CN119304200A - A kind of high sphericity ultrafine silver powder and its preparation method and application - Google Patents
A kind of high sphericity ultrafine silver powder and its preparation method and application Download PDFInfo
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Abstract
本发明提供了一种高球形度超细银粉及其制备方法和应用，上述高球形度超细银粉的制备方法在通过化学还原法制备超细银粉的同时，加入了水热法辅助，通过水热法对温度、反应时间等参数的调节，精确控制银粉的晶核生长过程，从而实现对颗粒尺寸和形貌的调控，制备了一种性能优异的粒径均一、具有高球形度的用于导电浆料制备的超细银粉，进而使得通过本发明中高球形度超细银粉制得的导电浆料具有优异的导电性能。
The present invention provides an ultrafine silver powder with high sphericity, a preparation method and application thereof. The preparation method of the ultrafine silver powder with high sphericity adds a hydrothermal method to assist while preparing the ultrafine silver powder by a chemical reduction method. The hydrothermal method adjusts parameters such as temperature and reaction time to accurately control the crystal nucleus growth process of the silver powder, thereby achieving regulation of particle size and morphology, and preparing an ultrafine silver powder with uniform particle size and high sphericity for preparing a conductive paste with excellent performance, thereby making the conductive paste prepared by the ultrafine silver powder with high sphericity in the present invention have excellent conductive properties.
Description
Technical Field
The invention relates to the technical field of noble metal powder materials, in particular to high sphericity superfine silver powder, a preparation method and application thereof.
Background
With global energy conversion and the proliferation of demand for clean energy, the photovoltaic industry is rapidly expanding worldwide. To cope with this demand, various large photovoltaic manufacturers are continually seeking methods for improving the efficiency of the battery and reducing the cost, and silver powder is one of the core targets of optimization as a key material of positive electrode silver paste. The superfine silver powder with high sphericity is taken as an important component of the light Fu Zheng silver, and the physical form and the particle size characteristic of the silver powder can directly influence the performance, the production cost and the overall market competitiveness of the photovoltaic cell by influencing the performance of the positive electrode silver paste, so that the silver powder has important effects on improving the efficiency of the photovoltaic cell, reducing the production cost and realizing material optimization.
At present, in the industrial production process, the liquid phase chemical reduction method is a main method for preparing spherical silver powder, has the advantages of lower production cost, relatively simple process route and the like, however, in the actual preparation process of superfine silver powder, the strict control of the particle size and the particle size distribution is very difficult, the phenomenon of uneven particle size or particle aggregation is easy to occur, and the sphericity of the silver powder is difficult to ensure. Therefore, there is a need for a high sphericity ultrafine silver powder, and a preparation method and application thereof, so as to meet the application requirements of clients.
Disclosure of Invention
The invention aims to solve the technical problems that sphericity is difficult to ensure and particle size is difficult to control in the existing silver powder preparation process.
In order to solve the technical problems, the invention firstly provides a preparation method of high sphericity superfine silver powder, which comprises the following steps:
s1, mixing a silver nitrate solution, a dispersing agent, a buffering agent, a coating agent, a reducing agent and a solvent to obtain a reaction suspension;
S2, carrying out heating and heat preservation treatment on the reaction suspension, and cooling to obtain a solid-liquid mixture, wherein the heating temperature of the heating and heat preservation treatment is 100-200 ℃, and the heat preservation time is 2-5 h;
S3, carrying out sedimentation treatment on the solid-liquid mixture to obtain a precipitate, and then carrying out washing and drying treatment on the precipitate to obtain the high-sphericity superfine silver powder.
Preferably, the reaction suspension in the step S1 comprises, by mass, 20-30 parts of silver nitrate solution, 1-10 parts of dispersing agent, 1-5 parts of buffering agent, 0.5-5 parts of coating agent, 5-20 parts of reducing agent and 300-600 parts of solvent.
Preferably, the step S1 specifically includes:
S11, mixing a reducing agent and a part of solvent, and stirring until the reducing agent and the part of solvent are dissolved to obtain a first mixed solution;
s12, mixing a buffering agent, a dispersing agent and another part of solvent, and stirring until the mixture is dissolved to obtain a second mixed solution;
And S13, sequentially adding the silver nitrate solution, the coating agent and the first mixed solution into the second mixed solution, and stirring at a uniform speed to obtain a reaction suspension.
Preferably, in the step S11, the reducing agent is at least one of ascorbic acid, formaldehyde, glucose, ethylene glycol and hydrazine hydrate.
Preferably, in the step S12, the buffer is at least one of acetic acid, sodium acetate, sodium citrate, phosphoric acid, boric acid, sodium borate and sodium bicarbonate, and the dispersing agent is at least one of polyvinylpyrrolidone, polyethylene glycol, sodium dodecyl sulfonate, sodium polyacrylate and tween.
Preferably, in the step S13, the coating agent is at least one of oleic acid, lauric acid, silane coupling agent and stearic acid.
Preferably, the solvent is water, and the stirring speed in the step S11, the step S12 and the step S13 is 300-500r/min.
Preferably, the step S3 specifically includes:
s31, carrying out sedimentation treatment on the solid-liquid mixture, and removing supernatant to obtain a precipitate;
S32, mixing the precipitate with ethanol, performing first centrifugation, mixing the precipitate with deionized water, and performing second centrifugation until the precipitate is washed until the conductivity is less than 20 mu S/m, so as to obtain wet silver powder;
s33, drying the wet silver powder at 60 ℃, and sieving the wet silver powder with a 300-mesh sieve to finally obtain the high-sphericity ultrafine silver powder.
Correspondingly, the invention also provides the high-sphericity superfine silver powder prepared by the preparation method of the high-sphericity superfine silver powder, wherein the particle size of the high-sphericity superfine silver powder is 0.82-3.53 mu m, the tap density is 6.24g/cm 3, and the specific surface area is 0.32m 2/g.
Correspondingly, the invention also provides application of the high sphericity superfine silver powder in preparing conductive silver paste.
The invention has the beneficial effects that the preparation method of the high-sphericity superfine silver powder is different from the situation of the prior art, is added with the assistance of a hydrothermal method while preparing the superfine silver powder by a chemical reduction method, and accurately controls the crystal nucleus growth process of the silver powder by adjusting parameters such as temperature, reaction time and the like by the hydrothermal method, so that the regulation and control of the particle size and morphology are realized, the superfine silver powder which has excellent performance and uniform particle size and high sphericity and is used for preparing the conductive paste is prepared, and the conductive paste prepared from the high-sphericity superfine silver powder has excellent conductive performance.
Drawings
FIG. 1 is a flow chart of a preparation method of high sphericity superfine silver powder provided by the embodiment of the invention;
FIG. 2 is an electron microscope image of the high sphericity ultrafine silver powder provided in example 1 of the present invention;
fig. 3 is an electron microscopic view of the high sphericity ultrafine silver powder provided in comparative example 1.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present invention without making any inventive effort, are intended to fall within the scope of the present invention.
Aiming at the problems that the morphology of particles is diversified due to unbalanced crystal growth in the existing preparation and production processes of superfine silver powder, irregular particles are generated, local supersaturation of chemical reaction or uneven reduction conditions can cause the morphology of the silver powder, the invention provides the preparation method of the superfine silver powder with high sphericity. The sample printed by the prepared conductive silver paste has low volume resistivity and excellent conductivity, and the silver powder synthesis process has the characteristics of simplicity and convenience in operation and no toxicity, and is suitable for mass production.
In order to achieve the technical purpose, the application adopts the following technical scheme:
In a first aspect, the present invention provides a method for preparing high sphericity ultrafine silver powder.
Referring to fig. 1, fig. 1 is a flowchart of a method for preparing high sphericity ultrafine silver powder according to an embodiment of the present invention, where the preparation method specifically includes:
s1, mixing a silver nitrate solution, a dispersing agent, a buffering agent, a coating agent, a reducing agent and a solvent to obtain a reaction suspension.
Specifically, the step S1 specifically includes:
S11, mixing a reducing agent and a part of solvent, and stirring until the reducing agent and the part of solvent are dissolved to obtain a first mixed solution;
s12, mixing a buffering agent, a dispersing agent and another part of solvent, and stirring until the mixture is dissolved to obtain a second mixed solution;
And S13, sequentially adding the silver nitrate solution, the coating agent and the first mixed solution into the second mixed solution, and stirring at a uniform speed to obtain a reaction suspension.
Further, the solvent in the step S11 and the step S12 is water, and the stirring speed in the step S11, the step S12 and the step S13 is set to 300-500 r/min.
Further, in the step S13, a silver nitrate solution is added first, and then a first mixed solution is added, wherein the adding time of the first mixed solution is 10-20S, and the stirring time is 15min, and the silver nitrate possibly plays a key initiating role in a system. The silver nitrate solution is added first to make the silver nitrate solution disperse fully in the system and react gradually with other components added later, so that the initiation and progress of the reaction can be controlled better. If the first mixed solution is added first, the reducing agent in the first mixed solution can react with other substances in the system prematurely, so that the reaction is difficult to control, and the quality and the performance of the product are affected.
In the step S11, the reducing agent is at least one of ascorbic acid, formaldehyde, glucose, glycol and hydrazine hydrate, wherein the silver nitrate solution and the reducing agent undergo oxidation-reduction reaction, so that silver ions in the solution are reduced into silver powder, and the consumption of the reducing agent is 5% -10% higher than the theoretical value of the stoichiometric ratio, so that the effect of thoroughly reducing the silver ions in the solution is achieved.
In the step S12, the buffer is at least one of acetic acid, sodium acetate, sodium citrate, phosphoric acid, boric acid, sodium borate and sodium bicarbonate, wherein the buffer is used for adjusting and stabilizing the pH value, so that the reduction process of silver ions is ensured to be carried out in a controllable range. The silver powder reducing agent not only can regulate and control the reducing rate and avoid particle agglomeration and side reaction, but also can influence the morphology and particle size distribution of the silver powder, and further improves the quality and performance of the silver powder.
In the step S12, the dispersing agent is at least one of polyvinylpyrrolidone, polyethylene glycol, sodium dodecyl sulfate, sodium polyacrylate and tween, wherein the dispersing agent mainly has the effects of preventing silver powder particles from agglomerating, improving particle dispersibility, controlling particle morphology, stabilizing a solution system and the like. By selecting a proper dispersing agent, the quality, uniformity and processing performance of the silver powder can be obviously improved, and the application effect of the silver powder in the fields of photovoltaics, electronics and the like is optimized.
In the step S13, the coating agent is at least one of oleic acid, lauric acid, silane coupling agent and stearic acid, wherein the coating agent mainly plays roles of preventing oxidation, controlling particle growth, avoiding agglomeration, improving dispersibility and sintering performance and the like by forming a protective layer on the surface of the particles. The proper coating agent can not only improve the quality of silver powder, but also improve the performance of silver powder in storage, transportation and subsequent application.
In the step S1, the reaction suspension comprises, by mass, 20-30 parts of silver nitrate solution, 1-10 parts of dispersing agent, 1-5 parts of buffering agent, 0.5-5 parts of coating agent, 5-20 parts of reducing agent and 300-600 parts of solvent.
Specifically, the silver nitrate solution is used in an amount of 20-30 parts, so that not only is enough silver ions ensured to participate in the reaction to obtain the required product amount, but also waste or unnecessary side reactions caused by excessive use amount are avoided.
The dispersing agent is used in an amount of 1-10 parts, so that aggregation of silver powder particles can be effectively prevented, the particles can keep good dispersibility through electrostatic repulsion or steric hindrance effect, and uniformly distributed superfine silver powder can be obtained, when the dispersing agent is used in an insufficient amount, aggregation of the particles cannot be effectively inhibited, mutual adsorption among the silver powder particles is caused, large particles or aggregation phenomenon is finally formed, particle size distribution and performance of a product are affected, when the dispersing agent is used in an excessive amount, an excessively thick molecular layer is formed on the surfaces of the particles, repulsive force among the particles is too large, the particles are difficult to approach, and sintering and conductivity are possibly affected. In addition, excessive dispersant residue may also affect the purity of silver powder.
Specifically, the buffer is used in an amount ranging from 1 to 5 parts, so that the pH value of the whole system can be effectively adjusted, and adverse effects on the reaction caused by excessive buffer use are avoided.
Specifically, the coating agent is used in an amount of 0.5 to 5 parts to effectively exert its coating effect, and excessive coating agent may affect the performance of silver particles or increase the cost.
Specifically, the amount of the reducing agent is 5-20 parts, which is required to be matched with the amount of the silver nitrate solution to ensure that silver ions can be sufficiently reduced. At the same time, the usage amount of the reducing agent cannot be too large so as not to generate side reactions or influence the quality of the product.
Specifically, the solvent is used in an amount of 300-600 parts, so that other reactants can be fully dissolved and dispersed, and a uniform reaction system is formed. At the same time, the solvent is not used too much to avoid affecting the concentration and efficiency of the reaction.
S2, carrying out heating and heat preservation treatment on the reaction suspension, and cooling to obtain a solid-liquid mixture, wherein the heating temperature of the heating and heat preservation treatment is 100-200 ℃, and the heat preservation time is 2-5 h.
Specifically, the step S2 further includes:
Firstly, transferring the reaction suspension into a high-pressure reaction kettle for heating and preserving heat, wherein the heating temperature is 100-200 ℃ and the preserving heat time is 2-5 h, in the temperature range, the thermal movement of molecules is aggravated, the collision frequency between reactants is increased, the reaction is facilitated, meanwhile, the higher temperature can reduce the activation energy of the reaction, so that the reaction is easier to occur, and meanwhile, the degree of the reaction can be adjusted by controlling the preserving heat time, and the excessive or insufficient reaction is avoided.
And then pouring out the solid-liquid mixture in the reaction kettle after the reaction kettle is cooled.
S3, carrying out sedimentation treatment on the solid-liquid mixture to obtain a precipitate, and then carrying out washing and drying treatment on the precipitate to obtain the high-sphericity superfine silver powder.
Specifically, the step S3 further includes:
s31, carrying out sedimentation treatment on the solid-liquid mixture, and removing supernatant to obtain a precipitate;
S32, mixing the precipitate with ethanol, performing first centrifugation, mixing the precipitate with deionized water, and performing second centrifugation until the precipitate is washed until the conductivity is less than 20 mu S/m to obtain wet silver powder, wherein the washing of the precipitate until the conductivity is less than 20 mu S/m indicates that the content of ionic impurities in the precipitate is very low, and the requirement of higher purity is met;
S33, drying the wet silver powder at 60 ℃ and sieving the wet silver powder with a 300-mesh sieve to finally obtain the high-sphericity ultrafine silver powder, wherein large-particle impurities and agglomerates in the silver powder can be removed through sieving treatment to obtain the high-sphericity ultrafine silver powder with uniform particle size, and the 300-mesh sieve has smaller pore diameter, so that silver powder particles meeting the requirements can be effectively screened out, and the quality and performance of products are improved.
Correspondingly, the invention also provides the high-sphericity superfine silver powder prepared by the preparation method of the high-sphericity superfine silver powder, wherein the particle size of the high-sphericity superfine silver powder is 0.82-3.53 mu m, the tap density is 6.24g/cm 3, and the specific surface area is 0.32m 2/g.
Specifically, in the high-sphericity ultrafine silver powder provided by the invention, the particle size distribution is uniform, the surface has certain roughness, and no agglomeration phenomenon occurs, so that the conductive paste prepared from the high-sphericity ultrafine silver powder has excellent conductive performance.
Correspondingly, the invention also provides application of the high sphericity superfine silver powder in preparing conductive silver paste.
The technical scheme of the invention is further described with reference to specific embodiments.
Example 1:
this embodiment 1 provides a high sphericity ultrafine silver powder and a preparation method thereof, the preparation method comprises the following steps:
step one, preparing liquid:
Taking 500ml of ethylene glycol, adding 500ml of deionized water, and uniformly stirring to obtain a solution A;
adding 160g of silver nitrate into a beaker, adding 500ml of deionized water, and stirring for dissolution to obtain a solution B;
Adding 10g of polyvinylpyrrolidone into a beaker, dissolving in 500ml of deionized water, stirring and dissolving, adding 3g of sodium citrate and 11.5g of sodium acetate, and stirring and dissolving to obtain solution C;
Adding 0.5g of oleic acid into a beaker, adding 10ml of absolute ethyl alcohol, and stirring for dissolution to obtain a solution D;
step two, silver powder preparation:
Adding the solution B into the solution C, starting stirring, setting the stirring speed to be 500rpm, adding the solution A into the solution C, controlling the time from the beginning to the end of the adding of the solution A to be 10-20 s, setting the stirring time to be 5min, adding the solution D after the stirring is ended, continuing stirring for 10min, and ending the reaction;
Transferring the reaction suspension prepared after the reaction is finished into a high-pressure reaction kettle, heating to 180 ℃, and preserving heat for 3 hours;
after the heat preservation is finished and the reaction kettle is cooled, carrying out sedimentation treatment on the reaction suspension, pouring out supernatant fluid to obtain reaction sediment;
washing and stirring the mixture by using absolute ethyl alcohol, wherein the stirring speed is set to 800rpm, and the stirring time is set to 10min; after stirring, separating absolute ethyl alcohol and silver powder through centrifugal treatment, cleaning and stirring through deionized water, wherein the stirring speed is set to 800rpm, and the stirring time is set to 10min;
The wet silver powder was dried at 60C for 12 hours, and after the drying was completed, it was sieved through a 300 mesh sieve to obtain high sphericity ultrafine silver powder, as shown in fig. 2.
Example 2:
step one, preparing liquid:
taking 86.4g of ascorbic acid, adding 500ml of deionized water, and uniformly stirring to obtain solution A;
adding 160g of silver nitrate into a beaker, adding 500ml of deionized water, and stirring for dissolution to obtain a solution B;
Adding 10g of polyvinylpyrrolidone into a beaker, dissolving in 500ml of deionized water, stirring and dissolving, adding 3g of boric acid and 11.5g of sodium borate, and stirring and dissolving to obtain solution C;
solution D is prepared by adding 0.5g oleic acid into a beaker, adding 10ml absolute ethanol, and stirring for dissolution.
Step two, silver powder preparation:
Adding the solution B into the solution C, starting stirring, setting the stirring speed to be 500rpm, adding the solution A into the solution C, controlling the time from the beginning to the end of the adding of the solution A to be 10-20 s, setting the stirring time to be 5min, adding the solution D after the stirring is ended, continuing stirring for 10min, and ending the reaction;
Transferring the reaction suspension prepared after the reaction is finished into a high-pressure reaction kettle, heating to 180 ℃, and preserving heat for 3 hours;
after the heat preservation is finished and the reaction kettle is cooled, carrying out sedimentation treatment on the reaction suspension, pouring out supernatant fluid to obtain reaction sediment;
washing and stirring the mixture by using absolute ethyl alcohol, wherein the stirring speed is set to 800rpm, and the stirring time is set to 10min; after stirring, separating absolute ethyl alcohol and silver powder through centrifugal treatment, cleaning and stirring through deionized water, wherein the stirring speed is set to 800rpm, and the stirring time is set to 10min;
and (3) drying the wet silver powder at 60 ℃ for 12 hours, and sieving the wet silver powder with a 300-mesh sieve after the drying is finished to obtain the high-sphericity superfine silver powder.
Example 3:
step one, preparing liquid:
taking 86.4g of glucose, adding 500ml of deionized water, and uniformly stirring to obtain solution A;
adding 160g of silver nitrate into a beaker, adding 500ml of deionized water, and stirring for dissolution to obtain a solution B;
Adding 10g of polyethylene glycol into a beaker, dissolving in 500ml of deionized water, stirring and dissolving, adding 3g of sodium citrate and 11.5g of sodium acetate, and stirring and dissolving to obtain solution C;
adding 0.5g of lauric acid into a beaker, adding 10ml of absolute ethyl alcohol, and stirring for dissolution to obtain a solution D;
step two, silver powder preparation:
Adding the solution B into the solution C, starting stirring, setting the stirring speed to be 500rpm, adding the solution A into the solution C, controlling the time from the beginning to the end of the adding of the solution A to be 10-20 s, setting the stirring time to be 5min, adding the solution D after the stirring is ended, continuing stirring for 10min, and ending the reaction;
Transferring the reaction suspension prepared after the reaction is finished into a high-pressure reaction kettle, heating to 180 ℃, and preserving heat for 3 hours;
after the heat preservation is finished and the reaction kettle is cooled, carrying out sedimentation treatment on the reaction suspension, pouring out supernatant fluid to obtain reaction sediment;
washing and stirring the mixture by using absolute ethyl alcohol, wherein the stirring speed is set to 800rpm, and the stirring time is set to 10min; after stirring, separating absolute ethyl alcohol and silver powder through centrifugal treatment, cleaning and stirring through deionized water, wherein the stirring speed is set to 800rpm, and the stirring time is set to 10min;
and (3) drying the wet silver powder at 60 ℃ for 12 hours, and sieving the wet silver powder with a 300-mesh sieve after the drying is finished to obtain the high-sphericity superfine silver powder.
Comparative example 1:
step one, preparing liquid:
Taking 500ml of ethylene glycol, adding 500ml of deionized water, and uniformly stirring to obtain a solution A;
adding 160g of silver nitrate into a beaker, adding 500ml of deionized water, and stirring for dissolution to obtain a solution B;
Adding 10g of polyvinylpyrrolidone into a beaker, dissolving in 500ml of deionized water, stirring and dissolving, adding 3g of sodium citrate and 11.5g of sodium acetate, and stirring and dissolving to obtain solution C;
Adding 0.5g of oleic acid into a beaker, adding 10ml of absolute ethyl alcohol, and stirring for dissolution to obtain a solution D;
step two, silver powder preparation:
Adding the solution B into the solution C, starting stirring, setting the stirring speed to be 500rpm, adding the solution A into the solution C, controlling the time from the beginning to the end of the adding of the solution A to be 10-20 s, setting the stirring time to be 5min, adding the solution D after the stirring is ended, continuing stirring for 10min, and ending the reaction;
Washing and stirring the silver powder by using absolute ethyl alcohol, wherein the stirring speed is set to 800rpm, and the stirring time is set to 10min;
washing and stirring with deionized water at 800rpm for 10min until the conductivity of the washing liquid is less than 20 mu S/m to obtain wet silver powder;
the wet silver powder was dried at 60C for 12 hours, and after the drying was completed, it was sieved through a 300 mesh sieve to obtain high sphericity ultrafine silver powder, as shown in fig. 3.
Performance tests were performed on the silver powders prepared in examples 1 to 3 and comparative example 1, and the test results are shown in table 1:
table 1 performance index of examples 1 to 3 and comparative example 1
Specifically, comparative example 1 was compared with examples 1 to 3, and the hydrothermal pot heat preservation treatment was not performed. Examples 1-3 all adopt a hydrothermal method to assist silver powder preparation, and the hydrothermal method has various advantages in silver powder preparation, including controllable particle size and morphology, good dispersibility, high purity, mild reaction conditions and the like. The advantages enable the hydrothermal method to have unique advantages when preparing high-quality superfine silver powder, and the hydrothermal method is suitable for the fields with high requirements on silver powder performance, such as conductive silver paste, conductive ink and the like.
As can be seen from Table 1, the high sphericity ultrafine silver powder prepared in example 1 has smaller particle size, D100 is kept below 3.53 μm, the particle size distribution is relatively uniform, the apparent density is 4.28g/cm 3, the tap density is higher, the tap density reaches 6.24g/cm 3, and the performance of the ultrafine silver powder prepared in example 1 is greatly improved compared with that of the ultrafine silver powder prepared in comparative example 1 without hydrothermal assistance.
The invention discloses high sphericity superfine silver powder, a preparation method and application thereof, and belongs to the field of noble metal powder materials. The grain size of the superfine silver powder prepared by the preparation method is 0.82-3.53 mu m, tap density is 6.24g/cm 3, and specific surface area is 0.32m 2/g. The spherical silver powder prepared by the invention has high sphericity, high dispersity, good particle size distribution and uniformity, and the surface of the silver powder has certain roughness. The sample printed by the prepared conductive silver paste has low volume resistivity and excellent conductivity, and the synthesis process of the silver powder has the characteristics of simple and convenient operation and no toxicity.
According to the invention, the hydrothermal method is added while preparing the superfine silver powder by the chemical reduction method, so that the novel silver powder preparation method is provided, and the crystal nucleus growth process of the silver powder is accurately controlled by adjusting parameters such as temperature, reaction time and the like by the hydrothermal method, so that the regulation and control of the particle size and morphology are realized, and the superfine silver powder which has excellent performance, uniform particle size and high sphericity and is used for preparing the conductive paste is prepared.
It should be noted that, the foregoing embodiments all belong to the same inventive concept, and the descriptions of the embodiments have emphasis, and where the descriptions of the individual embodiments are not exhaustive, reference may be made to the descriptions of the other embodiments.
The foregoing examples merely illustrate embodiments of the invention and are described in more detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (10)
1. The preparation method of the high sphericity superfine silver powder is characterized by comprising the following steps of:
s1, mixing a silver nitrate solution, a dispersing agent, a buffering agent, a coating agent, a reducing agent and a solvent to obtain a reaction suspension;
S2, carrying out heating and heat preservation treatment on the reaction suspension, and cooling to obtain a solid-liquid mixture, wherein the heating temperature of the heating and heat preservation treatment is 100-200 ℃, and the heat preservation time is 2-5 h;
s3, carrying out sedimentation treatment on the solid-liquid mixture to obtain a precipitate, and then carrying out cleaning and drying treatment on the precipitate to obtain the high sphericity superfine silver powder.
2. The preparation method of the high sphericity ultrafine silver powder according to claim 1, wherein the reaction suspension in the step S1 comprises the following components, by mass, 20-30 parts of silver nitrate solution, 1-10 parts of dispersing agent, 1-5 parts of buffering agent, 0.5-5 parts of coating agent, 5-20 parts of reducing agent and 300-600 parts of solvent.
3. The method for preparing high sphericity ultrafine silver powder according to claim 1, wherein the step S1 specifically comprises:
s11, mixing the reducing agent with a part of the solvent, and stirring until the reducing agent and the part of the solvent are dissolved to obtain a first mixed solution;
s12, mixing the buffer, the dispersing agent and the other part of the solvent, and stirring until the mixture is dissolved to obtain a second mixed solution;
and S13, sequentially adding the silver nitrate solution, the coating agent and the first mixed solution into the second mixed solution, and stirring at a uniform speed to obtain the reaction suspension.
4. The method for preparing high sphericity ultrafine silver powder according to claim 3, wherein in the step S11, the reducing agent is at least one of ascorbic acid, formaldehyde, glucose, ethylene glycol and hydrazine hydrate.
5. The method for preparing high sphericity ultrafine silver powder according to claim 3, wherein in the step S12, the buffer is at least one of acetic acid, sodium acetate, sodium citrate, phosphoric acid, boric acid, sodium borate and sodium bicarbonate, and the dispersant is at least one of polyvinylpyrrolidone, polyethylene glycol, sodium dodecyl sulfonate, sodium polyacrylate and tween.
6. The method for producing high sphericity ultrafine silver powder according to claim 3, wherein in the step S13, the coating agent is at least one of oleic acid, lauric acid, a silane coupling agent, and stearic acid.
7. The method for producing high sphericity ultrafine silver powder according to claim 3, wherein the solvent is water, and the stirring rates in the step S11, the step S12, and the step S13 are 300 to 500r/min.
8. The method for preparing high sphericity ultrafine silver powder according to claim 1, wherein the step S3 specifically comprises:
S31, carrying out sedimentation treatment on the solid-liquid mixture, and removing supernatant to obtain the precipitate;
s32, mixing the precipitate with ethanol, performing first centrifugation, mixing the precipitate with deionized water, and performing second centrifugation until the conductivity of the precipitate is less than 20 mu S/m, thereby obtaining wet silver powder;
and S33, drying the wet silver powder at 60 ℃, and sieving the wet silver powder with a 300-mesh sieve to finally obtain the high-sphericity ultrafine silver powder.
9. The high sphericity superfine silver powder is characterized by being prepared by the preparation method of the high sphericity superfine silver powder according to any one of claims 1 to 8, wherein the particle size of the high sphericity superfine silver powder is 0.82-3.53 mu m, the tap density is 6.24g/cm 3, and the specific surface area is 0.32m 2/g.
10. Use of the high sphericity ultrafine silver powder of claim 9 in the preparation of conductive silver paste.
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