CN110860700A - Preparation method of flaky nano silver powder - Google Patents
Preparation method of flaky nano silver powder Download PDFInfo
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- CN110860700A CN110860700A CN201911250739.7A CN201911250739A CN110860700A CN 110860700 A CN110860700 A CN 110860700A CN 201911250739 A CN201911250739 A CN 201911250739A CN 110860700 A CN110860700 A CN 110860700A
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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
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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
- B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
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Abstract
The invention discloses a preparation method of flaky nano silver powder, relating to the technical field of flaky nano silver powder preparation processes, wherein silver salt and ammonia water are mixed to obtain silver-ammonia solution; stirring and dissolving the dispersing agent at a high speed, adding the reducing agent, and continuously stirring and dissolving to obtain a mixed solution; adding the silver-ammonia solution into the mixed solution, and reacting under heating to obtain flaky nano silver powder; the dispersant is polymethacrylamide; the reducing agent is glucose. The preparation method of the flaky nano silver powder disclosed by the invention adopts the reducing agent which is nontoxic and harmless glucose, and the dispersing agent adopts the polymethacrylamide with good dispersibility, is easy to dissolve in water and is convenient to wash away; meanwhile, even if residues exist, the use of the flaky nano silver powder can not be influenced, and the conductivity of the silver powder used as silver paste is not influenced.
Description
Technical Field
The invention relates to the technical field of nano silver powder preparation, in particular to a preparation method of flaky nano silver powder.
Background
Metallic silver has excellent electrical and thermal conductivity and is widely used in the fields of printed electronics, catalysis, sensing, and the like. Research shows that the performance of metal nano-materials depends greatly on the shape, size, composition, crystallinity and structure of particles, and theoretically, people can finely adjust the properties of the nano-particles by controlling the parameters. The flaky nano silver powder has relatively large surface area, and the particles are in surface contact or line contact, so that the resistance is relatively low, and the conductivity is relatively good. In addition, the special surface plasma resonance performance of the flake nano silver powder enables the flake nano silver powder to show optical properties which are quite different from those of spherical particles and bulk phase materials. Therefore, the flaky nano silver powder has great application value in the fields of microelectronics, catalysis, surface enhanced Raman, metal enhanced fluorescence, infrared thermotherapy, biological markers, nano conductive adhesive, electronic packaging materials and the like.
Disclosure of Invention
Aiming at the prior art, the invention provides a preparation method of flaky nano silver powder, which adopts glucose as a reducing agent and polymethacrylamide as a dispersing agent to prepare the flaky nano silver powder.
The invention is realized by the following technical scheme: the preparation method of the flaky nano silver powder comprises the steps of dissolving silver salt in a solvent, adding ammonia water, and mixing to obtain a silver-ammonia solution; stirring and dissolving the dispersing agent at a high speed, adding the reducing agent, and continuously stirring and dissolving to obtain a mixed solution; adding the silver-ammonia solution into the mixed solution, and reacting under heating to obtain flaky nano silver powder; the dispersant is polymethacrylamide; the reducing agent is glucose.
According to the technical scheme, the flaky nano silver powder prepared by adopting the polymethacrylamide with good dispersion performance as the dispersing agent and the glucose as the reducing agent is used for obtaining the silver powder with the specific surface area of 8-11 m2The flake nano silver powder has good dispersing effect and large specific surface area.
Further, the silver salt, the reducing agent and the dispersing agent are as follows in parts by weight: 100-600 parts of silver salt, 100-500 parts of reducing agent and 5-50 parts of dispersing agent.
Further, the solvent of the mixed solution is deionized water; the concentration of the dispersant is as follows: 1-10 g/L; the concentration of the reducing agent is 20-100 g/L.
Further, the solvent of the silver ammonia solution is deionized water.
Further, the silver salt is any one of silver nitrate, silver acetate and silver citrate.
Further, the ammonia water is concentrated ammonia water with the mass fraction of 25-28%.
Further, the silver ammonia solution is dripped into the mixed solution at the speed of 5-50 mL/min.
Further, after the silver ammonia solution is added dropwise, continuing to react for 20-25 min at the reaction temperature of 30-60 ℃; and after the reaction is finished, centrifugally cleaning to obtain the flaky nano silver powder.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the yield of the flaky nano silver powder prepared by the preparation method of the flaky nano silver powder provided by the invention is about 90-95%.
(2) The flaky nano silver powder prepared by the preparation method of the flaky nano silver powder provided by the invention has uniform particle size distribution, and the particle size of the flaky nano silver powder is 50-150 nm; the thickness is 25-30 nm.
(3) The preparation method of the flaky nano silver powder provided by the invention adopts the reducing agent which is nontoxic and harmless glucose, and the dispersing agent adopts the polymethacrylamide with good dispersibility, is easy to dissolve in water and is convenient to wash away; meanwhile, even if residues exist, the use of the flaky nano silver powder can not be influenced, and the conductivity of the silver powder used as silver paste is not influenced.
(4) The preparation method of the flaky nano silver powder provided by the invention is simple, short in preparation process flow, lower in reaction temperature, low in energy consumption and convenient for large-scale process production.
Drawings
FIG. 1 is an electron microscope image of the flake nano silver powder prepared by the 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 nano silver powder, which specifically comprises the following steps:
s1) weighing silver salt, reducing agent and dispersing agent according to the mass fraction ratio of 100-600 parts of silver salt, 100-500 parts of reducing agent and 5-50 parts of dispersing agent; then stirring and adding the polymethacrylamide into deionized water, and stirring at a high speed of 2000-2500 r/min; then adding glucose powder, and continuing stirring to completely dissolve the glucose powder so that the concentration of the dispersing agent is as follows: 1-10 g/L; the concentration of the reducing agent is 20-100 g/L; obtaining a mixed solution;
s2) adding silver salt into deionized water, stirring and dissolving completely to enable the concentration of the silver salt to be 0.59-2.94 mol/L, then adding appropriate 25-28% ammonia water until the solution is gradually changed from brown to completely transparent, and preparing into a silver-ammonia solution;
s3) under the condition of 30-60 ℃, dropwise adding the mixed solution prepared in the step S1) into a silver ammonia solution at the speed of 5-50 mL/min, and continuing to react for 20-25 min after dropwise adding is finished, so that the reaction is finished;
s4), after the reaction is finished, centrifuging, and then washing and centrifuging by using deionized water to obtain a product; the yield is 90-95%.
Example 1
The specific implementation process of the preparation method of the flaky nano silver powder comprises the following steps:
s1) adding 5g of polymethacrylamide into 5L of deionized water by stirring, and stirring at a high speed of 2000 r/min; then adding 100g of glucose powder, and continuously stirring to completely dissolve the glucose powder to obtain a mixed solution;
s2) adding 100g of silver nitrate into 1L of deionized water, stirring and dissolving completely, and then adding 100mL of 25-28% ammonia water until the solution is gradually changed from brown to completely transparent to prepare a silver-ammonia solution;
s3) under the condition of 30 ℃, dropwise adding the mixed solution prepared in the step S1) into the silver-ammonia solution at the speed of 50mL/min, and continuing to react for 25min after the dropwise adding is finished, so that the reaction is finished;
s4), centrifuging, washing with deionized water, centrifuging and drying to obtain 58.13g of the flaky nano silver powder product; the yield was 91.5%.
The product prepared in the embodiment is characterized by a scanning electron microscope as shown in figure 1, and the obtained product is flaky nano silver powder, wherein the size distribution range of nano silver powder sheets is narrow and is 50-200 nm; the thickness distribution of the nano silver powder sheet is narrow, and the range of the thickness distribution is 28-30 nm, which shows that the nano silver powder sheet obtained by the method has a narrow size distribution range of the thickness although the shapes are different.
Wherein a small amount of nano silver powder particles can be separated in a separation and filtration mode, and the products using the conductive silver paste are all flaky nano silver powder.
The embodiment adopts glucose as a reducing agent, the reaction is mild and not violent, the reaction rate is easy to control, and the size distribution of the obtained product is narrow; meanwhile, the glucose is green, non-toxic, environment-friendly and suitable for industrial production; in addition, the glucose and the polymethacrylamide play a role in combined dispersion in the technical scheme, so that the reduction of the polymethacrylamide can also play a role in good dispersion, and a product with good dispersibility is obtained; the use of polymethacrylamide is reduced.
The polymethacrylamide has good water solubility and is easy to clean, so that the product after the reaction can be cleaned by deionized water without other solvents, the environmental pollution is low, and the cost is low; meanwhile, the residual polymethacrylamide after cleaning can be used as one of the components for preparing the conductive silver paste from the flaky nano silver powder, so that the conductivity of the product in the preparation of the conductive silver paste can not be influenced, and the product can be conveniently used.
In addition, in the reaction process, the change of the pH value of the reaction environment has a large influence on the size distribution range of the product, the larger the change of the pH value is, the wider the size distribution range of the product is, and the worse the conductivity is; in the invention, the pH value of the aqueous solution of the glucose is 6-7; the pH value of the silver-ammonia solution in the preparation process is about 7, so that the change range of the pH value in the whole reaction process is small, and the size distribution of the product is narrow.
Example 2
The specific implementation process of the preparation method of the flaky nano silver powder comprises the following steps:
s1) adding 50g of polymethacrylamide into 5L of deionized water by stirring, and stirring at a high speed of 2500 r/min; then adding 500g of glucose powder, and continuously stirring to completely dissolve the glucose powder to obtain a mixed solution;
s2) adding 600g of silver nitrate into 1L of deionized water, stirring and dissolving completely, and then adding 600mL of 25-28% ammonia water until the solution is gradually changed from brown to completely transparent to prepare a silver-ammonia solution;
s3) under the condition of 60 ℃, dropwise adding the mixed solution prepared in the step S1) into the silver-ammonia solution at the speed of 5mL/min, and continuing to react for 20min after the dropwise adding is finished, so that the reaction is finished;
s4), centrifuging, cleaning with deionized water, centrifuging and drying to obtain 343.8g of the flaky nano silver powder; the yield was 90.2%.
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 nano silver powder comprises the following steps:
s1) adding 25g of polymethacrylamide into 5L of deionized water by stirring, and stirring at a high speed of 2400 r/min; then adding 250g of glucose powder, and continuously stirring to completely dissolve the glucose powder to obtain a mixed solution;
s2) adding 300g of silver nitrate into 1L of deionized water, stirring and dissolving completely, and then adding 357mL of 25-28% ammonia water until the solution is gradually changed from brown to completely transparent to prepare a silver-ammonia solution;
s3) under the condition of 44 ℃, dropwise adding the mixed solution prepared in the step S1) into the silver-ammonia solution at the speed of 15mL/min, and continuing to react for 23min after the dropwise adding is finished, so that the reaction is finished;
s4), after the reaction is finished, centrifuging, and then cleaning and centrifuging by using deionized water to obtain 180.49g of a product; the yield was 94.7%.
Example 4
The specific implementation process of the preparation method of the flaky nano silver powder comprises the following steps:
s1) adding 7g of polymethacrylamide into 5L of deionized water by stirring, and stirring at a high speed of 2400 r/min; then adding 120g of glucose powder, and continuously stirring to completely dissolve the glucose powder to obtain a mixed solution;
s2) adding 120g of silver acetate into 1L of deionized water, stirring and dissolving completely, then adding 210mL of 25-28% ammonia water until the solution is gradually changed from brown to completely transparent, and preparing into a silver-ammonia solution;
s3) under the condition of 44 ℃, dropwise adding the mixed solution prepared in the step S1) into the silver-ammonia solution at the speed of 12mL/min, and continuing to react for 25min after the dropwise adding is finished, so that the reaction is finished;
s4), after the reaction is finished, centrifuging, and then washing and centrifuging by using deionized water to obtain 70.66g of a product; the yield thereof was 91.0%.
Example 5
The specific implementation process of the preparation method of the flaky nano silver powder comprises the following steps:
s1) adding 37g of polymethacrylamide into 5L of deionized water by stirring, and stirring at a high speed of 2400 r/min; then adding 120g of glucose powder, and continuously stirring to completely dissolve the glucose powder to obtain a mixed solution;
s2) adding 120g of silver acetate into 1L of deionized water, stirring and dissolving completely, then adding 210mL of 25-28% ammonia water until the solution is gradually changed from brown to completely transparent, and preparing into a silver-ammonia solution;
s3) under the condition of 44 ℃, dropwise adding the mixed solution prepared in the step S1) into the silver-ammonia solution at the speed of 15mL/min, and continuing to react for 25min after the dropwise adding is finished, so that the reaction is finished;
s4), after the reaction is finished, centrifuging, and then washing and centrifuging by using deionized water to obtain 72.58g of a product; the yield thereof was 93.5%.
Example 6
The specific implementation process of the preparation method of the flaky nano silver powder comprises the following steps:
s1) adding 37g of polymethacrylamide into 5L of deionized water by stirring, and stirring at a high speed of 2400 r/min; then adding 500g of glucose powder, and continuously stirring to completely dissolve the glucose powder to obtain a mixed solution;
s2) adding 500g of silver acetate into 1L of deionized water, stirring and dissolving completely, then adding 600mL of 25-28% ammonia water until the solution is gradually changed from brown to completely transparent, and preparing into a silver-ammonia solution;
s3) under the condition of 44 ℃, dropwise adding the mixed solution prepared in the step S1) into the silver-ammonia solution at the speed of 15mL/min, and continuing to react for 25min after the dropwise adding is finished, so that the reaction is finished;
s4), after the reaction is finished, centrifuging, and then cleaning and centrifuging by using deionized water to obtain 291.83g of a product; the yield was 90.2%.
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 nano silver powder is characterized by comprising the following steps: dissolving silver salt in a solvent, and adding ammonia water to mix to obtain a silver-ammonia solution; stirring and dissolving the dispersing agent at a high speed, adding the reducing agent, and continuously stirring and dissolving to obtain a mixed solution; adding the silver-ammonia solution into the mixed solution, and reacting under heating to obtain flaky nano silver powder; the dispersant is polymethacrylamide; the reducing agent is glucose.
2. The method for preparing the flaky nano silver powder according to claim 1, characterized in that: the silver salt, the reducing agent and the dispersing agent are as follows in parts by weight: 100-600 parts of silver salt, 100-500 parts of reducing agent and 5-50 parts of dispersing agent.
3. The method for preparing the flaky nano silver powder according to claim 2, characterized in that: the solvent of the mixed solution is deionized water; the concentration of the dispersant is as follows: 1-10 g/L; the concentration of the reducing agent is 20-100 g/L.
4. The method for preparing the flaky nano silver powder according to claim 1, characterized in that: the solvent of the silver ammonia solution is deionized water.
5. The method for preparing the flaky nano silver powder according to claim 4, characterized in that: the silver salt is any one of silver nitrate, silver acetate and silver citrate.
6. The method for preparing the flaky nano silver powder according to any one of claims 1 to 5, characterized in that: the ammonia water is concentrated ammonia water with the mass fraction of 25-28%.
7. The method for preparing the flaky nano silver powder according to any one of claims 1 to 5, characterized in that: the silver-ammonia solution is dripped into the mixed solution at the speed of 5-50 mL/min.
8. The method for preparing the flaky nano silver powder according to claim 7, characterized in that: after the silver ammonia solution is added dropwise, continuing to react for 20-25 min at the reaction temperature of 30-60 ℃; and after the reaction is finished, centrifugally cleaning to obtain the flaky nano silver powder.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112091233A (en) * | 2020-11-19 | 2020-12-18 | 西安宏星电子浆料科技股份有限公司 | Synthesis method of silver nanoparticles |
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