CN114226745B - Method for cleaning micron-sized flake silver powder - Google Patents
Method for cleaning micron-sized flake silver powder Download PDFInfo
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- CN114226745B CN114226745B CN202111509080.XA CN202111509080A CN114226745B CN 114226745 B CN114226745 B CN 114226745B CN 202111509080 A CN202111509080 A CN 202111509080A CN 114226745 B CN114226745 B CN 114226745B
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- silver powder
- silver
- cleaning
- micron
- impedance
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 95
- 238000004140 cleaning Methods 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 22
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 15
- 230000002209 hydrophobic effect Effects 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 238000010008 shearing Methods 0.000 claims abstract description 11
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 11
- 238000005406 washing Methods 0.000 claims abstract description 11
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 10
- 150000002497 iodine compounds Chemical class 0.000 claims abstract description 9
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims abstract description 8
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims abstract description 8
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims abstract description 8
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000005642 Oleic acid Substances 0.000 claims abstract description 8
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims abstract description 8
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims abstract description 8
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 5
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 9
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 2
- 229910000043 hydrogen iodide Inorganic materials 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 11
- 230000002776 aggregation Effects 0.000 abstract description 5
- 238000005054 agglomeration Methods 0.000 abstract description 4
- 230000003993 interaction Effects 0.000 abstract description 3
- 229910052709 silver Inorganic materials 0.000 description 13
- 239000004332 silver Substances 0.000 description 13
- 238000003756 stirring Methods 0.000 description 10
- 239000002245 particle Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 6
- 238000000926 separation method Methods 0.000 description 6
- 239000002002 slurry Substances 0.000 description 6
- 238000004537 pulping Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000009826 distribution Methods 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 3
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- 208000005156 Dehydration Diseases 0.000 description 2
- 239000013543 active substance Substances 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 238000009210 therapy by ultrasound Methods 0.000 description 2
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 229960005070 ascorbic acid Drugs 0.000 description 1
- 235000010323 ascorbic acid Nutrition 0.000 description 1
- 239000011668 ascorbic acid Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 125000005314 unsaturated fatty acid group Chemical group 0.000 description 1
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
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G5/00—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents
- C23G5/02—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using organic solvents
- C23G5/032—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using organic solvents containing oxygen-containing compounds
Abstract
The invention provides a method for cleaning micron-sized flake silver powder, which comprises the following steps: mixing silver nitrate, a reducing agent and a hydrophobic agent, and reacting to obtain a reaction product; dehydrating the reaction product until the mass content of silver powder is more than or equal to 95%, and adding ethanol for slurrying; adding iodine compound under ultrasonic condition, shearing and washing at 1500-2500 rpm, solid-liquid separating and stoving to obtain micron level silver flake. According to the method provided by the invention, the hydrophobic agent such as oleic acid is used for carrying out the surface hydrophobic treatment of the silver powder in the reaction process, so that the interaction force between the silver powder is changed, the surface free energy of the agglomeration of the silver powder is broken through washing in a high-speed shearing mode, the dispersibility of the silver powder in an oily system is reasonably improved, and the impedance of the silver powder is reduced. The impedance of silver powder obtained by cleaning by the cleaning method provided by the invention can be reduced by 10-20%; the impedance reaches 170Ω.
Description
Technical Field
The invention belongs to the technical field of noble metal cleaning, and particularly relates to a method for cleaning micron-sized flake silver powder.
Background
The low-impedance micron-sized flake silver powder is an important raw material for preparing the conductive silver paste of the circuit board. At present, research on micron-sized flake silver powder is mainly focused on a synthesis method, cooperation of a reaction device and control of reaction conditions, and little research is conducted on post-treatment steps after silver powder synthesis. The D50 of the micron-sized silver powder is generally concentrated at 3-5 mu m, the surface energy is large, and the aggregation is very easy.
The traditional silver powder cleaning method adopts a method of centrifugation and stirring soaking, can not fully break the agglomeration of flake silver powder, and the agglomerated particles enable micron-sized silver powder to form compact lamination in silver paste, so that impedance is increased, and conductivity is poor.
Disclosure of Invention
In view of the above, the present invention aims to provide a method for cleaning micron-sized plate-like silver powder, which can reduce the impedance of silver paste.
The invention provides a method for cleaning micron-sized flake silver powder, which comprises the following steps:
mixing silver nitrate, a reducing agent and a hydrophobic agent, and reacting to obtain a reaction product;
dehydrating the reaction product until the mass content of silver powder is more than or equal to 95%, and adding ethanol for slurrying;
adding iodine compound under ultrasonic condition, shearing and washing at 1500-2500 rpm, solid-liquid separating and stoving to obtain micron level silver flake.
In the present invention, the hydrophobic agent is selected from unsaturated fatty acids.
In the present invention, the hydrophobic agent is selected from oleic acid.
In the invention, the mass ratio of the hydrophobizing agent to the silver nitrate is 0.01-0.02:1.
In the present invention, the iodine compound is selected from potassium iodide and/or hydrogen iodide.
In the invention, the mass ratio of the iodine compound to the unsaturated fatty acid is 0.95-1.05:40.
In the invention, the mass ratio of the ethanol to the silver powder is 1:0.95 to 1.05.
In the invention, the mass concentration of the ethanol is 95-99%.
In the invention, the temperature of the drying is 65-75 ℃.
In the invention, the frequency of the ultrasonic wave is 3000-4000 Hz;
stirring at 1500-2500 rpm for 3000-4000 min.
The invention provides a method for cleaning micron-sized flake silver powder, which comprises the following steps: mixing silver nitrate, a reducing agent and a hydrophobic agent, and reacting to obtain a reaction product; dehydrating the reaction product until the mass content of silver powder is more than or equal to 95%, and adding ethanol for slurrying; adding iodine compound under ultrasonic condition, shearing and washing at 1500-2500 rpm, solid-liquid separating and stoving to obtain micron level silver flake. According to the method provided by the invention, the hydrophobic agent such as oleic acid is used for carrying out the surface hydrophobic treatment of the silver powder in the reaction process, so that the interaction force between the silver powder is changed, the surface free energy of the agglomeration of the silver powder is broken through washing in a high-speed shearing mode, the dispersibility of the silver powder in an oily system is reasonably improved, and the impedance of the silver powder is reduced.
Detailed Description
In order to further illustrate the present invention, a method for cleaning a micron-sized plate-like silver powder according to the present invention is described in detail with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
(1) The silver powder surface hydrophobization treatment of the micron silver powder is that silver nitrate (50 kg) is reduced into micron silver powder by taking ascorbic acid as a reducing agent, and unsaturated fatty acid (oleic acid, 400 g) serving as a hydrophobizing agent is added during the reduction to prepare initial silver powder;
(2) Dehydrating: adding the silver powder after the reaction into a filter press to carry out dehydration treatment, and controlling the mass fraction of the silver powder to be more than 95%;
(3) Pulping: adding alcohol with the weight ratio of 1:1 into the silver powder, and performing slurrying treatment;
(4) And (3) surface-active treatment: adding 10g of active substance potassium iodide under 3000Hz while performing ultrasonic treatment;
(5) High-speed shearing and washing: stirring the slurry in a high-speed dispersing machine at 1500-2000 rpm for 60min;
(6) Solid-liquid separation: carrying out solid-liquid separation on the slurry by using a centrifugal machine, wherein the centrifugal speed is 600rpm;
(7) And (3) drying: and (3) placing the silver powder subjected to solid-liquid separation into a vacuum oven at 70 ℃, and baking to constant weight to obtain the micron-sized flake silver powder.
The silver powder obtained in example 1 was prepared into a silver paste containing 53 silver and having an impedance of 170Ω, with the particle size of the silver flakes ranging from 2.8 to 3.2 μm and the particle size distribution being more uniform and concentrated.
Comparative example 1
(1) The reaction: directly reducing silver nitrate into silver powder by a reducing agent;
(2) Sedimentation: settling the silver powder after the reaction for more than half an hour;
(3) Controlling the water content of silver powder: pumping out the supernatant, and controlling the mass fraction of the silver powder to be about 80%;
(4) Pulping: adding pure water in a weight ratio of 1:1 into the silver powder, and performing slurrying treatment;
(5) Stirring, soaking and cleaning: placing the pulped slurry into a stirrer for stirring at the stirring speed of 500-800 rpm, and repeatedly cleaning for three times after suction filtration;
(6) And (3) drying: and placing the obtained silver powder in a vacuum oven at 70 ℃, and drying to constant weight to obtain the micron-sized flake silver powder.
The particle size of the micron-sized plate-like silver powder was 2.8 to 3.5. Mu.m, and the silver powder obtained in comparative example 1 was made into 53-silver-containing silver paste having an impedance of 200Ω.
The impedance of the silver paste was reduced by 30Ω, and the particle size distribution of the silver powder was narrower and better controlled, than in comparative example 1.
Example 2
(1) Hydrophobization treatment of silver powder surface: adding 400g of hydrophobic agent oleic acid into silver nitrate (50 kg) in the process of replacing silver powder;
(2) Dehydrating: adding the silver powder after the reaction into a filter press to carry out dehydration treatment, and controlling the mass fraction of the silver powder to be more than 90%;
(3) Pulping: adding alcohol with the weight ratio of 1:0.9 into the silver powder, and pulping;
(4) And (3) surface-active treatment: adding 10g of active substance potassium iodide under 3000Hz while performing ultrasonic treatment;
(5) High-speed shearing and washing: stirring the slurry in a high-speed dispersing machine at 2000-2500 rpm for 60min;
(6) Solid-liquid separation: carrying out solid-liquid separation on the slurry by using a centrifugal machine, wherein the centrifugal speed is 800rpm;
(7) And (3) drying: and (3) placing the silver powder subjected to solid-liquid separation into a vacuum oven at 65 ℃, and baking to constant weight to obtain the micron-sized flake silver powder.
The particle size of the micron-sized plate-like silver powder was 2.7 to 3.3. Mu.m, and the silver powder obtained in example 2 was made into a 53-silver-containing silver paste having an impedance of 185. OMEGA.
Comparative example 2
(1) The reaction: the silver nitrate is directly replaced;
(2) Sedimentation: settling the silver powder after the reaction for more than half an hour;
(3) Controlling the water content of silver powder: pumping out the supernatant, and controlling the mass fraction of the silver powder to be about 75%;
(4) Pulping: adding pure water with the weight ratio of 1:0.75 into the silver powder, and performing slurrying treatment;
(5) Stirring, soaking and cleaning: and placing the pulped slurry into a stirrer for stirring at the stirring speed of 800-1000 rpm, and repeatedly cleaning for three times after suction filtration.
(6) And (3) drying: and placing the obtained silver powder in a vacuum oven at 65 ℃, and drying to constant weight to obtain the micron-sized silver powder.
The particle size of the micron-sized plate-like silver powder was 2.6 to 3.6 microns, and the silver powder obtained in comparative example 2 was made into a 53-silver-containing silver paste having an impedance of 210. OMEGA.
Example 2 the resistance of the silver paste was reduced by 25 Ω and the particle size distribution of the silver powder was narrower and better controlled than comparative example 2.
As can be seen from the above examples, the present invention provides a method for cleaning micron-sized plate silver powder, comprising the following steps: mixing silver nitrate, a reducing agent and a hydrophobic agent, and reacting to obtain a reaction product; dehydrating the reaction product until the mass content of silver powder is more than or equal to 95%, and adding ethanol for slurrying; adding iodine compound under ultrasonic condition, shearing and washing at 1500-2500 rpm, solid-liquid separating and stoving to obtain micron level silver flake. According to the method provided by the invention, the hydrophobic agent such as oleic acid is used for carrying out the surface hydrophobic treatment of the silver powder in the reaction process, so that the interaction force between the silver powder is changed, the surface free energy of the agglomeration of the silver powder is broken through washing in a high-speed shearing mode, the dispersibility of the silver powder in an oily system is reasonably improved, and the impedance of the silver powder is reduced. The experimental results show that: the impedance of silver powder obtained by cleaning by the cleaning method provided by the invention can be reduced by 10-20%; the impedance reaches 170Ω.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (5)
1. The method for cleaning the micron-sized flake silver powder comprises the following steps of:
mixing silver nitrate, a reducing agent and a hydrophobic agent, and reacting to obtain a reaction product; the hydrophobizing agent is selected from oleic acid; the mass ratio of the hydrophobizing agent to the silver nitrate is 0.01-0.02:1;
dehydrating the reaction product until the mass content of silver powder is more than or equal to 95%, and adding ethanol for slurrying;
adding an iodine compound under the ultrasonic condition, shearing and washing at 1500-2500 rpm, separating solid from liquid, and drying to obtain micron-sized flake silver powder;
the iodine compound is selected from potassium iodide and/or hydrogen iodide; the mass ratio of the iodine compound to the oleic acid is 0.95-1.05:40.
2. The cleaning method according to claim 1, wherein the mass ratio of the ethanol to the silver powder is 1:0.95 to 1.05.
3. The method according to claim 1, wherein the mass concentration of the ethanol is 95 to 99%.
4. The cleaning method according to claim 1, wherein the temperature of the drying is 65 to 75 ℃.
5. The cleaning method according to claim 1, wherein the frequency of the ultrasonic wave is 3000 to 4000Hz;
the time of shearing and washing at 1500-2500 rpm is 30-60 min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111509080.XA CN114226745B (en) | 2021-12-10 | 2021-12-10 | Method for cleaning micron-sized flake silver powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111509080.XA CN114226745B (en) | 2021-12-10 | 2021-12-10 | Method for cleaning micron-sized flake silver powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114226745A CN114226745A (en) | 2022-03-25 |
| CN114226745B true CN114226745B (en) | 2024-03-22 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111509080.XA Active CN114226745B (en) | 2021-12-10 | 2021-12-10 | Method for cleaning micron-sized flake silver powder |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1686646A (en) * | 2005-04-26 | 2005-10-26 | 四川大学 | Preparation method of grain size controllable single dispersed nano silver powder |
| CN102407341A (en) * | 2011-10-27 | 2012-04-11 | 浙江光达电子科技有限公司 | surface modified particle diameter mixed silver powder and preparation method thereof |
| CN103079730A (en) * | 2011-06-16 | 2013-05-01 | 住友金属矿山株式会社 | Silver powder and method for producing same |
| CN106753026A (en) * | 2016-12-30 | 2017-05-31 | 中国科学院深圳先进技术研究院 | The modified method in surface, modified silver powder and the conductive silver glue comprising it are carried out to silver powder |
| CN109550933A (en) * | 2018-12-04 | 2019-04-02 | 苏州市贝特利高分子材料股份有限公司 | A kind of superthin section silver and its chemical synthesis process |
| CN112605394A (en) * | 2020-12-10 | 2021-04-06 | 广东先导稀材股份有限公司 | Preparation method of silver powder for conductive paste |
| CN113399679A (en) * | 2021-05-08 | 2021-09-17 | 东方电气集团科学技术研究院有限公司 | Preparation method of high-tap aging-resistant superfine silver powder for electronic paste |
-
2021
- 2021-12-10 CN CN202111509080.XA patent/CN114226745B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1686646A (en) * | 2005-04-26 | 2005-10-26 | 四川大学 | Preparation method of grain size controllable single dispersed nano silver powder |
| CN103079730A (en) * | 2011-06-16 | 2013-05-01 | 住友金属矿山株式会社 | Silver powder and method for producing same |
| CN102407341A (en) * | 2011-10-27 | 2012-04-11 | 浙江光达电子科技有限公司 | surface modified particle diameter mixed silver powder and preparation method thereof |
| CN106753026A (en) * | 2016-12-30 | 2017-05-31 | 中国科学院深圳先进技术研究院 | The modified method in surface, modified silver powder and the conductive silver glue comprising it are carried out to silver powder |
| CN109550933A (en) * | 2018-12-04 | 2019-04-02 | 苏州市贝特利高分子材料股份有限公司 | A kind of superthin section silver and its chemical synthesis process |
| CN112605394A (en) * | 2020-12-10 | 2021-04-06 | 广东先导稀材股份有限公司 | Preparation method of silver powder for conductive paste |
| CN113399679A (en) * | 2021-05-08 | 2021-09-17 | 东方电气集团科学技术研究院有限公司 | Preparation method of high-tap aging-resistant superfine silver powder for electronic paste |
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