CN110834100A - Preparation method of flaky porous silver powder - Google Patents
Preparation method of flaky porous silver powder Download PDFInfo
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- CN110834100A CN110834100A CN201911250743.3A CN201911250743A CN110834100A CN 110834100 A CN110834100 A CN 110834100A CN 201911250743 A CN201911250743 A CN 201911250743A CN 110834100 A CN110834100 A CN 110834100A
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- silver powder
- silver
- flaky
- reducing agent
- sodium carbonate
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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
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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
- B22F1/054—Nanosized particles
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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
- B22F1/054—Nanosized particles
- B22F1/0551—Flake form nanoparticles
-
- 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
- B22F1/068—Flake-like 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
- B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention discloses a preparation method of flaky porous silver powder, which relates to the technical field of flaky silver powder preparation processes, and is characterized in that silver salt is dissolved by a solvent, and then a sodium carbonate aqueous solution is added and mixed to form a suspension; dissolving a reducing agent to obtain a reducing agent solution; and directly adding the suspension into a reducing agent solution, reacting for 20-30 min under a heating condition, and centrifugally cleaning to obtain a product. According to the preparation method of the flaky porous silver powder, sodium carbonate is used as one of the raw materials, and no dispersant is added, so that the cost of the dispersant is reduced, meanwhile, a process of dispersant treatment is not needed in the post-treatment process of the product, and sintering residues generated in the sintering process of the dispersant are avoided; meanwhile, the generated product is flaky and porous in shape, so that the specific surface area of the flaky silver powder can be increased, the sintering temperature of the product can be reduced, low-temperature sintering at lower temperature can be realized, and the product can be used as a conductive adhesive for follow-up use, thereby saving energy.
Description
Technical Field
The invention relates to the technical field of nano silver powder preparation, in particular to a preparation method of flaky porous silver powder.
Background
The resistivity of the metallic silver is 1.59 x 10-6 omega.cm, the thermal conductivity is 408W/(m.K), and the electric conductivity and the thermal conductivity of the metallic silver are the best in metals at normal temperature; silver is chemically stable and is not easily oxidized, and even if the surface layer is oxidized, the oxide thereof has a certain conductivity, so that the silver powder has a very wide application in electronic pastes.
The proportion of the silver powder in the conductive silver paste is more than 50%, which is a key factor for determining the performances of the silver paste and the formed silver electrode, and the morphology of the silver powder has obvious influence on the sintering compactness and the conductivity of the conductive silver paste. Researches find that the flake silver powder has smaller volume resistivity compared with the spherical silver powder, and is more beneficial to sintering and compacting of the silver paste.
Disclosure of Invention
Aiming at the prior art, the invention provides a preparation method of flaky porous silver powder, which is used for preparing the flaky porous silver powder without adding a dispersing agent and post-processing the dispersing agent on silver powder particles.
The invention is realized by the following technical scheme: the preparation method of the flaky porous silver powder comprises the steps of dissolving silver salt by using a solvent, adding a sodium carbonate aqueous solution, and mixing to form a suspension; dissolving a reducing agent to obtain a reducing agent solution; and directly adding the suspension into a reducing agent solution, reacting for 20-30 min under a heating condition, and centrifugally cleaning to obtain a product.
In the technical scheme, a sodium carbonate aqueous solution is used as a pH value regulator and also used as a nucleation control agent of the silver powder; meanwhile, the silver carbonate generated by the sodium carbonate and the silver ions in the solvent can also play a role in etching, so that the surface of the product forms a porous structure, and the specific surface area is 4-5 m2The flake porous nano silver powder is/g.
Further, the molar ratio of the silver salt, the sodium carbonate and the reducing agent is as follows: 2-8: 1-5: 4-16.
Further, the concentration of silver salt in the suspension is 0.2-0.8 mol/L; the concentration of the sodium ions is 0.1-0.5 mol/L, and the solvent is deionized water.
Furthermore, the concentration of the reducing agent is 0.2-0.8 mol/L, and the solvent is deionized water.
Further, the silver salt is any one of silver nitrate, silver acetate and silver citrate.
Further, the reducing agent is ascorbic acid.
Further, the reaction temperature is 30-60 ℃.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the yield of the flaky porous silver powder prepared by the preparation method of the flaky porous silver powder is about 92-96%.
(2) The flaky nano silver powder prepared by the preparation method of the flaky porous silver powder provided by the invention has uniform particle size distribution, is columnar, has the length of 0.8-1.2 mu m and the width of 150-250 nm; the surface of each flake silver powder is provided with a plurality of hollow holes.
(3) According to the preparation method of the flaky porous silver powder, a dispersing agent is not added, the cost of the dispersing agent is reduced, a process of dispersing agent treatment is not needed in the post-treatment process of the product, and sintering residues generated in the sintering process of the dispersing agent are avoided.
Drawings
FIG. 1 is an electron microscope image of the flake porous silver powder prepared by the present invention.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
The invention discloses a preparation method of flaky porous silver powder, which specifically comprises the following steps:
s1) weighing silver salt and sodium carbonate crystals, respectively adding silver salt into deionized water to prepare silver salt solution, adding sodium carbonate into deionized water to prepare sodium carbonate solution, adding the sodium carbonate solution into the silver salt solution under the stirring condition to form light yellow suspension, wherein the concentration of the silver salt in the suspension is 0.2-0.8 mol/L, and the concentration of sodium ions is 0.1-0.5 mol/L;
s2) adding a reducing agent into deionized water, stirring and dissolving completely to prepare a reducing agent solution of 0.2-0.8 mol/L;
s3) directly pouring the reducing agent solution prepared in the step S2) into the suspension at the temperature of 30-60 ℃, and reacting for 20-30 min to finish the reaction;
s4), after the reaction is finished, centrifuging, and then washing and centrifuging by using deionized water to obtain a product; the yield is 92-96%.
Example 1
The specific implementation process of the preparation method of the flaky porous silver powder comprises the following steps:
s1) adding 34.0g of silver nitrate into 700mL of deionized water, and stirring to dissolve to obtain a silver nitrate solution for later use; weighing 10.6g of sodium carbonate, then adding the sodium carbonate into 300mL of deionized water, and stirring and dissolving to obtain a sodium carbonate solution; adding a sodium carbonate solution into a silver nitrate solution, and stirring to form a light yellow suspension;
s2), weighing 47.0g of ascorbic acid, adding the ascorbic acid into 2L of deionized water, stirring and dissolving completely to prepare a reducing agent solution of 0.25 mol/L;
s3) directly adding the reducing agent solution prepared in the step S2) into the suspension prepared in the step S1) at the temperature of 30 ℃, and stirring and reacting for 20 min;
s4), centrifuging, washing with deionized water, centrifuging and drying to obtain 20.46g of the flaky porous silver powder; the yield was 94.7%.
The product prepared in the embodiment is characterized by a scanning electron microscope as shown in figure 1, the obtained product is flaky particles, a plurality of holes are distributed on the surface of the flaky particles to form flaky porous silver powder, the length of the prepared silver powder is 0.8-1.2 mu m, the width of the prepared silver powder is 150-250 nm, and the distribution range of the prepared silver powder is narrow.
In the above embodiment, no dispersant is added in the preparation process, and simultaneously no ammonia water is added as a pH value regulator to generate silver ammonia, but a sodium carbonate aqueous solution is used as the pH value regulator. Before the reaction process, sodium carbonate reacts with silver nitrate to generate silver carbonate which is insoluble in water solution to form suspension, so that crystal nuclei are provided for the growth of the flake silver powder; in the reaction process, because part of silver ions do not form suspension with carbonate and react with the reducing agent firstly, when the silver ions are insufficient in the later period of the reaction, the silver carbonate is reduced by the reducing agent to generate metallic silver. In the reaction process, the silver carbonate provides crystal nuclei for the growth of the flake silver powder, and simultaneously has good etching effect, so that the generated silver powder is in a flake porous shape. Meanwhile, since crystal nuclei are generated before the reaction, the generated silver powder can achieve a good dispersion effect even without a dispersant.
The porous shape of the product can improve the specific surface area of the flake silver powder, and simultaneously can reduce the sintering temperature of the product, realize low-temperature sintering at lower temperature, and save energy for subsequent use as conductive adhesive.
The preparation method of the embodiment is simple and effective without adding a dispersing agent, has low cost, does not need to process the dispersing agent adsorbed on the silver powder at the later stage, and avoids sintering residues generated in the sintering process of the silver powder of the dispersing agent.
Example 2
The specific implementation process of the preparation method of the flaky porous silver powder comprises the following steps:
s1) adding 127.5g of silver nitrate into 700mL of deionized water, and stirring to dissolve to obtain a silver nitrate solution for later use; weighing 47.7g of sodium carbonate, then adding into 300mL of deionized water, and stirring for dissolving to obtain a sodium carbonate solution; adding a sodium carbonate solution into a silver nitrate solution, and stirring to form a light yellow suspension;
s2), weighing 150.4g of ascorbic acid, adding the ascorbic acid into 2L of deionized water, stirring and dissolving completely to prepare a reducing agent solution of 0.8 mol/L;
s3) directly adding the reducing agent solution prepared in the step S2) into the suspension prepared in the step S1) at the temperature of 60 ℃, and stirring and reacting for 20 min;
s4), centrifuging, cleaning with deionized water, centrifuging and drying to obtain 74.60g of the flaky porous silver powder; the yield was 92.1%.
Other parts in this embodiment are substantially the same as those in embodiment 1, and thus are not described in detail.
Example 3
The specific implementation process of the preparation method of the flaky porous silver powder comprises the following steps:
s1) adding 85.0g of silver nitrate into 700mL of deionized water, and stirring to dissolve to obtain a silver nitrate solution for later use; weighing 31.8g of sodium carbonate, then adding the sodium carbonate into 300mL of deionized water, and stirring and dissolving to obtain a sodium carbonate solution; adding a sodium carbonate solution into a silver nitrate solution, and stirring to form a light yellow suspension;
s2), weighing 103.4g of ascorbic acid, adding the ascorbic acid into 2L of deionized water, stirring and dissolving completely to prepare a reducing agent solution of 0.55 mol/L;
s3) directly adding the reducing agent solution prepared in the step S2) into the suspension prepared in the step S1) at 50 ℃, and stirring and reacting for 20 min;
s4), centrifuging, cleaning with deionized water, centrifuging and drying to obtain 51.41g of the flaky porous silver powder; the yield was 95.2%.
Example 4
The specific implementation process of the preparation method of the flaky porous silver powder comprises the following steps:
s1) adding 41.73g of silver acetate into 700mL of deionized water, and stirring and dissolving to obtain a silver acetate solution for later use; weighing 15.9g of sodium carbonate, then adding the sodium carbonate into 300mL of deionized water, and stirring and dissolving to obtain a sodium carbonate solution; adding a sodium carbonate solution into a silver acetate solution, and stirring to form a light yellow suspension;
s2), weighing 56.4g of ascorbic acid, adding the ascorbic acid into 2L of deionized water, stirring and dissolving completely to prepare a reducing agent solution of 0.55 mol/L;
s3) directly adding the reducing agent solution prepared in the step S2) into the suspension prepared in the step S1) at the temperature of 60 ℃, and stirring and reacting for 20 min;
s4), centrifuging, washing with deionized water, centrifuging and drying to obtain 25.30g of the flaky porous silver powder; the yield thereof was 93.7%.
Example 5
The specific implementation process of the preparation method of the flaky porous silver powder comprises the following steps:
s1) adding 116.8g of silver acetate into 700mL of deionized water, and stirring for dissolving to obtain a silver acetate solution for later use; weighing 53.0g of sodium carbonate, then adding the sodium carbonate into 300mL of deionized water, and stirring and dissolving to obtain a sodium carbonate solution; adding a sodium carbonate solution into a silver acetate solution, and stirring to form a light yellow suspension;
s2), weighing 141.0g of ascorbic acid, adding the ascorbic acid into 2L of deionized water, stirring and dissolving completely to prepare a reducing agent solution of 0.75 mol/L;
s3) directly adding the reducing agent solution prepared in the step S2) into the suspension prepared in the step S1) at the temperature of 45 ℃, and stirring and reacting for 25 min;
s4), centrifuging, washing with deionized water, centrifuging and drying to obtain 71.82g of the flaky porous silver powder; the yield was 95.0%.
Example 6
The specific implementation process of the preparation method of the flaky porous silver powder comprises the following steps:
s1) adding 83.45g of silver acetate into 700mL of deionized water, and stirring for dissolving to obtain a silver acetate solution for later use; weighing 31.8g of sodium carbonate, then adding the sodium carbonate into 300mL of deionized water, and stirring and dissolving to obtain a sodium carbonate solution; adding a sodium carbonate solution into a silver acetate solution, and stirring to form a light yellow suspension;
s2), weighing 103.4g of ascorbic acid, adding the ascorbic acid into 2L of deionized water, stirring and dissolving completely to prepare a reducing agent solution of 0.55 mol/L;
s3) directly adding the reducing agent solution prepared in the step S2) into the suspension prepared in the step S1) at 50 ℃, and stirring and reacting for 20 min;
s4), centrifuging, washing with deionized water, centrifuging and drying to obtain 51.14g of the flaky porous silver powder; the yield was 94.7%.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and all simple modifications and equivalent variations of the above embodiments according to the technical spirit of the present invention are included in the scope of the present invention.
Claims (8)
1. A preparation method of flaky porous silver powder is characterized by comprising the following steps: dissolving silver salt with a solvent, adding a sodium carbonate aqueous solution, and mixing to form a suspension; dissolving a reducing agent to obtain a reducing agent solution; and directly adding the suspension into a reducing agent solution, reacting for 20-30 min under a heating condition, and centrifugally cleaning to obtain a product.
2. The method for producing a flaky porous silver powder according to claim 1, characterized in that: the molar ratio of the silver salt to the sodium carbonate to the reducing agent is as follows: 2-8: 1-5: 4-16.
3. The method for producing a flaky porous silver powder according to claim 2, characterized in that: in the suspension, the concentration of silver salt is 0.2-0.8 mol/L; the concentration of the sodium ions is 0.1-0.5 mol/L, and the solvent is deionized water.
4. The method for producing a flaky porous silver powder according to claim 2, characterized in that: the concentration of the reducing agent is 0.2-0.8 mol/L, and the solvent is deionized water.
5. The method for producing a flaky porous silver powder according to claim 1, characterized in that: the solvent of the silver ammonia solution is deionized water.
6. The method for producing a flaky porous silver powder according to claim 4, characterized in that: the silver salt is any one of silver nitrate, silver acetate and silver citrate.
7. The method for producing a flaky porous silver powder according to any one of claims 1 to 6, characterized in that: the reducing agent is ascorbic acid.
8. The method for producing a flaky porous silver powder according to any one of claims 1 to 6, characterized in that: the reaction temperature is 30-60 ℃.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113084189A (en) * | 2021-04-08 | 2021-07-09 | 中船重工黄冈水中装备动力有限公司 | Preparation method of silver powder |
| CN113245554A (en) * | 2021-04-21 | 2021-08-13 | 中山大学 | Silver porous material and preparation method thereof |
| CN113547132A (en) * | 2021-07-29 | 2021-10-26 | 长沙新材料产业研究院有限公司 | Method for preparing nano silver powder by hydrothermal method and nano silver powder |
| CN114247896A (en) * | 2021-12-28 | 2022-03-29 | 成都市天甫金属粉体有限责任公司 | Simple preparation method and application of gold powder |
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Cited By (5)
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