CN109161358A - A kind of preparation method of conducting resinl - Google Patents
A kind of preparation method of conducting resinl Download PDFInfo
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- CN109161358A CN109161358A CN201810826715.0A CN201810826715A CN109161358A CN 109161358 A CN109161358 A CN 109161358A CN 201810826715 A CN201810826715 A CN 201810826715A CN 109161358 A CN109161358 A CN 109161358A
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- copper powder
- conducting resinl
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
- C09J9/02—Electrically-conducting adhesives
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/085—Copper
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Conductive Materials (AREA)
Abstract
The present invention relates to a kind of preparation methods of conducting resinl, belong to adhesive material preparation technical field.Copper salt solution and complexing agent reaction are generated complex solution first by the present invention, use hydrazine hydrate as reduction again, reduction obtains Micron Copper Powder, removal Micron Copper Powder oxide on surface is cleaned with dilute sulfuric acid later, obtain pretreatment copper powder, copper powder will be pre-processed again and complex reaction occurs for valine, complex protection layer is formed in Copper Powder Surface, obtain the Modified Micron copper powder with antioxygenic property, finally Modified Micron copper powder and other auxiliary materials are blended, conducting resinl is made, the copper conductive filler inoxidizability that the present invention generates is strong, it conducts electricity very well, ageing resistance is strong, high temperature resistant, resistivity is stablized, it is very outstanding conductive filler, it has broad application prospects.
Description
Technical field
The present invention relates to a kind of preparation methods of conducting resinl, belong to adhesive material preparation technical field.
Background technique
Conducting resinl is a kind of adhesive solidified or have certain electric conductivity after dry, it usually with matrix resin and leads
Electric filler, that is, conducting particles is main constituents, conducting particles is combined together by the bonding effect of matrix resin, shape
At conductive path, the conductive connection for being glued material is realized.Since the matrix resin of conducting resinl is a kind of adhesive, can choose suitable
Suitable solidification temperature is bonded, simultaneously as the miniaturization of electronic component, micromation and the densification of printed circuit board and
The rapid development of Highgrade integration, and slurry can be made in conducting resinl, realize very high linear resolution.And conductive adhesive process letter
It is single, it is easily operated, production efficiency can be improved, so conducting resinl is substitution slicker solder welding, realize the ideal chose of conductive connection.
Conductive filler is mainly metal powder (Ag, Cu, Ni etc.), and silver powder has both good conductivity and strong excellent of oxidation resistance
Point, but it is expensive, and silver-colored transport phenomena is easy to happen under hygrothermal environment, cause silver conductive adhesive resistance unstable；Copper powder
Price is lower, good conductivity, but its oxidation resistance is poor, is chronically exposed to surface in air and forms oxidation film easily to it
Electrical property has a significant impact.There is also some problems for the silver-plated copper powder prepared in industry at present: Copper Powder Surface is not completely silver-colored
Film covering, electric conductivity, inoxidizability still are below fine silver powder；The binding force of silvering and copper powder is not strong, leads to use process
The phenomenon that middle coating falls off.These problems limit silver-plated copper powder in the application in Electronic Packaging field.
Therefore, if copper gasket can be allowed to have superpower inoxidizability, a kind of low in cost, oxidation resistance can be invented
By force, good conductivity, the novel conductive glue that can be used for a long time, this has positive meaning in adhesive material preparation technical field
Justice.
Summary of the invention
Present invention mainly solves the technical issues of, although have both good conductivity and antioxygen for traditional silver powder filler at present
The strong advantage of change ability, expensive, although copper powder filler good conductivity, but inoxidizability is poor, is chronically exposed to sky
Surface forms oxidation film easily to have a significant impact to its electrical property in gas, provides a kind of preparation method of conducting resinl.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
A kind of preparation method of conducting resinl, it is characterised in that specific preparation step are as follows:
(1) copper-bath is mixed with ethylenediamine tetra-acetic acid at room temperature and is placed in beaker that be uniformly mixing to obtain complexing molten
Liquid, then the pH with sodium hydroxide solution adjusting complex solution；
(2) above-mentioned complex solution is heated up, while hydrazine hydrate solution is instilled into reactor, while being stirred, until in reactor
Reaction solution becomes to stop instilling when aubergine, continues to add polyvinylpyrrolidone into reaction solution, filter, isolated filter
Slag is respectively washed filter residue 3~5 times with distilled water and dehydrated alcohol, dry to get Micron Copper Powder；
It (3), is that 10% dilution heat of sulfuric acid is added in sonic oscillation instrument by Micron Copper Powder obtained above and mass fraction, ultrasound
It handles, is filtered after ultrasonic treatment, obtain filtering filter residue, be eluted 3~5 times with deionized water, obtain pretreatment copper powder；
(4) it is fitted into sonic oscillation instrument after mixing the valine ethanol solution that above-mentioned pretreatment copper powder and mass fraction are 10%,
It is ultrasonically treated, after ultrasonic treatment, filters, isolated filter cake, and be put into drying in vacuum drying oven, obtain Modified Micron copper
Powder；
(5) according to parts by weight, 50~55 parts of bisphenol A type epoxy resins, 52~57 parts of 1- methylhexahydrophthaacid acids are weighed
Acid anhydride and 1~3 part of ethylenediamine, 5~10 parts of above-mentioned Modified Micron copper powders are placed in agate mortar, are discharged after grinding, and tinning is to get leading
Electric glue.
The concentration of copper-bath as described in step (1) is 0.5~0.7mol/L, and copper-bath and ethylenediamine tetraacetic walk
Suddenly drop rate described in (2) is 5mL/min, and the temperature of heating is 60~70 DEG C, the concentration of hydrazine hydrate solution is 3~
4mol/L, the mass fraction of polyvinylpyrrolidone are 0.2%.
Micron Copper Powder described in step (3) and mass fraction are that the mass ratio of 10% dilute sulfuric acid is 1:10, and supersonic frequency is
25~30kHz, sonication treatment time are 40~50min.
The mass ratio for the valine ethanol solution that pretreatment copper powder and mass fraction are 10% described in step (4) is 1:
8。
Milling time described in step (5) is 30~40min.
The beneficial effects of the present invention are:
(1) copper salt solution and complexing agent reaction are generated complex solution first by the present invention, then use hydrazine hydrate as reduction, are restored
To Micron Copper Powder, removal Micron Copper Powder oxide on surface is cleaned with dilute sulfuric acid later, obtains pretreatment copper powder, then copper will be pre-processed
Complex reaction occurs for powder and valine, forms complex protection layer in Copper Powder Surface, obtains the Modified Micron with antioxygenic property
Finally Modified Micron copper powder and other auxiliary materials are blended for copper powder, and conducting resinl is made, and present invention maximum innovative point is using simultaneously
Valine with amino and carboxyl and branch is as film forming agent, and copper exposure can be oxidized in air, so that it can be reduced
Electric conductivity, and be that copper is avoided to be oxidized most effective method in copper surface plating layer protecting film, therefore, the present invention selects
Valine to generate one layer of organic matter coating in copper particle surface, can greatly increase the combination of protective film and copper particle in this way
Power, due to there is the presence of protective film, has completely cut off contact of the copper with air, has reached anti-oxidant to avoid falling off for protective layer
Purpose, the present invention select valine the reason of be, on the one hand, valine have organic acid property, can be generated with micron copper
Carboxylic acid mantoquita can play a protective role to copper powder, effectively promote the inoxidizability of particulate copper and the electrical property of conducting resinl, another
Aspect, valine have amino, possess the property of amine, and amine can be coordinated with exposed copper surface plays the role of protection, make conduction
Glue keeps body resistivity to stablize in degradation, and the Cu in carboxylic acid mantoquita2+It can also promote the coordination of amine and copper particle,
The nitrogen-atoms and copper particle of amine form coordinate bond, constitute stable comple, and as unit, constantly extend complexing, copper particle
It is constantly complexed with valine, to form organic copper coordination polymer film, which is cross-linked with each other with carboxylic acid mantoquita film, is formed two layers
Fine and close protective film, so that inoxidizability greatly reinforces, in addition, the molecule of valine is in dendritic morphology and other straight chain amino
Acid is compared, and better barrier action can be played to oxygen.It integrates, uses valine as organic film membrane-forming agent, energy
Improve the inoxidizability of particulate copper and the electrical property of conducting resinl, moreover it is possible to make conducting resinl resistivity keep stablizing, and possess resistance to height
The characteristic of temperature, whole operation process does not pollute, easy to operate, has broad application prospects.
Specific embodiment
It is at room temperature in mass ratio the copper-bath and ethylenediamine tetra-acetic acid that concentration is 0.5~0.7mol/L by 10:1
Mixing, which is placed in beaker, is uniformly mixing to obtain complex solution, then the pH to 9~11 of complex solution is adjusted with sodium hydroxide solution；
Above-mentioned complex solution is warming up to 60~70 DEG C, while instilling concentration with the drop rate of 5mL/min into beaker as 3~4mol/L
Hydrazine hydrate solution, until reaction solution becomes to stop instilling when aubergine in beaker, continues to add into reaction solution while being stirred
The polyvinylpyrrolidone that mass fraction is 0.2%, filtering, isolated filter residue are respectively washed filter with distilled water and dehydrated alcohol
It is slag 3~5 times, dry to get Micron Copper Powder；It is in mass ratio 1:10 by Micron Copper Powder obtained above and mass fraction is 10%
Dilution heat of sulfuric acid is added in sonic oscillation instrument, handles 40~50min with the frequency ultrasound of 25~30kHz, ultrasonic treatment terminates
After filter, obtain filter filter residue, with deionized water elute 3~5 times, obtain pretreatment copper powder；By above-mentioned pretreatment copper powder and matter
The valine ethanol solution that amount score is 10% is to be fitted into sonic oscillation instrument after 1:8 is mixed in mass ratio, with 25~30kHz's
Frequency ultrasound handles 40~50min, after ultrasonic treatment, filters, isolated filter cake, and be put into vacuum drying oven it is dry,
Obtain Modified Micron copper powder；According to parts by weight, 50~55 parts of bisphenol A type epoxy resins, 52~57 parts of 1- methyl hexahydros are weighed
Phthalic anhydride and 1~3 part of ethylenediamine, 5~10 parts of above-mentioned Modified Micron copper powders are placed in agate mortar, and grinding 30~
It discharges after 40min, tinning is to get conducting resinl.
Example 1
It is at room temperature in mass ratio that the copper-bath that concentration is 0.5mol/L is mixed postposition with ethylenediamine tetra-acetic acid by 10:1
It is uniformly mixing to obtain complex solution in beaker, then adjusts the pH to 9 of complex solution with sodium hydroxide solution；Above-mentioned complexing is molten
Liquid is warming up to 60 DEG C, while instilling concentration for 3mol/L hydrazine hydrate solution, while being stirred with the drop rate of 5mL/min into beaker
Mix, stop instilling when until reaction solution becoming aubergine in beaker, continue to add into reaction solution mass fraction be 0.2% it is poly-
Vinylpyrrolidone, filtering, isolated filter residue are respectively washed filter residue 3 times with distilled water and dehydrated alcohol, dry to get micro-
Rice copper powder；It is in mass ratio 1:10 by Micron Copper Powder obtained above and mass fraction is that 10% dilution heat of sulfuric acid is added to ultrasound
In shaker, 40min is handled with the frequency ultrasound of 30kHz, is filtered after ultrasonic treatment, obtains filtering filter residue, uses deionization
Water elutes 3 times, obtains pretreatment copper powder；The valine ethanol solution that above-mentioned pretreatment copper powder and mass fraction are 10% is pressed into matter
Amount handles 40min than being is fitted into sonic oscillation instrument after 1:8 mixing, with the frequency ultrasound of 30kHz, after ultrasonic treatment, pumping
Filter, isolated filter cake, and it is put into drying in vacuum drying oven, obtain Modified Micron copper powder；According to parts by weight, 50 parts pairs are weighed
Phenol A type epoxy resin, 52 parts of 1- methylhexahydrophthalic anhydrides and 1 part of ethylenediamine, 5 parts of above-mentioned Modified Micron copper powders are placed in Ma
In Nao mortar, discharge after grinding 30, tinning is to get conducting resinl.
Example 2
It is at room temperature in mass ratio that the copper-bath that concentration is 0.6mol/L is mixed postposition with ethylenediamine tetra-acetic acid by 10:1
It is uniformly mixing to obtain complex solution in beaker, then adjusts the pH to 10 of complex solution with sodium hydroxide solution；By above-mentioned complexing
Solution is warming up to 65 DEG C, while concentration is instilled as 3.5mol/L hydrazine hydrate solution with the drop rate of 5mL/min into beaker, Bian Jin
Row stirring continues to add mass fraction into reaction solution to be 0.2% until reaction solution becomes to stop instilling when aubergine in beaker
Polyvinylpyrrolidone, filtering, isolated filter residue is respectively washed filter residue 3 times with distilled water and dehydrated alcohol, dry, i.e.,
Obtain Micron Copper Powder；It is in mass ratio 1:10 by Micron Copper Powder obtained above and mass fraction is that 10% dilution heat of sulfuric acid is added to
In sonic oscillation instrument, 40min is handled with the frequency ultrasound of 30kHz, is filtered after ultrasonic treatment, obtains filtering filter residue, spend
Ionized water elutes 3 times, obtains pretreatment copper powder；The valine ethanol solution for being 10% by above-mentioned pretreatment copper powder and mass fraction
In mass ratio to be fitted into sonic oscillation instrument after 1:8 mixing, 40min is handled with the frequency ultrasound of 30kHz, ultrasonic treatment terminates
Afterwards, it filters, isolated filter cake, and is put into drying in vacuum drying oven, obtain Modified Micron copper powder；According to parts by weight, it weighs
52 parts of bisphenol A type epoxy resins, 55 parts of 1- methylhexahydrophthalic anhydrides and 2 parts of ethylenediamines, 7 parts of above-mentioned Modified Micron copper powders
It is placed in agate mortar, discharges after grinding 30min, tinning is to get conducting resinl.
Example 3
It is at room temperature in mass ratio that the copper-bath that concentration is 0.7mol/L is mixed postposition with ethylenediamine tetra-acetic acid by 10:1
It is uniformly mixing to obtain complex solution in beaker, then adjusts the pH to 11 of complex solution with sodium hydroxide solution；By above-mentioned complexing
Solution is warming up to 70 DEG C, while instilling concentration with the drop rate of 5mL/min into beaker as 4mol/L hydrazine hydrate solution, side is carried out
Stirring continues to add mass fraction into reaction solution to be 0.2% until reaction solution becomes to stop instilling when aubergine in beaker
Polyvinylpyrrolidone, filtering, isolated filter residue is respectively washed filter residue 3 times with distilled water and dehydrated alcohol, it is dry to get
Micron Copper Powder；It is super that be in mass ratio 1:10 by Micron Copper Powder obtained above and mass fraction be that 10% dilution heat of sulfuric acid is added to
In sound oscillation instrument, 40min is handled with the frequency ultrasound of 30kHz, is filtered after ultrasonic treatment, obtains filtering filter residue, spend from
Sub- water elutes 3 times, obtains pretreatment copper powder；The valine ethanol solution that above-mentioned pretreatment copper powder and mass fraction are 10% is pressed
Mass ratio is is fitted into sonic oscillation instrument after 1:8 mixing, with the frequency ultrasound of 30kHz processing 40min, after ultrasonic treatment,
It filters, isolated filter cake, and is put into drying in vacuum drying oven, obtain Modified Micron copper powder；According to parts by weight, 55 parts are weighed
Bisphenol A type epoxy resin, 57 parts of 1- methylhexahydrophthalic anhydrides and 3 parts of ethylenediamines, 10 parts of above-mentioned Modified Micron copper powders are set
In agate mortar, discharge after grinding 30min, tinning is to get conducting resinl.
Reference examples
By taking common silver-plated copper gasket conducting resinl as an example
Performance detection is carried out to the conducting resinl in the present invention obtained conducting resinl and reference examples, testing result is as shown in table 1:
Detection method: by the conducting resinl of preparation, 200 DEG C of solidification 1h carry out measured resistivity in nitrogen atmosphere；In nitrogen atmosphere,
With different temperature-curable 1h come measured resistivity；The aging 168h at air atmosphere, 85 DEG C, it is every by surveying primary conductive for 24 hours
Colloid resistivity measures ageing rate
1 performance test results of table
As can be seen from the above table, the particulate copper performance that example three generates is best, and the copper conductive filler that the invention generates is anti-oxidant
Property it is strong, conduct electricity very well, ageing resistance is strong, high temperature resistant, resistivity stablize, be very outstanding conductive filler, have it is wide
Application prospect.
Claims (6)
1. a kind of preparation method of conducting resinl, it is characterised in that specific preparation step are as follows:
(1) copper-bath is mixed with ethylenediamine tetra-acetic acid at room temperature and is placed in beaker that be uniformly mixing to obtain complexing molten
Liquid, then the pH with sodium hydroxide solution adjusting complex solution；
(2) above-mentioned complex solution is heated up, while hydrazine hydrate solution is instilled into reactor, while being stirred, until in reactor
Reaction solution becomes to stop instilling when aubergine, continues to add polyvinylpyrrolidone into reaction solution, filter, isolated filter
Slag is respectively washed filter residue 3~5 times with distilled water and dehydrated alcohol, dry to get Micron Copper Powder；
It (3), is that 10% dilution heat of sulfuric acid is added in sonic oscillation instrument by Micron Copper Powder obtained above and mass fraction, ultrasound
It handles, is filtered after ultrasonic treatment, obtain filtering filter residue, be eluted 3~5 times with deionized water, obtain pretreatment copper powder；
(4) it is fitted into sonic oscillation instrument after mixing the valine ethanol solution that above-mentioned pretreatment copper powder and mass fraction are 10%,
It is ultrasonically treated, after ultrasonic treatment, filters, isolated filter cake, and be put into drying in vacuum drying oven, obtain Modified Micron copper
Powder；
(5) according to parts by weight, 50~55 parts of bisphenol A type epoxy resins, 52~57 parts of 1- methylhexahydrophthaacid acids are weighed
Acid anhydride and 1~3 part of ethylenediamine, 5~10 parts of above-mentioned Modified Micron copper powders are placed in agate mortar, are discharged after grinding, and tinning is to get leading
Electric glue.
2. a kind of preparation method of conducting resinl according to claim 1, it is characterised in that: sulfuric acid as described in step (1)
The concentration of copper solution is 0.5~0.7mol/L, and copper-bath and ethylenediamine tetra-acetic acid mass ratio are 10:1, adjusts complex solution
PH to 9~11.
3. a kind of preparation method of conducting resinl according to claim 1, it is characterised in that: dropwise addition described in step (2)
Rate is 5mL/min, and the temperature of heating is 60~70 DEG C, and the concentration of hydrazine hydrate solution is 3~4mol/L, polyvinylpyrrolidone
Mass fraction be 0.2%.
4. a kind of preparation method of conducting resinl according to claim 1, it is characterised in that: micron described in step (3)
Copper powder and mass fraction are that the mass ratio of 10% dilute sulfuric acid is 1:10, and supersonic frequency is 25~30kHz, sonication treatment time 40
~50min.
5. a kind of preparation method of conducting resinl according to claim 1, it is characterised in that: pre- place described in step (4)
The mass ratio for managing the valine ethanol solution that copper powder and mass fraction are 10% is 1:8.
6. a kind of preparation method of conducting resinl according to claim 1, it is characterised in that: grinding described in step (5)
Time is 30~40min.
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Cited By (5)
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| CN109732099A (en) * | 2019-03-08 | 2019-05-10 | 辽宁大学 | A kind of preparation method of anti-oxidant micron copper |
| CN111673078A (en) * | 2020-05-14 | 2020-09-18 | 深圳第三代半导体研究院 | Anti-oxidation treatment method for micro-nano copper material |
| CN111995978A (en) * | 2020-09-08 | 2020-11-27 | 株洲飞鹿高新材料技术股份有限公司 | Low-temperature quick-drying polymer-based conductive adhesive and preparation method thereof |
| CN113480963A (en) * | 2021-05-24 | 2021-10-08 | 厦门大学 | Conductive adhesive, conductive adhesive tape and preparation method thereof |
| CN114875513A (en) * | 2022-06-02 | 2022-08-09 | 浙江理工大学 | Preparation method of nano-copper antibacterial and antiviral black fiber |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109732099A (en) * | 2019-03-08 | 2019-05-10 | 辽宁大学 | A kind of preparation method of anti-oxidant micron copper |
| CN111673078A (en) * | 2020-05-14 | 2020-09-18 | 深圳第三代半导体研究院 | Anti-oxidation treatment method for micro-nano copper material |
| CN111995978A (en) * | 2020-09-08 | 2020-11-27 | 株洲飞鹿高新材料技术股份有限公司 | Low-temperature quick-drying polymer-based conductive adhesive and preparation method thereof |
| CN111995978B (en) * | 2020-09-08 | 2022-03-15 | 株洲飞鹿高新材料技术股份有限公司 | Low-temperature quick-drying polymer-based conductive adhesive and preparation method thereof |
| CN113480963A (en) * | 2021-05-24 | 2021-10-08 | 厦门大学 | Conductive adhesive, conductive adhesive tape and preparation method thereof |
| CN114875513A (en) * | 2022-06-02 | 2022-08-09 | 浙江理工大学 | Preparation method of nano-copper antibacterial and antiviral black fiber |
| CN114875513B (en) * | 2022-06-02 | 2024-05-28 | 浙江理工大学 | Preparation method of nano-copper antibacterial antiviral black fiber |
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Application publication date: 20190108 |