CN111774583A - Preparation method of superfine silver powder with high tap mass and high specific surface - Google Patents
Preparation method of superfine silver powder with high tap mass and high specific surface Download PDFInfo
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 239000002270 dispersing agent Substances 0.000 claims abstract description 16
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 8
- 239000004094 surface-active agent Substances 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 22
- 239000007788 liquid Substances 0.000 claims description 21
- 238000000926 separation method Methods 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 12
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 10
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N EtOH Substances CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 229910052709 silver Inorganic materials 0.000 claims description 7
- 239000004332 silver Substances 0.000 claims description 7
- 239000000706 filtrate Substances 0.000 claims description 6
- BXWNKGSJHAJOGX-UHFFFAOYSA-N hexadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCO BXWNKGSJHAJOGX-UHFFFAOYSA-N 0.000 claims description 6
- 235000010489 acacia gum Nutrition 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 239000012065 filter cake Substances 0.000 claims description 5
- 238000012216 screening Methods 0.000 claims description 5
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000005635 Caprylic acid (CAS 124-07-2) Substances 0.000 claims description 4
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 4
- 229920000084 Gum arabic Polymers 0.000 claims description 4
- 241000978776 Senegalia senegal Species 0.000 claims description 4
- 239000000205 acacia gum Substances 0.000 claims description 4
- 229960002446 octanoic acid Drugs 0.000 claims description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 2
- DPUOLQHDNGRHBS-UHFFFAOYSA-N Brassidinsaeure Natural products CCCCCCCCC=CCCCCCCCCCCCC(O)=O DPUOLQHDNGRHBS-UHFFFAOYSA-N 0.000 claims description 2
- URXZXNYJPAJJOQ-UHFFFAOYSA-N Erucic acid Natural products CCCCCCC=CCCCCCCCCCCCC(O)=O URXZXNYJPAJJOQ-UHFFFAOYSA-N 0.000 claims description 2
- 235000021355 Stearic acid Nutrition 0.000 claims description 2
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 2
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 claims description 2
- 229960000541 cetyl alcohol Drugs 0.000 claims description 2
- DPUOLQHDNGRHBS-KTKRTIGZSA-N erucic acid Chemical compound CCCCCCCC\C=C/CCCCCCCCCCCC(O)=O DPUOLQHDNGRHBS-KTKRTIGZSA-N 0.000 claims description 2
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 2
- 229920002401 polyacrylamide Polymers 0.000 claims description 2
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 2
- 229920000053 polysorbate 80 Polymers 0.000 claims description 2
- 239000008117 stearic acid Substances 0.000 claims description 2
- 239000000243 solution Substances 0.000 abstract description 38
- 239000002245 particle Substances 0.000 abstract description 11
- 238000009826 distribution Methods 0.000 abstract description 5
- 238000002425 crystallisation Methods 0.000 abstract description 2
- 230000008025 crystallization Effects 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 230000006911 nucleation Effects 0.000 abstract description 2
- 238000010899 nucleation Methods 0.000 abstract description 2
- 239000012266 salt solution Substances 0.000 abstract description 2
- 238000006722 reduction reaction Methods 0.000 description 5
- 239000007791 liquid phase Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical group [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- XTYFHDXUXGBDGD-KVVVOXFISA-N (z)-docos-13-enoic acid;ethanol Chemical compound CCO.CCCCCCCC\C=C/CCCCCCCCCCCC(O)=O XTYFHDXUXGBDGD-KVVVOXFISA-N 0.000 description 1
- 239000001785 acacia senegal l. willd gum Substances 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- KYIDJMYDIPHNJS-UHFFFAOYSA-N ethanol;octadecanoic acid Chemical compound CCO.CCCCCCCCCCCCCCCCCC(O)=O KYIDJMYDIPHNJS-UHFFFAOYSA-N 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
- B22F1/147—Making a dispersion
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- Condensed Matter Physics & Semiconductors (AREA)
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Abstract
The invention discloses a preparation method of superfine silver powder with high tap height ratio, which adopts a reaction base solution to add a morphology regulator solution and a metal salt solution in parallel flow, prepares reducing powder by controlling the temperature of a reaction system, and has the advantages of narrow particle size distribution, good dispersibility, high tap density and high specific surface area, the average particle size is 1.0-3.0 mu m, and the specific surface area is 0.6-0.8m2The tap density is 4.0-5.5g/cm3The high tap height ratio table of the superfine silver powder. The selection of the reducing agent is the key for controlling the uniform and concentrated granularity, and the purpose of obtaining the silver powder product with narrow particle size distribution and good dispersibility can be better achieved by controlling the nucleation and the growth rate of the silver powder in the preparation process; morphology modulatorsThe selection is to control the crystallization property and the apparent morphology of the silver powder to achieve the aim of obtaining the silver powder product with high specific surface area. The prepared silver powder is ensured to have no dispersant residue after being washed and dried by the dispersant; the dispersibility and tap density of the synthesized silver powder are improved by the surfactant.
Description
Technical Field
The invention relates to the technical field of precious metal material preparation, in particular to a preparation method of superfine silver powder with high tap mass and high specific surface.
Background
With the rapid development of the technical fields of electronic industry, new energy and the like, the ultrafine silver powder is used as a functional material with very high surface activity and excellent electrical conductivity, and is widely applied to the fields of conductive paste, energy industry, composite materials, catalysts, antibacterial materials and the like. The conductive paste is used as a functional material and is widely applied to the production of various electronic components. Silver powder is the most important raw material of the conductive paste, has important influence on parameters such as film forming property, film thickness, electrical property, weldability and adhesiveness in the preparation process, and the quality of the silver powder directly influences the conductive paste and the performance of a finally formed conductor. Particularly, in recent years, the rapid development of the photovoltaic industry puts forward higher requirements on silver powder, and the silver powder is required to have the characteristics of high tap density, good dispersibility and the like. At present, a plurality of methods for preparing silver powder at home and abroad mainly comprise a grinding method, an atomization method, an evaporation and condensation method, an electrochemical deposition method, a sol-gel method, a liquid phase reduction method and the like. The liquid phase reduction method is characterized in that silver is reduced from a solution of salt or a complex of the silver in a form of powder through chemical reduction reaction under the protection action of a dispersing agent. The liquid phase reduction method has the advantages of simple operation process, small investment, high yield, low loss and good performance, and is one of the preparation methods with the most development prospects at present.
Disclosure of Invention
The invention aims to provide a preparation method of superfine silver powder with a high tap-height ratio. The invention utilizes a liquid phase reduction method to scientifically and reasonably control a reducing agent and a dispersing agent in the reduction process, and prepares the high-tap-height ratio table superfine silver powder with narrow particle size distribution, good silver powder dispersibility, high tap density, high specific surface area, environmental protection and no pollution.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of superfine silver powder with high tap mass and high specific surface comprises the following steps:
step one, dissolving a morphology regulator in pure water to obtain a morphology regulator solution A1L-2L with the mass volume concentration of 100-; dissolving a reducing agent and a dispersing agent in pure water to obtain reaction bottom liquid B1L-2L, wherein the mass volume concentration of the reducing agent in the reaction bottom liquid B is 100-170g/L and the mass volume concentration of the dispersing agent in the reaction bottom liquid B is 100-200 g/L;
step two, adding 1L-2L of silver nitrate solution with the mass volume concentration of 150-50 ℃ and the morphology regulator solution A prepared in the step one into the reaction base solution B in a concurrent flow manner at the temperature of 30-50 ℃, wherein the liquid adding time is 20-40min, stirring is carried out while adding, the stirring speed is 500-1000rpm, after reacting for 20-40min, surfactant-ethanol solution with the concentration of 0.01-0.1g/L is added while stirring, the stirring speed is 500rpm, stirring is carried out for 10-20min, then standing is carried out for 1-2h, and then the solution after reacting is subjected to solid-liquid separation;
step three, washing the solid obtained by separation in the step two for several times by pure water until the conductivity of the filtrate is less than or equal to 50 mu s/cm, carrying out solid-liquid separation, and drying the filter cake Ag powder in an oven for 10-20h at the temperature of 80 ℃;
step four, crushing and screening the silver powder obtained in the step three to obtain the silver powder with the average grain diameter of 1.0-3.0 mu m, and detecting that the specific surface area of the prepared silver powder is 0.6-0.8m2The tap density is 4.0-5.5g/cm3The silver content is more than 99.95 percent, and the silver powder is the superfine silver powder with high tap height ratio.
Preferably, the morphology regulator is one of ethylenediamine or triethanolamine.
Preferably, the reducing agent is one of gum arabic, formaldehyde or hydrazine hydrate.
Preferably, the preparation method of the surfactant-ethanol solution is to dissolve the surfactant in an absolute ethanol solution; the surfactant is one of isomeric stearic acid, erucic acid or polyacrylamide.
Preferably, the dispersant is one of polyethylene glycol, caprylic acid, succinic acid, tween 80 or cetyl alcohol.
The method detects Ag in the filtrate in the third step+The reagent used for the ionic content is a sodium chloride solution with a percentage concentration of 1%.
The method adopts the reaction base solution to add the morphology regulator solution and the metal salt solution in parallel, and prepares the reduced silver powder by controlling the temperature of the reaction system, the obtained silver powder has narrow particle size distribution, good dispersibility, high tap density and high specific surface area, the average particle size is 1.0-3.0 mu m, and the specific surface area is 0.6-0.8m2The tap density is 4.0-5.5g/cm3The high tap height ratio table of the superfine silver powder.
The invention adopts good appearance regulator, reducer and dispersant, and controls the granularity of the powder through the reaction time under the condition of controlling the reaction temperature of the reaction system; the selection of the reducing agent is the key for controlling the uniform and concentrated granularity, and the purpose of obtaining the silver powder product with narrow particle size distribution and good dispersibility can be better achieved by controlling the nucleation and the growth rate of the silver powder in the preparation process; the morphology regulator is selected to control the crystallization performance and the apparent morphology of the silver powder so as to achieve the aim of obtaining the silver powder product with high specific surface area. The prepared silver powder is ensured to have no dispersant residue after being washed and dried by the dispersant; the dispersibility and tap density of the synthesized silver powder are improved by the surfactant.
The method has no waste and pollutant discharge in the process of preparing the silver powder, is environment-friendly and is easy for large-scale production.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is an electron micrograph of the ultrafine silver powder according to the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following examples, but the present invention is not limited to the following embodiments and can be carried out by arbitrarily changing the examples.
Example 1
A preparation method of superfine silver powder with high tap mass and high specific surface comprises the following steps:
step one, dissolving 200g of ethylenediamine in 1L of pure water to obtain a morphology regulator solution A with the mass volume concentration of 200 g/L; dissolving 200g of polyethylene glycol and 170g of Arabic gum in 1L of pure water to obtain a reaction base solution B, wherein the mass volume concentration of a reducing agent in the reaction base solution B is 200g/L, and the mass volume concentration of a dispersing agent is 170 g/L;
step two, adding 1L of silver nitrate solution with the mass volume concentration of 250g/L and 1L of morphology regulator solution A prepared in the step one into reaction base solution B in a concurrent flow manner at 30 ℃, wherein the liquid adding time is 30min, the stirring speed is 500rpm while adding, after reacting for 20min, adding polyacrylamide-ethanol solution with the concentration of 0.04g/L while stirring, the stirring speed is 100rpm, stirring for 20min, standing for 2.0h, and then carrying out solid-liquid separation on the reacted solution;
step three, washing the solid obtained by separation in the step two for a plurality of times by pure water until the Ag of the filtrate+When the ionic conductivity is less than or equal to 50 mu s/cm, carrying out solid-liquid separation, and drying the filter cake Ag powder in an oven for 15h at the temperature of 80 ℃;
step four, crushing and screening the silver powder obtained in the step three to obtain the silver powder with the average grain diameter of 1.93 mu m, and detecting that the specific surface area of the prepared silver powder is 0.79m2(g) tap density of 4.65g/cm3The silver content is more than 99.95 percent and is a high tap height ratio tableSuperfine silver powder.
The data for the measurements of the two samples prepared in two portions according to the above method are shown in Table 1.
TABLE 1
| Example 1 | Average particle diameter (μm) | Tap density (g/cm)3） | Specific surface area (m)2/g） |
| Sample 1 | 1.93 | 4.65 | 0.79 |
| Sample 2 | 1.88 | 4.4 | 0.76 |
Example 2
A preparation method of superfine silver powder with high tap mass and high specific surface comprises the following steps:
step one, dissolving 100g of triethanolamine in 1L of pure water to obtain a morphology regulator solution A with the mass volume concentration of 100 g/L; dissolving 150g of caprylic acid and 100g of gum arabic in 1L of pure water to obtain a reaction base solution B, wherein the mass volume concentration of a reducing agent, i.e. caprylic acid, in the reaction base solution B is 150g/L, and the mass volume concentration of a dispersing agent, i.e. gum arabic, is 100 g/L;
step two, adding 1L of silver nitrate solution with the mass volume concentration of 250g/L and the morphology regulator solution A prepared in the step one into the reaction base solution B at the temperature of 30 ℃ in a parallel flow manner, wherein the liquid adding time is 30min, the stirring speed is 500rpm while adding, after reacting for 20min, adding isomeric stearic acid-ethanol solution with the concentration of 0.08g/L while stirring, the stirring speed is 100rpm, stirring for 20min, standing for 1h, and then carrying out solid-liquid separation on the reacted solution;
step three, washing the solid obtained by separation in the step two for a plurality of times by pure water until the Ag of the filtrate+When the ionic conductivity is less than or equal to 50 mu s/cm, carrying out solid-liquid separation, and drying the filter cake Ag powder in an oven for 15h at the temperature of 80 ℃;
step four, crushing and screening the silver powder obtained in the step three to obtain the silver powder with the average grain diameter of 2.97 mu m, and detecting that the specific surface area of the prepared silver powder is 0.601m2(g) tap density of 5.25g/cm3The silver content is more than 99.95 percent, and the silver powder is the superfine silver powder with high tap height ratio.
The data for the measurements of the two samples prepared in two portions according to the above method are shown in Table 2.
TABLE 2
| Example 2 | Average particle diameter (μm) | Tap density (g/cm)3） | Specific surface area (m)2/g） |
| Sample 1 | 2.97 | 5.25 | 0.601 |
| Sample 2 | 2.54 | 5.12 | 0.63 |
Example 3
A preparation method of superfine silver powder with high tap mass and high specific surface comprises the following steps:
step one, dissolving 300g of ethylenediamine in 2L of pure water to obtain a morphology regulator solution A with the mass volume concentration of 150 g/L; 300g of hexadecanol and 270g of formaldehyde are dissolved in 2L of pure water to obtain reaction base solution B, the mass volume concentration of the reducing agent hexadecanol in the reaction base solution B is 150g/L, and the mass volume concentration of the dispersing agent formaldehyde is 135 g/L;
step two, adding 2L of silver nitrate solution with the mass volume concentration of 250g/L and the morphology regulator solution A2L prepared in the step one into the reaction base solution B in a concurrent flow manner at 30 ℃, wherein the liquid adding time is 30min, the stirring speed is 500rpm while adding, after reacting for 20min, adding erucic acid-ethanol solution with the concentration of 0.04g/L while stirring, the stirring speed is 100rpm, stirring for 20min, standing for 1.5h, and then carrying out solid-liquid separation on the reacted solution;
step three, washing the solid obtained by separation in the step two for a plurality of times by pure water until the Ag of the filtrate+When the ionic conductivity is less than or equal to 50 mu s/cm, performing solid-liquid separation, and drying the filter cake Ag powder in an oven for 10 hours at the temperature of 80 ℃;
step four, crushing and screening the silver powder obtained in the step three to obtain the silver powder with the average particle size of 2.37 mu m, and detecting that the specific surface area of the prepared silver powder is 0.69m2(g) tap density of 4.85g/cm3The silver content is more than 99.95 percent, and the silver powder is the superfine silver powder with high tap height ratio.
The data of the measurements of the two samples prepared in two portions according to the above method are shown in Table 3.
TABLE 3
| Example 3 | Average particle diameter (μm) | Tap density (g/cm)3） | Specific surface area (m)2/g） |
| Sample 1 | 2.37 | 4.85 | 0.69 |
| Sample 2 | 2.67 | 4.45 | 0.66 |
Claims (5)
1. A preparation method of superfine silver powder with high tap mass and high specific surface is characterized by comprising the following steps: it comprises the following steps:
step one, dissolving a morphology regulator in pure water to obtain a morphology regulator solution A1L-2L with the mass volume concentration of 100-; dissolving a reducing agent and a dispersing agent in pure water to obtain reaction bottom liquid B1L-2L, wherein the mass volume concentration of the reducing agent in the reaction bottom liquid B is 100-170g/L and the mass volume concentration of the dispersing agent in the reaction bottom liquid B is 100-200 g/L;
step two, adding 1L-2L of silver nitrate solution with the mass volume concentration of 150-50 ℃ and the morphology regulator solution A prepared in the step one into the reaction base solution B in a concurrent flow manner at the temperature of 30-50 ℃, wherein the liquid adding time is 20-40min, stirring is carried out while adding, the stirring speed is 500-1000rpm, after reacting for 20-40min, surfactant-ethanol solution with the concentration of 0.01-0.1g/L is added while stirring, the stirring speed is 500rpm, stirring is carried out for 10-20min, then standing is carried out for 1-2h, and then the solution after reacting is subjected to solid-liquid separation;
step three, washing the solid obtained by separation in the step two for several times by pure water until the conductivity of the filtrate is less than or equal to 50 mu s/cm, carrying out solid-liquid separation, and drying the filter cake Ag powder in an oven for 10-20h at the temperature of 80 ℃;
step four, crushing and screening the silver powder obtained in the step three to obtain the silver powder with the average grain diameter of 1.0-3.0 mu m, and detecting that the specific surface area of the prepared silver powder is 0.6-0.8m2The tap density is 4.0-5.5g/cm3The silver content is more than 99.95 percent, and the silver powder is the superfine silver powder with high tap height ratio.
2. The method for preparing the ultrafine silver powder with high tap-height ratio according to claim 1, wherein the method comprises the following steps: the morphology regulator is one of ethylenediamine or triethanolamine.
3. The method for preparing the ultrafine silver powder having a high tap-to-height ratio according to claim 1 or 2, wherein: the reducing agent is one of gum arabic, formaldehyde or hydrazine hydrate.
4. The method for preparing the ultrafine silver powder with high tap-height ratio according to claim 3, wherein the method comprises the following steps: the preparation method of the surfactant-ethanol solution is to dissolve the surfactant in the absolute ethanol solution; the surfactant is one of isomeric stearic acid, erucic acid or polyacrylamide.
5. The method for preparing the ultrafine silver powder with high tap-height ratio according to claim 3, wherein the method comprises the following steps: the dispersant is one of polyethylene glycol, caprylic acid, succinic acid, tween 80 or cetyl alcohol.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110026564A (en) * | 2019-03-15 | 2019-07-19 | 安徽宝生元新材料有限公司 | A kind of flake silver powder of low-apparent-density and preparation method thereof |
| CN113305298A (en) * | 2021-05-28 | 2021-08-27 | 金川集团股份有限公司 | Preparation method of small-particle size medium-tap-density ultrafine silver powder |
| CN114871444A (en) * | 2022-07-12 | 2022-08-09 | 长春黄金研究院有限公司 | Preparation method of silver powder with high tap density and narrow particle size distribution |
Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1817524A (en) * | 2006-01-09 | 2006-08-16 | 四川大学 | Production of nanometer silver powder by liquid-phase and solid-liquid separating method |
| CN101347841A (en) * | 2008-09-03 | 2009-01-21 | 西北大学 | Method for preparing high tap density silver powder with controllable graininess |
| CN101618462A (en) * | 2008-07-03 | 2010-01-06 | 东进世美肯株式会社 | Method for manufacturing metal nanometer particle |
| CN102328094A (en) * | 2011-09-28 | 2012-01-25 | 上海交通大学 | Method for preparing ultrafine silver powder with uniform particle size |
| CN104148665A (en) * | 2014-07-22 | 2014-11-19 | 西北大学 | Preparation method of crystalized sliver powder |
| JP2015054975A (en) * | 2013-09-10 | 2015-03-23 | 住友金属鉱山株式会社 | Silver powder and method for producing the same |
| CN106623971A (en) * | 2016-12-08 | 2017-05-10 | 中国科学院深圳先进技术研究院 | Nano-silver particles for conductive ink and preparation method of nano-silver particles |
| CN106825544A (en) * | 2017-02-17 | 2017-06-13 | 江苏欧耐尔新型材料股份有限公司 | Improve the high-specific surface area silver powder and preparation method of electrode of solar battery electric conductivity |
| CN107876799A (en) * | 2017-12-18 | 2018-04-06 | 西安宏星电子浆料科技有限责任公司 | High-tap density low specific surface area super fine silver powder 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 |
| CN109365830A (en) * | 2018-11-19 | 2019-02-22 | 金川集团股份有限公司 | A kind of preparation method of the spherical super fine silver powder of high jolt ramming |
| CN110947953A (en) * | 2019-12-19 | 2020-04-03 | 苏州银瑞光电材料科技有限公司 | Preparation method of spherical silver powder with high sintering activity for solar front silver paste |
-
2020
- 2020-07-30 CN CN202010750957.3A patent/CN111774583A/en active Pending
Patent Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1817524A (en) * | 2006-01-09 | 2006-08-16 | 四川大学 | Production of nanometer silver powder by liquid-phase and solid-liquid separating method |
| CN101618462A (en) * | 2008-07-03 | 2010-01-06 | 东进世美肯株式会社 | Method for manufacturing metal nanometer particle |
| CN101347841A (en) * | 2008-09-03 | 2009-01-21 | 西北大学 | Method for preparing high tap density silver powder with controllable graininess |
| CN102328094A (en) * | 2011-09-28 | 2012-01-25 | 上海交通大学 | Method for preparing ultrafine silver powder with uniform particle size |
| JP2015054975A (en) * | 2013-09-10 | 2015-03-23 | 住友金属鉱山株式会社 | Silver powder and method for producing the same |
| CN104148665A (en) * | 2014-07-22 | 2014-11-19 | 西北大学 | Preparation method of crystalized sliver powder |
| CN106623971A (en) * | 2016-12-08 | 2017-05-10 | 中国科学院深圳先进技术研究院 | Nano-silver particles for conductive ink and preparation method of nano-silver particles |
| CN106825544A (en) * | 2017-02-17 | 2017-06-13 | 江苏欧耐尔新型材料股份有限公司 | Improve the high-specific surface area silver powder and preparation method of electrode of solar battery electric conductivity |
| CN107876799A (en) * | 2017-12-18 | 2018-04-06 | 西安宏星电子浆料科技有限责任公司 | High-tap density low specific surface area super fine silver powder 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 |
| CN109365830A (en) * | 2018-11-19 | 2019-02-22 | 金川集团股份有限公司 | A kind of preparation method of the spherical super fine silver powder of high jolt ramming |
| CN110947953A (en) * | 2019-12-19 | 2020-04-03 | 苏州银瑞光电材料科技有限公司 | Preparation method of spherical silver powder with high sintering activity for solar front silver paste |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110026564A (en) * | 2019-03-15 | 2019-07-19 | 安徽宝生元新材料有限公司 | A kind of flake silver powder of low-apparent-density and preparation method thereof |
| CN113305298A (en) * | 2021-05-28 | 2021-08-27 | 金川集团股份有限公司 | Preparation method of small-particle size medium-tap-density ultrafine silver powder |
| CN114871444A (en) * | 2022-07-12 | 2022-08-09 | 长春黄金研究院有限公司 | Preparation method of silver powder with high tap density and narrow particle size distribution |
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Application publication date: 20201016 |