CN113290252A - Preparation method of superfine silver powder with low tap mass and high specific surface - Google Patents
Preparation method of superfine silver powder with low tap mass and high specific surface Download PDFInfo
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- CN113290252A CN113290252A CN202110588498.8A CN202110588498A CN113290252A CN 113290252 A CN113290252 A CN 113290252A CN 202110588498 A CN202110588498 A CN 202110588498A CN 113290252 A CN113290252 A CN 113290252A
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 51
- 239000003223 protective agent Substances 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002245 particle Substances 0.000 claims abstract description 11
- 229910052709 silver Inorganic materials 0.000 claims abstract description 9
- 239000004332 silver Substances 0.000 claims abstract description 9
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 7
- 229920000642 polymer Polymers 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 17
- 238000000926 separation method Methods 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 13
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 7
- 239000003638 chemical reducing agent Substances 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 6
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000003607 modifier Substances 0.000 claims description 4
- 229920002401 polyacrylamide Polymers 0.000 claims description 4
- 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 3
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 3
- 108010010803 Gelatin Proteins 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- 235000021355 Stearic acid Nutrition 0.000 claims description 3
- 239000008273 gelatin Substances 0.000 claims description 3
- 229920000159 gelatin Polymers 0.000 claims description 3
- 235000019322 gelatine Nutrition 0.000 claims description 3
- 235000011852 gelatine desserts Nutrition 0.000 claims description 3
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 238000012216 screening Methods 0.000 claims description 3
- 239000008117 stearic acid Substances 0.000 claims description 3
- 239000001384 succinic acid Substances 0.000 claims description 3
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 2
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 2
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 2
- 239000005642 Oleic acid Substances 0.000 claims description 2
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 230000006911 nucleation Effects 0.000 abstract description 2
- 238000010899 nucleation Methods 0.000 abstract description 2
- 230000035484 reaction time Effects 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 3
- 238000012360 testing method Methods 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- 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
- 238000010586 diagram Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
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
- B22F2301/00—Metallic composition of the powder or its coating
- B22F2301/25—Noble metals, i.e. Ag Au, Ir, Os, Pd, Pt, Rh, Ru
- B22F2301/255—Silver or gold
Abstract
The invention discloses a preparation method of low-tap high-ratio table superfine silver powder, which comprises the steps of firstly adding a high-molecular protective agent solution into a silver nitrate solution, then adding a strong base solution, and preparing reduced silver powder by controlling the temperature of a reaction system, wherein the average particle size of the obtained silver powder is 0.54-0.79 mu m, and the specific surface area is 2.12-2.48 m2The tap density is 2.02-2.49 g/cm3The silver content is more than 99.95 percent, and the obtained silver powder has small particle size, high specific surface area and low tap density. The invention adopts good polymer protective agent, and controls the granularity of the silver powder through the reaction time under the condition of controlling the reaction temperature of the reaction system. The selection of sodium hydroxide is the key for controlling the uniform and concentrated granularity, and the purpose of obtaining the silver powder product with small grain diameter and high specific surface area can be better achieved by controlling the nucleation and growth rate of the silver powder. The preparation method is simple and convenient, high in yield, good in repeatability and easy for large-scale production.
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 a low tap mass and a high specific surface.
Background
With the rapid development of the electronic industry, new energy and other technical fields, microelectronic products tend to be miniaturized, integrated and intelligent. The superfine silver powder with the particle size of less than 1.0 mu m is used as a functional material with high surface activity and excellent conductivity and is widely applied to the fields of conductive paste, energy industry, composite materials, catalysts, antibacterial materials and the like. In order to adapt to the trend, developed countries are dedicated to research and development of thick film slurry, noble metal powder and the like, and research in the field of China is greatly developed. 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 low tap density and high specific surface area, which utilizes a liquid phase reduction method to scientifically and reasonably control a reducing agent and a dispersing agent in a reduction process to prepare the superfine silver powder with small particle size, low tap density and high specific surface area.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of superfine silver powder with a low tap-height ratio table comprises the following steps:
dissolving a macromolecular protective agent in pure water to obtain 1L of macromolecular protective agent solution with the mass volume concentration of 0.1-0.2 g/L; dissolving sodium hydroxide solid in pure water to obtain 1L of sodium hydroxide solution with the mass volume concentration of 50-100 g/L, and dissolving a surface modifier in an absolute ethyl alcohol solution to obtain a surface modifier-absolute ethyl alcohol solution with the mass volume concentration of 0.01-0.1 g/L;
step two, firstly adding the macromolecular protective agent solution prepared in the step one into a silver nitrate solution with the mass volume concentration of 150-300 g/L, then adding the sodium hydroxide solution prepared in the step one, stirring while adding the solution for 4-8 min, then adding a reducing agent to perform synthetic reaction for 10-30min, standing for 1-2h, and then performing solid-liquid separation on the reacted solution;
step three, washing the solid obtained by separation in the step two with pure water for several times until the conductivity of the filtrate is less than or equal to 50 mu s/cm, carrying out solid-liquid separation, adding the surface modifier-absolute ethyl alcohol solution prepared in the step one, and drying in an oven at 60 ℃ for 10-20 h to obtain silver powder;
step four, screening the silver powder obtained in the step three to obtain the silver powder with the average particle size of 0.54-0.79 mu m and the specific surface area of 2.12-2.48 m2The tap density is 2.02-2.49 g/cm3The silver content is more than 99.95 percent, and the superfine silver powder has a low tap-height ratio.
Preferably, the polymeric protective agent in the first step is one of polyethylene glycol, gelatin or succinic acid.
Preferably, the reducing agent in the first step is one of ethylenediamine, hydrazine hydrate or formaldehyde.
Preferably, in the first step, the surface modifier is one of isomeric stearic acid, oleic acid or polyacrylamide.
The preparation method is simple and convenient, high in yield, good in repeatability and easy for large-scale production.
And the reagent for detecting the conductivity in the filtrate in the third step is a sodium chloride solution with the mass percentage concentration of 1%.
The method comprises the steps of firstly adding a high-molecular protective agent solution into a silver nitrate solution, then adding a strong base solution, and preparing the reduced silver powder by controlling the temperature of a reaction system, wherein the average particle size of the obtained silver powder is 0.54-0.79 mu m, and the specific surface area is 2.12-2.48 m2The tap density is 2.02-2.49 g/cm3The silver content is more than 99.95 percent, and the obtained silver powder has small particle size, high specific surface area and low tap density.
The invention adopts good polymer protective agent, and controls the granularity of the silver powder through the reaction time under the condition of controlling the reaction temperature of the reaction system. The selection of sodium hydroxide is the key for controlling the uniform and concentrated granularity, and the purpose of obtaining the silver powder product with small grain diameter and high specific surface area can be better achieved by controlling the nucleation and growth rate of the silver powder.
In the present invention, the surfactant is selected to improve the dispersibility of the synthesized small-particle-size silver powder.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a photograph of a micromirror plate made of ultrafine silver powder according to an example of the present invention.
Detailed Description
The technical solution of the present invention will be further described in detail with reference to the accompanying drawings and specific embodiments.
Example 1
A preparation method of superfine silver powder with a low tap-height ratio table comprises the following steps:
step one, 10g of gelatin is dissolved in pure water to obtain 1L of macromolecular protective agent solution with mass volume concentration of 0.1 g/L; dissolving 50g of sodium hydroxide in pure water to obtain 1L of sodium hydroxide solution with the mass volume concentration of 50g/L, and dissolving 5g of isomeric stearic acid and fatty acid in absolute ethyl alcohol to obtain 50ml of surface modifier-absolute ethyl alcohol solution with the mass volume concentration of 0.1 g/L;
step two, firstly adding the macromolecular protective agent solution prepared in the step one into 1L of silver nitrate solution with the mass volume concentration of 300g/L, then adding the sodium hydroxide solution prepared in the step one, wherein the total liquid adding time is 8min, stirring is carried out while adding, and the stirring speed is 200 rpm; adding 500g of ethylenediamine to carry out synthetic reaction for 10min, standing for 1h, and then carrying out solid-liquid separation on the solution after the reaction;
step three, washing the solid obtained by separation in the step two with pure water for several times until the conductivity of the filtrate is less than or equal to 50 mus/cm, carrying out solid-liquid separation, adding the surface modifier-absolute ethyl alcohol solution prepared in the step one, and drying in an oven for 20 hours at 60 ℃ to obtain silver powder;
step four, repeating the step 5 times, screening the silver powder obtained in the step three, and checking to obtain the silver powder with the average particle size of 0.75-0.79 mu m and the specific surface area of 2.12-2.20 m2The tap density is 2.49-2.32 g/cm3The silver content is more than 99.96 percent, and the superfine silver powder has a low tap-height ratio. The test data are shown in table 1.
TABLE 1
Example 2
A preparation method of superfine silver powder with a low tap-height ratio table comprises the following steps:
step one, dissolving 20g of succinic acid in pure water to obtain 1L of macromolecular protective agent solution with the mass volume concentration of 0.2 g/L; dissolving 80g of sodium hydroxide in pure water to obtain 1L of sodium hydroxide solution with the mass volume concentration of 80g/L, and dissolving 2g of polyacrylamide in absolute ethyl alcohol to obtain 50ml of surface modifier-absolute ethyl alcohol solution with the mass volume concentration of 0.04 g/L;
step two, firstly adding the macromolecular protective agent solution prepared in the step one into 1L of silver nitrate solution with the mass volume concentration of 150g/L, then adding the sodium hydroxide solution prepared in the step one, wherein the total liquid adding time is 4min, stirring is carried out while adding, the stirring speed is 600rpm, 720g of hydrazine hydrate is added for carrying out synthetic reaction for 30min, then standing is carried out for 1.5h, and then the solution after the reaction is subjected to solid-liquid separation;
step three, washing the solid obtained by separation in the step two with pure water for several times until the conductivity of the filtrate is less than or equal to 50 mus/cm, carrying out solid-liquid separation, adding the surface modifier-absolute ethyl alcohol solution prepared in the step one, and drying in an oven for 12 hours at 60 ℃ to obtain silver powder;
step four, repeating the step 5 times, and sieving the silver powder obtained in the step three to obtain the silver powder with the average particle size of 0.54-0.62 mu m and the specific surface area of 2.48-2.33 m2The tap density is 2.02-2.12 g/cm3The silver content is more than 99.95 percent, and the superfine silver powder has a low tap-height ratio. The test data are shown in table 2.
TABLE 2
Example 3
A preparation method of superfine silver powder with a low tap-height ratio table comprises the following steps:
step one, dissolving 15g of polyethylene glycol in pure water to obtain 1L of macromolecular protective agent solution with the mass volume concentration of 0.15 g/L; dissolving 100g of sodium hydroxide in pure water to obtain 1L of sodium hydroxide solution with the mass volume concentration of 100g/L, and dissolving 1g of polyacrylamide in absolute ethyl alcohol to obtain 50ml of surface modifier-absolute ethyl alcohol solution with the mass volume concentration of 0.01 g/L;
step two, firstly adding the macromolecular protective agent solution prepared in the step one into 1L of silver nitrate solution with the mass volume concentration of 250g/L, then adding the sodium hydroxide solution prepared in the step one, wherein the total liquid adding time is 6min, stirring is carried out while adding, and the stirring speed is 500 rpm; adding 480g of formaldehyde for synthetic reaction for 25min, standing for 2h, and then carrying out solid-liquid separation on the reacted solution;
step three, washing the solid obtained by separation in the step two with pure water for several times until the conductivity of the filtrate is less than or equal to 50 mus/cm, carrying out solid-liquid separation, adding the surface modifier-absolute ethyl alcohol solution prepared in the step one, and drying in an oven for 10 hours at 60 ℃ to obtain silver powder;
step four, repeating the step 5 times, and sieving the silver powder obtained in the step three to obtain the silver powder with the average particle size of 0.65-0.74 mu m and the specific surface area of 2.19-2.13 m2The tap density is 2.13-2.32 g/cm3The silver content is more than 99.97 percent, and the superfine silver powder has a low tap-height ratio. The test data are shown in table 3.
TABLE 3
Claims (4)
1. A preparation method of superfine silver powder with a low tap-height ratio table is characterized by comprising the following steps: the method comprises the following steps:
dissolving a macromolecular protective agent in pure water to obtain 1L of macromolecular protective agent solution with the mass volume concentration of 0.1-0.2 g/L; dissolving sodium hydroxide solid in pure water to obtain 1L of sodium hydroxide solution with the mass volume concentration of 50-100 g/L, and dissolving a surface modifier in an absolute ethyl alcohol solution to obtain a surface modifier-absolute ethyl alcohol solution with the mass volume concentration of 0.01-0.1 g/L;
step two, firstly adding the macromolecular protective agent solution prepared in the step one into a silver nitrate solution with the mass volume concentration of 150-300 g/L, then adding the sodium hydroxide solution prepared in the step one, stirring while adding the solution for 4-8 min, then adding a reducing agent to perform synthetic reaction for 10-30min, standing for 1-2h, and then performing solid-liquid separation on the reacted solution;
step three, washing the solid obtained by separation in the step two with pure water for several times until the conductivity of the filtrate is less than or equal to 50 mu s/cm, carrying out solid-liquid separation, adding the surface modifier-absolute ethyl alcohol solution prepared in the step one, and drying in an oven at 60 ℃ for 10-20 h to obtain silver powder;
step four, screening the silver powder obtained in the step three to obtain the silver powder with the average particle size of 0.54-0.79 mu m and the specific surface area of 2.12-2.48 m2The tap density is 2.02-2.49 g/cm3The silver content is more than 99.95 percent, and the superfine silver powder has a low tap-height ratio.
2. The method for preparing the ultrafine silver powder with the low tap height ratio according to claim 1, wherein the method comprises the following steps: the polymer protective agent in the first step is one of polyethylene glycol, gelatin or succinic acid.
3. The method for preparing the ultrafine silver powder having a low tap height ratio according to claim 1 or 2, wherein: in the first step, the reducing agent is one of ethylenediamine, hydrazine hydrate or formaldehyde.
4. The method for preparing the ultrafine silver powder with the low tap height ratio according to claim 3, wherein the method comprises the following steps: in the first step, the surface modifier is one of isomeric stearic acid, oleic acid or polyacrylamide.
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| 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 |
| CN110666184A (en) * | 2019-10-28 | 2020-01-10 | 苏州银瑞光电材料科技有限公司 | Preparation method of sphere-like silver powder |
| CN111889698A (en) * | 2020-09-01 | 2020-11-06 | 苏州银瑞光电材料科技有限公司 | Preparation method of superfine spherical silver powder |
| CN112296351A (en) * | 2020-09-29 | 2021-02-02 | 湖南诺尔得材料科技有限公司 | Preparation method of high-tap-density ultrafine silver powder |
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