CN102332324A - Composite conducting particles and preparation method thereof - Google Patents
Composite conducting particles and preparation method thereof Download PDFInfo
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- CN102332324A CN102332324A CN 201110253712 CN201110253712A CN102332324A CN 102332324 A CN102332324 A CN 102332324A CN 201110253712 CN201110253712 CN 201110253712 CN 201110253712 A CN201110253712 A CN 201110253712A CN 102332324 A CN102332324 A CN 102332324A
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Abstract
The invention relates to a preparation method for conducting particles which can substitute pure silver conducting particles and take a polymer matrix as an outer layer of a core for plating copper and silver. In the method, copper and silver are plated on the surface of insulating epoxy resin powder by using a palladium-free activated chemical plating method on the surface of non-metal powder, namely epoxy resin powder, to prepare the composite conducting particles in which a copper-silver composite plating layer is plated on the polymer. Compared with the normal metal conducting filler, the conducting particles have the advantages that: the preparation process is simple, the cost is low, the prepared conducting particles have high performance, and the conventional silver powder and copper powder conducting metal filler can be substituted.
Description
Technical field
The present invention relates to a kind of composite conducting particle and preparation method thereof, particularly a kind of with polymeric matrix, conducting particles that outer copper facing is silver-plated and preparation method thereof.
Background technology
Conducting particles is an important component part in the compound-type conducting material, has determined the electric conductivity of material.Metal species conductive fillers such as silver, copper, nickel are the conductive fillers of one type of extensive use.Copper and mickel class conducting particles price is lower, but has the shortcoming that is easy to oxidation and reduces electric conductivity.Plurality of advantages such as argent has that contact resistance is little, good conductivity, thermal conductivity and excellent corrosion resistance; So in the electronics industry in recent years; A large amount of attritive powders that use Ag are as the conductive filler of conducting resinl etc.; But there is problems such as costing an arm and a leg, be easy to the silver migration in argent, so its application is restricted.For improving performance, reduce cost, comparatively extensive to the research of compounded mix, mainly realize through metal covering metallic or inorganic organic non-conductive particles surface.
Summary of the invention
The object of the present invention is to provide a kind of composite conducting particle, this conducting particles can replace fine silver as conductive particle.
Two of the object of the invention is to provide the preparation method of this composite conducting particle.
For achieving the above object, the present invention adopts following technical scheme:
A kind of composite conducting particle is characterized in that this conducting particles is matrix with epoxy resin, and with copper and silver, wherein the quality of copper is 24.0%～44.1% of a substrate quality in the plating of the skin of this matrix; The quality of silver is 36.3% ~ 56.4% of a substrate quality.
A kind of method for preparing above-mentioned composite conducting particle is characterized in that the concrete steps of this method are following:
A. epoxy resin and amine curing agent are cured in than scope in the quality of 3.78:1～4.25:1; Epoxy resin after the curing that will obtain is then pulverized grinding, and sieving with 200 purpose sieves afterwards obtains the epoxy powder of alligatoring;
B. step a gained epoxy powder is carried out sensitization and activation processing;
C. prepare 0.06～0.1 mol/L copper-bath, 0.08～0.12 mol/L disodium EDTA solution, 0.2～0.4 mol/L sodium hydroxide solution and 3.8 ~ 4.1 mol/L formalins.Stir down, add copper sulphate, the sodium hydroxide solution of being prepared, and use ammoniacal liquor to regulate the pH value to be 12.5～13.3, to obtain copper plating solution at the medium volume of above-mentioned disodium EDTA solution;
D. stir down, step b gained epoxy resin powder is dispersed in the step c gained copper plating bath, add step c gained formalin, and the mass ratio of control formaldehyde and raw material sulphuric acid copper is: 1:2.5～1:4.5; Stir copper facing 45～60 min under the room temperature, suction filtration and with the distilled water washing for several times obtains copper coating/epoxy resin particle after the drying then;
E. soluble silver salt is soluble in water, it is transparent fully to stir following concentrated ammonia liquor to the solution that dropwise adds, and uses the concentration of distilled water diluting to silver ion to be: 0.02～0.1 mol/L gets silver-colored ammonia activating solution; Under agitation, steps d gained copper facing/epoxy powder is dispersed in the silver-colored ammonia activating solution, adds formalin, wherein the mass ratio of formaldehyde and copper facing/epoxy powder is: 1:1～1:2; Silver-plated 45～60 min of stirring at room, suction filtration and with distilled water washing for several times then obtains the silver-plated epoxy resin composite conducting particle with copper of outer surface after the drying.
The sensitization of above-mentioned epoxy powder and the concrete steps of activation processing are:
A. stannous chloride is dissolved in the concentrated hydrochloric acid, treats that the concentration of its dissolving back thin up to stannous chloride is the sensitizing solution of 0.10～0.20mol/L; The epoxy powder of step a gained alligatoring is immersed in the sensitizing solution, and the room temperature lower magnetic force stirs 30～40 min, suction filtration, and with deionized water rinsing for several times, drying for standby;
B. soluble silver salt is soluble in water, it is transparent fully to stir following concentrated ammonia liquor to the solution that dropwise adds, and uses the concentration of distilled water diluting to silver ion to be: 0.02～0.1 mol/L gets silver-colored ammonia activating solution; Step a gained epoxy powder is immersed in the silver-colored ammonia activating solution, and the room temperature lower magnetic force stirs 30～40 min, suction filtration and with deionized water rinsing for several times after, drying.
Gained composite conducting particle of the present invention has metallic luster, and average conductivity is 139.53 S/cm.
Precious metal chemical complexs such as employing palladiums more than in the traditional chemical plating improve the cost of chemical plating as activator.The present invention adopts the chemical plating method of no-palladium activating; The non-metallic powder epoxy powder is carried out preliminary treatment; Copper facing and silver outside on the insulating epoxy powder surface; Having prepared a kind of is the composite conducting particle of the outer copper facing of nuclear silver with the polymeric matrix, silver-platedly outside in its conductivity of assurance can prevent copper layer generation oxidation.Be that activator is compared with the palladium bichloride in the traditional chemical plating; Composite conducting particle of the present invention is activator with the soluble silver salt; Cost is lower and whole preparation process is easy to operate, and prepared conducting particles conductivity is good, can replace traditional silver powder and copper powder conducting metal filler.The conductive filler cost of this nonmetal system is lower, and functional, can replace traditional silver powder and copper powder conducting metal filler, has more wide application prospect.
Embodiment
The sensitization of epoxy resin and activating treatment method have been used for reference the work in seminar's early stage, Lei Zhihong, the research of novel anisotropy conductiving glue, 2007 (Master's thesis) simultaneously with reference to the surface treatment method of common non-metallic powder
Embodiment one:
1, the preparation of epoxy powder and preliminary treatment
(1) preparation of epoxy powder
Be that 4:1 is cured with the amine curing agent ratio at normal temperatures at first with epoxy resin (E51).Epoxy resin after the curing that will obtain is then pulverized grinding, and sieving with 200 purpose sieves afterwards obtains the epoxy powder of alligatoring.
(2) sensitization
Take by weighing 4.7246 g SnCl
2Be dissolved in the 20 mL concentrated hydrochloric acids, it is subsequent use to treat that its dissolving back thin up to 200 mL is mixed with sensitizing solution.
Epoxy powder 1.2097 g that take by weighing alligatoring add the inferior tin sensitizing solution of 200 mL chlorine in conical flask, and the room temperature lower magnetic force stirs 35 min, suction filtration, and with the deionization flushing for several times, drying for standby.
(3) activation
Take by weighing 1.6421 g silver nitrates and be dissolved in the 10 mL water, it is transparent fully under continue stirring, dropwise to add concentrated ammonia liquor to solution, and with distilled water diluting to 250 mL.
Epoxy powder after the above-mentioned sensitization is added in the 200 mL silver ammonia activating solution, and the room temperature lower magnetic force stirs 35 min, suction filtration and with deionized water rinsing for several times after, drying for standby, it is yellow that dried powder is.
2, electroless copper
(1) preparation of chemical copper plating solution
Accurately take by weighing copper sulphate 4.5011 g, disodium EDTA 10.0003 g, NaOH 3.0011 g, formaldehyde 8 mL, use 20 mL deionized water dissolvings respectively.Then with copper-bath constantly stirring down, join in the complexing agent disodium EDTA solution, again sodium hydroxide solution is added wherein under stirring condition, with ammoniacal liquor adjusting pH value between 12.5～13.3 and to be diluted to 250 mL subsequent use.
(2) electroless copper
Get 200 mL copper plating baths in beaker, under magnetic agitation will on the epoxy powder crossed of joint activation processing add in the beaker, after magnetic agitation 5 min are uniformly dispersed it, add 8 mL reducing agent formalins.Stir copper facing 50 min under the room temperature, suction filtration and with the distilled water washing for several times obtains copper coating/epoxy resin particle after the drying then, and compound particle is kermesinus.
3, chemical silvering
Get 200 mL silver ammino solutions and place beaker; Under magnetic agitation will on copper facing/epoxy powder of obtaining of joint join in the beaker after premix 5 min treat that it is uniformly dispersed, add 8 mL reducing agent formalins, silver-plated 50 min of stirring at room; Suction filtration and for several times then with distilled water washing; Obtain after the drying outer surface silver-plated/copper/epoxy resin composite conducting particle, particle is silver gray, has metallic luster.
Adopting the composite conducting particle of above-mentioned steps preparation to have metallic luster, is 138.89 S/cm through measuring its conductivity.
Embodiment two:
1, the preparation of epoxy powder and preliminary treatment
(1) preparation of epoxy powder
Be that 4:1 is cured with the amine curing agent ratio at normal temperatures at first with epoxy resin (E51).Epoxy resin after the curing that will obtain is then pulverized grinding, and sieving with 200 purpose sieves afterwards obtains the epoxy powder of alligatoring.
(2) sensitization
Take by weighing 4.9126 g SnCl
2Be dissolved in the 20 mL concentrated hydrochloric acids, it is subsequent use to treat that its dissolving back thin up to 200 mL is mixed with sensitizing solution.
Epoxy powder 1.2085 g that take by weighing alligatoring add the inferior tin sensitizing solution of 200 mL chlorine in conical flask, and the room temperature lower magnetic force stirs 30 min, suction filtration, and with the deionization flushing for several times, drying for standby.
(3) activation
Take by weighing 1.7141 g silver nitrates and be dissolved in the 10 mL water, it is transparent fully under continue stirring, dropwise to add concentrated ammonia liquor to solution, and with distilled water diluting to 250 mL.
Epoxy powder after the above-mentioned sensitization is added in the 200 mL silver ammonia activating solution, and the room temperature lower magnetic force stirs 30 min, suction filtration and with deionized water rinsing for several times after, drying for standby, it is yellow that dried powder is.
2, electroless copper
(1) preparation of chemical copper plating solution
Accurately take by weighing copper sulphate 4.5023 g, disodium EDTA 10.0012 g, NaOH 3.0007 g, formaldehyde 8 mL, use 20 mL deionized water dissolvings respectively.Then with copper-bath constantly stirring down, join in the complexing agent disodium EDTA solution, again sodium hydroxide solution is added wherein under stirring condition, with ammoniacal liquor adjusting pH value between 12.5～13.3 and to be diluted to 250 mL subsequent use.
(2) electroless copper
Get 200 mL copper plating baths in beaker, under magnetic agitation will on the epoxy powder crossed of joint activation processing add in the beaker, after magnetic agitation 5 min are uniformly dispersed it, add 8 mL reducing agent formalins.Stir copper facing 55 min under the room temperature, suction filtration and with the distilled water washing for several times obtains copper coating/epoxy resin particle after the drying then, and compound particle is kermesinus.
3, chemical silvering
Get 200 mL silver ammino solutions and place beaker; Under magnetic agitation will on copper facing/epoxy powder of obtaining of joint join in the beaker after premix 5 min treat that it is uniformly dispersed, add 6 mL reducing agent formalins, silver-plated 55 min of stirring at room; Suction filtration and for several times then with distilled water washing; Obtain after the drying outer surface silver-plated/copper/epoxy resin composite conducting particle, particle is silver gray, has metallic luster.
Adopting the composite conducting particle of above-mentioned steps preparation to have metallic luster, is 156.25 S/cm through measuring its conductivity.
Embodiment three:
1, the preparation of epoxy powder and preliminary treatment
(1) preparation of epoxy powder
Be that 4:1 is cured with the amine curing agent ratio at normal temperatures at first with epoxy resin (E51).Epoxy resin after the curing that will obtain is then pulverized grinding, and sieving with 200 purpose sieves afterwards obtains the epoxy powder of alligatoring.
(2) sensitization
Take by weighing 5.4146 g SnCl
2Be dissolved in the 20 mL concentrated hydrochloric acids, it is subsequent use to treat that its dissolving back thin up to 200 mL is mixed with sensitizing solution.
Epoxy powder 1.2034 g that take by weighing alligatoring add the inferior tin sensitizing solution of 200 mL chlorine in conical flask, and the room temperature lower magnetic force stirs 30 min, suction filtration, and with the deionization flushing for several times, drying for standby.
(3) activation
Take by weighing 1.8021 g silver nitrates and be dissolved in the 10 mL water, it is transparent fully under continue stirring, dropwise to add concentrated ammonia liquor to solution, and with distilled water diluting to 250 mL.
Epoxy powder after the above-mentioned sensitization is added in the 200 mL silver ammonia activating solution, and the room temperature lower magnetic force stirs 30 min, suction filtration and with deionized water rinsing for several times after, drying for standby, it is yellow that dried powder is.
2, electroless copper
(1) preparation of chemical copper plating solution
Accurately take by weighing copper sulphate 4.5008 g, disodium EDTA 10.0023 g, NaOH 3.0001 g, formaldehyde 8 mL, use 20 mL deionized water dissolvings respectively.Then with copper-bath constantly stirring down, join in the complexing agent disodium EDTA solution, again sodium hydroxide solution is added wherein under stirring condition, with ammoniacal liquor adjusting pH value between 12.5～13.3 and to be diluted to 250 mL subsequent use.
(2) electroless copper
Get 200 mL copper plating baths in beaker, under magnetic agitation will on the epoxy powder crossed of joint activation processing add in the beaker, after magnetic agitation 5 min are uniformly dispersed it, add 8 mL reducing agent formalins.Stir copper facing 55 min under the room temperature, suction filtration and with the distilled water washing for several times obtains copper coating/epoxy resin particle after the drying then, and compound particle is kermesinus.
3, chemical silvering
Get 200 mL silver ammino solutions and place beaker; Under magnetic agitation will on copper facing/epoxy powder of obtaining of joint join in the beaker after premix 5 min treat that it is uniformly dispersed, add 7 mL reducing agent formalins, silver-plated 55 min of stirring at room; Suction filtration and for several times then with distilled water washing; Obtain after the drying outer surface silver-plated/copper/epoxy resin composite conducting particle, particle is silver gray, has metallic luster.
Adopting the composite conducting particle of above-mentioned steps preparation to have metallic luster, is 123.46 S/cm through measuring its conductivity.
Claims (3)
1. a composite conducting particle is characterized in that this conducting particles is matrix with epoxy resin, and with copper and silver, wherein the quality of copper is 24.0%～44.1% of a substrate quality in the plating of the skin of this matrix; The quality of silver is 36.3% ~ 56.4% of a substrate quality.
2. method for preparing composite conducting particle according to claim 1 is characterized in that the concrete steps of this method are following:
A. epoxy resin and amine curing agent are cured in than scope in the quality of 3.78:1～4.25:1; Epoxy resin after the curing that will obtain is then pulverized grinding, and sieving with 200 purpose sieves afterwards obtains the epoxy powder of alligatoring;
B. step a gained epoxy powder is carried out sensitization and activation processing;
C. prepare 0.06～0.1 mol/L copper-bath, 0.08～0.12 mol/L disodium EDTA solution, 0.2～0.4 mol/L sodium hydroxide solution and 3.8 ~ 4.1 mol/L formalins; Stir down, add copper sulphate, the sodium hydroxide solution of being prepared, and use ammoniacal liquor to regulate the pH value to be 12.5～13.3, to obtain copper plating solution at the medium volume of above-mentioned disodium EDTA solution;
D. stir down, step b gained epoxy resin powder is dispersed in the step c gained copper plating bath, add step c gained formalin, and the mass ratio of control formaldehyde and raw material sulphuric acid copper is: 1:2.5～1:4.5; Stir copper facing 45～60 min under the room temperature, suction filtration and with the distilled water washing for several times obtains copper coating/epoxy resin particle after the drying then;
E. soluble silver salt is soluble in water, it is transparent fully to stir following concentrated ammonia liquor to the solution that dropwise adds, and uses the concentration of distilled water diluting to silver ion to be: 0.02～0.1 mol/L gets silver-colored ammonia activating solution; Under agitation, steps d gained copper facing/epoxy powder is dispersed in the silver-colored ammonia activating solution, adds formalin, wherein the mass ratio of formaldehyde and copper facing/epoxy powder is: 1:1～1:2; Silver-plated 45～60 min of stirring at room, suction filtration and with distilled water washing for several times then obtains the silver-plated epoxy resin composite conducting particle with copper of outer surface after the drying.
3. according to the preparation method of the said composite conducting particle of claim 2, it is characterized in that the sensitization of described epoxy powder and the concrete steps of activation processing are:
A. stannous chloride is dissolved in the concentrated hydrochloric acid, treats that the concentration of its dissolving back thin up to stannous chloride is the sensitizing solution of 0.10～0.20mol/L; The epoxy powder of step a gained alligatoring is immersed in the sensitizing solution, and the room temperature lower magnetic force stirs 30～40 min, suction filtration, and with deionized water rinsing for several times, drying for standby;
B. soluble silver salt is soluble in water, it is transparent fully to stir following concentrated ammonia liquor to the solution that dropwise adds, and uses the concentration of distilled water diluting to silver ion to be: 0.02～0.1 mol/L gets silver-colored ammonia activating solution; Step a gained epoxy powder is immersed in the silver-colored ammonia activating solution, and the room temperature lower magnetic force stirs 30～40 min, suction filtration and with deionized water rinsing for several times after, drying.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103668131A (en) * | 2013-12-16 | 2014-03-26 | 天诺光电材料股份有限公司 | Silver-plated graphite and production technology thereof |
| CN103695978A (en) * | 2013-12-16 | 2014-04-02 | 天诺光电材料股份有限公司 | Nickel-plated graphite and preparation method thereof |
| CN104098277A (en) * | 2014-07-14 | 2014-10-15 | 上海奇微新材料科技有限公司 | Method for copperizing and silvering on surface of glass bead, and copperized and silvered glass bead |
| CN104152882A (en) * | 2014-07-17 | 2014-11-19 | 广东致卓精密金属科技有限公司 | Preparation method of chemically-silvered active carbon as composite conductive filler |
| CN105063798A (en) * | 2015-08-25 | 2015-11-18 | 无锡市长安曙光手套厂 | Conductive fabric |
| CN105172286A (en) * | 2015-08-25 | 2015-12-23 | 无锡市长安曙光手套厂 | High temperature resistant electro-conductive fabric |
| CN105965010A (en) * | 2016-05-23 | 2016-09-28 | 济南大学 | Preparation method for silver-plating copper powder |
| CN107573647A (en) * | 2017-10-18 | 2018-01-12 | 常州中翔科技有限公司 | A kind of preparation method of conductive nano composite material |
| CN107699179A (en) * | 2017-11-17 | 2018-02-16 | 苏州锐特捷化工制品有限公司 | A kind of high heat-conductivity conducting environment-protective adhesive and preparation method thereof |
| CN109137011A (en) * | 2018-09-20 | 2019-01-04 | 吕莉 | A kind of preparation method of high voltage isolator contact material |
| CN110467863A (en) * | 2019-08-16 | 2019-11-19 | 广东华祐新材料有限公司 | Conductive coating, plating solution, PCB circuit board and PCB circuit board production method |
| CN114605894A (en) * | 2022-04-11 | 2022-06-10 | 西安热工研究院有限公司 | Based on AgNWs/Ti3AlC2Corrosion-resistant coating of conductive filler and preparation method thereof |
| GR1010610B (en) * | 2022-12-16 | 2024-01-23 | Εθνικο Μετσοβιο Πολυτεχνειο, | Hybrid thermosetting microbeads having deposited silver nanoparticles |
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| CN103695978A (en) * | 2013-12-16 | 2014-04-02 | 天诺光电材料股份有限公司 | Nickel-plated graphite and preparation method thereof |
| CN103668131B (en) * | 2013-12-16 | 2015-12-09 | 天诺光电材料股份有限公司 | A kind of silvering graphite and production technique thereof |
| CN103695978B (en) * | 2013-12-16 | 2016-04-27 | 天诺光电材料股份有限公司 | A kind of Ni-coated graphite and preparation method thereof |
| CN103668131A (en) * | 2013-12-16 | 2014-03-26 | 天诺光电材料股份有限公司 | Silver-plated graphite and production technology thereof |
| CN104098277B (en) * | 2014-07-14 | 2017-02-15 | 上海奇微新材料科技有限公司 | Method for copperizing and silvering on surface of glass bead, and copperized and silvered glass bead |
| CN104098277A (en) * | 2014-07-14 | 2014-10-15 | 上海奇微新材料科技有限公司 | Method for copperizing and silvering on surface of glass bead, and copperized and silvered glass bead |
| CN104152882A (en) * | 2014-07-17 | 2014-11-19 | 广东致卓精密金属科技有限公司 | Preparation method of chemically-silvered active carbon as composite conductive filler |
| CN104152882B (en) * | 2014-07-17 | 2017-02-01 | 广东致卓精密金属科技有限公司 | Preparation method of chemically-silvered active carbon as composite conductive filler |
| CN105063798A (en) * | 2015-08-25 | 2015-11-18 | 无锡市长安曙光手套厂 | Conductive fabric |
| CN105172286A (en) * | 2015-08-25 | 2015-12-23 | 无锡市长安曙光手套厂 | High temperature resistant electro-conductive fabric |
| CN105965010A (en) * | 2016-05-23 | 2016-09-28 | 济南大学 | Preparation method for silver-plating copper powder |
| CN107573647A (en) * | 2017-10-18 | 2018-01-12 | 常州中翔科技有限公司 | A kind of preparation method of conductive nano composite material |
| CN107699179A (en) * | 2017-11-17 | 2018-02-16 | 苏州锐特捷化工制品有限公司 | A kind of high heat-conductivity conducting environment-protective adhesive and preparation method thereof |
| CN109137011A (en) * | 2018-09-20 | 2019-01-04 | 吕莉 | A kind of preparation method of high voltage isolator contact material |
| CN110467863A (en) * | 2019-08-16 | 2019-11-19 | 广东华祐新材料有限公司 | Conductive coating, plating solution, PCB circuit board and PCB circuit board production method |
| CN114605894A (en) * | 2022-04-11 | 2022-06-10 | 西安热工研究院有限公司 | Based on AgNWs/Ti3AlC2Corrosion-resistant coating of conductive filler and preparation method thereof |
| GR1010610B (en) * | 2022-12-16 | 2024-01-23 | Εθνικο Μετσοβιο Πολυτεχνειο, | Hybrid thermosetting microbeads having deposited silver nanoparticles |
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Application publication date: 20120125 |