CN110434355B - Preparation method of high-tap-density and high-dispersibility spherical silver powder - Google Patents
Preparation method of high-tap-density and high-dispersibility spherical silver powder Download PDFInfo
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Abstract
The invention discloses a preparation method of spherical silver powder with high tap density and high dispersibility, which comprises the following steps: (1) preparation of silver crystal nucleus: mixing the first dispersing agent solution and the first reducing agent solution, stirring and heating to boil, quickly adding the first silver nitrate solution, and stirring and reacting for 30-60 min to obtain a silver crystal nucleus solution; (2) and (3) crystal nucleus growth: and (2) adding a second dispersing agent solution and a second reducing agent solution into the silver crystal nucleus solution prepared in the step (1), and stirring. Heating to 25-65 ℃, adjusting the pH value to 2.5-5.5, adding a second silver nitrate solution, then adding a coating agent, stirring for 0.5-2 h, and carrying out solid-liquid separation to obtain a solid, thereby obtaining the silver powder. The method can control the particle size of the silver powder, and the prepared silver powder has higher tap density, better sphericity and monodispersity; and the method is simple, the conditions are controllable, and the industrial production is easy to realize.
Description
Technical Field
The invention relates to a preparation method of silver powder, in particular to a preparation method of spherical silver powder with high tap density and high dispersibility.
Background
The silver powder has excellent conductivity, particularly in the field of solar cells, the silver powder is the most important raw material of the conductive paste, and the silver powder with excellent performance can effectively improve the photoelectric conversion efficiency of the solar cells. In particular, in recent years, rapid development of the photovoltaic industry has made higher requirements on the properties of silver powder, such as high tap density, excellent dispersibility, good sphericity, and the like. The solar cell silver powder is prepared by a plurality of methods at present, and mainly comprises a ball milling method, an atomization method, a sol-gel method, a hydrothermal method, a liquid phase reduction method and the like. The liquid phase method is characterized in that silver is reduced from a salt solution thereof in a powder form through a chemical reduction method under the protection of a dispersing agent. The liquid phase method has the advantages of simple process, small investment, large output, controllable performance and suitability for industrial production, and therefore, the liquid phase method is the superfine silver powder preparation method with the most development prospect at present.
Patent CN 104400000 a describes a method for preparing spherical silver powder, which comprises adjusting the pH of silver nitrate solution with ammonium sulfate solution, adding prepared ascorbic acid solution into silver nitrate solution, stirring, washing, filtering, drying, and powdering. The silver powder prepared by the method has the advantages of good sphericity, concentrated particle size distribution, high tap density, poor dispersibility and poor intersolubility with an organic solvent, and the prepared silver paste has the problems of layering and uneven printing.
Patent CN 107000050A describes a method for preparing silver powder, which comprises adding strong ammonia water into silver nitrate solution, adding sodium hydroxide solution to adjust pH, and getting silver ammonia solution; keeping a certain temperature and stirring, adding a hydrazine hydrate solution into a silver-ammonia solution, adding a certain amount of phytic acid alcohol solution into the silver-ammonia solution, stirring and curing, filtering, washing with water, drying, and crushing to obtain the silver powder. The silver powder prepared by the method has good hydrophobicity, and the method has the defects of generating a large amount of ammonia nitrogen wastewater and having low yield.
Patent CN 109365830 a describes a method for preparing silver powder, which comprises preparing silver nitrate and dispersant solution, adding dispersant solution into silver nitrate solution as base solution, adding reducing solution into base solution, after reaction, washing, drying, sieving, and packaging. The silver powder produced by the method has wide particle size distribution, is in a sphere-like shape or an irregular shape, and generates a large amount of wastewater.
In view of the above disadvantages, there is a need for a new method for preparing silver powder.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide the preparation method of the spherical silver powder with high tap density and high dispersibility.
In order to achieve the purpose, the invention adopts the technical scheme that: a preparation method of spherical silver powder with high tap density and high dispersibility comprises the following steps:
(1) preparation of silver crystal nucleus:
mixing the first dispersing agent solution and the first reducing agent solution, stirring and heating to boil, adding the first silver nitrate solution, and stirring and reacting for 30-60 min to obtain a silver crystal nucleus solution;
(2) and (3) crystal nucleus growth:
adding a second dispersing agent solution and a second reducing agent solution into the silver crystal nucleus solution prepared in the step (1), stirring, heating to 25-65 ℃, adjusting the pH value to 2.5-5.5, adding a second silver nitrate solution, then adding a coating agent, stirring for 0.5-2 h, and performing solid-liquid separation to obtain a solid, thereby obtaining the silver powder; the coating agent is octadecyl amine.
The synthesis process of the silver powder consists of a chemical reduction method with two stages of nucleation and growth control, crystal nuclei are provided for the growth of silver particles through the nucleation, and the granularity of the required silver particles is obtained through the growth control; meanwhile, the dispersing agent is added at different stages of nucleation and growth of silver particles, so that the growth of silver ions on the surface of crystal nuclei is ensured, and the obtained silver powder has good dispersibility. The control of the particle size of the silver particles is realized by controlling the reaction conditions of the nucleation step (the preparation step of the silver crystal nucleus) and the growth step of the crystal nucleus, and the effect of controlling the performance of the silver particles is further achieved.
In the step (1), the first silver nitrate solution is added by one-time rapid pouring. The silver crystal nucleus D50 prepared in the step (1) is 50-150 nm.
In the step (2), after solid-liquid separation and solid taking, the method also comprises a step of washing the solid; the washing end point is that the conductivity in the washing liquid is less than or equal to 20 mu s/cm; the washing step further comprises the steps of drying, crushing and grading, wherein the drying temperature is 60-80 ℃, and the drying time is 10-20 hours; the pH adjustment is preferably carried out using sodium hydroxide solution.
As a preferred embodiment of the method for preparing the high tap density and high dispersibility spherical silver powder according to the present invention, the first dispersant comprises at least one of polyvinylpyrrolidone, polyethylene glycol, tannic acid, polyvinyl alcohol, and tween 80. The nano silver colloid with better granularity can be prepared by adopting the dispersing agent.
As a preferred embodiment of the method for preparing the high tap density and high dispersibility spherical silver powder according to the present invention, the second dispersant comprises at least one of polyethylene glycol, polyvinyl alcohol, polyvinylpyrrolidone, and gelatin. The first dispersant and the second dispersant may be the same or different in kind, and a dispersant commonly used in the art may be selected, and the above kind of dispersant is preferred, and polyvinylpyrrolidone is preferred as the second dispersant. Compared with other dispersants, the silver particles prepared by adopting polyvinylpyrrolidone have better appearance, more uniform granularity and higher tap density.
As a preferred embodiment of the method for preparing the high tap density and high dispersibility spherical silver powder according to the present invention, the first reducing agent comprises sodium citrate; the second reducing agent is at least one of formaldehyde, glucose, hydrazine hydrate and ascorbic acid. The types of the first reducing agent and the second reducing agent ensure the reduction speed, and finally determine the granularity and tap density of the obtained silver powder.
As a preferred embodiment of the method for preparing the high tap density and high dispersibility spherical silver powder according to the present invention, the molar ratio of the first silver nitrate to the second silver nitrate is: first silver nitrate: the second silver nitrate is 1: 1200-4400. When the silver powder and the silver powder are mixed according to the proportion, the silver powder meeting the requirement of the particle size can be prepared.
As a preferred embodiment of the method for preparing the high tap density and high dispersibility spherical silver powder according to the present invention, the molar ratio of the first silver nitrate to the first reducing agent is: first silver nitrate: the first reducing agent is 3: 1.25-1.5.
As a preferred embodiment of the method for preparing the spherical silver powder with high tap density and high dispersibility according to the present invention, the second reducing agent is ascorbic acid, and the molar ratio of the second silver nitrate to the second reducing agent is: second silver nitrate: second reducing agent ═ 2: 1; the concentration of the second reducing agent is 0.8-1.5 mol/L.
As a preferable embodiment of the method for preparing the spherical silver powder with high tap density and high dispersibility, the concentration of the first silver nitrate solution is 8-12 mM, and the concentration of the second silver nitrate solution is 0.3-1M. When the concentration of the first silver nitrate solution is the above concentration, the formation of colloidal silver is facilitated, and when the concentration is too high, the granularity of the formed silver is large, the quantity of the formed silver is small, the formed silver is easy to precipitate and separate out, and the subsequent growth of silver nitrate is not facilitated; when the second silver nitrate solution has the above concentration, the growth of silver particles is facilitated.
As a preferred embodiment of the method for preparing the spherical silver powder with high tap density and high dispersibility, the mass ratio of the first dispersing agent to the first silver nitrate is as follows: a first dispersant: the first silver nitrate is 40-80: 1; the addition amount of the second dispersing agent is 8-12% of silver equivalent. When the dispersant is added in the above amount, a good dispersing effect can be ensured, and the COD value of the produced wastewater is reduced while the system stability is ensured. The silver equivalent is the theoretical mass of the silver powder.
In a preferred embodiment of the method for preparing the spherical silver powder with high tap density and high dispersibility according to the present invention, the concentration of the first reducing agent solution is 0.5 to 1.5 mM.
As a preferable embodiment of the preparation method of the spherical silver powder with high tap density and high dispersibility, the addition amount of the coating agent is 0.3-1% of the mass of the silver powder. The amount of the coating agent added is more preferably 0.5% by mass of the silver powder. The addition of the capping agent can increase the hydrophobicity of the surface of the silver powder, where the mass of the silver powder represents the theoretical mass of silver. As a preferred embodiment of the method for preparing the spherical silver powder with high tap density and high dispersibility, the adding speed of the second silver nitrate solution is 30mL/min to 90 mL/min. The reduction speed of the silver nitrate, namely the growth speed of silver particles can be controlled by adopting the dripping speed, so that the silver powder with better sphericity and higher tap density is prepared.
The invention has the beneficial effects that: the invention provides a preparation method of high-tap-density high-dispersibility spherical silver powder, the particle size of the silver powder can be controlled by adopting the method, and the prepared silver powder has higher tap density, better sphericity and monodispersity; and the method is simple, the conditions are controllable, and the industrial production is easy to realize.
Drawings
FIG. 1 is a scanning electron micrograph of the silver powder obtained in example 1, at a magnification of 3.00 KX;
FIG. 2 is a scanning electron micrograph of the silver powder obtained in example 2, at a magnification of 3.00 KX;
FIG. 3 is a scanning electron micrograph of the silver powder obtained in example 3, at a magnification of 3.00 KX;
FIG. 4 is a scanning electron micrograph of the silver powder obtained in comparative example 1, at a magnification of 3.00 KX.
Detailed Description
To better illustrate the objects, technical solutions and advantages of the present invention, the present invention will be further described with reference to specific examples.
Example 1
The embodiment of the preparation method of the spherical silver powder with high tap density and high dispersibility, provided by the invention, comprises the following steps:
(1) preparation of silver crystal nucleus:
firstly preparing 400mL of a tannic acid solution with the concentration of 2.5mM, adding 80mL of 1mM sodium citrate into the tannic acid solution, stirring and heating the tannic acid solution to boiling, pouring 20mL of the prepared 10mM silver nitrate solution into the tannic acid solution, and stirring and reacting for half an hour to obtain a silver crystal nucleus solution;
(2) and (3) crystal nucleus growth:
1249.5g of silver nitrate solution containing 149.5g of silver nitrate is prepared, 600mL of dispersant solution containing 9.5g of polyvinylpyrrolidone is prepared, and 400mL of reducing agent solution containing 79.3g of ascorbic acid is prepared; adding a dispersant solution and a reducing agent solution into the silver crystal nucleus solution, stirring and heating, and adjusting the pH to 4.0 by using 8.4g of 1M sodium hydroxide solution; adding silver nitrate solution at the speed of 90mL/min under stirring, adding 0.48g of octadecylamine after the addition is finished, and stirring for 1 h; and filtering, washing, drying, powdering and screening the reaction liquid containing the silver powder to obtain the silver powder.
The silver powder obtained in this example was measured for particle size distribution using a Malvern 2000 laser particle size analyzer, BET using a nitrogen adsorption method, and tap density using a JZ-7 powder tap densitometer.
The silver powder obtained was evaluated, and the results were as follows: BET specific surface area of 0.5365m2Per g, cumulative 10% particle diameter (D)10) 1.134 μm, cumulative 50% particle size (D)50) 1.708 μm, 90% cumulative particle size (D)90) 2.570 μm, tap density of 6.39g/cm3。
As shown in a scanning electron micrograph of the silver powder in figure 1, the silver powder has uniform particles, better sphericity and good dispersibility as shown in figure 1.
Example 2
The embodiment of the preparation method of the spherical silver powder with high tap density and high dispersibility, provided by the invention, comprises the following steps:
(1) preparation of silver crystal nucleus: the preparation method of the silver crystal nucleus is the same as that of example 1;
(2) and (3) crystal nucleus growth:
795.1g of silver nitrate solution containing 95.1g of silver nitrate was prepared, 381.8mL of dispersant solution containing 6.0g of polyvinylpyrrolidone was prepared, and 254.5mL of reducing agent solution containing 50.3g of ascorbic acid was prepared. Adding a dispersant solution and a reducing agent solution into the silver crystal nucleus solution, stirring and heating, and adjusting the pH to 4.0 by using 5.5g of 1M sodium hydroxide solution; adding silver nitrate solution at the speed of 90mL/min under stirring, adding 0.3g of octadecylamine after the addition is finished, and fully stirring for 1 h; and filtering, washing, drying, powdering and screening the reaction liquid containing the silver powder to obtain the silver powder.
The silver powder obtained in this example was evaluated as follows: BET specific surface area of 0.8354m2(g) cumulative 10% particle size (D)10) 0.851 μm, cumulative 50% particle diameter (D)50) 1.213 μm, cumulative 90% particle size (D)90) 1.894 μm, tap density of 5.43g/cm3。
As shown in a scanning electron micrograph in FIG. 2, the silver powder has uniform particles, better sphericity and good dispersibility as shown in FIG. 2.
Example 3
The embodiment of the preparation method of the spherical silver powder with high tap density and high dispersibility, provided by the invention, comprises the following steps:
(1) preparation of silver crystal nucleus: the preparation method of the silver crystal nucleus is the same as that of the example 1;
(2) and (3) crystal nucleus growth:
340.8g of silver nitrate solution containing 40.8g of silver nitrate was prepared, 163.6mL of dispersant solution containing 2.6g of polyvinylpyrrolidone was prepared, and 109.1mL of reducing agent solution containing 21.6g of ascorbic acid was prepared. Adding a dispersant solution and a reducing agent solution into the silver crystal nucleus solution, stirring and heating, and adjusting the pH to 4.0 by using 2.4g of 1M sodium hydroxide solution; adding silver nitrate solution at the speed of 90mL/min under stirring, adding 0.13g of octadecylamine after the addition is finished, and fully stirring for 1 h; and filtering, washing, drying, powdering and screening the reaction liquid containing the silver powder to obtain the silver powder.
The silver powder obtained in this example was evaluated as follows: BET specific surface area of 1.056m2(g) cumulative 10% particle size (D)10) 0.534 μm, cumulative 50% particle size (D)50) 0.843 μm, cumulative 90% particle size (D)90) 1.345 μm and a tap density of 4.34g/cm3。
The scanning electron micrograph is shown in FIG. 3, and it can be seen from FIG. 3 that the silver powder has uniform particles, better sphericity and good dispersibility.
Example 4
The embodiment of the preparation method of the spherical silver powder with high tap density and high dispersibility, provided by the invention, comprises the following steps:
(1) preparation of silver crystal nucleus:
firstly, preparing 110mL of solution containing 3.3g of polyvinylpyrrolidone, adding 80mL of 1.25mM sodium citrate, stirring and heating to boil, pouring 20mL of prepared 12mM silver nitrate solution into the polyvinylpyrrolidone solution, and stirring and reacting for half an hour to obtain a silver crystal nucleus solution;
(2) and (3) crystal nucleus growth:
preparing 580g of silver nitrate solution containing 98.7g of silver nitrate, 625mL of dispersant solution containing 7.5g of polyvinylpyrrolidone and 232mL of reducing agent solution containing 51g of ascorbic acid; adding a dispersant solution and a reducing agent solution into the silver crystal nucleus solution, stirring and heating, and adjusting the pH to 2.5 by using a sodium hydroxide solution; adding silver nitrate solution at the speed of 90mL/min under stirring, adding 0.18g of octadecylamine after the addition is finished, and stirring for 0.5 h; and filtering, washing, drying, powdering and screening the reaction liquid containing the silver powder to obtain the silver powder.
The silver powder obtained in this example was evaluated as follows: BET specific surface area of 0.532m2(g) cumulative 10% particle size (D)10) 1.261 μm, cumulative 50% particle size (D)50) 1.803 μm, cumulative 90% particle size (D)90) 2.903 μm, tap density of 5.60g/cm3。
Example 5
One embodiment of the preparation method of the spherical silver powder with high tap density and high dispersibility, which is disclosed by the invention, comprises the following steps of:
(1) preparation of silver crystal nucleus:
preparing 38mL of solution containing 1.88g of polyvinyl alcohol, adding 80mL of 1mM sodium citrate, stirring and heating to boil, pouring 20mL of prepared 8mM silver nitrate solution into the polyvinyl alcohol solution, and stirring and reacting for half an hour to obtain a silver crystal nucleus solution;
(2) and (3) crystal nucleus growth:
preparing 1529g of silver nitrate solution containing 78g of silver nitrate, 333mL of dispersant solution containing 4g of polyvinylpyrrolidone and 232mL of reducing agent solution containing 40.4g of ascorbic acid; adding a dispersant solution and a reducing agent solution into the silver crystal nucleus solution, stirring and heating, and adjusting the pH to 5.5 by using a sodium hydroxide solution; adding silver nitrate solution at the speed of 30mL/min under stirring, adding 0.5g of octadecylamine after the addition is finished, and stirring for 2 hours; and filtering, washing, drying, powdering and screening the reaction liquid containing the silver powder to obtain the silver powder.
The silver powder obtained in this example was evaluated as follows: BET specific surface area of 0.514m2Per g, cumulative 10% particle diameter (D)10) 0.608 μm, cumulative 50% particle size (D)50) 1.105 μm, cumulative 90% particle diameter (D)90) 1.943 μm, tap density of 4.15g/cm3。
Comparative example 1
A comparative example of the method for preparing a spherical silver powder having a high tap density and high dispersibility according to the present invention, which does not include the step (1) of preparing silver crystal nuclei and the step (2) is the same as example 1, is compared to example 1.
The silver powder obtained was evaluated, and the results thereof were as follows: BET specific surface area of 1.056m2Per g, cumulative 10% particle diameter (D)10) 0.621 μm, cumulative 50% particle diameter (D)50) 1.443 μm, cumulative 90% particle diameter (D)90) 2.683 μm, tap density 4.83g/cm3。
The scanning electron micrograph of the silver powder obtained by the method of the present comparative example is shown in FIG. 4, and it can be seen from FIG. 4 that the particle size distribution of the silver powder obtained by comparative example 1 is not uniform.
The results of the particle size distribution, specific surface area, tap density, etc. of the silver powders obtained in examples 1 to 5 and comparative example 1 are shown in Table 1.
TABLE 1 analysis of particle size distribution, specific surface area and tap density of silver powders described in examples 1 to 5 and comparative example 1
From Table 1 (D)90-D10)/D50As can be seen, the particle size distribution of the silver powder prepared by the methods of examples 1-5 is significantly better in concentratability than that of comparative example 1.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (4)
1. A preparation method of spherical silver powder with high tap density and high dispersibility is characterized by comprising the following steps:
(1) preparation of silver crystal nucleus:
mixing a first dispersant solution and a first reducing agent solution, stirring and heating to boil, adding a first silver nitrate solution, stirring and reacting for 30-60 min to obtain a silver crystal nucleus solution, wherein the first reducing agent comprises sodium citrate, the first dispersant comprises at least one of polyvinylpyrrolidone, polyethylene glycol, tannic acid, polyvinyl alcohol and tween-80, and the concentration of the first silver nitrate solution is 8-12 mM;
(2) and (3) crystal nucleus growth:
adding a second dispersing agent solution and a second reducing agent solution into the silver crystal nucleus solution prepared in the step (1), stirring, heating to 25-65 ℃, adjusting the pH value to 2.5-5.5, adding a second silver nitrate solution, then adding a coating agent, stirring for 0.5-2 h, and performing solid-liquid separation to obtain a solid, thereby obtaining the silver powder; the coating agent is octadecylamine, the adding amount of the coating agent is 3-10% of the mass of the silver powder, the second reducing agent comprises at least one of formaldehyde, glucose, hydrazine hydrate and ascorbic acid, the second dispersing agent comprises polyvinylpyrrolidone, the concentration of the second silver nitrate solution is 0.3-1M, and the molar ratio of the first silver nitrate to the second silver nitrate is as follows: first silver nitrate: the second silver nitrate is 1: 1200-4400.
2. The method for preparing a high tap density and high dispersibility spherical silver powder according to claim 1, wherein the molar ratio of the first silver nitrate to the first reducing agent is: first silver nitrate: the first reducing agent is 3: 1.25-1.5.
3. The method for preparing the spherical silver powder with high tap density and high dispersibility according to claim 1, wherein the mass ratio of the first dispersing agent to the first silver nitrate is: a first dispersant: the first silver nitrate is 40-80: 1; the addition amount of the second dispersing agent is 8-12% of silver equivalent.
4. The method for preparing a spherical silver powder with high tap density and high dispersibility according to claim 1, wherein the second silver nitrate solution is added at a rate of 30mL/min to 90 mL/min.
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