentration, the reducing agent are one of potassium borohydride, sodium borohydride or combinations thereof;Reduction is added The mole of agent is 12~25 times of Cu atomic mol in reaction system.
4. prepared by a kind of preparation method of printed wiring board as described in claims 1 to 3 any one with PPTC adhesive Printed wiring board PPTC adhesive, the input and/or output end for electronic component is bonded and plays the role of conducting, works as electricity When flowing through big or element over-temperature, resistance, which sharply increases, realizes circuit shutdown, can be self-healing conducting after troubleshooting.
CN201810721988.9A 2018-06-26 2018-06-26 A kind of preparation method of printed wiring board PPTC adhesive Withdrawn CN109135629A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201810721988.9A CN109135629A (en) 2018-06-26 2018-06-26 A kind of preparation method of printed wiring board PPTC adhesive

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Application Number Priority Date Filing Date Title
CN201810721988.9A CN109135629A (en) 2018-06-26 2018-06-26 A kind of preparation method of printed wiring board PPTC adhesive

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CN109135629A true CN109135629A (en) 2019-01-04

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1759157A (en) * 2003-03-10 2006-04-12 蒂萨股份公司 Intrinsically heatable pressure-sensitive adhesive planar structures
CN1786096A (en) * 2004-12-08 2006-06-14 Lg电线株式会社 Anisotropic conductive adhesive having PTC characteristics
CN1925070A (en) * 2006-09-19 2007-03-07 谭富彬 Composition and preparation of aluminum conductive electric slurry for positive temperature coefficient heat-variable resistor
CN103436197A (en) * 2013-09-02 2013-12-11 南京萨特科技发展有限公司 Conductive adhesive for over-temperature overcurrent protective element and production method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1759157A (en) * 2003-03-10 2006-04-12 蒂萨股份公司 Intrinsically heatable pressure-sensitive adhesive planar structures
CN1786096A (en) * 2004-12-08 2006-06-14 Lg电线株式会社 Anisotropic conductive adhesive having PTC characteristics
CN1925070A (en) * 2006-09-19 2007-03-07 谭富彬 Composition and preparation of aluminum conductive electric slurry for positive temperature coefficient heat-variable resistor
CN103436197A (en) * 2013-09-02 2013-12-11 南京萨特科技发展有限公司 Conductive adhesive for over-temperature overcurrent protective element and production method thereof

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
李宝库 等主编: "《胶粘剂应用技术》", 31 December 1989, 中国商业出版社 *
田甜 等: "化学原位还原法制备石墨烯-铜纳米颗粒复合物", 《电子显微学报》 *
钟力生 等编: "《工程电介质物理与介电现象》", 31 March 2013, 西安交通大学出版社 *

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Application publication date: 20190104