CN110102778B - Preparation method of low-temperature sintered high-crystallinity silver powder - Google Patents
Preparation method of low-temperature sintered high-crystallinity silver powder Download PDFInfo
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 106
- 238000002360 preparation method Methods 0.000 title claims description 11
- 229910052709 silver Inorganic materials 0.000 claims abstract description 42
- 239000004332 silver Substances 0.000 claims abstract description 42
- 238000000034 method Methods 0.000 claims abstract description 30
- 239000013078 crystal Substances 0.000 claims abstract description 28
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 26
- 239000002245 particle Substances 0.000 claims abstract description 25
- ZNBNBTIDJSKEAM-UHFFFAOYSA-N 4-[7-hydroxy-2-[5-[5-[6-hydroxy-6-(hydroxymethyl)-3,5-dimethyloxan-2-yl]-3-methyloxolan-2-yl]-5-methyloxolan-2-yl]-2,8-dimethyl-1,10-dioxaspiro[4.5]decan-9-yl]-2-methyl-3-propanoyloxypentanoic acid Chemical compound C1C(O)C(C)C(C(C)C(OC(=O)CC)C(C)C(O)=O)OC11OC(C)(C2OC(C)(CC2)C2C(CC(O2)C2C(CC(C)C(O)(CO)O2)C)C)CC1 ZNBNBTIDJSKEAM-UHFFFAOYSA-N 0.000 claims abstract description 21
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 21
- PLKATZNSTYDYJW-UHFFFAOYSA-N azane silver Chemical compound N.[Ag] PLKATZNSTYDYJW-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910000378 hydroxylammonium sulfate Inorganic materials 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 239000002101 nanobubble Substances 0.000 claims abstract description 11
- 238000006722 reduction reaction Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 238000004140 cleaning Methods 0.000 claims abstract description 5
- 239000012295 chemical reaction liquid Substances 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 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 14
- 239000000243 solution Substances 0.000 claims description 14
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 10
- 229910052751 metal Inorganic materials 0.000 claims description 10
- 239000002184 metal Substances 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 10
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 9
- 238000002347 injection Methods 0.000 claims description 8
- 239000007924 injection Substances 0.000 claims description 8
- 229960005070 ascorbic acid Drugs 0.000 claims description 7
- 235000010323 ascorbic acid Nutrition 0.000 claims description 7
- 239000011668 ascorbic acid Substances 0.000 claims description 7
- 230000001590 oxidative effect Effects 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 4
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 3
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 3
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 3
- 239000008103 glucose Substances 0.000 claims description 3
- 239000007800 oxidant agent Substances 0.000 claims description 3
- 240000007594 Oryza sativa Species 0.000 claims 1
- 235000007164 Oryza sativa Nutrition 0.000 claims 1
- 235000009566 rice Nutrition 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 238000000151 deposition Methods 0.000 abstract description 3
- 210000004027 cell Anatomy 0.000 description 18
- 238000005245 sintering Methods 0.000 description 11
- 238000003756 stirring Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 6
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 229910001961 silver nitrate Inorganic materials 0.000 description 3
- 101001073212 Arabidopsis thaliana Peroxidase 33 Proteins 0.000 description 2
- 101001123325 Homo sapiens Peroxisome proliferator-activated receptor gamma coactivator 1-beta Proteins 0.000 description 2
- 102100028961 Peroxisome proliferator-activated receptor gamma coactivator 1-beta Human genes 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000009766 low-temperature sintering Methods 0.000 description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000006479 redox reaction Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000004913 activation Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 210000002858 crystal cell Anatomy 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- -1 dispersibility Chemical compound 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
- B22F2009/245—Reduction reaction in an Ionic Liquid [IL]
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Abstract
The inventionA process for preparing low-temp sintered silver powder with high crystallinity includes such steps as chemical reduction to obtain silver particles from silver-ammonia solution, mixing with hydroxylamine sulfate, and reaction while N is generated2Gas, forming micro-nano bubbles in a solution environment, and depositing silver on the micro-nano bubbles to form nano silver seed crystals with hollow structures; and then, mixing one or more weak reducing agents, injecting the mixture into a reactor, dispersing reaction liquid in the reactor by ultrasonic waves by using an ultrasonic generator to enable silver crystal seeds to independently grow to form silver powder, and finally, centrifugally separating, cleaning and drying to obtain the low-temperature sintered high-crystallinity silver powder. The production process is simple and stable, the production cost is low, large-scale continuous industry is realized, and the method can be widely applied to the production of various high-end conductive silver pastes.
Description
Technical Field
The invention relates to the field of chemistry, in particular to a production technology of silver powder, particularly relates to silver paste for a front electrode of a solar cell, and particularly relates to a preparation method of low-temperature sintered high-crystallinity silver powder.
Background
Silver powder, which is the most important conductive material in the silver conductive paste, is an essential component of the front electrode of the solar cell. With the great demand of high-efficiency solar cells, the solar cells are developing from polycrystalline cells to single-crystal high-efficiency cells, especially the development of PERC high-efficiency single-crystal cells, so that the conversion efficiency of the solar cells is more than 25%, and the high-efficiency single-crystal cells can be expected to dominate the market in the future. With the development of single-crystal high-efficiency solar cells, higher requirements are put forward on the properties of silver powder such as dispersibility, sinterability, crystallinity and particle size distribution. Especially, the PERC high-efficiency single crystal cell has higher requirements on the sintering property and the crystallinity of the silver powder, because the lower the sintering temperature of the silver paste is, the less the PN junction of the solar cell is damaged, and the higher the photoelectric conversion efficiency is. The solid content of the silver powder in the front conductive paste of the solar cell on the market at present is as high as about 90%, and the solid content is low because the sintering activity is low, the sintering temperature is required to be as high as 800-900 ℃ in the sintering process, and the silver powder can not be suitable for the high-efficiency single crystal solar cell. In addition, the higher the crystallinity of the silver powder is, most of the silver powder particles are formed by independent growth of single crystal nucleus, and the tap density of the silver powder is high. When the solar cell conductive silver paste prepared from the high-crystallinity silver powder is sintered, the shrinkage rate of the electrode grid line on the front surface of the solar cell is low, and the internal porosity is small, so that the conductivity and compactness of the electrode grid line are directly determined, and the final grid line resistance and the photoelectric conversion efficiency of a solar cell piece are influenced. The key properties of the conductive paste are determined by the properties of the silver powder.
In order to solve the problems of low-temperature sinterability and high crystallinity of silver powder, the following patents are included: CN 106041123B 'a high-activity hollow silver powder for solar cell front silver and a preparation method thereof', provides a preparation method of the high-activity hollow silver powder for solar cell front silver, and the silver powder prepared by the method has narrow particle size distribution, good sphericity, uniform dispersion, hollow interior and high sintering activity. However, since the silver powder has a microcrystalline structure, the silver powder has low crystallinity. Silver powder is easy to collapse and form pores during sintering, so that the conductivity of the electrode wire is reduced. The patent: CN 101347841B, "preparation method of silver powder with controllable particle size and high tap density", performs redox reaction by pouring method, so that nucleation and growth time of each silver powder particle is kept consistent, and uniformity of particle size is ensured. More importantly, the controllable production of the granularity, the morphology and the tap density of the silver powder is realized, the problem of the crystallinity of the silver powder is well solved, but the silver powder is solid and is similar to the common silver powder, and the sintering temperature is high.
Disclosure of Invention
The invention aims to provide a method for preparing low-temperature sintering high-crystallinity silver powder, which aims to solve the technical problems of high sintering temperature and low crystallinity of the silver powder in the prior art.
The invention provides a preparation method of low-temperature sintering high-crystallinity silver powder, which comprises a process of obtaining metal silver particles from a silver-ammonia solution by using a chemical reduction method in a reactor, wherein in the process of obtaining the metal silver particles from the silver-ammonia solution by using the chemical reduction method, the silver-ammonia solution is used as an oxidant, the silver-ammonia solution is added into the reactor, hydroxylamine sulfate is used as a reducing agent, hydroxylamine sulfate is added into the reactor in a jet flow mode, the hydroxylamine sulfate and the silver-ammonia solution are fully mixed in the reactor, N2 gas generated in the reaction process is used for forming micro-nano bubbles in a solution environment, and silver is deposited on the micro-nano bubbles to form nano silver seed crystals with hollow structures; and then injecting the mixture of one or more weak reducing agents into a reactor, dispersing the reaction liquid in the reactor by using ultrasonic waves by using an ultrasonic generator to independently grow silver crystal seeds to form silver powder, and finally performing centrifugal separation, cleaning and drying to obtain the low-temperature sintered high-crystallinity silver powder.
Furthermore, in the preparation process of the silver seed crystal, the concentration of the strong reducing agent hydroxylamine sulfate is 0.1-3.0 g/L.
Further, the injection speed of the hydroxylamine sulfate into the reactor is less than 100 milliliters per minute.
Further, the weak reducing agent is one or a mixture of more than two of ascorbic acid, glucose, formaldehyde and triethanolamine.
Further, in the process of obtaining the metal silver particles from the silver-ammonia solution by using the chemical reduction method, the reducing solution and the oxidizing solution are respectively injected into the reactor in a constant speed mode.
Further, the injection speed of the weak reducing agent into the reactor is more than 500 milliliters per minute.
Specifically, the finally generated metal silver particles and the residual liquid are conveyed into a centrifuge, the metal silver particles and the residual liquid are separated by the centrifuge to obtain metal silver particles, then the metal silver particles are washed by deionized water until the conductivity is less than 50us, the silver powder is taken out and then is heated and dried by an oven to obtain a finished silver powder product, and the heating and drying temperature is controlled below 70 ℃.
The working principle of the invention is as follows: and (3) synthesizing a hollow micro-nano structure by using bubbles generated in the reaction process as a soft template. The synthesis principle is that gas is generated in the synthesis reaction process, micro-nano bubbles are formed in a solution environment, and target products are deposited on the micro-nano bubbles to form a hollow structure. Firstly, N2 gas is generated during the redox reaction of silver ammonia solution and hydroxylamine sulfate, and the reaction conditions are precisely controlled to realize the control of the growth speed and the size of a silver crystal nucleus, so that the hollow nano silver crystal seed is prepared. Then, one or a plurality of ascorbic acid, glucose or formaldehyde or triethanolamine is/are mixed and used as a weak reducing agent to be injected into the reactor, so that the reaction speed is effectively controlled, and the growth speed of the silver seed crystal is effectively controlled. Meanwhile, the silver seed crystals are prevented from agglomerating by ultrasonic dispersion, and the independent growth of the silver seed crystals is realized. Thereby controlling the growth of silver crystal nucleus and obtaining the silver powder with high crystallinity. The whole process can be divided into two stages of silver seed crystal preparation and silver particle growth, and the size and the shape of the silver particles can be controlled by adjusting reaction conditions;
compared with the prior art, the method effectively solves the problems of mononuclear crystal growth and high sintering activation of the silver powder in the preparation process, and has positive and obvious effect. The method has the advantages of simple feeding reaction mode, good stability of the prepared silver powder, low production cost and realization of large-scale continuous industrial production. The prepared silver powder has a crystal structure, the average particle diameter is 0.8-2.2 um, and the tap density is more than 6.0 g/cm3And can be widely applied to the production of various high-end conductive silver pastes.
Drawings
FIG. 1 is a process flow diagram of a method for preparing a low-temperature sintered high-crystallinity silver powder according to the present invention.
FIG. 2 is a schematic illustration of a reactor in one embodiment of the invention.
The part names are as follows:
1: a stirring paddle; 2: an ultrasonic generator; 3: an ammonia water feeding hole; 4: a hydroxylamine sulfate feed port; 5: a stirring motor; 6: a deionized water feed port; 7: a weak reducing agent feed inlet; 8: a reactor; 9, a centrifugal machine; 10: silver powder;
FIG. 3 is an electron micrograph of silver powder prepared according to one embodiment of the present invention.
Detailed Description
Example 1
As shown in FIG. 1, the present invention provides a method for preparing a low-temperature sintered silver powder having high crystallinity, comprising a process of obtaining metallic silver particles from a silver-ammonia solution in a reactor 8 by a chemical reduction method, in which the metallic silver particles are obtained from the silver-ammonia solution by the chemical reduction methodAdding silver ammonia solution into a reactor 8 by taking the silver ammonia solution as an oxidant, adding hydroxylamine sulfate into the reactor 8 by using hydroxylamine sulfate as a reducing agent in a jet flow mode, fully mixing the hydroxylamine sulfate and the silver ammonia solution in the reactor 8, and utilizing N generated in the reaction process2Gas, forming micro-nano bubbles in a solution environment, and depositing silver on the micro-nano bubbles to form nano silver seed crystals with hollow structures; then one or more weak reducing agents are mixed and injected into a reactor 8, an ultrasonic generator 2 is adopted at the same time, the reaction liquid in the reactor 8 is dispersed by ultrasonic waves to prevent the agglomeration of silver seed crystals and realize the independent growth of the silver seed crystals, silver powder 10 with different particle sizes, different sintering activities and different crystallinities is prepared, finally, the silver powder with high crystallinity is sintered at low temperature through centrifugal separation, cleaning and drying,
further, the concentration of the strong reducing agent hydroxylamine sulfate is 0.13 g/L;
further, the injection rate of hydroxylamine sulfate into the reactor 8 was 37 ml per minute;
further, the weak reducing agent is ascorbic acid;
further, the reducing solution and the oxidizing solution are injected into the reactor 8 in a constant rate manner, respectively;
further, the ascorbic acid was injected into the reactor 8 at a rate of 2.7 liters per minute.
Example 2
As shown in FIG. 2, the present invention provides a method for preparing a low-temperature sintered silver powder with high crystallinity, comprising the following steps:
1) weighing 5Kg of silver nitrate solid, placing the silver nitrate solid in a reactor 8, adding 95L of deionized water through a deionized water feeding hole 6, and then starting a stirring motor 5 to drive a stirring paddle 1 to stir for dissolution at the stirring speed of 60 revolutions per minute. After the dissolution is finished, ammonia water with the mass percentage concentration of 25% is added through an ammonia water feeding hole 3 and is adjusted until the silver nitrate is precipitated and then is completely dissolved, and the pH value of the system is 9-10. Finally, 650g of dispersant PVP (polyvinylpyrrolidone) solid is weighed and placed in a reactor 8, stirred and dissolved to prepare silver ammonia solution oxidation liquid, and heated and kept at 37 ℃;
2)137 ml of hydroxylamine sulfate aqueous solution with the mass concentration of 0.13 g/L is injected through the hydroxylamine sulfate inlet 4, the injection speed is 37 ml/min, the stirring speed is 200 r/min, the hydroxylamine sulfate solution and the silver ammonia solution are enabled to rotate and fully mix in the reactor 8, and N generated in the reaction process is utilized2Gas, forming micro-nano bubbles in a solution environment, and depositing silver on the micro-nano bubbles to form nano silver seed crystals with hollow structures;
3) 2.9Kg of ascorbic acid aqueous solution with the mass percentage concentration of 27.4 percent is injected through a weak reducing agent feed port 7, the injection speed is 2.7 liters per minute, the stirring speed is 500 r/min for reaction, and the adding time is controlled within 15 min. Simultaneously, the ultrasonic generator 2 is started, the ultrasonic frequency is 68Hz, and the ultrasonic power is 600W. The reaction solution is dispersed by ultrasonic waves, so that the silver seed crystals are prevented from agglomerating, and the independent growth of the silver seed crystals is realized;
4) after the injection of the ascorbic acid aqueous solution was completed, it was aged for 25 min. Discharging the silver paste solution to a centrifuge 9 for separation, filtration and cleaning until the conductivity of the filtrate is less than or equal to 20 us/cm; transferring the obtained silver powder 10 into a drying oven, setting the drying temperature to be 55 ℃, drying for 8 hours to obtain about 3.17 Kg of silver powder;
5) the obtained silver powder has uniform particle size, high crystallinity, face-centered cubic structure, average particle diameter of 1.2um, and tap density of 6.3 g/cm3 。
Claims (4)
1. A preparation method of low-temperature sintered high-crystallinity silver powder is characterized by comprising the following steps: the method comprises the steps of obtaining metal silver particles from a silver-ammonia solution by a chemical reduction method in a reactor, adding the silver-ammonia solution into the reactor by taking the silver-ammonia solution as an oxidizing agent in the process of obtaining the metal silver particles from the silver-ammonia solution by the chemical reduction method, and using hydroxylamine sulfate as a reducing agent, wherein the concentration of the hydroxylamine sulfate is 0.1-3.0 g/L; adding hydroxylamine sulfate into a reactor in a jet flow mode, fully mixing the hydroxylamine sulfate and the silver ammonia solution in the reactor, and utilizing N generated in the reaction process2Gas, forming micro-nano bubbles in the solution environment, and silver in the micro-nanoDepositing on the rice bubbles to form nano silver seed crystals with hollow structures; then injecting the mixture of one or more weak reducing agents into the reactor; the weak reducing agent is one or a mixture of more than two of ascorbic acid, glucose, formaldehyde and triethanolamine, an ultrasonic generator is adopted, the reaction liquid in the reactor is dispersed by ultrasonic waves, so that silver crystal seeds independently grow to form silver powder, and finally the silver powder with high crystallinity is obtained by centrifugal separation, cleaning and drying.
2. The method for preparing a low-temperature-sintered high-crystallinity silver powder according to claim 1, wherein:
the injection speed of the hydroxylamine sulfate into the reactor is less than 100 ml per minute.
3. The method for preparing a low-temperature-sintered high-crystallinity silver powder according to claim 1, wherein: in the process of obtaining the metal silver particles from the silver-ammonia solution by using the chemical reduction method, the reducing solution and the oxidizing solution are respectively injected into the reactor in a constant speed mode.
4. The method for preparing a low-temperature-sintered high-crystallinity silver powder according to claim 1, wherein: the injection speed of the weak reducing agent into the reactor is more than 500 milliliters per minute.
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| CN110355382B (en) * | 2019-08-23 | 2022-06-14 | 山东建邦胶体材料有限公司 | Preparation method of microcrystalline silver powder containing hollow structure |
| CN117380966B (en) * | 2023-10-16 | 2024-05-07 | 上海镭立激光科技有限公司 | Preparation method of polycrystalline structure silver powder with controllable grain size |
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| GB1514805A (en) * | 1974-06-26 | 1978-06-21 | Eastman Kodak Co | Photographic silver halide developer compositions |
| CN1142204A (en) * | 1993-11-22 | 1997-02-05 | 利利工业(美国)有限公司 | Ammonia-free deposition of copper by disproportionation |
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| CN102101061A (en) * | 2009-09-30 | 2011-06-22 | 朗盛德国有限责任公司 | Method for improved removal of cations using chelate resins |
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