CN104858415B - A kind of washing methods of super fine silver powder - Google Patents
A kind of washing methods of super fine silver powder Download PDFInfo
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- CN104858415B CN104858415B CN201510195970.6A CN201510195970A CN104858415B CN 104858415 B CN104858415 B CN 104858415B CN 201510195970 A CN201510195970 A CN 201510195970A CN 104858415 B CN104858415 B CN 104858415B
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Abstract
The present invention provides a kind of washing methods of super fine silver powder, settles first, controls quality of cathode silver fraction in slurry to be 60 ~ 80%;Fatty acid is added to carry out surface-hydrophobicized process in the slurry after sedimentation;Homogenizing washing in rotor stator type homogenizer is added after stirring pulp;After solid-liquid separation, Solid Silver dried bean noodles is dry obtains super fine silver powder product.The argentum powder tap density that the super fine silver powder tap density being obtained using this washing methods is obtained than traditional agitator treating improves 20 ~ 40%.
Description
Technical field
The invention belongs to precious metal smelting technical field is and in particular to a kind of washing methods of super fine silver powder.
Background technology
High-tap density super fine silver powder is the important source material preparing high-temperature sintered silver paste.At present, the research to super fine silver powder
It is concentrated mainly on synthetic method and reaction unit, and the research to handling process such as the washing after argentum powder synthesis, dryings is less.Super
The granule of thin argentum powder is less than 2 μm, and surface energy is larger, easily forms aggregate.Conventional washing silver powder is typically using centrifugation, immersion
Or the method for stirring is it is impossible to fully open the reunion between super fine silver powder.Agglomerated particle makes super fine silver powder can not form fine and close heap
Long-pending, lead to tap density relatively low.
Content of the invention
In order to overcome deficiency of the prior art, the present invention provides a kind of washing methods of super fine silver powder, ultra-fine to improve
The tap density of argentum powder.
The present invention is achieved by the following technical solutions:
A kind of washing methods of super fine silver powder is it is characterised in that comprise the steps:
(1)Sedimentation
Super fine silver powder synthesis after slurry is settled, pour out supernatant so that in slurry quality of cathode silver fraction be 60 ~
80%;
(2)Surface-hydrophobicized process
Add fatty acid in the slurry after sedimentation, the quality of addition fatty acid with theoretical output quality of cathode silver ratio is
0.001~0.01:1;Theoretical output quality of cathode silver is to generate during the yield 100% being calculated according to the raw material of argentum powder synthetic reaction
The quality of argentum powder, the preferred stearic acid of wherein said fatty acid;
(3)Stirring pulp
Pulp is sufficiently stirred for the slurry after surface-hydrophobicized process, makes the uniform dispersion of formation, mixing speed is
200 ~ 400rpm, mixing time 20 ~ 60min;
(4)Homogenizing is washed
Slurry after pulp adds homogenizing washing in rotor-stator homogenizer, then settles, solid-liquid separation, obtains
To argentum powder, the rotor of homogenizer and stator gap are 0.25 ~ 0.50mm, and rotor speed is 3000 ~ 6000rpm;
(5)It is dried
The argentum powder obtaining puts oven drying, obtains super fine silver powder product.
Surface hydrophobic process is carried out by fatty acid to argentum powder, surface-treated uniform argentum powder slurry passes through homogenizing
Machine washing is washed, and so that agglomerated particle is opened by the high intensity shearing force between the rotor of high-speed rotation and stator.The method improve argentum powder
The dispersibility of granule, has reached the purpose improving argentum powder tap density.
Brief description
A kind of flow chart of the washing methods of super fine silver powder of Fig. 1 present invention.
Specific embodiment
Hereinafter the principle and feature of the present invention is described, example is served only for explaining the present invention, is not intended to limit
Determine the scope of the present invention.
Embodiment 1
The present embodiment is the comparative example using traditional agitator treating method:
(1)Sedimentation, is 1 kilogram through the theoretical output quality of cathode silver that argentum powder synthetic reaction calculates, right after super fine silver powder synthesis
Slurry is settled, and pours out supernatant;
(2)Agitator treating, is followed by stirring and washing to super fine silver powder with washing kettle, then settles again, repeat above-mentioned sedimentation and
Agitator treating process 3 times;
(3)Ethanol wash, adds ethanol that super fine silver powder is washed, then settles again in washing kettle;After removing ethanol
Super fine silver powder washing completes;
(4)It is dried, product is put in baking oven 70 DEG C and 12h is dried.
The spherical argentum powder that super fine silver powder is 1 μm about for particle diameter;The tap density of the super fine silver powder that the method obtains is
3.3g/cm3.
Embodiment 2
(1)Sedimentation
It is 1 kilogram through the theoretical output quality of cathode silver that argentum powder synthetic reaction calculates, after super fine silver powder synthesis, slurry is carried out
Sedimentation, pours out supernatant, pours out water content in disposed slurry and is 0.25 kilogram;
(2)Surface-hydrophobicized process
Add stearic acid in the slurry after sedimentation, the stearic quality of addition is 1g;
(3)Stirring pulp
Being sufficiently stirred for pulp to the slurry after surface-hydrophobicized process makes the uniform dispersion of formation, and mixing speed is
400rpm, mixing time 40min;
(4)Homogenizing is washed
Slurry after pulp adds the homogenizing washing of rotor-stator homogenizer, then settles, solid-liquid separation, obtains
Argentum powder, the rotor of homogenizer and stator gap are 0.50mm, and rotor speed is 3000rpm;
(5)It is dried
The argentum powder obtaining is put 70 DEG C of baking oven and 12h is dried, and obtains super fine silver powder product.
The spherical argentum powder that super fine silver powder is 1 μm about for particle diameter;The tap density of the super fine silver powder that the method obtains is
4.0g/cm3.
Embodiment 3
(1)Sedimentation
Single theoretical output quality of cathode silver through the calculating of argentum powder synthetic reaction is 1 kilogram, after super fine silver powder synthesis, slurry is entered
Row sedimentation, pours out supernatant, pours out water content in disposed slurry and is 0.33 kilogram;
(2)Surface-hydrophobicized process
Add stearic acid in the slurry after sedimentation, add stearic quality 1g;
(3)Stirring pulp
Being sufficiently stirred for pulp to the slurry after surface-hydrophobicized process makes the uniform dispersion of formation, and mixing speed is
200rpm, mixing time 20min;
(4)Homogenizing is washed
Slurry after pulp adds the homogenizing washing of rotor-stator homogenizer, then settles, solid-liquid separation, obtains
Argentum powder, the rotor of homogenizer and stator gap are 0.25mm, and rotor speed is 6000rpm;
(5)It is dried
The argentum powder obtaining is put 70 DEG C of baking oven and 12h is dried, and obtains super fine silver powder product.
The spherical argentum powder that super fine silver powder is 1 μm about for particle diameter;The tap density of the super fine silver powder that the method obtains is
4.5g/cm3.
Improved using the argentum powder tap density that the argentum powder tap density of the inventive method washing obtains than traditional agitator treating
20~40%.
Claims (2)
1. a kind of washing methods of super fine silver powder is it is characterised in that comprise the steps:
(1)Sedimentation
After super fine silver powder synthesis, slurry is settled, pour out supernatant so that quality of cathode silver fraction is 60 ~ 80% in slurry;
(2)Surface-hydrophobicized process
Add fatty acid in the slurry after sedimentation, add quality and the theoretical output quality of cathode silver of fatty acid than for 0.001 ~
0.01:1;
(3)Stirring pulp
To surface-hydrophobicized process after slurry be sufficiently stirred for pulp, make the uniform dispersion of formation, mixing speed be 200 ~
400rpm, mixing time 20 ~ 60min;
(4)Homogenizing is washed
Slurry after pulp adds homogenizing washing in rotor-stator homogenizer, then settles, solid-liquid separation, obtains silver
Powder, the rotor of homogenizer and stator gap are 0.25 ~ 0.50mm, and rotor speed is 3000 ~ 6000rpm;
(5)It is dried
The argentum powder obtaining puts oven drying, obtains super fine silver powder product.
2. as claimed in claim 1 a kind of washing methods of super fine silver powder it is characterised in that:Described fatty acid is stearic acid.
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CN109550933B (en) * | 2018-12-04 | 2021-06-29 | 苏州市贝特利高分子材料股份有限公司 | Ultrathin silver sheet and chemical synthesis method thereof |
CN112475284B (en) * | 2020-11-24 | 2021-10-12 | 西南科技大学 | Surface modification method of micro-nano silver powder for conductive silver paste |
CN115519129B (en) * | 2022-08-05 | 2023-04-18 | 南通领跑者新材料科技有限公司 | Preparation method of silver powder for conductive paste |
CN115351285B (en) * | 2022-10-21 | 2023-01-17 | 陕西斯瑞新材料股份有限公司 | Method for preparing CuCrNb powder for additive manufacturing based on EIGA process |
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JPH04246102A (en) * | 1991-01-29 | 1992-09-02 | Daido Steel Co Ltd | Method for cleaning surface of pulverized metal powder |
CN1686593A (en) * | 2005-03-22 | 2005-10-26 | 温州市东瓯微孔过滤有限公司 | Filtration and washing technology in preparing metal or non metal fine granular powder |
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Effective date of registration: 20180604 Address after: 730101 Heping Town Economic Development Zone, Yuzhong County, Lanzhou, Gansu Patentee after: Jinchuan Lanzhou science and Technology Park Co., Ltd. Address before: No. 98 Jinchuan Road, Jinchang, Gansu Patentee before: Jinchuan Group Co., Ltd. |