CN102990061B - Preparation method of tightly-combined silver-coated copper powder - Google Patents
Preparation method of tightly-combined silver-coated copper powder Download PDFInfo
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- CN102990061B CN102990061B CN201210440784.0A CN201210440784A CN102990061B CN 102990061 B CN102990061 B CN 102990061B CN 201210440784 A CN201210440784 A CN 201210440784A CN 102990061 B CN102990061 B CN 102990061B
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Abstract
The invention discloses a preparation method of tightly-combined silver-coated copper powder. The preparation method comprises the following steps of: washing off an oxidized layer on the surface of copper powder by using diluted sulfuric acid with the concentration of 3-10%; washing off acid liquid and adding the copper powder into an EDTA (Ethylene Diamine Tetraacetic Acid) disodium solution; agitating and adding a silver ammonia solution; reacting for 5-60 minutes to obtain silver-coated copper powder; mixing and stirring the silver-coated copper powder, a grinding aid and zirconium oxide beads; then, carrying out planet ball grinding; sieving a ball grinding mixture by using a sieve with the size of 100-500 meshes; collecting the sieved silver-coated copper powder; washing and collecting washed-off suspension liquid; standing and settling for 3-6 hours; removing liquid supernatant and centrifuging and separating lower-layer mixing liquid; washing obtained sediment for 3-5 times by using alcohol; and carrying out vacuum drying or blowing drying at the temperature of 40-70 DEG C to obtain the tightly-combined silver coated copper powder. The coated copper powder disclosed by the invention replaces the common silver coated copper powder, and has the advantages of good electric conductivity, tight combination, good anti-oxidization, low cost and tight combination.
Description
Technical field
The present invention relates to a kind of preparation method's technical field of used in electronic industry silver-coated copper powder, be specifically related to a kind of preparation method of compact silver-coated copper powder.
Background technology
Coating mostly made by submicron order metal powder or powder metallurgy uses, and electronics industry is flourish, widen the application of metal dust, some noble metals and base metal powder are the important materials of electronic component, at present in common printed circuit board extensive use be sliver-powder conducting glue, and flake silver powder conducting resinl is capacitor, wave filter, carbon-film potentiometer, the main electrode material of the electronic components such as thin film switch, along with the increase of flake silver powder conducting resinl consumption, in order to reduce costs, electronics industry circle expects to have high-performance, the appearance of conducting resinl of new generation cheaply, silver-coated copper powder conducting resinl is considered to desirable substitute products, but the problem running into is that the surface coating layer deposition of silver-coated copper powder is not fine and close, should there is part exposed at the Copper Powder Surface of internal layer, easily oxidation, and the conjugation of silver-bearing copper is not high, caducous problem in the time of high temperature sintering, result causes the electric conductivity of silver-coated copper powder conducting resinl to be fallen greatly.
Summary of the invention
The present invention is directed to the above-mentioned deficiency of prior art, a kind of good electric conductivity that has is provided, in conjunction with closely, have good non-oxidizability, and the preparation method of the low compact silver-coated copper powder of cost.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is: a kind of preparation method of compact silver-coated copper powder, and concrete steps are as follows:
(1) oxide layer that washes Copper Powder Surface of the diluted acid that is first 3% ~ 10% by mass percent, then removes with deionized water washing the acid solution that remains in Copper Powder Surface, filters the copper powder that must clean up after ionized water; Be added to copper powder as reducing agent in EDETATE SODIUM salting liquid, be made into reducing solution; With silver nitrate and ammoniacal liquor configuration silver ammino solution, in the situation that stirring, silver ammino solution is joined in reducing solution, stirring reaction completes the chemical silvering of Copper Powder Surface after 5 ~ 60 minutes; Isolated by filtration washing, after vacuum drying, obtaining silver-coated copper powder is silver-plated copper powder;
(2) silver-coated copper powder of step (1) gained is mixed with grinding aid and zirconium oxide bead, put into jar, on power-assisted agitator, stir, then airtight jar;
(3) jar is put in planetary ball mill, adjusting planetary ball mill rotating speed is 100 ~ 500 revs/min, after operation 0.5 ~ 1.5h, stops ball milling;
(4) in-tank mixing thing 100 ~ 500 eye mesh screens that stop ball milling being sieved, collect the silver-coated copper powder that is mixed with zirconium pearl after sieving; Clean to wash off the silver-coated copper powder being attached on zirconium pearl with alcohol or acetone, collect the suspension washing down;
(5) by the suspension washing down, staticly settle 3 ~ 6h, remove supernatant, lower floor's mixed liquor is separated with ultracentrifuge, alcohol washing 3 ~ 5 times for gained precipitation, then at 40 ~ 70 DEG C of temperature, vacuum drying or forced air drying, the metal dust (color increases with particle diameter and silver-colored covering amount increases, and color bleaches gradually) that obtains blush or silvery white is the compact silver-coated copper powder of final goal product.
The each component of silver-coated copper powder and percentage by weight thereof that step (1) is described: silver: 15 ~ 50%; Copper 50 ~ 85%.
The described EDETATE SODIUM salt of step (1) is that one or more in ethylenediamine tetra-acetic acid one sodium, disodium ethylene diamine tetraacetate, sodium versenate, tetrasodium ethylenediamine tetraacetate mix.The concentration of EDETATE SODIUM salting liquid is 25 ~ 100g/L.
The described grinding aid of step (2) is that one or more in formaldehyde, ethanol, isopropyl alcohol, stearic acid mix, and the weight proportion of grinding aid and silver-coated copper powder is 1 ~ 5:1.
Described zirconium oxide bead and the silver-coated copper powder size ratio of step (2) is that 50 ~ 600:1, weight ratio are 10 ~ 20:1.Advantage of the present invention and beneficial effect:
The present invention adopts the silver-coated copper powder after grinding to substitute common coated silver-coated copper powder, and it has good electric conductivity, in conjunction with closely, has good non-oxidizability, and low, the compact advantage of cost.
Brief description of the drawings
Fig. 1 is the XRD collection of illustrative plates of the prepared silver-coated copper powder of the embodiment of the present invention 1.
The TGA curve of Fig. 2 copper powder.
Fig. 3 is the TGA curve of the prepared silver-coated copper powder of the embodiment of the present invention 1.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further described:
Embodiment 1
Get particle diameter and be 87 grams of the copper powders of 1.0 microns, add 100 milliliters of 5% spirit of vinegars, remove the oxide of Copper Powder Surface, then, by deionized water washing for copper powder 3 times, filter ionized water.Get 49 grams of silver nitrates and add 1 liter of deionized water, add 80 grams of toluidines, stir, obtaining clear solution is silver ammino solution.Get 80gEDTA mono-sodium, add 2L deionized water, be uniformly mixed EDTA mono-sodium solution obtaining, then the copper powder of above-mentioned processing is added in EDTA mono-sodium solution, after stirring, mix; The silver ammino solution of above-mentioned configuration, join in copper powder EDTA mono-sodium mixed liquor, stirring reaction 45 minutes, isolated by filtration obtains silver-coated copper powder.Gained silver-coated copper powder washed with de-ionized water 3 times after filtering, absolute ethyl alcohol cleans 2 times, filters, and 75 DEG C of vacuum drying obtain silver-plated copper powder.Get 200 grams of the zirconium oxide beads of 300 microns of particle diameters, put into 500 milliliters of plastics jars, add 20 grams of above-mentioned silver-coated copper powders, then add 60 milliliters of isopropyl alcohols, stir after 5 minutes airtight jar with power-assisted agitator.Jar is put into planetary ball mill, rotating speed is 200 revs/min, ball milling 40 minutes, in-tank mixing thing is sieved and obtains being mixed with the flaky silver coated copper powder of zirconium oxide bead with 200 eye mesh screens, clean to wash off the sheet silver-coated copper powder being attached on zirconium pearl with alcohol, the suspension washing down staticly settles after 4h layering, lower floor's mixed liquor is carried out centrifugal with tube centrifuge, the precipitation obtaining is cleaned three times with alcohol, at 60 DEG C, 1h is dried in forced air drying, and the silvery white powder that obtains metallic luster is sheet silver-coated copper powder.
Embodiment 2
Get 98 grams of 5.0um copper powders, add 100 milliliters, 5% watery hydrochloric acid, remove the oxide of Copper Powder Surface, deionized water washing 3 times, filtering water.Get 25 grams of silver nitrates and add 0.5 liter of deionized water, adding concentration is 20 grams of triethylene tetramines, stirs, and obtaining clear solution is silver ammino solution.Get 52gEDTA disodium, add 2L deionized water mixed dissolution to obtain the EDETATE SODIUM solution as reducing solution, then the copper powder of processing is added in EDETATE SODIUM solution, after stirring, mix; The silver ammino solution of above-mentioned configuration, join in copper powder EDETATE SODIUM mixed liquor, stir 30 minutes.Washed with de-ionized water 3 times after filtering, absolute ethyl alcohol cleans 2 times, filters, and 75 DEG C of vacuum drying obtain silver-plated copper powder.Get 200 grams of the zirconium oxide beads of 300 microns, put into 500 milliliters of plastics jars, add 15 grams of above-mentioned silver-coated copper powders, then add 50 milliliters of formaldehyde, stir after 5 minutes airtight jar with power-assisted agitator.Jar is put into planetary ball mill, and rotating speed is 300 revs/min, and ball milling 30 minutes sieves in-tank mixing thing with 150 eye mesh screens, collects the silver-coated copper powder sieving; Clean the silver-coated copper powder of zirconium oxide bead surface adhesion with alcohol, the suspension washing down, staticly settle after 3h, lower floor's mixed liquor is carried out centrifugal with tube centrifuge, the precipitation obtaining is cleaned three times with alcohol, at 50 DEG C, 1h is dried in forced air drying, and the silvery white powder that obtains metallic luster is sheet silver-coated copper powder.
Embodiment 3
Get 71 grams of 0.5um copper powders, add 100 milliliters of 5% phosphoric acid,diluteds, remove the oxide of Copper Powder Surface, deionized water washing 3 times, filtering water.Get 83 grams of silver nitrates and add 1.2 liters of deionized waters, adding concentration is 83 milliliters of 28% ammoniacal liquor, stirs, and obtaining clear solution is silver ammino solution.Get 200gEDTA trisodium, add 2L deionized water dissolving to be configured to EDTA tri-sodium solutions, then the copper powder of processing is added in EDTA tri-sodium solutions, after stirring, mix; The silver ammino solution of above-mentioned configuration, join in copper powder EDTA trisodium mixed liquor, stir 60 minutes.Washed with de-ionized water 3 times after filtering, absolute ethyl alcohol cleans 2 times, filters, and 75 DEG C of vacuum drying obtain silver-plated copper powder.Get 300 grams, the zirconium pearl of 200 microns, put into 800 milliliters of plastics jars, add 25 grams of above-mentioned silver-coated copper powders, then add 80 milliliters of stearic acid alcoholic solutions, stir after 10 minutes airtight jar with power-assisted agitator.Jar is put into planetary ball mill, and rotating speed is 150 revs/min, and ball milling 60 minutes sieves in-tank mixing thing with 300 eye mesh screens, collects the silver-coated copper powder sieving; Clean the sheet silver-coated copper powder of zirconium surface adhesion with alcohol, the suspension washing down, staticly settle after 5h, lower floor's mixed liquor is carried out centrifugal with tube centrifuge, the precipitation obtaining is cleaned three times with alcohol, at 40 DEG C, 2h is dried in vacuum drying, and the silvery white powder that obtains metallic luster is sheet silver-coated copper powder.
Embodiment 4
Get 98 grams of 1.0um copper powders, add 100 milliliters of 5% dilute sulfuric acids, remove the oxide of Copper Powder Surface, deionized water washing 3 times, filtering water.Get 25 grams of silver nitrates and add 0.5 liter of deionized water, add 16 grams of triethylene triamines, stir, obtaining clear solution is silver ammino solution.Get 80gEDTA tetra-sodium, add 2L deionized water mixed dissolution to be configured to EDTA tetra-sodium solutions, then the copper powder of processing is added in EDTA tetra-sodium solutions, after stirring, mix; The silver ammino solution of above-mentioned configuration, join in copper powder EDTA tetra-sodium mixed liquors, stir 30 minutes.Washed with de-ionized water 3 times after filtering, absolute ethyl alcohol cleans 2 times, filters, and 75 DEG C of vacuum drying obtain silver-plated copper powder.Get 200 grams, the zirconium pearl of 300 microns, put into 500 milliliters of plastics jars, add 20 grams of above-mentioned silver-coated copper powders, then add 60 milliliters of isopropyl alcohols, stir after 5 minutes airtight jar with power-assisted agitator.Jar is put into planetary ball mill, and rotating speed is 200 revs/min, and ball milling 30 minutes sieves in-tank mixing thing with 200 eye mesh screens, collects the silver-coated copper powder sieving; Clean the sheet silver-coated copper powder of zirconium surface adhesion with alcohol, the suspension washing down, staticly settle after 4h, lower floor's mixed liquor is carried out centrifugal with tube centrifuge, the precipitation obtaining is cleaned three times with alcohol, at 50 DEG C, 1.5h is dried in vacuum drying, and the metal dust slightly redly that obtains metallic luster is sheet silver-coated copper powder.
Embodiment 1 gained flaky silver coated copper powder is detected, as described below:
The XRD curve of Fig. 1 embodiment 1 silver-coated copper powder: as can be seen from the figure, powder is silver and two kinds of element compositions of copper, non-oxidation copper or cuprous oxide, prove powder top layer be not oxidized (be silver-coated copper powder outer surface without copper expose, copper and silver is in conjunction with closely), silver layer is evenly coated on copper core top layer.
Fig. 2 raw material copper powder TGA curve (non-oxidizability sign), Fig. 3 embodiment 1 gained flaky silver coated copper powder TGA curve: can find out from above two figure, the initial oxidation temperature of copper powder is at 238 degree, and the initial oxidation temperature of silver-coated copper powder is at 390 degree, prove that prepared silver-coated copper powder has excellent non-oxidizability.
Claims (5)
1. the preparation method of a compact silver-coated copper powder, it is characterized in that: silver ammino solution is joined in the reducing solution that contains copper powder, obtain silver-plated copper powder, this silver-plated copper powder is ground, is dried, obtain the compact silver-plated copper powder of silver-bearing copper layer, concrete preparation process comprises:
(1) first wash the oxide layer of Copper Powder Surface with the diluted acid that mass percent is 3% ~ 10%, then remove with deionized water washing the acid solution that remains in Copper Powder Surface, filter the copper powder that must clean up after ionized water; Be added to copper powder as reducing agent in EDETATE SODIUM salting liquid, be made into reducing solution; With silver nitrate and ammoniacal liquor configuration silver ammino solution, in the situation that stirring, silver ammino solution is joined in reducing solution, stirring reaction completes the chemical silvering of Copper Powder Surface after 5 ~ 60 minutes; Isolated by filtration washing, after vacuum drying, obtaining silver-coated copper powder is silver-plated copper powder;
(2) silver-coated copper powder of step (1) gained is mixed with grinding aid and zirconium oxide bead, put into jar, on power-assisted agitator, stir, then airtight jar;
(3) the airtight jar of step (2) gained is put in planetary ball mill, adjusting planetary ball mill rotating speed is 100 ~ 500 revs/min, after operation 0.5 ~ 1.5h, stops ball milling;
(4) in-tank mixing thing 100 ~ 500 eye mesh screens that stop ball milling being sieved, collect the silver-coated copper powder that is mixed with zirconium oxide bead after sieving; Clean to wash off the silver-coated copper powder being attached on zirconium oxide bead with alcohol or acetone, collect the suspension washing down;
(5) by the suspension washing down, staticly settle 3 ~ 6h, remove supernatant, lower floor's mixed liquor is separated with ultracentrifuge, and alcohol washing 3 ~ 5 times for gained precipitation, then at 40 ~ 70 DEG C of temperature, vacuum drying or forced air drying, obtain blush or silvery white silver-coated copper powder;
The each component of silver-coated copper powder and percentage by weight thereof that step (1) is described: silver: 15 ~ 50%, copper 50 ~ 85%.
2. according to the preparation method of compact silver-coated copper powder claimed in claim 1, it is characterized in that: the described EDETATE SODIUM salt of step (1) is that one or more in ethylenediamine tetra-acetic acid one sodium, disodium ethylene diamine tetraacetate, sodium versenate, tetrasodium ethylenediamine tetraacetate mix.
3. according to the preparation method of compact silver-coated copper powder claimed in claim 2, it is characterized in that: the concentration of the described EDETATE SODIUM salting liquid of step (1) is 25 ~ 100 g/L.
4. according to the preparation method of compact silver-coated copper powder claimed in claim 1, it is characterized in that: the described grinding aid of step (2) is that one or more in formaldehyde, ethanol, isopropyl alcohol, stearic acid mix, and the weight proportion of the grinding aid described in step (2) and silver-coated copper powder is 1 ~ 5:1.
5. the preparation method of compact silver-coated copper powder according to claim 1, is characterized in that: the zirconium oxide bead described in step (2) and silver-coated copper powder size ratio are 50 ~ 600:1; Weight ratio is 10 ~ 20:1.
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| CN103752842A (en) * | 2013-11-11 | 2014-04-30 | 南京工业大学 | Preparation of nano silver-coated copper powder by replacement and chemical deposition composite method |
| CN103949635B (en) * | 2014-05-13 | 2016-05-11 | 中南大学 | A kind of preparation method of flaky silver coated copper powder |
| CN105355541A (en) * | 2015-10-23 | 2016-02-24 | 乐山新天源太阳能科技有限公司 | Solar cell recycling method |
| 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 |
| 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 |
| CN116060610B (en) * | 2023-03-07 | 2023-10-20 | 东方电气集团科学技术研究院有限公司 | Silver-coated copper powder and preparation method and application thereof |
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| JP5778941B2 (en) * | 2011-02-15 | 2015-09-16 | Ｄｏｗａエレクトロニクス株式会社 | Method for producing silver-coated flake copper powder |
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| CN101905321A (en) * | 2010-08-20 | 2010-12-08 | 中国兵器工业集团第五三研究所 | Preparation method of flake silver-plated copper powder |
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Effective date of registration: 20161028 Address after: 223801 Suqian province high tech Development Zone, Jiangshan Road, No. 23, No. Patentee after: Jiangsu Bo move new materials Limited by Share Ltd Address before: Yinzhou District Shiqi car 315153 Zhejiang city in Ningbo province where extensive science and Technology Park Patentee before: Ningbo Guangbo New Nanomaterials Stock Co.,Ltd. |