CN102328076A - Preparation method of silver coated copper powder for electronic slurry - Google Patents
Preparation method of silver coated copper powder for electronic slurry Download PDFInfo
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- CN102328076A CN102328076A CN201110165977A CN201110165977A CN102328076A CN 102328076 A CN102328076 A CN 102328076A CN 201110165977 A CN201110165977 A CN 201110165977A CN 201110165977 A CN201110165977 A CN 201110165977A CN 102328076 A CN102328076 A CN 102328076A
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Abstract
The invention provides a preparation method of silver coated copper powder for electronic slurry, which comprises the following operation steps of: (1) adding a certain mass of copper powder raw materials into a reaction container, adding acid solution, carrying out ultrasonic stirring for 5 to 15 min, filtering materials, and collecting filter residue; (2) weighing a proper amount of complexing agents, adding the complexing agents into deionized water, then, adding copper powder after acid washing, carrying out stirring dispersion, and obtaining reducing liquid; (3) weighing a proper amount of silver nitrate, adding the silver nitrate into the deionized water, adding ammonia water, stirring the solution until the solution is transparent, and obtaining silver-ammonia solution; (4) adding the silver-ammonia solution into the reducing liquid for taking reaction under the dispersion stirring of an ultrasonic dispersing device; and (5) filtering the solution after the reaction, washing the filter residue by the deionized water and/or absolute ethyl alcohol, carrying out vacuum drying, and obtaining the product of the silver coated copper powder for the electronic slurry. The preparation method has the advantages that the raw material ingredients are simple, the technical steps are simple, the preparation method can be used for large-scale production, and in addition, a silver layer can not be deposited on the surface of the reaction container.
Description
Technical field
The present invention relates to the metal-powder technical field, be specifically related to the preparation method of a kind of electric slurry with silver-coated copper powder.
Background technology
Along with the mankind march toward informationized society at a quick pace; Processes such as the miniaturization of various electronic components, chip type, multiple stratification are accelerated day by day, to being that the demand of electric slurry (electrically-conducting paint, conducting resinl) of major function phase is also more and more with metal dusts such as silver, gold, nickel, copper.Electric slurry is as the electrode of resistance, electric capacity, inductance etc., and all is widely used at the aspects such as curtain coating of anti-electromagnetic interference.Super fine silver powder is a kind of electrically-conducting paint commonly used and the main component of electrocondution slurry, and it has high conductivity (ρ v=1.62 * 10
-6Ω CM), high antioxidant and high-ductility; Be to be used for conductive filler in all metals the earliest; US military just is used as electromagnetic shielding material with it as far back as the sixties in 20th century, but silver migration very easily takes place under wet heat condition or under the DC voltage effect and causes short circuit, and costs an arm and a leg; So the application of silver powder in electrically-conducting paint at present is not a lot, only in special special coatings such as military field, uses.The electric conductivity of copper (ρ v=1.70 * 10
-6Ω CM) be only second to silver, and anti-transfer ability is superior to silver greatly, and originate wide, cheap (only be silver 1/20th); But because copper is very active; Superfine cupper powder is difficult to stable existence, and phenomenons such as gathering, oxidation are serious, are not suitable for directly being used for the electrically-conducting paint application.In order to give full play to the high conductivity and the non-oxidizability of silver; And advantage such as low cost of copper, satisfactory electrical conductivity; Coat one deck silver on the copper powder surface, make it to become the composite conducting function phase of electric slurry, this silver-coated copper powder has high performance price ratio; Can reach the saving noble metal, the purpose of protection environment.
Metal, nonmetallic surface chemistry coating technology are very ripe, and the chemical silvering on copper powder surface also has report.
Application number is that 200610089631 Chinese invention patent " the silver-plated method of a kind of copper powder surface chemistry " discloses and a kind ofly prepares the method that silver coats copper powder with displacement reaction; With being made into a certain proportion of reducing solution in dispersant, the stabilizing agent adding copper powder solution, chemical plating is carried out in the silver ammino solution adding that then ammoniacal liquor, silver nitrate, NaOH proportioning is become.
Application number is the preparation method that 02139151.3 Chinese invention patent " a kind of silver-plated copper powder and preparation method thereof " discloses a kind of silver-colored copper facing powder, adopts aminated compounds that silver nitrate is carried out complexing, and need carry out chemical plating at a certain temperature.
Application number is the method that 200410037056.0 Chinese invention patent " a kind of preparation method of silver-plated copper powder " discloses a kind of silver-plated copper powder, huge legendary turtle is closed extractant mix with silver ammino solution, adds copper powder and under 40～90 ℃ of conditions, carries out electroless copper.
Application number is the method that 200810020025.2 Chinese invention patent " method of a kind of chemical silvering copper powder and chemical plating fluid and chemical plating " discloses a kind of chemical silvering copper powder and chemical plating fluid and chemical plating, silver nitrate aqueous solution, formaldehyde ethanolic solution and rare earth nitrades (cerium, lanthanum, the yttrium class salt) aqueous solution is added successively carry out chemical plating.
The above-mentioned silver-plated method of copper powder surface chemistry of carrying out; The shortcoming that exists is that raw material components is complicated, processing step is complicated; And the reagent such as the silver cyanide that have are poisonous, some also need carry out chemical plating etc. being higher than under the condition of room temperature; And in the plating process, the reaction vessel inwall deposits silver layer easily and causes silver-colored waste.
Summary of the invention
Technical problem to be solved by this invention is the deficiency that overcomes above prior art; Provide that a kind of raw material components is simple, processing step is simple, can be used for the preparation method of the electric slurry of large-scale production with silver-coated copper powder, and this preparation method can be at reaction vessel surface deposition silver layer.
The technical scheme that the present invention adopted is:
A kind of electric slurry has following operating procedure with the preparation method of silver-coated copper powder:
(1) in reaction vessel, adds the copper powder raw material (copper powder raw material particle size scope is at 0.5～30 micron, that pattern can be is spherical, sheet or near-spherical) of certain mass; Add mass concentration then and be 3%～10% acid solution, the acid solution volume is 3～20 times of copper powder raw material weight, ultrasonic agitation 5～15min; Purpose is to carry out the acid of copper powder raw material is cleaned, and to remove the oxide on copper powder raw material surface, filters then; Collect filter residue, filter residue cleaned with distilled water, the copper powder after the pickling;
(2) take by weighing the complexing agent that weight is copper powder raw material weight 65%～150%; Add in the deionized water and form complex liquid; The deionized water volume is 20～60 times of complexing agent weight, add the copper powder after the pickling that step (1) obtains then in the complex liquid and carry out dispersed with stirring, reducing solution;
(3) take by weighing in the silver nitrate adding deionized water that weight is copper powder raw material weight 30%～65%; The deionized water volume is 15～50 times of silver nitrate weight; Add mass concentration then and be 20%～30% ammoniacal liquor; It is in this step in the deionized water 2%～8% of volume that ammoniacal liquor adds volume, and stirring makes solution transparent, obtains silver ammino solution;
(4) be under the ultrasonic disperser dispersion stirring of 0.3～6kW at power; The silver ammino solution that step (3) is obtained joins in the reducing solution that step (2) obtains with the rate of addition of 0.05～1.2L/min and reacts; Reaction temperature is 20～60 ℃, and the reaction time is 30～60min;
(5) step (4) reacted solution is filtered; Collect filter residue; Filter residue is carried out deionized water washing and/or absolute ethanol washing; Promptly only carry out deionized water washing or only carry out absolute ethanol washing or carry out the deionized water washing after absolute ethanol washing again, 50～80 ℃ of vacuum drying then obtain the product electric slurry and use silver-coated copper powder.
Acid solution is nitric acid or sulfuric acid or formic acid in the said step (1).
Complexing agent is the amine organic matter in the said step (2), further is preferably ethylenediamine tetra-acetic acid (EDTA) or disodium ethylene diamine tetraacetate (EDTA-2Na) or diethylenetriamine or TEPA.
Electric slurry with above-mentioned preparation method obtains is used silver-coated copper powder, and silver-colored weight percent content is 10%～30%, and the weight of copper degree is 70%～90%.
Compared with prior art, the present invention has following remarkable advantage and beneficial effect: electric slurry provided by the invention is with the preparation method of silver-coated copper powder, and its raw material components is simple, processing step is simple, meets the environmental protection needs, is easy to large-scale production; And reducing solution added in the silver ammino solution, can reduce or eliminate the silvering on the reactor vessel wall, cut the waste, silver-colored conversion ratio is high.The silver-coated copper powder resistivity that obtains is less than 2xl0
-4Ω cm; With epoxy resin is matrix, adds the silver-coated copper powder of 60～75% percentage by weights, and the isotropism heat cure conducting resinl resistivity of preparation is less than 6xl0
-4Ω cm has higher oxidation resistance.The silver-coated copper powder that utilizes this method to obtain prepares electric slurry, under the condition that electrical property meets the demands, can reduce the cost of electric slurry.
The specific embodiment
Below in conjunction with embodiment the present invention is made further specific descriptions, but be not limited to this.
Embodiment 1:
Take by weighing 500nm spherical copper powder raw material 10 gram, add in the reaction vessel, add mass concentration then and be 5% nitric acid 200ml; Ultrasonic agitation 5min is to remove the oxide on copper powder raw material surface; Filter to collect filter residue then, filter residue cleaned 3 times with distilled water, the copper powder after the pickling.Take by weighing in EDTA 12 gram addings 400 ml deionized water and form complex liquid, then the copper powder after the pickling is added in this complex liquid, stirring obtains reducing solution.Take by weighing silver nitrate 3 gram and add in 150 ml deionized water, and then to add mass concentration be 3 milliliters of 28% ammoniacal liquor, stir, obtain transparent silver ammino solution.At power is under the ultrasonic disperser of 500W disperse to stir, and silver ammino solution is joined with the rate of addition of 0.05L/min it is reacted, and reaction temperature is 35 ℃, and the reaction time is 30min.Question response after accomplishing filters reaction solution, collects filter residue, and filter residue is carried out deionized water washing 3 times, absolute ethanol washing 2 times, and 50 ℃ of vacuum drying then obtain the product electric slurry and use silver-coated copper powder.Utilize this preparation method to make behind the silver-coated copper powder to not find to deposit silver layer on the reaction vessel surface.
Embodiment 2:
Take by weighing 800nm spherical copper powder raw material 52 gram, add in the reaction vessel, add mass concentration then and be 5% sulfuric acid 200ml; Ultrasonic agitation 10min is to remove the oxide on copper powder raw material surface; Filter to collect filter residue then, filter residue cleaned 3 times with distilled water, the copper powder after the pickling.Take by weighing in EDTA-2Na 74.43 gram addings 2000 ml deionized water and form complex liquid, then the copper powder after the pickling is added in this complex liquid, stirring obtains reducing solution.Take by weighing silver nitrate 31.4 gram and add in 600 ml deionized water, and then to add mass concentration be 42.9 milliliters of 25% ammoniacal liquor, stir, obtain transparent silver ammino solution.At power is under the ultrasonic disperser of 300W disperse to stir, and silver ammino solution is joined with the rate of addition of 0.05L/min it is reacted, and reaction temperature is 40 ℃, and the reaction time is 35min.Question response after accomplishing filters reaction solution, collects filter residue, and filter residue is carried out deionized water washing 3 times, and 60 ℃ of vacuum drying then obtain the product electric slurry and use silver-coated copper powder.Utilize this preparation method to make behind the silver-coated copper powder to not find to deposit silver layer on the reaction vessel surface.
Embodiment 3:
Take by weighing 3um flake copper raw material 100 gram, add in the reaction vessel, add mass concentration then and be 8% formic acid 400ml; Ultrasonic agitation 15min is to remove the oxide on copper powder raw material surface; Filter to collect filter residue then, filter residue cleaned 3 times with distilled water, the copper powder after the pickling.Take by weighing in EDTA 68.89 gram addings 4000 ml deionized water and form complex liquid, then the copper powder after the pickling is added in this complex liquid, stirring obtains reducing solution.Take by weighing silver nitrate 33.05 gram and add in 600 ml deionized water, and then to add mass concentration be 45.1 milliliters of 25% ammoniacal liquor, stir, obtain transparent silver ammino solution.At power is under the ultrasonic disperser of 300W disperse to stir, and silver ammino solution is joined with the rate of addition of 0.06L/min it is reacted, and reaction temperature is 50 ℃, and the reaction time is 45min.Question response after accomplishing filters reaction solution, collects filter residue, and filter residue is carried out alcohol wash 3 times, and 50 ℃ of vacuum drying then obtain the product electric slurry and use silver-coated copper powder.Utilize this preparation method to make behind the silver-coated copper powder to not find to deposit silver layer on the reaction vessel surface.
Above embodiment explains that this electric slurry is not only applicable to the preparation of small scale experiments chamber with the preparation method of silver-coated copper powder, also is applicable to large-scale production.
The raw material that embodiment is used unless otherwise indicated, is common commercially available industrial goods.
The above embodiment of the present invention is can not be used to limit the present invention to explanation of the present invention, and implication suitable with claims of the present invention and any change in the scope all should be thought to be included in the scope of claims.
Claims (4)
1. an electric slurry is characterized in that having following operating procedure with the preparation method of silver-coated copper powder:
(1) in reaction vessel, add the copper powder raw material of certain mass, add mass concentration then and be 3%～10% acid solution; The acid solution volume is 3～20 times of copper powder raw material weight; Ultrasonic agitation 5～15min filters then, collects filter residue; With distilled water filter residue is cleaned, the copper powder after the pickling;
(2) take by weighing the complexing agent that weight is copper powder raw material weight 65%～150%; Add in the deionized water and form complex liquid; The deionized water volume is 20～60 times of complexing agent weight, add the copper powder after the pickling that step (1) obtains then in the complex liquid and carry out dispersed with stirring, reducing solution;
(3) take by weighing in the silver nitrate adding deionized water that weight is copper powder raw material weight 30%～65%; The deionized water volume is 15～50 times of silver nitrate weight; Add mass concentration then and be 20%～30% ammoniacal liquor; It is in this step in the deionized water 2%～8% of volume that ammoniacal liquor adds volume, and stirring makes solution transparent, obtains silver ammino solution;
(4) be under the ultrasonic disperser dispersion stirring of 0.3～6kW at power; The silver ammino solution that step (3) is obtained joins in the reducing solution that step (2) obtains with the rate of addition of 0.05～1.2L/min and reacts; Reaction temperature is 20～60 ℃, and the reaction time is 30～60min;
(5) step (4) reacted solution is filtered, collect filter residue, filter residue is carried out deionized water washing and/or absolute ethanol washing, 50～80 ℃ of vacuum drying then obtain the product electric slurry and use silver-coated copper powder.
2. according to the preparation method of the said electric slurry of claim 1 with silver-coated copper powder, it is characterized in that: acid solution is nitric acid or sulfuric acid or formic acid in the said step (1).
3. according to the preparation method of the said electric slurry of claim 1 with silver-coated copper powder, it is characterized in that: complexing agent is the amine organic matter in the said step (2).
4. according to the preparation method of the said electric slurry of claim 3 with silver-coated copper powder, it is characterized in that: complexing agent is ethylenediamine tetra-acetic acid or disodium ethylene diamine tetraacetate or diethylenetriamine or TEPA in the said step (2).
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Cited By (22)
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| CN102814496A (en) * | 2012-08-14 | 2012-12-12 | 烟台德邦科技有限公司 | Silver-plated copper powder and preparation method thereof |
| CN102950282A (en) * | 2012-10-15 | 2013-03-06 | 宁波广博纳米新材料股份有限公司 | Preparation method of silver-copper coating powder |
| CN102990061A (en) * | 2012-11-07 | 2013-03-27 | 宁波广博纳米新材料股份有限公司 | Preparation method of tightly-combined silver-coated copper powder |
| CN103752842A (en) * | 2013-11-11 | 2014-04-30 | 南京工业大学 | Substitution and chemistry deposition compound preparation method for nano silver coated copper powder |
| CN103785828A (en) * | 2014-02-25 | 2014-05-14 | 朱晓云 | Method for preparing silver-coated copper powder through light induction |
| CN105149575A (en) * | 2015-10-23 | 2015-12-16 | 乐山新天源太阳能科技有限公司 | Preparation method of silver coated copper powder |
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| CN102814496A (en) * | 2012-08-14 | 2012-12-12 | 烟台德邦科技有限公司 | Silver-plated copper powder and preparation method thereof |
| CN102950282A (en) * | 2012-10-15 | 2013-03-06 | 宁波广博纳米新材料股份有限公司 | Preparation method of silver-copper coating powder |
| CN102950282B (en) * | 2012-10-15 | 2015-03-18 | 宁波广博纳米新材料股份有限公司 | Preparation method of silver-copper coating powder |
| CN102990061A (en) * | 2012-11-07 | 2013-03-27 | 宁波广博纳米新材料股份有限公司 | Preparation method of tightly-combined silver-coated copper powder |
| CN102990061B (en) * | 2012-11-07 | 2014-11-12 | 宁波广博纳米新材料股份有限公司 | Preparation method of tightly-combined silver-coated copper powder |
| CN103752842A (en) * | 2013-11-11 | 2014-04-30 | 南京工业大学 | Substitution and chemistry deposition compound preparation method for nano silver coated copper powder |
| CN103785828A (en) * | 2014-02-25 | 2014-05-14 | 朱晓云 | Method for preparing silver-coated copper powder through light induction |
| CN103785828B (en) * | 2014-02-25 | 2015-09-30 | 昆明贵信凯科技有限公司 | The method of silver-coated copper powder is prepared in photoinduction |
| CN106148926B (en) * | 2015-04-23 | 2019-08-02 | 广州北峻工业材料有限公司 | Silver-coated copper powder and preparation method thereof |
| CN105149575A (en) * | 2015-10-23 | 2015-12-16 | 乐山新天源太阳能科技有限公司 | Preparation method of silver coated copper powder |
| CN105567012A (en) * | 2016-03-14 | 2016-05-11 | 宁波江东索雷斯电子科技有限公司 | Preparation method of stable photocuring conductive ink |
| CN105855538A (en) * | 2016-04-08 | 2016-08-17 | 广东工业大学 | Nano silver-coated copper powder and preparation method and application thereof |
| CN107498064A (en) * | 2017-08-14 | 2017-12-22 | 昆明高聚科技有限公司 | A kind of preparation method of high temperature electric slurry ultra-fine copper galactic nucleus shell composite powder |
| CN107740145A (en) * | 2017-10-16 | 2018-02-27 | 广州市天承化工有限公司 | A kind of highly conductive carbon pores liquid of pcb board and its preparation method and application |
| CN108176849A (en) * | 2017-12-12 | 2018-06-19 | 南京邮电大学 | A kind of silver coated copper nano-powder and its preparation method and application |
| CN108080651A (en) * | 2017-12-14 | 2018-05-29 | 湖南兴威新材料有限公司 | The preparation method of electric slurry nanometer silver-coated copper powder |
| CN108941539B (en) * | 2018-06-22 | 2020-09-15 | 深圳市绚图新材科技有限公司 | Preparation method and equipment of silver-coated copper powder with low waste liquid discharge |
| CN108941539A (en) * | 2018-06-22 | 2018-12-07 | 深圳市绚图新材科技有限公司 | A kind of preparation method and equipment of the silver-coated copper powder of low discharging of waste liquid |
| CN109355034A (en) * | 2018-10-24 | 2019-02-19 | 焦作市高森建电子科技有限公司 | A kind of conducting resinl silver-coated copper powder and preparation method thereof |
| CN109570814A (en) * | 2019-01-14 | 2019-04-05 | 哈尔滨理工大学 | A kind of composite solder paste adding micro-nano granules |
| CN111360246A (en) * | 2020-04-24 | 2020-07-03 | 刘勤华 | Silver-coated copper powder with high coating rate and excellent quality and preparation method thereof |
| CN112280512A (en) * | 2020-10-30 | 2021-01-29 | 无锡帝科电子材料股份有限公司 | Preparation method of conductive adhesive for 5G ceramic filter |
| CN112935244A (en) * | 2021-01-27 | 2021-06-11 | 刘勤华 | Silver-coated copper composite powder process for photovoltaic use and replacing pure silver slurry |
| CN113000837A (en) * | 2021-03-10 | 2021-06-22 | 昆明理工大学 | Preparation method of silver-coated copper composite powder with zinc intermediate layer |
| CN113000837B (en) * | 2021-03-10 | 2022-11-18 | 昆明理工大学 | Preparation method of silver-coated copper composite powder with zinc intermediate layer |
| CN115475937A (en) * | 2021-05-28 | 2022-12-16 | 季华实验室 | Method for rapidly coating silver shell on copper particles |
| CN116197396A (en) * | 2023-02-09 | 2023-06-02 | 苏州星翰新材料科技有限公司 | Preparation method of submicron silver-coated copper powder |
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Application publication date: 20120125 |