CN102990061A - 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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- CN102990061A CN102990061A CN2012104407840A CN201210440784A CN102990061A CN 102990061 A CN102990061 A CN 102990061A CN 2012104407840 A CN2012104407840 A CN 2012104407840A CN 201210440784 A CN201210440784 A CN 201210440784A CN 102990061 A CN102990061 A CN 102990061A
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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 the submicron order metal powder or powder metallurgy uses, and electronics industry is flourish, widened 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 the 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, increase along with flake silver powder conducting resinl consumption, in order to reduce cost, the expectation of electronics industry circle has high-performance, the cheaply appearance of conducting resinl of new generation, the silver-coated copper powder conducting resinl is considered to desirable substitute products, but the problem that runs into is that the surface coating layer deposition of silver-coated copper powder is not fine and close, should there be at the Copper Powder Surface of internal layer part exposed, easily oxidation, and the conjugation of silver-bearing copper is not high, caducous problem when high temperature sintering, result cause 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, good non-oxidizability is arranged, 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) is first the oxide layer that washes Copper Powder Surface of 3% ~ 10% diluted acid with mass percent, then removes the acid solution that remains in Copper Powder Surface with the deionized water washing, filter the copper powder that must clean up behind the ionized water; Copper powder is added in the EDETATE SODIUM salting liquid as reducing agent, is made into reducing solution; With silver nitrate and ammoniacal liquor configuration silver ammino solution, in situation about stirring, silver ammino solution is joined in the reducing solution, stirring reaction is finished the chemical silvering of Copper Powder Surface after 5 ~ 60 minutes; The isolated by filtration washing, obtaining silver-coated copper powder after the vacuum drying is silver-plated copper powder;
(2) silver-coated copper powder with step (1) gained mixes with grinding aid and zirconium oxide bead, puts into jar, stirs at the power-assisted agitator, then airtight jar;
(3) jar is put in the planetary ball mill, adjusting the planetary ball mill rotating speed is 100 ~ 500 rev/mins, behind operation 0.5 ~ 1.5h, stops ball milling;
The in-tank mixing thing that (4) will stop ball milling sieving with 100 ~ 500 eye mesh screens, collects the silver-coated copper powder that is mixed with the zirconium pearl after sieving; Clean to wash off the silver-coated copper powder that is attached on the zirconium pearl with alcohol or acetone, collect the suspension that washes down;
(5) with the suspension that washes down, staticly settle 3 ~ 6h, remove supernatant, lower floor's mixed liquor is separated with ultracentrifuge, gained precipitation is with alcohol washing 3 ~ 5 times, then under 40 ~ 70 ℃ of temperature, and 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 gets blush or silvery white is the compact silver-coated copper powder of final goal product.
Step (1) each component of described silver-coated copper powder and percentage by weight thereof: silver: 15 ~ 50%; Copper 50 ~ 85%.
The described EDETATE SODIUM salt of step (1) is that in ethylenediamine tetra-acetic acid one sodium, disodium ethylene diamine tetraacetate, sodium versenate, the tetrasodium ethylenediamine tetraacetate one or more mix.The concentration of EDETATE SODIUM salting liquid is 25 ~ 100g/L.
The described grinding aid of step (2) is that in formaldehyde, ethanol, isopropyl alcohol, the stearic acid one or more mix, and the weight proportion of grinding aid and silver-coated copper powder is 1 ~ 5:1.
The described zirconium oxide bead of step (2) and silver-coated copper powder size ratio are 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 the grinding to substitute the silver-coated copper powder of common coating, and it has good electric conductivity, in conjunction with closely, good non-oxidizability is arranged, and low, the compact advantage of cost.
Description of drawings
Fig. 1 is the XRD collection of illustrative plates of the prepared silver-coated copper powder of the embodiment of the 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 invention 1.
The specific embodiment 39
The present invention is further described below in conjunction with specific embodiment:
Embodiment 1
Get particle diameter and be 1.0 microns copper powder 87 grams, add 100 milliliters of 5% spirit of vinegars, remove the oxide of Copper Powder Surface, then with copper powder with deionized water washing 3 times, filter ionized water.Get 49 gram silver nitrates and add 1 liter of deionized water, add toluidines 80 grams, stir, obtaining clear solution is silver ammino solution.Get 80gEDTA one sodium, add the 2L deionized water, mix EDTA one sodium solution that obtains, then the copper powder with above-mentioned processing adds in EDTA one sodium solution, mixes after the stirring; The silver ammino solution of above-mentioned configuration, join in the copper powder EDTA one 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 is 3 times after filtering, and absolute ethyl alcohol cleans 2 times, filters, and 75 ℃ of vacuum drying obtain silver-plated copper powder.Get zirconium oxide bead 200 grams of 300 microns of particle diameters, put into 500 milliliters of plastics jars, add above-mentioned silver-coated copper powder 20 grams, add again 60 milliliters of isopropyl alcohols, use the power-assisted agitator to stir after 5 minutes airtight jar.Jar is put into planetary ball mill, rotating speed is 200 rev/mins, ball milling 40 minutes, the in-tank mixing thing sieved with 200 eye mesh screens obtain being mixed with the flaky silver coated copper powder of zirconium oxide bead, clean to wash off the sheet silver-coated copper powder that is attached on the zirconium pearl with alcohol, after the suspension that washes down staticly settles the 4h layering, carry out lower floor's mixed liquor centrifugal with tube centrifuge, the precipitation that obtains alcohol wash three times, under 60 ℃, forced air drying oven dry 1h, the silvery white powder that obtains metallic luster is the sheet silver-coated copper powder.
Embodiment 2
Get 5.0um copper powder 98 gram, add 100 milliliters in 5% watery hydrochloric acid, remove the oxide of Copper Powder Surface, deionized water washing 3 times, filtering water.Get 25 gram silver nitrates and add 0.5 liter of deionized water, adding concentration is triethylene tetramine 20 grams, stirs, and obtaining clear solution is silver ammino solution.Get the 52gEDTA disodium, adding 2L deionized water mixed dissolution obtains the EDETATE SODIUM solution as reducing solution, and the copper powder that then will process adds in the EDETATE SODIUM solution, mixes after the stirring; The silver ammino solution of above-mentioned configuration, join in the copper powder EDETATE SODIUM mixed liquor, stirred 30 minutes.Washed with de-ionized water is 3 times after filtering, and absolute ethyl alcohol cleans 2 times, filters, and 75 ℃ of vacuum drying obtain silver-plated copper powder.Get 300 microns zirconium oxide bead 200 grams, put into 500 milliliters of plastics jars, add above-mentioned silver-coated copper powder 15 grams, add again 50 milliliters of formaldehyde, use the power-assisted agitator to stir after 5 minutes airtight jar.Jar is put into planetary ball mill, and rotating speed is 300 rev/mins, and ball milling 30 minutes sieves the in-tank mixing thing with 150 eye mesh screens, collects the silver-coated copper powder that sieves; Clean the silver-coated copper powder of zirconium oxide bead surface adhesion with alcohol, the suspension that washes down, after staticly settling 3h, carry out lower floor's mixed liquor centrifugal with tube centrifuge, the precipitation that obtains alcohol wash three times, under 50 ℃, forced air drying oven dry 1h, the silvery white powder that obtains metallic luster is the sheet silver-coated copper powder.
Embodiment 3
Get 0.5um copper powder 71 gram, add 100 milliliters of 5% phosphoric acid,diluteds, remove the oxide of Copper Powder Surface, deionized water washing 3 times, filtering water.Get 83 gram 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 the 200gEDTA trisodium, add the 2L deionized water dissolving and be configured to EDTA three sodium solutions, the copper powder that then will process adds in EDTA three sodium solutions, mixes after the stirring; The silver ammino solution of above-mentioned configuration, join in the copper powder EDTA trisodium mixed liquor, stirred 60 minutes.Washed with de-ionized water is 3 times after filtering, and absolute ethyl alcohol cleans 2 times, filters, and 75 ℃ of vacuum drying obtain silver-plated copper powder.Get 200 microns zirconium pearl 300 grams, put into 800 milliliters of plastics jars, add above-mentioned silver-coated copper powder 25 grams, add again 80 milliliters of stearic acid alcoholic solutions, use the power-assisted agitator to stir after 10 minutes airtight jar.Jar is put into planetary ball mill, and rotating speed is 150 rev/mins, and ball milling 60 minutes sieves the in-tank mixing thing with 300 eye mesh screens, collects the silver-coated copper powder that sieves; Clean the sheet silver-coated copper powder that zirconium surface adheres to alcohol, the suspension that washes down, after staticly settling 5h, carry out lower floor's mixed liquor centrifugal with tube centrifuge, the precipitation that obtains alcohol wash three times, under 40 ℃, vacuum drying oven dry 2h, the silvery white powder that obtains metallic luster is the sheet silver-coated copper powder.
Embodiment 4
Get 1.0um copper powder 98 gram, add 100 milliliters of 5% dilute sulfuric acids, remove the oxide of Copper Powder Surface, deionized water washing 3 times, filtering water.Get 25 gram silver nitrates and add 0.5 liter of deionized water, add triethylene triamine 16 grams, stir, obtaining clear solution is silver ammino solution.Get 80gEDTA four sodium, add 2L deionized water mixed dissolution and be configured to EDTA four sodium solutions, the copper powder that then will process adds in EDTA four sodium solutions, mixes after the stirring; The silver ammino solution of above-mentioned configuration, join in the copper powder EDTA four sodium mixed liquors, stirred 30 minutes.Washed with de-ionized water is 3 times after filtering, and absolute ethyl alcohol cleans 2 times, filters, and 75 ℃ of vacuum drying obtain silver-plated copper powder.Get 300 microns zirconium pearl 200 grams, put into 500 milliliters of plastics jars, add above-mentioned silver-coated copper powder 20 grams, add again 60 milliliters of isopropyl alcohols, use the power-assisted agitator to stir after 5 minutes airtight jar.Jar is put into planetary ball mill, and rotating speed is 200 rev/mins, and ball milling 30 minutes sieves the in-tank mixing thing with 200 eye mesh screens, collects the silver-coated copper powder that sieves; Clean the sheet silver-coated copper powder that zirconium surface adheres to alcohol, the suspension that washes down, after staticly settling 4h, carry out lower floor's mixed liquor centrifugal with tube centrifuge, the precipitation that obtains alcohol wash three times, under 50 ℃, vacuum drying oven dry 1.5h, the slightly redly metal dust that obtains metallic luster is the 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 that silver and two kinds of elements of copper form, non-oxidation copper or cuprous oxide, prove the powder top layer do not have oxidation (be silver-coated copper powder outer surface without copper expose, copper and silver is in conjunction with closely), silver layer evenly is coated on copper nuclear 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 proves that at 390 degree prepared silver-coated copper powder has excellent non-oxidizability.
Claims (7)
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, obtains silver-plated copper powder, with this silver-plated copper powder grind, drying, obtain the compact silver-plated copper powder of silver-bearing copper layer, concrete preparation process comprises:
(1) is first the oxide layer that washes Copper Powder Surface of 3% ~ 10% diluted acid with mass percent, then removes the acid solution that remains in Copper Powder Surface with the deionized water washing, filter the copper powder that must clean up behind the ionized water; Copper powder is added in the EDETATE SODIUM salting liquid as reducing agent, is made into reducing solution; With silver nitrate and ammoniacal liquor configuration silver ammino solution, in situation about stirring, silver ammino solution is joined in the reducing solution, stirring reaction is finished the chemical silvering of Copper Powder Surface after 5 ~ 60 minutes; The isolated by filtration washing, obtaining silver-coated copper powder after the vacuum drying is silver-plated copper powder;
(2) silver-coated copper powder with step (1) gained mixes with grinding aid and zirconium oxide bead, puts into jar, stirs at the power-assisted agitator, then airtight jar;
(3) the airtight jar of step (2) gained is put in the planetary ball mill, adjusting the planetary ball mill rotating speed is 100 ~ 500 rev/mins, behind operation 0.5 ~ 1.5h, stops ball milling;
The in-tank mixing thing that (4) will stop ball milling sieving with 100 ~ 500 eye mesh screens, collects the silver-coated copper powder that is mixed with zirconium oxide bead after sieving; Clean to wash off the silver-coated copper powder that is attached on the zirconium oxide bead with alcohol or acetone, collect the suspension that washes down;
(5) with the suspension that washes down, staticly settle 3 ~ 6h, remove supernatant, lower floor's mixed liquor is separated with ultracentrifuge, and the gained precipitation is with alcohol washing 3 ~ 5 times, then under 40 ~ 70 ℃ of temperature, vacuum drying or forced air drying get blush or silvery white silver-coated copper powder.
2. the preparation method of compact silver-coated copper powder according to claim 1 is characterized in that: step (1) each component of described silver-coated copper powder and percentage by weight thereof: silver: 15 ~ 50%, and copper 50 ~ 85%.
3. 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 in ethylenediamine tetra-acetic acid one sodium, disodium ethylene diamine tetraacetate, sodium versenate, the tetrasodium ethylenediamine tetraacetate one or more mix.
4. according to the preparation method of compact silver-coated copper powder claimed in claim 3, it is characterized in that: the concentration of the described EDETATE SODIUM salting liquid of step (1) is 25 ~ 100g/L.
5. 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 in formaldehyde, ethanol, isopropyl alcohol, the stearic acid one or more mix
6. the preparation method of compact silver-coated copper powder according to claim 5, it is characterized in that: the weight proportion of the grinding aid described in the step (2) and silver-coated copper powder is 1 ~ 5:1.
7. the preparation method of compact silver-coated copper powder according to claim 1, it is characterized in that: the zirconium oxide bead described in the step (2) and silver-coated copper powder size ratio are 50 ~ 600:1; Weight ratio is 10 ~ 20:1.
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| CN103949635A (en) * | 2014-05-13 | 2014-07-30 | 中南大学 | Preparation method for flaky silver coated copper powder |
| 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 |
| 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 |
| 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 |
| CN116060610A (en) * | 2023-03-07 | 2023-05-05 | 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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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN103949635A (en) * | 2014-05-13 | 2014-07-30 | 中南大学 | Preparation method for flaky silver coated copper powder |
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| 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 |
| 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 |
| 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 |
| CN116060610A (en) * | 2023-03-07 | 2023-05-05 | 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 |
| 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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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. |