CN104001930B - The preparation method of high-temperature electronic slurry lead/galactic nucleus shell composite powder - Google Patents
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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
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000002002 slurry Substances 0.000 title claims abstract description 13
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 53
- 238000007747 plating Methods 0.000 claims abstract description 21
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 238000005516 engineering process Methods 0.000 claims abstract description 8
- 239000000428 dust Substances 0.000 claims abstract description 6
- 230000004913 activation Effects 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims abstract description 5
- 239000000126 substance Substances 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
- 239000000243 solution Substances 0.000 claims description 22
- 229960005070 ascorbic acid Drugs 0.000 claims description 19
- 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
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 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 7
- 239000008139 complexing agent Substances 0.000 claims description 7
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 7
- 229910001379 sodium hypophosphite 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
- 239000012153 distilled water Substances 0.000 claims description 5
- 239000000203 mixture 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
- 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
- 238000001035 drying Methods 0.000 claims description 3
- 239000012530 fluid Substances 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 239000002994 raw material Substances 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
- 238000000034 method Methods 0.000 abstract description 17
- 238000006722 reduction reaction Methods 0.000 abstract description 8
- 239000011246 composite particle Substances 0.000 abstract description 3
- 239000011248 coating agent Substances 0.000 abstract description 2
- 238000000576 coating method Methods 0.000 abstract description 2
- 239000006185 dispersion Substances 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 239000004020 conductor Substances 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 238000005245 sintering 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
- 230000007812 deficiency Effects 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
- 239000002245 particle Substances 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 present invention relates to the preparation method of a kind of high-temperature electronic slurry lead/galactic nucleus shell composite powder, belong to new material technology field.High dispersiveness spherical micron/submicron silver powder is first prepared by chemical reduction method, the silver powder of preparation is dispersed in water, then prepare with certain order the electroless lead plating liquid had good stability by a certain percentage, again silver powder solution is joined in the electroless lead plating solution of stirring, be settled out the lead/silver-colored composite particles of high-tap density, high conductivity and controlled morphology.The present invention first uses chemical preparation micron/submicron silver powder, and behind dust technology activation silver powder surface, the growth of subsequent chemistry lead plating is carried out in silver-colored core surfaces with regard to preferential, and can completely parcel Argent grain, thickness of coating is controlled.
Description
Technical field
The present invention relates to the preparation method of a kind of high-temperature electronic slurry lead/galactic nucleus shell composite powder, 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 the pattern of conducting wire.Then these circuits are dry and roasting is volatilized and is removed liquid organic carrier, then sinters Argent grain.
More intensive and the more accurate electronic circuit of printed wire technical requirement, for meeting these requirements, the width of wire has become narrower, and 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 of semiconductor devices that solar energy can be converted to electric energy, and under the condition of illumination, solar cell can generation current, to be got up by electric collecting and transfer out by grid line and electrode.Front electrode of solar battery and grid line all have conductive silver paste to be made by the technique such as serigraphy, low temperature drying, high temperature sintering of high-speed, high precision.Solar cell front side silver paste mainly contain silver powder, glass dust, additive and organic carrier four part composition.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 surface topography of silver powder simultaneously and improve the tap density of powder.
The many methods being used for manufacturing silver powder at present can be applicable to manufacture silver powder.Such as, can adopt thermal decomposition method, electrochemical process, physical method are as atomization or grinding, and chemical reduction method.Voluminous powder that thermal decomposition method probably produces sponge matter, that reunite, and electrochemical process is produced as the larger powder of crystalline form.General employing physical method prepares 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 liquid-phase reduction method to prepare.Silver powder can adopt chemical reduction method to prepare, and makes the aqueous solution of the soluble-salt of silver and suitable reducing agent react under the condition that can precipitate silver powder 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 of reuniting.Organic reducing agent is alcohols, sugar or aldehydes such as, 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 display of these types is difficult to control sintering, the lack of resolution of wire in thick film conductor circuits.
Therefore, the present invention wishes the preparation method developing a kind 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, high dispersiveness spherical micron/submicron silver powder is first prepared by chemical reduction method in the method, the silver powder of preparation is dispersed in water, then prepare with certain order the electroless lead plating liquid had good stability by a certain percentage, again silver powder solution is joined in the electroless lead plating solution of stirring, 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 high-temperature electronic slurry lead/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: first prepare high dispersiveness spherical micron/submicron silver powder by chemical reduction method, the silver powder of preparation is dispersed in water, then prepare with certain order the electroless lead plating liquid had good stability by a certain percentage, again silver powder solution is joined in the electroless lead plating solution of stirring, 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 after then being cleaned respectively with alcohol and distilled water successively by silver powder;
(2) first prepare sodium hypophosphite solution, then add pyrovinic acid, pyrovinic acid lead, EDTA, complexing agent A, ascorbic acid and thiocarbamide successively, obtained electroless lead plating liquid after fully dissolving;
(3) be 0.03 ~ 0.3mol/L dust technology washing activation step (1) dispersed micron/submicron ball shape silver powder of preparing by concentration, and then this silver powder to be dispersed in concentration be 4 × 10
-6~ 8 × 10
-4in the dispersant PVP of mol/L and PEG-4000 solution, then joined by this mixed solution in the chemical plating fluid in stirring and react 20 ~ 45 minutes, reaction temperature is 40 ~ 95 DEG C, and centrifugation is stand-by; Then use deionized water and alcohol centrifugal deposition and ultrasonic dispersion cycle to clean, remove reaction residue, finally obtain single dispersing lead/galactic nucleus shell composite powder.
In described step (1), the preparation of polymolecularity micron/submicron ball shape silver powder is that first compound concentration is the liquor argenti nitratis ophthalmicus of 0.25 ~ 1.5mol/L, concentration is the ascorbic acid solution of 0.3 ~ 4.5mol/L, then be that 0.01 ~ 0.1:1 gets the raw materials ready according to the mass ratio of dispersant and silver nitrate, dispersant is divided into two parts, add in liquor argenti nitratis ophthalmicus and ascorbic acid solution respectively, be 3 ~ 6 by ammoniacal liquor adjust ph, again liquor argenti nitratis ophthalmicus is poured in ascorbic acid solution, first stir 5 minutes with the speed being less than 50r/min, 15 ~ 25min is stirred again with the speed of 150 ~ 500r/min, centrifugation obtains dispersed micron/submicron ball shape silver powder.
Silver powder cleans 4 times respectively with alcohol and distilled water successively in described step (1), then drying 4 hours under vacuum condition at 50 DEG C.
The concrete composition of described electroless lead plating liquid is 4 ~ 25g/L sodium hypophosphite, 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, often plants after the material added dissolves completely and add lower one again during preparative chemistry plating solution.
The invention has the beneficial effects as follows: the present invention first uses chemical preparation micron/submicron silver powder, behind dust technology activation silver powder surface, the growth of subsequent chemistry lead plating is carried out in silver-colored core surfaces with regard to preferential, and can completely parcel Argent grain, thickness of coating is controlled.Due to the stabilization of dispersant, the nucleocapsid composite powder good dispersion obtained.Silver powder sphere size is homogeneous, determines the dimensional homogeneity of nucleocapsid composite powder.Gained lead of the present invention/galactic nucleus shell composite powder can be used for the conductive phase of high-temperature electronic slurry.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the invention will be further described.
The preparation method of the high-temperature electronic slurry lead/galactic nucleus shell composite powder of embodiment 1 ~ 10 is:
(1) take ascorbic acid as reducing agent, silver nitrate is silver salt, PVP and PEG-4000 are dispersant, first compound concentration is the liquor argenti nitratis ophthalmicus of 0.25 ~ 1.5mol/L, concentration is the ascorbic acid solution of 0.3 ~ 4.5mol/L, then be that 0.01 ~ 0.1:1 gets the raw materials ready according to the mass ratio of dispersant and silver nitrate, dispersant is divided into two parts, add in liquor argenti nitratis ophthalmicus and ascorbic acid solution respectively, be 3 ~ 6 by ammoniacal liquor adjust ph, again liquor argenti nitratis ophthalmicus is poured in ascorbic acid solution, first stir 5 minutes with the speed being less than 50r/min, 15 ~ 25min is stirred again with the speed of 150 ~ 500r/min, centrifugation obtains dispersed micron/submicron ball shape silver powder, then silver powder is cleaned 4 times respectively with alcohol and distilled water successively, then at 50 DEG C under vacuum condition dry 4 hours,
(2) first prepare sodium hypophosphite solution, then add pyrovinic acid, pyrovinic acid lead, EDTA, complexing agent A, ascorbic acid and thiocarbamide successively, obtained electroless lead plating liquid after fully dissolving; The concrete composition of electroless lead plating liquid is 4 ~ 25g/L sodium hypophosphite, 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 ~ 25g/L sodium hypophosphite, 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, often plants after the material added dissolves completely and add lower one again during preparative chemistry plating solution.
(3) be 0.03 ~ 0.3mol/L dust technology washing activation step (1) dispersed micron/submicron ball shape silver powder of preparing by concentration, and then this silver powder to be dispersed in concentration be 4 × 10
-6~ 8 × 10
-4in the dispersant PVP of mol/L and PEG-4000 solution, then joined by this mixed solution in the chemical plating fluid in stirring and react 20 ~ 45 minutes, reaction temperature is 40 ~ 95 DEG C, and centrifugation is stand-by; Then use deionized water and alcohol centrifugal deposition and ultrasonic dispersion cycle to clean, remove reaction residue, obtain single dispersing lead/galactic nucleus shell composite powder.Silver powder sphere size is homogeneous, determines the dimensional homogeneity of nucleocapsid composite powder.
The parameter distribution of table 1 detailed description of the invention 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 that those of ordinary skill in the art possess, various change can also be made under the prerequisite not departing from present inventive concept.
Claims (4)
1. a preparation method for high-temperature electronic slurry lead/galactic nucleus shell composite powder, 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 after then being cleaned respectively with alcohol and distilled water successively by silver powder;
(2) first prepare sodium hypophosphite solution, then add pyrovinic acid, pyrovinic acid lead, EDTA, complexing agent, ascorbic acid and thiocarbamide successively, obtained electroless lead plating liquid after fully dissolving;
(3) be 0.03 ~ 0.3mol/L dust technology washing activation step (1) dispersed micron/submicron ball shape silver powder of preparing by concentration, and then this silver powder to be dispersed in concentration be 4 × 10
-6~ 8 × 10
-4in the dispersant PVP of mol/L and PEG-4000 solution, then joined by this mixed solution in the chemical plating fluid in stirring and react 20 ~ 45 minutes, reaction temperature is 40 ~ 95 DEG C, and centrifugation is stand-by; Then use deionized water and alcohol centrifugal deposition and ultrasonic dispersion cycle to clean, remove reaction residue, finally obtain single dispersing lead/galactic nucleus shell composite powder.
2. the preparation method of high-temperature electronic slurry lead according to claim 1/galactic nucleus shell composite powder, be characterised in that: in described step (1), the preparation of polymolecularity micron/submicron ball shape silver powder is that first compound concentration is the liquor argenti nitratis ophthalmicus of 0.25 ~ 1.5mol/L, concentration is the ascorbic acid solution of 0.3 ~ 4.5mol/L, then be that 0.01 ~ 0.1:1 gets the raw materials ready according to the mass ratio of dispersant and silver nitrate, dispersant is divided into two parts, add in liquor argenti nitratis ophthalmicus and ascorbic acid solution respectively, be 3 ~ 6 by ammoniacal liquor adjust ph, again liquor argenti nitratis ophthalmicus is poured in ascorbic acid solution, first stir 5 minutes with the speed being less than 50r/min, 15 ~ 25min is stirred again with the speed of 150 ~ 500r/min, centrifugation obtains dispersed micron/submicron ball shape silver powder.
3. the preparation method of high-temperature electronic slurry lead according to claim 1/galactic nucleus shell composite powder, is characterized in that: silver powder cleans 4 times respectively with alcohol and distilled water successively in described step (1), then drying 4 hours under vacuum condition at 50 DEG C.
4. the preparation method of high-temperature electronic slurry lead according to claim 1/galactic nucleus shell composite powder, it is characterized in that: the concrete composition of described electroless lead plating liquid is 4 ~ 25g/L sodium hypophosphite, 10 ~ 50g/L pyrovinic acid, 4 ~ 20g/L pyrovinic acid lead, 15 ~ 35g/LEDTA, 5 ~ 20g/L complexing agent, 2 ~ 10g/L ascorbic acid and 10 ~ 80g/L thiocarbamide, often plants after the material added dissolves completely and add lower one again during preparative chemistry plating solution.
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| CN112916851B (en) * | 2021-01-25 | 2023-11-28 | 江苏博迁新材料股份有限公司 | Preparation method of silver-nickel composite powder |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| 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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| 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 |
| 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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Effective date of registration: 20240811 Address after: No. 858 Xihu 1st Road, Xincheng Office Street, Tongguan District, Tongling City, Anhui Province, 244002 Patentee after: Tongling Baoshengyuan New Material Technology Co.,Ltd. Country or region after: China Address before: 650106 No. 1369 Kegao Road, high tech Development Zone, Kunming, Yunnan Patentee before: KUNMING GAOJU TECHNOLOGY CO.,LTD. Country or region before: China |