CN113399679A - Preparation method of high-tap aging-resistant superfine silver powder for electronic paste - Google Patents
Preparation method of high-tap aging-resistant superfine silver powder for electronic paste Download PDFInfo
- Publication number
- CN113399679A CN113399679A CN202110497975.XA CN202110497975A CN113399679A CN 113399679 A CN113399679 A CN 113399679A CN 202110497975 A CN202110497975 A CN 202110497975A CN 113399679 A CN113399679 A CN 113399679A
- Authority
- CN
- China
- Prior art keywords
- silver
- silver powder
- aging
- tap
- preparing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- 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
-
- 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
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
-
- 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
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
Abstract
The invention discloses a preparation method of high-tap aging-resistant superfine silver powder for electronic paste, which comprises the following steps: firstly, preparing silver oxide mother liquor with high crystallinity, then obtaining soft agglomerated coarse silver particles, optimizing washing, filtering and dispersing processes to obtain dispersed silver mud, carrying out surface modification on the silver mud to obtain super-hydrophobic silver powder, and finally carrying out a special ball-milling dispersing process to obtain a target product. The method shortens the production process on the basis of the existing silver powder preparation process, does not need to add a dispersing agent, does not need to adjust the pH value of a system, is difficult to optimize the solid-liquid separation of the superfine powder by adopting a special washing and dispersing mode, and adopts a special modification method and a ball milling process to disperse the silver powder. The granularity of the silver powder can be regulated and controlled between nanometer and micron,good dispersibility, high tap density, and tap density of micro-nano silver powder up to 5.5g/cm3The aging tension applied to the photovoltaic silver paste reaches more than 5.5N, and the aging tension reaches the leading level of the industry under the same test condition.
Description
Technical Field
The invention relates to a preparation method of high-tap aging-resistant superfine silver powder for electronic paste, belonging to the technical field of superfine powder preparation and application.
Background
The superfine silver powder is a functional powder material, and has the characteristics of good conductivity, chemical stability, higher surface energy and the like, so that the superfine silver powder has wide application prospects in the fields of optics, electromagnetic shielding materials, biomedical treatment, electronic paste and the like. Along with the rapid development of the electronic industry and the photovoltaic industry, the demand of the ultrafine silver powder is larger and larger, and along with the development trend of the electronic industry of increasingly high precision and integration, the performance requirement of the ultrafine silver powder is higher and higher.
The silver powder for the crystalline silicon solar cell slurry is divided into front silver powder and back silver powder, so that the front silver localization rate is low, and the back silver localization rate is slightly high. The back silver paste mainly plays a role in leading out electrode current and welding electrodes of the assembly string, so that the requirement on the performance of the back silver powder is not very high. However, with the increasing market share of the high-efficiency battery, the demand of the back silver paste is also increased continuously, and through more than ten years of technical competition, the current mainstream photovoltaic module factory in China puts higher requirements on the back silver paste silver powder. First, the back silver powder should have basic physical and chemical properties such as uniform particle size distribution, high tap density, and slurry sintering activity. Secondly, the silver powder is prepared into silver paste which has good adhesive force and higher aging tension after being sintered. The photovoltaic module is installed in the open air and is subjected to wind, rain and sunshine for a long time, and parts can be slowly aged, researches show that the key factors influencing the output power and the service life of the photovoltaic module are the ageing-resistant capacity of the back electrode, the ageing of the back electrode can cause the series resistance of the module to rise and even the electrode to fall, and the efficiency of the module is reduced. At present, the back silver made in China can meet the requirements of electrical performance and conventional adhesive force, but the aging-resistant tension is low or even none, the research on the aging mechanism of the back electrode is insufficient, and the silver powder with high aging tension is not provided. Silver paste with aging tension is an urgent requirement for component manufacturers, so that silver powder manufacturers can develop silver powder with high aging tension to meet the next silver-backed market. Meanwhile, silver paste is required to have higher tensile force in the 5G ceramic filter, and the silver powder is the most main component of the silver paste and has a decisive effect on the performance of the sintered silver paste.
Disclosure of Invention
Aiming at the problems and the defects in the prior art, the invention provides the preparation method of the high-tap aging-resistant PERC battery back silver powder, which reduces the cost and shortens the production procedure on the basis of the existing silver powder preparation process, does not need to add a dispersing agent or adjust the pH value of a system, optimizes a solid-liquid separation process by adopting a quick washing mode, disperses and depolymerizes the silver powder by adopting a special modification method and a ball milling process, realizes excellent performance on the slurry end of the silver powder prepared by the method, and solves the problem of low aging tension of the existing silver powder. The invention is realized by the following technical scheme.
A preparation method of high-tap aging-resistant superfine silver powder for electronic paste is characterized by comprising the following specific steps:
1) preparing silver nitrate solution and complexing agent solution, and respectively preheating and dissolving the silver nitrate solution and the complexing agent solution uniformly;
2) adding a complexing agent solution into a silver nitrate solution at a constant speed to obtain a crystalline silver oxide suspension of 200-600 nm, and performing heat preservation and aging;
3) preparing a reducing agent solution, and adding the reducing agent solution into the aged silver oxide suspension at a constant speed to obtain soft agglomerated coarse silver powder;
4) washing, dispersing and dehydrating the obtained soft agglomerated coarse silver powder to form paste dispersed silver mud;
5) carrying out surface modification on the dispersed silver mud, and drying the obtained modified silver paste to obtain dry silver powder;
6) carrying out ball milling, dispersing and screening on the dried silver powder to obtain a high-dispersion target product, wherein the indexes of the high-dispersion target product are as follows: the macroscopic average particle size measured by the laser particle size is 0.3-1.5 mu m, and the error of the macroscopic average particle size measured by the laser particle size and the single-particle average particle size counted by a high-resolution electron microscope picture is less than 10%.
The complexing agent in the step 1) is an alkaline solution, and the alkaline solution is one of sodium hydroxide, potassium hydroxide or ammonia water. Preferably selecting a sodium hydroxide solution, and keeping the temperature of the silver nitrate solution and the temperature of the sodium hydroxide solution to be 25-70 ℃.
In the step 2), the adding speed of the complexing agent is 2-20L/min, high-speed shearing and mixing are carried out in the reaction process, so that the produced silver oxide single particles are fine and uniform, and then heat preservation and aging are carried out for 1-3 h.
The reducing agent in the step 3) is one of formaldehyde, ascorbic acid, a compound of formaldehyde and ascorbic acid and a hydrazine hydrate solution, the concentration is 0.3-5 mol/L, the temperature is consistent with that of the aged silver oxide solution, and the temperature is 25-60 ℃. The uniformity of reduction reaction is increased by adopting a multi-pipeline spraying and dripping mode, the speed of adding the reducing agent solution into the silver oxide suspension is 2-20L/min, the mixture is continuously stirred for about 10min after dripping is finished, and the particles are sheared and mixed at a high speed in the reduction process, so that the particles are prevented from forming large hard aggregates.
And in the step 4), adding pure water into the washing device, stirring and washing the soft agglomerated coarse silver powder obtained in the step 3), continuously discharging the washing liquid while washing, increasing the washing effect, quickly stirring and shearing the washed silver powder to separate out water adsorbed among particles after washing until the conductivity of the supernatant is less than 1ms/cm, and then dehydrating, thereby finally keeping the solid content in the dispersed silver mud to be 60-80%.
And 5) stirring and dispersing the silver mud by using a high-speed dispersion machine, adding a modifier, mixing for 10-40 min under stirring and shearing at 1000-4000 rpm, and drying the modified silver paste in an oven at 60-80 ℃. Wherein the modifier is one or more than two of phosphate, linolenic acid, oleic acid, linoleic acid and stearic acid which are dissolved in absolute ethyl alcohol, and the dosage of the modifier is 0.1-0.5 percent of the mass of the silver.
The density of 0.5-4.0 g/cm is adopted in the step 6)3The rubber balls, the PVC balls, the polyurethane balls and the like are used as grinding media, the grinding balls can also be high-density balls coated with the materials, the ball-material ratio is 1-5: 1, the materials are further ground and dispersed in a ball mill for 2-20 hours, and finally, the ball-material separation is carried out to obtain the target silver powder.
Compared with the prior art, the invention has the beneficial effects that:
(1) reaction materials are balanced, and a dispersing agent is not required to be added in a special reduction process for particle protection, so that the cost is saved, and the environment is protected; the process of the silver powder washing, filtering and dispersing process is optimized, and the process time is saved; the dispersibility and tap density of the silver powder are improved by a special modification process and a special ball milling process.
(2) The obtained silver powder is pure, the granularity can be regulated and controlled between nanometer and micron, the prepared silver powder has super hydrophobicity and good dispersibility, and the tap density of the micro-nanometer silver powder can reach 5.5g/cm3The high tap density of the silver paste can reach an aging tension of more than 5.5N when being applied to photovoltaic silver paste or other high-temperature sintered silver pastes, and reaches the domestic leading level.
Drawings
FIG. 1 is a process flow diagram of the present invention.
FIG. 2 is a scanning electron micrograph of silver powder prepared in example 1 of the present invention.
Detailed Description
The invention is further described with reference to the following drawings and detailed description.
Example 1
1) Weighing 4720g of silver nitrate in a reaction kettle, adding 34.73L of pure water with the temperature of 40 ℃ for dissolution, and starting a stirring paddle; weighing 1122g of sodium hydroxide solid particles, dissolving the sodium hydroxide solid particles in 28L of normal-temperature pure water, and adjusting the temperature to 40 ℃ after heat release of the solution;
2) adding the sodium hydroxide solution into the silver nitrate solution at a constant speed of 4.0L/min under high-speed stirring to obtain silver oxide precipitate, and preserving heat and aging for 1h after the silver oxide precipitate is added;
3) weighing 2900g of ascorbic acid into a reaction kettle, adding 54L of pure water with the temperature of 43 ℃ to prepare a reducing agent solution, and adding the ascorbic acid solution into the silver oxide suspension at a constant speed of 10L/min to reduce to obtain soft agglomerated coarse silver powder;
5) transferring the soft agglomerated coarse silver powder obtained by reduction to washing equipment for quick washing, washing until the conductivity of the supernatant is 900 mu s/cm, quickly stirring the silver mud to separate out water, and then dehydrating the water to obtain dispersed silver mud;
6) adding the dispersed silver mud obtained in the last step into a dispersion machine, stirring for 10min, adding a modifier for surface modification, dissolving 14.9g of phosphate into 200ml of alcohol, shearing and mixing at 3500rpm for 10min, and drying the silver paste;
7) and smashing the dried silver powder, pouring the smashed silver powder into a ball mill, adding 3kg of polyurethane balls for ball milling, taking out the silver powder after 2 hours, and removing the balls through a vibrating screen to obtain the target silver powder.
2990g of highly dispersed silver powder was obtained in example 1, with a yield of 99.66%, and a particle size distribution: d10-0.22 μm, D50-0.51 μm, D90-1.1 μm, bulk density: 3.0g/cm3And tap density: 5.55g/cm3Preparing slurry, printing and sintering the slurry on the back of the PERC battery to manufacture a back electrode, welding a tin bar with the width of 0.9mm on the back electrode at 360 ℃, stripping a welding strip by a tensile machine at 180 degrees, carrying out the average of 6.7N in a conventional tensile test, putting the battery piece into an oven, and carrying out aging under the condition of keeping the temperature at 170 ℃ for 1h, wherein the aging tensile test is 5.6N.
Example 2
1) Weighing 7874g of silver nitrate in a reaction kettle, adding 23.2L of pure water with the temperature of 55 ℃ for dissolution, and starting a stirring paddle; weighing 1855g of potassium hydroxide solid particles, dissolving in 20L of pure water at normal temperature, releasing heat, and adjusting the temperature to 55 ℃;
2) adding the potassium hydroxide solution into the silver nitrate solution at a constant speed of 7L/min under high-speed stirring to obtain silver oxide precipitate, and preserving heat and aging for 3h after the silver oxide precipitate is added;
3) 2334g of formaldehyde solution with the concentration of 37 percent is weighed, 9.6L of pure water with the temperature of 50 ℃ is added to prepare reducing agent solution, and the reducing agent solution is added into the silver oxide suspension at a constant speed of 20L/min to be reduced to obtain soft agglomerated coarse silver powder;
4) continuously stirring for 10min, transferring the soft agglomerated coarse silver powder into washing equipment for quick washing, quickly stirring and shearing the silver mud when the conductivity of the washed supernatant is 600 mu s/cm to separate out water, and then draining the water to obtain dispersed silver mud;
5) adding the dispersed silver mud obtained in the last step into a dispersion machine, stirring for 10min, adding a modifier for surface modification, dissolving 15g of linoleic acid in 300ml of alcohol, stirring and mixing at 2500rpm for 20min, and drying the silver paste;
6) and smashing the dried silver powder, pouring the smashed silver powder into a ball mill, adding 15kg of rubber balls for ball milling, taking out the silver powder after 20 hours, and removing the balls through a vibrating screen to obtain the target silver powder.
Example 2 preparation of highly dispersed silver4972g powder, yield 99.44%, particle size distribution: d10-0.21 μm, D50-0.72 μm, D90-1.97 μm, apparent density: 2.8g/cm3And tap density: 5.1g/cm3Preparing slurry, printing and sintering the slurry on the back of the PERC battery to manufacture a back electrode, welding a tin bar with the width of 0.9mm on the back electrode at 360 ℃, stripping a welding strip by a tensile machine at 180 degrees, aging the battery piece in an oven under the condition of keeping the temperature at 170 ℃ for 1h, and aging the battery piece at the tensile test of 5.4N.
Example 3
1) Weighing 7874g of silver nitrate in a reaction kettle, adding 33.1L of pure water with the temperature of 60 ℃ for dissolution, and starting a stirring paddle; 1909g of sodium hydroxide solid particles are weighed and dissolved in 30L of normal-temperature pure water, and the temperature is adjusted to 60 ℃ after heat release;
2) adding the sodium hydroxide solution into the silver nitrate solution at a constant speed of 10L/min under high-speed stirring to obtain silver oxide precipitate, and aging for 1.5h after the addition is finished to reduce the temperature of the silver oxide to 35 ℃;
3) 2410g of ascorbic acid is weighed and dissolved in 11.6L of pure water, 1170g of formaldehyde solution with the concentration of 37 percent is added, the temperature of the mixed reducing agent solution is stabilized at 35 ℃, and the reducing agent solution is added into the silver oxide suspension at a constant speed of 10L/min for reduction to obtain soft agglomerated coarse silver powder;
4) continuously stirring for 5min, transferring the soft agglomerated coarse silver powder into washing equipment for quick washing, quickly stirring the silver mud when the conductivity of the washing liquid is 400 mu s/cm to separate out water, and then draining the water to obtain dispersed silver mud;
5) adding the dispersed silver mud obtained in the last step into a dispersion machine, stirring for 10min, adding a modifier for surface modification, dissolving 25g of oleic acid in 300ml of alcohol as the modifier, shearing and mixing at 2000rpm for 40min, and drying the silver paste;
6) and smashing the dried silver powder, pouring the smashed silver powder into a ball mill, adding 10kg of polyurethane balls for ball milling, taking out the silver powder after 10 hours, and removing the balls through a vibrating screen to obtain the target silver powder.
4960g of high-dispersion silver powder prepared in example 3, yield 99.2%, particle size distribution: d10-0.18 μm, D50-0.85 μm, D90-1.78 μm, bulk density: 2.5g/cm3And tap density: 5.0g/cm3Mixing ofThe prepared slurry is printed and sintered on the back of the PERC battery to prepare a back electrode, a tin bar with the width of 0.9mm is welded on the back electrode at 360 ℃, a tensile machine is used for stripping a welding strip at 180 degrees, the average tensile test is 6.6N, the battery piece is placed into a common oven to be aged under the condition of keeping the temperature at 170 ℃ for 1h, and the aging tensile test is 6.7N.
Example 4
1) Weighing 7874g of silver nitrate in a reaction kettle, and adding 46.35L of pure water for dissolving;
2) measuring 8L of 25% ammonia water, adding into silver nitrate solution at a rate of 10L/min, and stabilizing the system temperature to 25 deg.C;
3) weighing 4920g ascorbic acid, adding 55.7L pure water at 25 deg.C to obtain reducing agent solution, and adding the reducing agent solution into the silver oxide system at constant speed of 20L/min for reduction to obtain soft agglomerated coarse silver powder;
4) continuously stirring for 10min, transferring the soft agglomerated coarse silver powder into washing equipment for quick washing, quickly stirring the silver mud when the conductivity of the washing liquid is 650 mu s/cm to separate out water, and then draining the water to obtain dispersed silver mud;
5) putting the dispersed silver mud obtained in the last step into a dispersion machine, stirring for 10min, adding a modifier for surface modification, dissolving 15g of oleic acid in 300ml of alcohol, shearing and mixing at 1500rpm for 10min, then shearing and mixing at 3000rpm for 25min, and drying the silver paste;
6) and smashing the dried silver powder, pouring the smashed silver powder into a ball mill, adding 15kg of rubber balls for ball milling, taking out the silver powder after 20 hours, and removing the balls through a vibrating screen to obtain the target silver powder.
4985g of highly dispersed silver powder prepared in example 4, yield 99.7%, particle size distribution: d10-0.14 μm, D50-0.45 μm, D90-0.9 μm, apparent density: 2.3g/cm3And tap density: 5.4g/cm3Preparing slurry, printing and sintering the slurry on the back of the PERC battery to manufacture a back electrode, welding a tin bar with the width of 0.9mm on the back electrode at 360 ℃, stripping a welding strip by a tensile machine at 180 degrees, aging the battery piece in a common oven under the condition of keeping the temperature at 170 ℃ for 1h, and aging the battery piece at the tensile test of 5.8N.
Example 5
In comparison with example 4, the different conditions are: in the step 3), the reduction temperature is raised to 40 ℃; in the step 5), the modifier is 30g of oleic acid dissolved in 300ml of absolute ethyl alcohol, and the rest conditions are consistent.
4980g of high-dispersion silver powder prepared in example 5, yield 99.6%, particle size distribution: d10-0.17 μm, D50-0.39 μm, D90-1.13 μm, apparent density: 2.2g/cm3And tap density: 5.2g/cm3Preparing slurry, printing and sintering the slurry on the back of the PERC battery to manufacture a back electrode, welding a tin bar with the width of 0.9mm on the back electrode at 360 ℃, stripping a welding strip by a tensile machine at 180 degrees, aging the battery piece in a common oven under the condition of keeping the temperature at 170 ℃ for 1h, wherein the aging tension is 5.6N.
Example 6
Compared to example 3, the different conditions are: in the step 3), the reducing agent solution is dissolved in 300ml of alcohol at a rate of 2L/min, the modifier is 25g of stearic acid, and the rest conditions are consistent.
Example 6 prepared highly dispersed silver powder 4971g, yield 99.42%, particle size distribution: d10-0.16 μm, D50-1.1 μm, D90-1.51 μm, bulk density: 3.2g/cm3And tap density: 5.61g/cm3Preparing slurry, printing and sintering the slurry on the back of the PERC battery to manufacture a back electrode, welding a tin bar with the width of 0.9mm on the back electrode at 360 ℃, stripping a welding strip by a tensile machine at 180 degrees, aging the battery piece in a common oven under the condition of keeping the temperature at 170 ℃ for 1h, wherein the aging tension is 7.3N.
The highly dispersed silver powders prepared by the above examples have different indices as shown in table 1.
TABLE 1
Claims (10)
1. A preparation method of high-tap aging-resistant superfine silver powder for electronic paste is characterized by comprising the following preparation steps:
1) preparing silver nitrate solution and complexing agent solution, and respectively preheating and dissolving the silver nitrate solution and the complexing agent solution uniformly;
2) adding a complexing agent solution into a silver nitrate solution at a constant speed to obtain a crystalline silver oxide suspension of 200-600 nm, and performing heat preservation and aging;
3) preparing a reducing agent solution, and adding the reducing agent solution into the aged silver oxide suspension at a constant speed to obtain soft agglomerated coarse silver powder;
4) washing, dispersing and dehydrating the obtained soft agglomerated coarse silver powder to form paste dispersed silver mud;
5) carrying out surface modification on the dispersed silver mud, and drying the obtained modified silver paste to obtain dry silver powder;
6) carrying out ball milling, dispersing and screening on the dried silver powder to obtain a high-dispersion target product, wherein the indexes of the high-dispersion target product are as follows: the macroscopic average particle size measured by the laser particle size is 0.3-1.5 mu m, and the error of the macroscopic average particle size measured by the laser particle size and the single-particle average particle size counted by a high-resolution electron microscope picture is less than 10%.
2. The method for preparing the high-tap aging-resistant ultrafine silver powder for electronic paste according to claim 1, wherein the method comprises the following steps: the complexing agent in the step 1) is alkaline solution, and the alkaline solution is one of sodium hydroxide, potassium hydroxide and ammonia water.
3. The method for preparing the high-tap aging-resistant ultrafine silver powder for electronic paste according to claim 1, wherein the method comprises the following steps: the temperature of the complexing agent in the step 1) is kept consistent with that of the preheated silver nitrate solution, and is 25-70 ℃.
4. The method for preparing the high-tap aging-resistant ultrafine silver powder for electronic paste according to claim 1, wherein the method comprises the following steps: in the step 2), the adding speed of the complexing agent is 2-20L/min, shearing and mixing are carried out in the reaction process, and the heat preservation and aging time is 1-3 h.
5. The method for preparing the high-tap aging-resistant ultrafine silver powder for electronic paste according to claim 1, wherein the method comprises the following steps: in the step 3), the reducing agent solution is one of formaldehyde, ascorbic acid, a compound of formaldehyde and ascorbic acid and a hydrazine hydrate solution, the concentration is 0.3-5 mol/L, the temperature of the reducing agent solution is consistent with that of the aged silver oxide suspension, and the temperature is 25-60 ℃.
6. The method for preparing the high-tap aging-resistant ultrafine silver powder for electronic paste according to claim 1, wherein the method comprises the following steps: in the step 3), the rate of adding the reducing agent solution into the silver oxide suspension is 2-20L/min, and shearing and mixing are carried out in the adding process.
7. The method for preparing the high-tap aging-resistant ultrafine silver powder for electronic paste according to claim 1, wherein the method comprises the following steps: and in the step 4), adding pure water, stirring and washing the soft agglomerated coarse silver powder obtained in the step 3) in a washing device, continuously discharging a washing liquid in the washing process, washing until the conductivity of the supernatant liquid is less than 1ms/cm, stirring, shearing and separating out water from the washed silver powder, and dehydrating to obtain dispersed silver mud, wherein the solid content in the dispersed silver mud is kept at 60-80%.
8. The method for preparing the high-tap aging-resistant ultrafine silver powder for electronic paste according to claim 1, wherein the method comprises the following steps: in the step 5), a high-speed dispersion machine is adopted to stir and disperse the silver mud, then the modifier is added, the silver mud is mixed for 10-40 min under the stirring and shearing of 1000-4000 rpm, and then the modified silver paste is dried in an oven at the temperature of 60-80 ℃.
9. The method for preparing the high-tap aging-resistant ultrafine silver powder for electronic paste according to claim 8, wherein the method comprises the following steps: the modifier is one or a combination of more of phosphate, linolenic acid, oleic acid, linoleic acid and stearic acid dissolved in absolute ethyl alcohol, and the dosage of the modifier is 0.1-0.5% of the mass of the silver.
10. The method for preparing high-tap aging-resistant ultrafine silver powder for electronic paste according to claim 1The method is characterized in that: the density of 0.5-4.0 g/cm is adopted in the step 6)3Taking one of the rubber balls, the PVC balls and the polyurethane balls as a grinding medium, further grinding and dispersing the rubber balls, the PVC balls and the polyurethane balls in a ball mill for 2-20 hours at a ball material weight ratio of 1-5: 1, and finally separating the ball materials to obtain the target silver powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110497975.XA CN113399679A (en) | 2021-05-08 | 2021-05-08 | Preparation method of high-tap aging-resistant superfine silver powder for electronic paste |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110497975.XA CN113399679A (en) | 2021-05-08 | 2021-05-08 | Preparation method of high-tap aging-resistant superfine silver powder for electronic paste |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113399679A true CN113399679A (en) | 2021-09-17 |
Family
ID=77678078
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110497975.XA Pending CN113399679A (en) | 2021-05-08 | 2021-05-08 | Preparation method of high-tap aging-resistant superfine silver powder for electronic paste |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113399679A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114226745A (en) * | 2021-12-10 | 2022-03-25 | 江西贝特利新材料有限公司 | Method for cleaning micron-sized flake silver powder |
| CN114799198A (en) * | 2022-04-14 | 2022-07-29 | 有研亿金新材料有限公司 | High-dispersity nanogold powder and preparation method thereof |
| CN115570141A (en) * | 2022-12-09 | 2023-01-06 | 长春黄金研究院有限公司 | Preparation method of superfine silver powder for conductive paste |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4938868A (en) * | 1972-08-18 | 1974-04-11 | ||
| JPS5798606A (en) * | 1980-12-10 | 1982-06-18 | Mitsubishi Metal Corp | Production of fine silver powder |
| JPH1088207A (en) * | 1996-09-12 | 1998-04-07 | Dowa Mining Co Ltd | Silver powder and its manufacture |
| KR20040047100A (en) * | 2002-11-29 | 2004-06-05 | (주)창성 | Method for manufacturing nano-scale silver powders by wet reducing process |
| CN101088678A (en) * | 2006-06-13 | 2007-12-19 | 上海宝银电子材料有限公司 | Chemical reduction process of preparing silver powder |
| CN101554664A (en) * | 2009-05-20 | 2009-10-14 | 广东风华高新科技股份有限公司 | Method for preparing nano-scale silver powder |
| CN101707062A (en) * | 2009-12-03 | 2010-05-12 | 北京有色金属研究总院 | Nano-silver powder, manufacturing method and application thereof |
| CN101941078A (en) * | 2010-09-27 | 2011-01-12 | 彩虹集团公司 | Silver powder for electrode paste of solar cell and preparation method thereof |
| CN108907226A (en) * | 2018-07-13 | 2018-11-30 | 金川集团股份有限公司 | A kind of preparation method for laser ablation electrode circuit super fine silver powder |
| CN110997198A (en) * | 2017-06-05 | 2020-04-10 | 大州电子材料有限公司 | Silver particles and method for producing same |
-
2021
- 2021-05-08 CN CN202110497975.XA patent/CN113399679A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4938868A (en) * | 1972-08-18 | 1974-04-11 | ||
| JPS5798606A (en) * | 1980-12-10 | 1982-06-18 | Mitsubishi Metal Corp | Production of fine silver powder |
| JPH1088207A (en) * | 1996-09-12 | 1998-04-07 | Dowa Mining Co Ltd | Silver powder and its manufacture |
| KR20040047100A (en) * | 2002-11-29 | 2004-06-05 | (주)창성 | Method for manufacturing nano-scale silver powders by wet reducing process |
| CN101088678A (en) * | 2006-06-13 | 2007-12-19 | 上海宝银电子材料有限公司 | Chemical reduction process of preparing silver powder |
| CN101554664A (en) * | 2009-05-20 | 2009-10-14 | 广东风华高新科技股份有限公司 | Method for preparing nano-scale silver powder |
| CN101707062A (en) * | 2009-12-03 | 2010-05-12 | 北京有色金属研究总院 | Nano-silver powder, manufacturing method and application thereof |
| CN101941078A (en) * | 2010-09-27 | 2011-01-12 | 彩虹集团公司 | Silver powder for electrode paste of solar cell and preparation method thereof |
| CN110997198A (en) * | 2017-06-05 | 2020-04-10 | 大州电子材料有限公司 | Silver particles and method for producing same |
| CN108907226A (en) * | 2018-07-13 | 2018-11-30 | 金川集团股份有限公司 | A kind of preparation method for laser ablation electrode circuit super fine silver powder |
Non-Patent Citations (1)
| Title |
|---|
| 刘漫红等: "《纳米材料及其制备技术》", 31 August 2014 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114226745A (en) * | 2021-12-10 | 2022-03-25 | 江西贝特利新材料有限公司 | Method for cleaning micron-sized flake silver powder |
| CN114226745B (en) * | 2021-12-10 | 2024-03-22 | 江西贝特利新材料有限公司 | Method for cleaning micron-sized flake silver powder |
| CN114799198A (en) * | 2022-04-14 | 2022-07-29 | 有研亿金新材料有限公司 | High-dispersity nanogold powder and preparation method thereof |
| CN115570141A (en) * | 2022-12-09 | 2023-01-06 | 长春黄金研究院有限公司 | Preparation method of superfine silver powder for conductive paste |
| CN115570141B (en) * | 2022-12-09 | 2023-03-07 | 长春黄金研究院有限公司 | Preparation method of superfine silver powder for conductive paste |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN113399679A (en) | Preparation method of high-tap aging-resistant superfine silver powder for electronic paste | |
| CN110434355B (en) | Preparation method of high-tap-density and high-dispersibility spherical silver powder | |
| CN110355380B (en) | Preparation method of hexagonal flaky micron-crystal silver powder | |
| CN112475311A (en) | Quasi-spherical silver powder with accurately controllable particle size and preparation method thereof | |
| CN104308183A (en) | Preparation method for flake silver powder for electronic paste | |
| CN110421179A (en) | A kind of low-temperature cured conductive elargol silver powder and preparation method thereof | |
| CN108672718A (en) | A kind of preparation method of the spherical silver powder of high specific area and its silver powder obtained | |
| CN115780824A (en) | Preparation method and application of silver powder with high sintering activity | |
| CN116251961A (en) | Method for preparing silver powder with assistance of ultrasonic waves, silver powder prepared by method and application of silver powder | |
| CN111774575A (en) | Preparation method of high-tap-density large-sheet-diameter flaky silver powder | |
| KR20190048316A (en) | Surface-treated silver powder and method for producing the same | |
| US20230211410A1 (en) | Silver powder for conductive paste having improved viscosity stability, and preparation method therefor | |
| CN106229026B (en) | Alloy silver powder and preparation method thereof and solar energy electrocondution slurry prepared therefrom | |
| CN115055691B (en) | Cluster-shaped silver powder with large particle size and preparation method thereof | |
| CN111590086A (en) | Ultrathin flake silver powder with smooth surface and preparation method thereof | |
| CN116422896A (en) | Conductive silver paste, silver powder and method for preparing silver powder by utilizing ionic dispersing agent | |
| JP5500237B1 (en) | Silver powder | |
| CN114188066A (en) | High-crystallization silver powder and low-cost heterojunction silver paste as well as preparation method and application thereof | |
| CN107755711A (en) | A kind of square micro-nano silver powder, preparation method thereof | |
| CN105817646B (en) | A kind of preparation method of the ball shape silver powder of high-tap density | |
| CN111014717A (en) | Silver powder for low-temperature curing conductive silver paste and preparation method thereof | |
| CN110434352A (en) | A kind of low-temperature cured conductive silver paste silver powder and preparation method thereof | |
| CN111659901A (en) | Preparation method of submicron silver powder | |
| CN113414401B (en) | Silver powder of crystalline silicon solar PERC battery silver paste and preparation method thereof | |
| CN116174739B (en) | Microcrystal nano-sheet aggregation type spheroidal silver powder and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |