CN115121804A - Synthesis method of micron-sized hollow sphere silver particles sprayed by electrode aerosol of solar cell - Google Patents
Synthesis method of micron-sized hollow sphere silver particles sprayed by electrode aerosol of solar cell Download PDFInfo
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- CN115121804A CN115121804A CN202210830607.7A CN202210830607A CN115121804A CN 115121804 A CN115121804 A CN 115121804A CN 202210830607 A CN202210830607 A CN 202210830607A CN 115121804 A CN115121804 A CN 115121804A
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- solar cell
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 33
- 239000004332 silver Substances 0.000 title claims abstract description 33
- 239000002245 particle Substances 0.000 title claims abstract description 31
- 239000000443 aerosol Substances 0.000 title claims abstract description 18
- 238000001308 synthesis method Methods 0.000 title claims description 9
- 239000000243 solution Substances 0.000 claims abstract description 43
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000008367 deionised water Substances 0.000 claims abstract description 23
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 239000011259 mixed solution Substances 0.000 claims abstract description 13
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 12
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 9
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 9
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 7
- 239000000725 suspension Substances 0.000 claims abstract description 7
- 235000010489 acacia gum Nutrition 0.000 claims abstract description 6
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 6
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 6
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 6
- 229920000084 Gum arabic Polymers 0.000 claims abstract description 5
- 241000978776 Senegalia senegal Species 0.000 claims abstract description 5
- 239000000205 acacia gum Substances 0.000 claims abstract description 5
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 22
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 11
- 239000002244 precipitate Substances 0.000 claims description 9
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000000967 suction filtration Methods 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 3
- 230000002194 synthesizing effect Effects 0.000 claims 5
- 238000005507 spraying Methods 0.000 abstract description 11
- 239000007788 liquid Substances 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000002699 waste material Substances 0.000 abstract description 5
- 231100000252 nontoxic Toxicity 0.000 abstract description 3
- 230000003000 nontoxic effect Effects 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000009689 gas atomisation Methods 0.000 abstract description 2
- 239000007787 solid Substances 0.000 abstract description 2
- 238000010189 synthetic method Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 7
- 238000002360 preparation method Methods 0.000 description 6
- 239000000843 powder Substances 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 231100000481 chemical toxicant Toxicity 0.000 description 2
- 239000011094 fiberboard Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 239000003440 toxic substance Substances 0.000 description 2
- 241000282414 Homo sapiens Species 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000001785 acacia senegal l. willd gum Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000003380 propellant Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- -1 smart phones Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 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
- 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
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
- B22F1/0655—Hollow particles
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0224—Electrodes
- H01L31/022408—Electrodes for devices characterised by at least one potential jump barrier or surface barrier
- H01L31/022425—Electrodes for devices characterised by at least one potential jump barrier or surface barrier for solar cells
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
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- Condensed Matter Physics & Semiconductors (AREA)
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Abstract
The invention is suitable for the technical field of solar cell production, and provides a synthetic method for spraying micron-sized hollow sphere silver particles on electrode aerosol of a solar cell, which comprises the following steps: step one, adding a certain amount of ascorbic acid and gum arabic into deionized water with different masses respectively to obtain a reducing agent solution A and a reducing agent solution B; step two, adding a certain proportion of citric acid and polyethylene glycol into deionized water to obtain a growth agent C; and step three, adding the solution B into the reducing agent solution A to obtain a mixed solution D, and uniformly stirring the mixed solution D. According to the special performance requirements of the aerosol spraying process of the electrode silver grid of the solar cell on the conductive silver paste, the invention develops a novel hollow spherical silver particle which has the characteristics of light weight, small density, good dispersibility, good suspension property, good gas atomization performance of the prepared paste and the like compared with a solid silver particle, and meanwhile, the required raw materials are nontoxic, and the subsequent waste liquid does not need to be specially treated.
Description
Technical Field
The invention belongs to the technical field of solar cell production, and particularly relates to a synthesis method for spraying micron-sized hollow sphere silver particles on electrode aerosol of a solar cell.
Background
The 21 st century is an era of rapid development of electronic information manufacturing industry, electronic products such as smart phones, tablet computers, electronic books and wearable watches are ubiquitous, and the life style of human beings is thoroughly changed. With the development of high-tech industries, research and development of new related conductive materials have attracted much attention from governments and research institutions of various countries around the world. The micro-nano material has the characteristics of high surface activity, large surface area and the like, so that the micro-nano material becomes a 'pet' in the research field of related new materials, and particularly, the micro-nano structure material with optical and electric characteristics, such as micro-nano noble metal gold and silver, becomes a very active topic in the research field. Among them, the micro-nano silver powder is widely used in the production of products such as electronic tags, solar cell electrodes, membrane switches, flexible printed circuit boards, organic light emitting diodes, transparent conductive films and the like because of its advantages of excellent conductivity, oxidation resistance, low-temperature sintering property, stable chemical properties, easy processing and the like. In recent years, each country has great investment in preparing high-performance micro-nano silver powder, and silver powder manufacturers such as DuPont, Sumitomo and Tianzhong in Japan occupy most of the global market due to the advanced production process.
The aerosol spraying is to fill the paint and the gas propellant into a metal can, and a plurality of steel balls or glass balls are also placed into the can. The publication No. CN1325762A discloses for the first time an aerosol jet printing apparatus, which performs organic solvent mixed jet printing, and is suitable for spraying a binder mixture to cement, metal, vinyl, fiberboard (e.g., medium density fiberboard), and the like. Publication No. CN 101605924a discloses a non-electrolytic method that provides metallization of arbitrary substrates by spraying an aerosol of a solution containing oxidized metal cations and a reducing agent.
The aerosol spray technique is mentioned in the above patent and no attempt is made to spray silver paste. And the prior micron-sized hollow spherical silver particles need to treat waste liquid in the preparation process, and have complex operation and long preparation time.
Disclosure of Invention
The embodiment of the invention aims to provide a synthesis method for spraying micron-sized hollow sphere silver particles by using aerosol of a solar cell electrode, and aims to solve the problems that waste liquid needs to be treated, the operation is complex and the preparation time is long in the existing preparation process of the micron-sized hollow sphere silver particles.
The invention discloses a synthesis method for spraying micron-sized hollow sphere silver particles by using aerosol of a solar cell electrode, which comprises the following steps:
step one, adding a certain amount of ascorbic acid and gum arabic into deionized water with different masses respectively to obtain a reducing agent solution A and a reducing agent solution B;
step two, adding a certain proportion of citric acid and polyethylene glycol into deionized water to obtain a growth agent C;
step three, adding the solution B into the reducing agent solution A to obtain a mixed solution D, and uniformly stirring the mixed solution D;
step four, adding a certain amount of silver nitrate into deionized water to prepare a silver nitrate solution; dropwise adding a silver nitrate solution into the mixed solution D in the third step, and stirring for 30 minutes to obtain a suspension E;
step five, adding a growth agent C into the suspension E obtained in the step four, and stirring for 2 hours at normal temperature
Step six, stirring the solution obtained in the step five, and collecting the solution by using a centrifugal tube;
step seven, carrying out ultrasonic treatment on the solution collected in the step six;
step eight, centrifuging the solution subjected to the ultrasonic treatment in the step seven in a centrifuge for 5 minutes, and then removing the supernatant to leave precipitate silver powder;
and step nine, adding alcohol into the precipitate silver powder collected in the step eight for suction filtration, and then putting the precipitate silver powder into an oven to dry for 2 hours at the temperature of 60 ℃ to obtain the hollow spherical silver particles.
According to a further technical scheme, 0.88g of ascorbic acid is added into 5mL of deionized water in the step one to obtain a reducing agent solution A, and 0.2g of Arabic gum is added into 10mL of deionized water in the step one to obtain a solution B.
According to a further technical scheme, in the second step, the concentration of the citric acid, the concentration of the polyethylene glycol and the concentration of the deionized water are respectively 0.01mL, 4mL and 1.25mL, and the solution of the citric acid, the polyethylene glycol and the deionized water is stirred for 5 minutes.
According to a further technical scheme, the mixed solution D in the third step is stirred for 10 minutes at room temperature.
According to a further technical scheme, in the fourth step, the silver nitrate is 0.425g, and the deionized water is 5 mL.
In a further technical scheme, the speed of the centrifuge in the step eight is 7000 rps.
The invention provides a synthesis method for spraying micron-sized hollow sphere silver particles by using aerosol of a solar cell electrode, which develops a novel hollow sphere silver particle according to the special performance requirement of the aerosol spraying process of a solar cell electrode silver grid on conductive silver paste, the particle has the characteristics of light weight, small density, good dispersibility, good suspensibility, good gas atomization performance of prepared slurry and the like compared with solid silver particles, simultaneously, required raw materials are nontoxic, subsequent waste liquid does not need to be specially treated, and the shape control and continuous preparation of the silver particles smaller than 5 microns can be realized without adding other toxic chemical reagents, the process is simple, the product is widely applied, the powder yield is high, the product is green and environment-friendly, the method has great potential for further commercial development, and the difference exists between high-end silver powder products and abroad, therefore, the method has high product quality and very important theoretical significance and practical significance for replacing the micro-nano spherical silver powder imported at the high end.
Drawings
FIG. 1 is a schematic diagram of a micron-sized hollow spherical silver particle provided by an embodiment of the present invention;
fig. 2 and fig. 3 are macro topography diagrams of micron-sized hollow spherical silver particles provided by the embodiment of the invention;
fig. 4 and 5 are microstructure diagrams of micron-sized hollow spherical silver particles provided by an embodiment of the present invention;
fig. 6 is a structural view of the inside of a micron-sized hollow spherical silver particle according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Specific implementations of the present invention are described in detail below with reference to specific embodiments.
Example one
The synthesis method of the micron-sized hollow sphere silver particles sprayed by the aerosol of the solar cell electrode comprises the following steps:
step one, 0.88g of ascorbic acid and 0.2g of gum arabic are respectively added into 5mL of deionized water and 10mL of deionized water to obtain a reducing agent solution A and a reducing agent solution B;
step two, adding 0.01mL of citric acid and 4mL of polyethylene glycol into 1.25mL of deionized water to obtain a growth agent C; and stirring the solution of citric acid, polyethylene glycol and deionized water for 5 minutes;
step three, adding the solution B into the reducing agent solution A to obtain a mixed solution D, and stirring the mixed solution D for 10 minutes at room temperature;
step four, adding 0.425g of silver nitrate into 5mL of deionized water to prepare a silver nitrate solution; dropwise adding a silver nitrate solution into the mixed solution D in the third step, and stirring for 30 minutes to obtain a suspension E;
step five, adding a growth agent C into the suspension E obtained in the step four, and stirring for 2 hours at normal temperature
Step six, stirring the solution obtained in the step five, and collecting the solution by using a centrifugal tube;
step seven, performing ultrasonic treatment on the solution collected in the step six;
step eight, centrifuging the solution subjected to ultrasonic treatment in the step seven in a centrifuge at the speed of 7000rps for 5 minutes, and then removing the supernatant to leave precipitate silver powder;
step nine, adding alcohol into the precipitate silver powder collected in the step eight for suction filtration, and then putting the precipitate silver powder into an oven to dry for 2 hours at the temperature of 60 ℃ to obtain hollow spherical silver particles
The synthesis method for spraying the micron-sized hollow sphere silver particles by using the aerosol of the solar cell electrode is provided in the embodiment of the invention, the required raw materials are nontoxic, subsequent waste liquid does not need to be specially treated, the shape control and continuous preparation of the nano silver particles can be realized without adding other toxic chemical reagents, the process is simple, the product is widely applied, the powder yield is high, and the method is green and environment-friendly and has feasibility of industrial production.
The above description is intended to be illustrative of the preferred embodiment of the present invention and should not be taken as limiting the invention, but rather, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention.
Claims (6)
1. The synthesis method of the micron-sized hollow sphere silver particles sprayed by the aerosol of the solar cell electrode is characterized by comprising the following steps of:
step one, adding a certain amount of ascorbic acid and gum arabic into deionized water with different masses respectively to obtain a reducing agent solution A and a reducing agent solution B;
step two, adding a certain proportion of citric acid and polyethylene glycol into deionized water to obtain a growth agent C;
step three, adding the solution B into the reducing agent solution A to obtain a mixed solution D, and uniformly stirring the mixed solution D;
step four, adding a certain amount of silver nitrate into deionized water to prepare a silver nitrate solution; dropwise adding a silver nitrate solution into the mixed solution D in the third step, and stirring for 30 minutes to obtain a suspension E;
step five, adding a growth agent C into the suspension E obtained in the step four, and stirring for 2 hours at normal temperature
Step six, stirring the solution obtained in the step five, and collecting the solution by using a centrifugal tube;
step seven, carrying out ultrasonic treatment on the solution collected in the step six;
step eight, centrifuging the solution subjected to the ultrasonic treatment in the step seven in a centrifuge for 5 minutes, and then removing the supernatant to leave precipitate silver powder;
and step nine, adding alcohol into the precipitate silver powder collected in the step eight for suction filtration, and then putting the precipitate silver powder into an oven to dry for 2 hours at the temperature of 60 ℃ to obtain the hollow spherical silver particles.
2. The method for synthesizing the silver micro-sized hollow sphere particles sprayed by the aerosol of the solar cell electrode according to claim 1, wherein 0.88g of ascorbic acid is added into 5mL of deionized water to obtain a reducing agent solution A in the first step, and 0.2g of gum arabic is added into 10mL of deionized water to obtain a solution B in the first step.
3. The method for synthesizing the silver particles as claimed in claim 1, wherein the concentration of citric acid, polyethylene glycol and deionized water in the second step is 0.01mL, 4mL and 1.25mL, and the solution of citric acid, polyethylene glycol and deionized water is stirred for 5 minutes.
4. The method for synthesizing the silver particles as the solar cell electrode aerosol-sprayed micron-sized hollow spheres of claim 1, wherein the mixed solution D in the third step is stirred at room temperature for 10 minutes.
5. The method for synthesizing the aerosol-sprayed micron-sized hollow sphere silver particles for the solar cell electrode according to claim 1, wherein silver nitrate in the fourth step is 0.425g, and deionized water is 5 mL.
6. The method for synthesizing the silver particles as the solar cell electrode aerosol-coated micron-sized hollow spheres of claim 1, wherein the speed of the centrifuge in the step eight is 7000 rps.
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KR20150116927A (en) * | 2014-04-08 | 2015-10-19 | 에이비씨나노텍 주식회사 | the producing method of hollow sliver powder and the hollow sliver powder using the method and the low specific gravity silver paste composite |
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CN110355382A (en) * | 2019-08-23 | 2019-10-22 | 山东建邦胶体材料有限公司 | A kind of preparation method of the crystallite silver powder containing hollow structure |
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CN113600825A (en) * | 2021-07-22 | 2021-11-05 | 厦门大学 | Micron-sized spherical silver powder and preparation method thereof |
CN114743716A (en) * | 2022-04-15 | 2022-07-12 | 北京大学深圳研究生院 | Silver powder capable of being sintered at low temperature and preparation method and application thereof |
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KR20150116927A (en) * | 2014-04-08 | 2015-10-19 | 에이비씨나노텍 주식회사 | the producing method of hollow sliver powder and the hollow sliver powder using the method and the low specific gravity silver paste composite |
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CN110355382A (en) * | 2019-08-23 | 2019-10-22 | 山东建邦胶体材料有限公司 | A kind of preparation method of the crystallite silver powder containing hollow structure |
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Non-Patent Citations (1)
Title |
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T. PREUKSARATTANAWUT等: "Fabrication of silver hollow microspheres by sodium hydroxide in glycerol solution", MATERIALS CHEMISTRY AND PHYSICS, vol. 130, no. 1, pages 481 - 486, XP028389163, DOI: 10.1016/j.matchemphys.2011.07.013 * |
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