CN114985758B - Preparation method of flake silver powder - Google Patents
Preparation method of flake silver powder Download PDFInfo
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- CN114985758B CN114985758B CN202210903879.5A CN202210903879A CN114985758B CN 114985758 B CN114985758 B CN 114985758B CN 202210903879 A CN202210903879 A CN 202210903879A CN 114985758 B CN114985758 B CN 114985758B
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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
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/068—Flake-like 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
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention provides a preparation method of flake silver powder, which takes ascorbic acid as a reducing agent and utilizes the interaction among the ascorbic acid, nitric acid, silver nitrate and an adsorbent to efficiently and simply prepare the flake silver powder with excellent performance. The growth of silver atoms is controlled by introducing an adsorbent into a reaction system, and the reaction is carried out at a lower temperature to control the reaction rate, so that the morphology of the silver powder is controlled; after silver ions are reduced to obtain silver powder, a small amount of ascorbic acid is added into a reaction system to prevent the silver powder from being dissolved, the flaky silver powder is prepared by the method in one step, the diameter of the prepared silver powder is 10-30 mu m, the diameter-thickness ratio is 20-60, and the flaky silver powder has the characteristics of high diameter-thickness ratio and high brightness.
Description
Technical Field
The invention relates to the technical field of conductive metal powder and a preparation method thereof, in particular to a preparation method of flaky silver powder.
Background
The silver powder is widely applied to conductive silver paste in various electronic related industries due to the unique conductivity and oxidation resistance of the silver powder. The morphology and size of silver powder particles are required to be different according to different specific applications. Compared with spherical silver powder, the flake silver powder is easier to lap to form a conductive path, and the prepared silver paste has higher glossiness. Roughly classified into submicron and micron sizes according to the sheet diameter. Submicron flake silver powder is mostly used for high precision circuit printing, such as photovoltaic and microelectronic industries; the micron-sized flake silver powder is mainly used for circuit printing with lower printing precision requirement, conductive adhesive, electromagnetic shielding coatings and high-end silver coatings for decoration.
At present, the industrial production of the flake silver powder is mainly carried out through a two-step method, the process steps are complicated, uncontrollable variables are easily introduced, the preparation reproducibility is poor, and the product quality is unstable. In the prior art, the invention patent with the application number of 200910074642.5 and the publication date of 2009, 11, month and 4, entitled "a method for preparing flaky micron silver powder" makes silver nitrate and a reducing agent react under an acidic condition, and adds a surfactant and alcohol into a reaction system to further control the reaction rate, so as to achieve the purposes of improving the silver powder preparation efficiency and controlling the morphology of the silver powder. However, in the above technical scheme, a large amount of surfactant and alcohol need to be introduced to achieve the effects of reducing the reaction rate and controlling the morphology of the silver powder.
In view of the above, there is a need for an improved method for preparing a silver flake powder to solve the above problems.
Disclosure of Invention
The invention aims to provide a preparation method of flake silver powder.
In order to achieve the above object, the present invention provides a method for preparing flake silver powder, comprising the steps of:
s1, preparing HNO with pH of 0~2 3 An aqueous solution to the HNO 3 Adding an adsorbent with a certain mass into the aqueous solution, uniformly mixing, adding silver nitrate, and stirring until the silver nitrate is completely dissolved to obtain a silver solution; the adsorbent is citric acid or citrate, and each 100mL of HNO 3 The mass of the silver nitrate added into the aqueous solution is 14 to 18g, and the mass of the adsorbent added into the aqueous solution is 0.05 to 0.1g;
s2, pouring an excessive ascorbic acid aqueous solution with the concentration of 1 to 3mol/L into the silver solution prepared in the step S1 at one time under the conditions of constant temperature of 0 to 25 ℃ and stirring, so that the ascorbic acid aqueous solution reacts with silver ions in the silver solution to obtain a product silver powder; then, fully dispersing the silver powder adhered together in the mixed solution through dispersion treatment; and finally, standing and aging the mixed solution for 1 to 3 hours at room temperature, and then filtering, washing and drying to obtain the flaky silver powder.
Preferably, in step S2, the dispersion treatment is performed by ultrasonic treatment, and a certain amount of ascorbic acid is further added to the mixed solution during the aging process.
Preferably, the rule of addition of the ascorbic acid during the aging process is that every 100mL of the HNO 3 0.5 to 1.5g of the aqueous solution was added.
Preferably, in step S2, the flake silver powder has a flake diameter of 10 to 30 μm and a ratio of diameter to thickness of 20 to 40.
Preferably, in step S1, a low-molecular-weight water-soluble polymer is added to the silver solution, the water-soluble polymer is polyvinyl alcohol or polyethylene glycol, and the addition rule of the water-soluble polymer is that every 100mL of the HNO is added 3 0 to 2g of the aqueous solution is added.
Preferably, in step S2, the ascorbic acid aqueous solution and the silver solution are mixed and then continuously stirred for 3 to 7min.
Preferably, in step S2, the washing is performed by: washing the silver powder with deionized water until the pH value of the surface of the silver powder is neutral, and then fully washing the silver powder with ethanol.
The invention has the beneficial effects that:
1. according to the preparation method of the flake silver powder, ascorbic acid is used as a reducing agent, the growth of silver atoms is controlled by introducing an adsorbent into a reaction system, and the reaction is carried out at a lower temperature, so that the reaction rate is controlled, and the morphology of the silver powder is controlled; after silver ions are reduced to obtain silver powder, a small amount of ascorbic acid is added into a reaction system to prevent the silver powder from being dissolved, the flaky silver powder is prepared by the method in one step, the diameter of the prepared silver powder is 10 to 30 mu m, the diameter-thickness ratio is 20 to 60, and the flaky silver powder has the characteristics of high diameter-thickness ratio and high brightness.
2. According to the preparation method of the flake silver powder, the adsorbent is introduced during preparation of the silver solution, so that on one hand, reduced silver atoms can grow into crystal nuclei, and a large number of crystal nuclei are convenient for the subsequent reduced silver atoms to grow on the crystal nuclei; the morphology of the silver powder is further controlled by controlling the pH and the using amount of the adsorbent; by adding a small amount of ascorbic acid into the system after the silver powder is obtained, the problem that the silver powder is dissolved in the aging process to reduce the yield can be avoided. Particularly, the method provided by the invention can also be used for carrying out surface modification on silver atoms by adding macromolecules, so that the affinity of the powder surface to organic matters is improved, and the method is favorable for further carrying out post-treatment such as organic matter coating on the flaky silver powder and is more suitable for application. In the process, the interaction among the ascorbic acid, the nitric acid, the silver nitrate and the adsorbent can be utilized to efficiently and simply prepare the flake silver powder with excellent performance only by adding a small amount of the adsorbent into a reaction system and carrying out the reaction in an acidic environment.
Drawings
FIG. 1 is an SEM photograph of the plate-like silver powder obtained in example 1 of the present invention;
FIG. 2 is an SEM photograph of the plate-like silver powder obtained in example 2 of the present invention;
FIG. 3 is an SEM photograph of the plate-like silver powder obtained in example 3 of the present invention;
FIG. 4 is an SEM photograph of the plate-like silver powder obtained in example 4 of the present invention;
FIG. 5 is an SEM photograph of the plate-like silver powder obtained in comparative example 1 of the present invention;
FIG. 6 is an SEM image of a plate-like silver powder produced by comparative example 2 of the present invention;
FIG. 7 is an SEM photograph of the plate-like silver powder obtained in comparative example 3 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 will be described in detail with reference to the accompanying drawings and specific embodiments.
It should be noted that, in order to avoid obscuring the present invention with unnecessary details, only the structures and/or processing steps closely related to the aspects of the present invention are shown in the drawings, and other details not closely related to the present invention are omitted.
In addition, it is also to be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
The invention provides a preparation method of flake silver powder, which comprises the following steps:
s1, solution preparation:
preparing HNO with certain pH value 3 Aqueous solution, and to HNO 3 Adding an adsorbent with a certain mass into the aqueous solution, uniformly mixing, adding silver nitrate, and stirring until the silver nitrate is completely dissolved to obtain a silver solution;
s2, preparing silver powder:
under the conditions of certain temperature and stirring, pouring the ascorbic acid aqueous solution into the silver solution prepared in the step S1 at one time, and continuously stirring for 5min to enable the ascorbic acid aqueous solution to react with silver ions in the silver solution to obtain a product silver powder; then, fully dispersing the silver powder adhered together in the mixed solution through dispersion treatment; and finally, adding a certain amount of ascorbic acid into the mixed solution after the reaction, standing and aging the solution for 1 to 3 hours, and filtering, washing and drying the solution to obtain the flaky silver powder.
Preferably, in step S1, a low-molecular-weight water-soluble polymer may be further added to the silver solution, and the surface of the silver flake can be modified by adding the water-soluble polymer, so as to improve the affinity of the surface of the silver flake for organic substances, and facilitate further post-treatment such as organic matter coating of the silver flake; wherein the water soluble polymer is polyvinyl alcohol or polyethylene glycol, etc., and the addition rule of the water soluble polymer is HNO per 100mL 3 0 to 2g of the aqueous solution is added.
Preferably, in step S1, HNO 3 The pH of the aqueous solution is 0 to 2 3 The aqueous solution is used for adjusting the pH value of the silver solution, so that an acid environment is provided for oxidizing and reducing silver ions into silver atoms subsequently, the acid environment can slow down the oxidation-reduction reaction rate, and the shape of the silver powder can be favorably adjusted.
Preferably, inIn step S1, the adsorbent is added according to the rule of every 100mL of HNO 3 Adding 0.05 to 0.1g of silver nitrate into the aqueous solution according to the rule of adding per 100mL of HNO 3 14 to 18g of the aqueous solution was added.
Preferably, in step S1, the adsorbent is citric acid or citrate, and the added adsorbent can adsorb on the specific crystal surface of the crystal nucleus to hinder the growth of silver atoms on the specific crystal surface of the crystal nucleus, thereby finally obtaining the plate-like silver powder product, and when the amount of the adsorbent is in the above range, the final silver powder having a high aspect ratio can be ensured.
Preferably, in step S2, the concentration of the aqueous ascorbic acid solution is 1 to 3mol/L, and the amount of the aqueous ascorbic acid solution added is excessive so that the content of the ascorbic acid in the aqueous ascorbic acid solution is 1.1 to 1.5 times the theoretical amount used for sufficiently reducing silver ions in the silver solution, and the theoretical amount used herein refers to the mass or amount of the substance required for the reaction between the reactants according to the stoichiometric ratio.
Preferably, in step S2, the dispersion treatment is performed by ultrasonic treatment.
Preferably, the ascorbic acid is added on a regular basis per 100mL of HNO during aging 3 0.5 to 1.5g of ascorbic acid is added into the aqueous solution, so that the reaction system can keep reducibility all the time in the aging process, thereby improving the reaction yield.
Preferably, in step S2, the washing process is performed by: washing the silver powder with deionized water until the pH value of the surface of the silver powder is neutral, and then fully washing the silver powder with ethanol.
Preferably, in step S2, the temperature is 0 to 25 ℃.
Preferably, in step S2, the prepared sheet-like silver powder has a diameter of 10 to 30 μm and a ratio of diameter to thickness of 20 to 40.
The invention is further illustrated by the following specific examples:
example 1
Adding 2mL of concentrated nitric acid into 100mL of deionized water to obtain a solution with the pH value of 0.6, adding 0.05g of citric acid into the solution, fully mixing, adding 16g of silver nitrate, and stirring until the silver nitrate is completely dissolved to obtain a silver solution. 8.5g of ascorbic acid was added to 100mL of deionized water, and stirred until completely dissolved, to obtain an aqueous ascorbic acid solution. Adding ascorbic acid aqueous solution into silver solution at a constant temperature of 25 deg.C under mechanical stirring, and maintaining mechanical stirring for 5min. And adding 1g of ascorbic acid into the mixed solution obtained by the reaction, treating the mixture by ultrasonic waves to disperse the silver powder adhered together, standing and aging the mixture for 1h, filtering the mixture, washing the mixture by deionized water until the pH value of the surface of the silver powder is neutral, fully washing the silver powder by ethanol, and drying the silver powder to obtain the target silver powder product. The SEM image of the silver flake prepared in this example is shown in FIG. 1, and it can be seen that the silver flake exhibits a more regular hexagonal-like shape, and has the characteristics of high aspect ratio and high brightness.
Example 2
Adding 10mL of concentrated nitric acid into 100mL of deionized water to obtain a solution with the pH value of 0, adding 0.15g of citric acid and 2g of polyvinyl alcohol into the solution, fully mixing, adding 16g of silver nitrate, and stirring until the silver nitrate is completely dissolved to obtain the silver solution. 12g of ascorbic acid was added to 100mL of deionized water, and stirred until completely dissolved, to obtain an aqueous ascorbic acid solution. Adding ascorbic acid water solution into silver solution at 0 deg.C under mechanical stirring, and maintaining mechanical stirring for 5min. And adding 0.1g of ascorbic acid into the mixed solution obtained by the reaction, treating the mixed solution by ultrasonic waves to disperse the silver powder adhered together, standing and aging the mixture for 3 hours, filtering the mixture, washing the mixture by deionized water until the pH value of the surface of the silver powder is neutral, fully washing the silver powder by ethanol, and drying the silver powder to obtain the target silver powder product. The SEM image of the silver flake prepared in this example is shown in FIG. 2, and it can be seen that the silver flake exhibits a more regular hexagonal-like shape, and has the characteristics of high aspect ratio and high brightness. Since the reaction in this example was carried out at 0 ℃ which is lower than that in example 1, the rate of formation of silver atoms was slow, and the rate of further growth of silver atoms on the crystal nuclei was faster than that of silver atoms, so that a silver powder having a larger plate diameter could be obtained. In addition, as can be seen from fig. 2, the introduction of the polyvinyl alcohol does not affect the morphology of the silver powder, and the polyvinyl alcohol is used for modifying the surface of the silver powder, so as to improve the affinity of the surface of the powder to organic matters and reduce the difficulty of organic coating of the silver powder.
Example 3
Adding 8mL of concentrated nitric acid into 100mL of deionized water to obtain a solution with the pH value of 0, adding 0.1g of citric acid into the solution, mixing fully, adding 16g of silver nitrate, and stirring until the silver nitrate is completely dissolved to obtain a silver solution. 12g ascorbic acid is added into 100mL deionized water and stirred until the ascorbic acid is completely dissolved, thus obtaining an ascorbic acid aqueous solution. Adding ascorbic acid water solution into silver solution at 25 deg.C under mechanical stirring, and maintaining mechanical stirring for 5min. And adding 0.1g of ascorbic acid into the mixture obtained by the reaction, treating the mixture by ultrasonic waves to disperse the silver powder adhered together, standing and aging the mixture for 3 hours, filtering the mixture, washing the mixture by deionized water until the pH value of the surface of the silver powder is neutral, fully washing the silver powder by ethanol, and drying the silver powder to obtain the target silver powder product. The SEM image of the silver flake powder obtained in this example is shown in FIG. 3, and it can be seen that the silver flake powder obtained exhibits a more regular hexagonal-like shape, and has the characteristics of high aspect ratio and high brightness.
Example 4
Adding 6mL of concentrated nitric acid into 100mL of deionized water to obtain a solution with the pH value of 0, adding 0.10g of citric acid into the solution, mixing fully, adding 16g of silver nitrate, and stirring until the silver nitrate is completely dissolved to obtain a silver solution. 12g of ascorbic acid was added to 100mL of deionized water, and stirred until completely dissolved, to obtain an aqueous ascorbic acid solution. Adding ascorbic acid water solution into silver solution at 25 deg.C under mechanical stirring, and maintaining mechanical stirring for 5min. And adding 0.1g of ascorbic acid into the mixture obtained by the reaction, treating the mixture by ultrasonic waves to disperse the silver powder adhered together, standing and aging the mixture for 2 hours, filtering the mixture, washing the mixture by deionized water until the pH value of the surface of the silver powder is neutral, fully washing the silver powder by ethanol, and drying the silver powder to obtain the target silver powder product. As shown in FIG. 4, the SEM image of the silver flake obtained in this example shows that the silver flake exhibits a more regular hexagonal-like shape, and has the characteristics of high aspect ratio and high brightness. As can be seen by comparing FIG. 3 with FIG. 4, the morphology of the silver powder is different, and the result shows that the aging time has an influence on the morphology of the silver powder.
Comparative example 1
Comparative example 1 differs from example 1 only in that: the adsorbent citric acid was not added, and the other steps were substantially the same as in example 1 and will not be described herein. The SEM image of the silver powder obtained in this example is shown in FIG. 5, from which it can be seen that the product silver powder exhibits a spheroidal state with high crystallinity, since the reduced silver atoms are directly deposited on the surface of the crystal nuclei and grow.
Comparative example 2
Comparative example 2 differs from example 1 only in that: the mass of citric acid was 0.2g, and other steps were substantially the same as in example 1 and will not be described herein again. The SEM image of the silver powder prepared in this example is shown in FIG. 6, from which it can be seen that the product exhibits a highly crystallized slab-like shape, because the excessive amount of the adsorbent adsorbs to the crystal planes, reducing the growth variability of the crystal planes.
Comparative example 3
Comparative example 3 differs from example 1 only in that: the aging process was carried out without adding ascorbic acid, and the other steps were substantially the same as in example 1, and thus, detailed description thereof is omitted. The SEM image of the silver powder obtained in this example is shown in FIG. 7, from which it can be seen that the edges of the silver flakes exhibited some traces of corrosion.
In summary, the method for preparing the silver flake according to the present invention uses ascorbic acid as a reducing agent, and utilizes the interaction between ascorbic acid, nitric acid, silver nitrate and an adsorbent to efficiently and easily prepare the silver flake with excellent performance. The growth of silver atoms is controlled by introducing an adsorbent into a reaction system, and the reaction is carried out at a lower temperature to control the reaction rate, so that the morphology of the silver powder is controlled; after silver ions are reduced to obtain silver powder, a small amount of ascorbic acid is added into a reaction system to prevent the silver powder from being dissolved, the flaky silver powder is prepared by the method in one step, the diameter of the prepared silver powder is 10-30 mu m, the diameter-thickness ratio is 20-60, and the flaky silver powder has the characteristics of high diameter-thickness ratio and high brightness. Because the consumption of raw materials in the preparation process is low, the organic matter content in the wastewater is effectively reduced, and the cost of the preparation process can be reduced.
Although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the spirit and scope of the present invention.
Claims (6)
1. A preparation method of flaky silver powder is characterized by comprising the following steps:
s1, preparing HNO with pH of 0~2 3 An aqueous solution to the HNO 3 Adding an adsorbent with a certain mass into the aqueous solution, uniformly mixing, adding silver nitrate, and stirring until the silver nitrate is completely dissolved to obtain a silver solution; the adsorbent is citric acid or citrate, and each 100mL of HNO 3 The mass of the silver nitrate added into the aqueous solution is 14 to 18g, and the mass of the adsorbent added into the aqueous solution is 0.05 to 0.1g;
s2, pouring an excessive ascorbic acid aqueous solution with the concentration of 1 to 3mol/L into the silver solution prepared in the step S1 at one time under the conditions of constant temperature of 0 to 25 ℃ and stirring, and reacting the ascorbic acid aqueous solution with silver ions in the silver solution to obtain a product silver powder; then, fully dispersing the silver powder adhered together in the mixed solution through dispersion treatment; and finally, standing and aging the mixed solution for 1 to 3 hours at room temperature, and then filtering, washing and drying to obtain the sheet-shaped silver powder with the diameter of 10 to 30 mu m and the diameter-thickness ratio of 20 to 40.
2. The method for producing the silver flake according to claim 1, wherein the dispersion treatment is performed by ultrasonic treatment in step S2, and a certain amount of ascorbic acid is added to the mixture during the aging process.
3. The method for producing the plate-like silver powder according to claim 2, wherein the ascorbic acid is added in a regular amount per 100mL of the HNO during the aging process 3 0.5 to 1.5g of the aqueous solution was added.
4. The method for producing the plate-like silver powder according to claim 1, further comprising adding a low molecular weight water-soluble polymer to the silver solution in step S1, wherein the water-soluble polymer is polyvinyl alcohol or polyethylene glycol, and the water-soluble polymer is added in a regular amount of HNO per 100mL 3 0 to 2g of the aqueous solution is added.
5. The method for producing the silver flake powder according to claim 1, wherein the aqueous ascorbic acid solution and the silver solution are mixed together and then continuously stirred for 3 to 7min in step S2.
6. The method for producing the plate-like silver powder according to claim 1, wherein in step S2, the washing is performed by: washing the silver powder with deionized water until the pH value of the surface of the silver powder is neutral, and then fully washing the silver powder with ethanol.
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