CN104001930A - Preparing method of lead/silver nuclear shell composite powder for high-temperature electronic paste - Google Patents
Preparing method of lead/silver nuclear shell composite powder for high-temperature electronic paste Download PDFInfo
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- CN104001930A CN104001930A CN201410181549.5A CN201410181549A CN104001930A CN 104001930 A CN104001930 A CN 104001930A CN 201410181549 A CN201410181549 A CN 201410181549A CN 104001930 A CN104001930 A CN 104001930A
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- 239000000843 powder Substances 0.000 title claims abstract description 28
- 239000002131 composite material Substances 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title abstract description 21
- 229910052709 silver Inorganic materials 0.000 title abstract description 5
- 239000004332 silver Substances 0.000 title abstract description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 53
- 238000007747 plating Methods 0.000 claims abstract description 22
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000126 substance Substances 0.000 claims abstract description 10
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims abstract description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 5
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 38
- 229960005070 ascorbic acid Drugs 0.000 claims description 19
- 239000000243 solution Substances 0.000 claims description 19
- 238000002360 preparation method Methods 0.000 claims description 17
- 235000010323 ascorbic acid Nutrition 0.000 claims description 15
- 239000011668 ascorbic acid Substances 0.000 claims description 15
- 239000002253 acid Substances 0.000 claims description 14
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 14
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 14
- 239000002270 dispersing agent Substances 0.000 claims description 13
- 239000002002 slurry Substances 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000008139 complexing agent Substances 0.000 claims description 7
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- 229920001030 Polyethylene Glycol 4000 Polymers 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000012530 fluid Substances 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 5
- 235000000069 L-ascorbic acid Nutrition 0.000 claims description 4
- 239000002211 L-ascorbic acid Substances 0.000 claims description 4
- 230000004913 activation Effects 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- -1 sodium hypophosphites Chemical class 0.000 claims description 4
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 3
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 3
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 230000008021 deposition Effects 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 3
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical group [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 claims description 3
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 150000007513 acids Chemical class 0.000 claims 1
- 238000006722 reduction reaction Methods 0.000 abstract description 9
- 239000002245 particle Substances 0.000 abstract description 4
- 239000011246 composite particle Substances 0.000 abstract description 3
- 230000003213 activating effect Effects 0.000 abstract 1
- 239000006185 dispersion Substances 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 239000004020 conductor Substances 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000001298 alcohols Chemical group 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 150000004675 formic acid derivatives Chemical class 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical compound [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention relates to a preparing method of lead/silver nuclear shell composite powder for high-temperature electronic paste and belongs to the technical field of new materials. Through a chemical reduction method, high-dispersity spherical micron/submicron silver powder is prepared first, the prepared silver powder is dispersed in water, then according to a certain ratio and a certain order, chemical lead plating liquid with good stability is prepared, a silver powder solution is then added into the stirred chemical lead plating liquid, and high-tap-density high-conductivity and controlled-shape lead/silver composite particles are precipitated. According to the preparing method, a chemical reduction method is used first for preparing the micron/submicron silver powder, dilute nitric acid is used for activating a silver powder surface, then following chemical lead plating growing can be carried out on a silver core surface, silver particles can be wrapped completely, and the plating layer thickness can be controlled.
Description
Technical field
The present invention relates to a kind of preparation method of lead/galactic nucleus shell composite powder for high-temperature electronic slurry, belong to new material technology field.
Background technology
Silver powder can be used for electronics industry and manufactures conductor thick film slurry.Thick film ink serigraphy is formed on substrate to the pattern of conducting wire.Then liquid organic carrier is removed in these circuits are dry and roasting volatilization, then silver-colored particle is carried out to sintering.
More intensive and the more accurate electronic circuit of printed wire specification requirement, for meeting these requirements, it is narrower that the width of wire has become, and the spacing between wire is also less.The silver powder that forming intensive closelypacked fine rule road needs must be as far as possible close to the spheroid of the dense packing of single size.Such as solar cell is a kind ofly solar energy can be converted to the semiconductor devices of electric energy, under the condition of illumination, solar cell can generation current, by grid line and electrode, electric collecting is got up and transferred out.Front electrode of solar battery and grid line are all to have the techniques such as the serigraphy of conductive silver paste by high-speed, high precision, low temperature drying, high temperature sintering to make.Solar cell front side silver paste mainly contains silver powder, glass dust, additive and organic carrier four parts and forms.Wherein, the performance of silver powder is particularly important.But silver powder is expensive, if plate the thin lead of one deck at silver powder, so not only can reduce the cost of electric slurry, also can improve the tap density of surface topography and the raising powder of silver powder simultaneously.
The many methods that are used at present manufacturing silver powder can be applicable to manufacture silver powder.For example, can adopt thermal decomposition method, electrochemical process, physical method are as atomization or grinding, and chemical reduction method.Thermal decomposition method probably produces voluminous powder sponge matter, that reunite, and electrochemical process is produced as the larger powder of crystalline form.The general physical method that adopts is prepared sheeting and very large spheric granules.Chemical deposition produces the silver powder of certain size scope and shape.Silver powder for electronic application generally adopts the preparation of liquid-phase reduction method.Silver powder can adopt chemical reduction method preparation, makes the aqueous solution of silver-colored soluble-salt react under the condition that can precipitate silver powder with suitable reducing agent in the method.Inorganic reducing agent comprises hydrazine hydrate, sulphite and formates, and inorganic reducing agent may produce very thick, the in irregular shape powder of granularity, and this powder has large size distribution because reunite.Organic reducing agent is alcohols, sugar or aldehydes for example, and organic reducing can be used from reduction silver nitrate with alkali metal hydroxide one.Reduction reaction rate is very fast; Therefore be difficult to control, the powder of generation is polluted by residual alkali ions.Although the granularity of these powder is very little, the out-of-shape of these powder, broad particle distribution, can not well pile up.The silver powder demonstration of these types is difficult to control sintering, the lack of resolution of wire in thick film conductor circuit.
Therefore, the present invention wishes to develop a kind of preparation method of lead/galactic nucleus shell structure composite powder, and described composite powder can high degree of dispersion, high conductivity and high-tap density.Method of the present invention is a kind of method of reducing, in the method, by chemical reduction method, first prepare high dispersiveness spherical micron/submicron silver powder, the silver powder of preparation is dispersed in water, then prepare with certain order the electroless lead plating liquid having good stability by a certain percentage, silver powder solution is joined in the electroless lead plating solution of stirring again, be settled out the lead/silver-colored composite particles of high-tap density, high conductivity and controlled morphology.
Summary of the invention
For overcoming the deficiencies in the prior art, the invention provides the preparation method of lead for high-temperature electronic slurry/galactic nucleus shell composite powder, the composite powder that the method is prepared has the performances such as high degree of dispersion, high conductivity and high-tap density.
Technical scheme of the present invention is: by chemical reduction method, first prepare high dispersiveness spherical micron/submicron silver powder, the silver powder of preparation is dispersed in water, then prepare with certain order the electroless lead plating liquid having good stability by a certain percentage, silver powder solution is joined in the electroless lead plating solution of stirring again, be settled out the lead/silver-colored composite particles of high-tap density, high conductivity and controlled morphology.Concrete preparation process comprises:
(1) take ascorbic acid as reducing agent, silver nitrate is silver salt, and PVP and PEG-4000 are dispersant, prepares polymolecularity micron/submicron ball shape silver powder, dry under vacuum condition after then silver powder being cleaned respectively with alcohol and distilled water successively;
(2) first prepare sodium hypophosphite solution, then add successively pyrovinic acid, pyrovinic acid lead, EDTA, complexing agent A, ascorbic acid and thiocarbamide, after fully dissolving, make electroless lead plating liquid;
(3) by concentration, be dispersed micron/submicron ball shape silver powder prepared by 0.03～0.3 mol/L rare nitric acid washing activation step (1), and then this silver powder is dispersed in to concentration is 4 * 10
-6～8 * 10
-4in the dispersant PVP and PEG-4000 solution of mol/L, then this mixed solution is joined in the chemical plating fluid in stirring and reacted 20～45 minutes, reaction temperature is 40～95 ℃, and centrifugation is stand-by; Then use deionized water and alcohol centrifugal deposition and ultrasonic dispersion wash cycles, remove reaction residue, finally obtain single lead/galactic nucleus shell composite powder that disperses.
In described step (1), the preparation of polymolecularity micron/submicron ball shape silver powder is the liquor argenti nitratis ophthalmicus that first compound concentration is 0.25 ~ 1.5mol/L, concentration is the ascorbic acid solution of 0.3～4.5mol/L, then according to the mass ratio of dispersant and silver nitrate, be that 0.01～0.1:1 gets the raw materials ready, dispersant is divided into two parts, add respectively in liquor argenti nitratis ophthalmicus and ascorbic acid solution, with ammoniacal liquor, regulating pH value is 3～6, again liquor argenti nitratis ophthalmicus is poured in ascorbic acid solution, first to be less than the speed of 50r/min, stir 5 minutes, speed with 150～500r/min stirs 15～25min again, centrifugation obtains dispersed micron/submicron ball shape silver powder.
In described step (1), silver powder cleans respectively 4 times with alcohol and distilled water successively, then at 50 ℃, under vacuum condition, is dried 4 hours.
The concrete composition of described electroless lead plating liquid is 4～25 g/L sodium hypophosphites, 10～50g/L pyrovinic acid, 4～20g/L pyrovinic acid lead, 10～30g/LEDTA, 5～20g/L complexing agent A, 2～10g/L ascorbic acid and 10～80g/L thiocarbamide, and the material that while preparing chemical plating fluid, every kind adds adds lower a kind of again after dissolving completely.
The invention has the beneficial effects as follows: the present invention first uses chemical preparation micron/submicron silver powder, with behind rare nitric acid activation silver powder surface, the growth of subsequent chemistry lead plating is just preferentially carried out in silver-colored core surfaces, and can completely wraps up silver-colored particle, and thickness of coating is controlled.Due to the stabilization of dispersant, the nucleocapsid composite powder good dispersion obtaining.Silver powder sphere size homogeneous, has determined the dimensional homogeneity of nucleocapsid composite powder.Gained lead/galactic nucleus shell composite powder of the present invention can be used for the conductive phase of high-temperature electronic slurry.
The specific embodiment
Below in conjunction with the specific embodiment, the invention will be further described.
The preparation method of lead/galactic nucleus shell composite powder for high-temperature electronic slurry of embodiment 1～10 is:
(1) take ascorbic acid as reducing agent, silver nitrate is silver salt, PVP and PEG-4000 are dispersant, first the liquor argenti nitratis ophthalmicus that compound concentration is 0.25 ~ 1.5mol/L, concentration is the ascorbic acid solution of 0.3～4.5mol/L, then according to the mass ratio of dispersant and silver nitrate, be that 0.01～0.1:1 gets the raw materials ready, dispersant is divided into two parts, add respectively in liquor argenti nitratis ophthalmicus and ascorbic acid solution, with ammoniacal liquor, regulating pH value is 3～6, again liquor argenti nitratis ophthalmicus is poured in ascorbic acid solution, first to be less than the speed of 50r/min, stir 5 minutes, speed with 150～500r/min stirs 15～25min again, centrifugation obtains dispersed micron/submicron ball shape silver powder, then silver powder is cleaned respectively 4 times with alcohol and distilled water successively, then at 50 ℃, under vacuum condition, be dried 4 hours,
(2) first prepare sodium hypophosphite solution, then add successively pyrovinic acid, pyrovinic acid lead, EDTA, complexing agent A, ascorbic acid and thiocarbamide, after fully dissolving, make electroless lead plating liquid; The concrete composition of electroless lead plating liquid is 4～25 g/L sodium hypophosphites, 10～50g/L pyrovinic acid, 4～20g/L pyrovinic acid lead, 10～30g/LEDTA, 5～20g/L complexing agent A, 2～10g/L ascorbic acid and 10～80g/L thiocarbamide, the concrete composition of electroless lead plating liquid is 4～25 g/L sodium hypophosphites, 10～50g/L pyrovinic acid, 4～20g/L pyrovinic acid lead, 10～30g/LEDTA, 5～20g/L complexing agent A, 2～10g/L ascorbic acid and 10～80g/L thiocarbamide, and the material that while preparing chemical plating fluid, every kind adds adds lower a kind of again after dissolving completely.
(3) by concentration, be dispersed micron/submicron ball shape silver powder prepared by the rare nitric acid of 0.03～0.3mol/L washing activation step (1), and then this silver powder is dispersed in to concentration is 4 * 10
-6～8 * 10
-4in the dispersant PVP and PEG-4000 solution of mol/L, then this mixed solution is joined in the chemical plating fluid in stirring and reacted 20～45 minutes, reaction temperature is 40～95 ℃, and centrifugation is stand-by; Then use deionized water and alcohol centrifugal deposition and ultrasonic dispersion wash cycles, remove reaction residue, obtain single lead/galactic nucleus shell composite powder that disperses.Silver powder sphere size homogeneous, has determined the dimensional homogeneity of nucleocapsid composite powder.
The parameter distribution of table 1 specific embodiment 1～10
Above the specific embodiment of the present invention is explained in detail, but the present invention is not limited to above-mentioned embodiment, in the ken possessing those of ordinary skills, can also under the prerequisite that does not depart from aim of the present invention, makes various variations.
Claims (4)
1. a preparation method for lead/galactic nucleus shell composite powder for high-temperature electronic slurry, is characterized in that concrete steps comprise:
(1) take ascorbic acid as reducing agent, silver nitrate is silver salt, and PVP and PEG-4000 are dispersant, prepares polymolecularity micron/submicron ball shape silver powder, dry under vacuum condition after then silver powder being cleaned respectively with alcohol and distilled water successively;
(2) first prepare sodium hypophosphite solution, then add successively pyrovinic acid, pyrovinic acid lead, EDTA, complexing agent A, ascorbic acid and thiocarbamide, after fully dissolving, make electroless lead plating liquid;
(3) by concentration, be dispersed micron/submicron ball shape silver powder prepared by the rare nitric acid of 0.03～0.3mol/L washing activation step (1), and then this silver powder is dispersed in to concentration is 4 * 10
-6～8 * 10
-4in the dispersant PVP and PEG-4000 solution of mol/L, then this mixed solution is joined in the chemical plating fluid in stirring and reacted 20～45 minutes, reaction temperature is 40～95 ℃, and centrifugation is stand-by; Then use deionized water and alcohol centrifugal deposition and ultrasonic dispersion wash cycles, remove reaction residue, finally obtain single lead/galactic nucleus shell composite powder that disperses.
2. the preparation method of lead/galactic nucleus shell composite powder for high-temperature electronic slurry according to claim 1, it is characterized in that: in described step (1), the preparation of polymolecularity micron/submicron ball shape silver powder is the liquor argenti nitratis ophthalmicus that first compound concentration is 0.25 ~ 1.5mol/L, concentration is the ascorbic acid solution of 0.3～4.5mol/L, then according to the mass ratio of dispersant and silver nitrate, be that 0.01～0.1:1 gets the raw materials ready, dispersant is divided into two parts, add respectively in liquor argenti nitratis ophthalmicus and ascorbic acid solution, with ammoniacal liquor, regulating pH value is 3～6, again liquor argenti nitratis ophthalmicus is poured in ascorbic acid solution, first to be less than the speed of 50r/min, stir 5 minutes, speed with 150～500r/min stirs 15～25min again, centrifugation obtains dispersed micron/submicron ball shape silver powder.
3. the preparation method of lead/galactic nucleus shell composite powder for high-temperature electronic slurry according to claim 1, is characterized in that: in described step (1), silver powder cleans respectively 4 times with alcohol and distilled water successively, then at 50 ℃, under vacuum condition, is dried 4 hours.
4. the preparation method of lead/galactic nucleus shell composite powder for high-temperature electronic slurry according to claim 1, it is characterized in that: the concrete composition of described electroless lead plating liquid is 4～25 g/L sodium hypophosphites, 10～50 g/L pyrovinic acids, 4～20 g/L pyrovinic acid lead, 15～35g/LEDTA, 5～20g/L, complexing agent A, 2～10g/L ascorbic acid and 10～80g/L thiocarbamide, and the material that while preparing chemical plating fluid, every kind adds adds lower a kind of again after dissolving completely.
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| CN104001930B CN104001930B (en) | 2016-03-30 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107742696A (en) * | 2017-10-10 | 2018-02-27 | 吉林省凯禹电化学储能技术发展有限公司 | A kind of preparation method for lead charcoal negative pole charcoal based additive |
| CN112916851A (en) * | 2021-01-25 | 2021-06-08 | 江苏博迁新材料股份有限公司 | Preparation method of silver-nickel composite powder |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101716685A (en) * | 2009-12-14 | 2010-06-02 | 昆明理工大学 | Method for preparing spherical superfine silver powder by using chemical reduction method |
| US20110223350A1 (en) * | 2010-03-10 | 2011-09-15 | Industrial Technology Research Institute | Method for producing thermoelectric material |
| CN103506630A (en) * | 2012-06-29 | 2014-01-15 | 中国科学院理化技术研究所 | Preparation method of flaky silver powder with ultralow apparent density |
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2014
- 2014-05-04 CN CN201410181549.5A patent/CN104001930B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101716685A (en) * | 2009-12-14 | 2010-06-02 | 昆明理工大学 | Method for preparing spherical superfine silver powder by using chemical reduction method |
| US20110223350A1 (en) * | 2010-03-10 | 2011-09-15 | Industrial Technology Research Institute | Method for producing thermoelectric material |
| CN103506630A (en) * | 2012-06-29 | 2014-01-15 | 中国科学院理化技术研究所 | Preparation method of flaky silver powder with ultralow apparent density |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107742696A (en) * | 2017-10-10 | 2018-02-27 | 吉林省凯禹电化学储能技术发展有限公司 | A kind of preparation method for lead charcoal negative pole charcoal based additive |
| CN112916851A (en) * | 2021-01-25 | 2021-06-08 | 江苏博迁新材料股份有限公司 | Preparation method of silver-nickel composite powder |
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| CN104001930B (en) | 2016-03-30 |
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