CN102418118A - Method for electrochemically aided preparation of silver powder with special form - Google Patents
Method for electrochemically aided preparation of silver powder with special form Download PDFInfo
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- CN102418118A CN102418118A CN2011103639206A CN201110363920A CN102418118A CN 102418118 A CN102418118 A CN 102418118A CN 2011103639206 A CN2011103639206 A CN 2011103639206A CN 201110363920 A CN201110363920 A CN 201110363920A CN 102418118 A CN102418118 A CN 102418118A
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Abstract
The invention provides a method for electrochemically aided preparation of silver powder with a special form. According to the invention, carbonic or metallic electrodes are used as a working electrode and a counter electrode; after cleaning with ultrasonic wave, the working electrode and the counter electrode are immersed into a solution or sol containing silver ions prepared by using ultra pure deionized water; the working electrode is used as a cathode, the counter electrode is used as an anode, and an electrochemical reaction is carried out under an air-tight condition and the condition of a constant current; after the reaction, a resultant is separated and dried to obtain nanometer silver powder. Through control of the variety of electrodes, the amount of current flowing and the variety of electrolytes, dendritic nanometer silver powder, flake nanometer silver powder, laminated flake nanometer silver powder, fibrous nanometer silver powder, cubic cage nanometer silver powder and tetrahedron cubic cage nanometer silver powder can be prepared. The method provided in the invention enables form control and continuous preparation of nanometer silver particles to be realized without addition of any other chemical reagents; the method has the advantages of a simple process, a widely applicable product, high yield of the powder, greenness, environmental protection and feasibility in industrial production.
Description
Technical field
The present invention relates to a kind of method of electrochemical reduction method aid preparation specific form nano silver powder.
Background technology
In recent years, the nanostructure of noble metal granule is because its superior chemistry, electronics, magnetic, optics, calorifics and catalytic performance more and more receive people's attention.Nano-silver powder is used more in electronic industry as a kind of functional materials, is mainly used in to make argentiferous electrocondution slurry, and the electrode of some electron device and high-grade Alkaline Zinc silver accumulator.In the microelectronics industry that develops rapidly now, the market requirement of high-purity nm silver powder is also constantly significantly being increased.Nano silver particles also is splendid biomaterial and environmentally conscious materials simultaneously, has to the human non-toxic evil characteristics of efficient sterilizing sterilization; Nano-silver powder is all used aspect many in catalysis, heat transfer, medical treatment etc. to some extent.As everyone knows, catalytic activity and selectivity all depend on the size and dimension of metal nanoparticle.Therefore, shape and size control is vital for the application of synthetic silver well.
The method that tradition is made silver powder generally has: silver suboxide thermal decomposition method, organic silver thermal decomposition method, reductive agent reduction method, electrolysis cathode sedimentation etc.(publication number: CN1227148) in people's such as Wang Lu work; With the silver ingot is raw material, uses salpeter solution, processes high purity silver nitrate solution; Add ammoniacal liquor with dispersant and process silver ammino ion solution; Mix through the speciality shower nozzle with reductant solution, stir with the high-energy stirring device simultaneously, process high dispersiveness spherical ultra micro silver powder.The process procedure that chemical process prepares nano-silver powder is complicated, and the cycle is longer, and the process difficulty is big, and the silver powder form is difficult to control.Physical method prepares nano silver particles such as vacuum-evaporation, high energy beam bombardment evaporation etc., and the productive rate of silver powder is lower.In people's such as Liao Xuehong work (Huang gang college of education journal, 2001,21,5), adopt platinum filament-platinized platinum electrode system, be working electrode with the platinized platinum electrode, under nitrogen protection, 25min obtains nano-silver powder with the 10mA current electroanalysis.With the method for the electrochemical preparation nano-silver powder of present existence relatively, the selectable electrode of method of the present invention is varied, required electric current is extremely faint, need not to add other chemical reagent, and the final product form is controlled.
Summary of the invention
The objective of the invention is specific form nano-silver powder, provide a kind of electrochemistry to assist reduction, controlled shape, specific form nano-silver powder preparation simple to operation, to overcome the deficiency that prior art exists for the stable performance of production regular shape.
For realizing above-mentioned purpose, the present invention adopts following technical scheme:
A kind of method of electrochemistry aid preparation specific form nano-silver powder comprises step: with carbon-containing electrode or metal electrode as working electrode and counter electrode; With working electrode and counter electrode are ultrasonic clean after, immerse in the argentiferous ion solution or colloidal sol that disposes with ultrapure deionized water; With the working electrode is negative electrode, is anode with the counter electrode, and lucifuge passes to constant current and carries out electrochemical reaction; Reaction makes the specific form nano-silver powder after accomplishing after separated product and the drying.
Said ultrapure deionized water both was meant almost completely to be removed the conducting medium in the water, again with dissociative colloidalmaterial, gas and organism all are not removed to the very water of low degree in the water.Its resistivity is greater than 18M Ω .cm.
Preferable, said carbon-containing electrode is selected from Graphite Electrodes, glassy carbon electrode, activated carbon electrodes and the bamboo charcoal electrode of various forms; Said metal electrode is selected from platinum electrode, the gold electrode of various forms.
Preferable, described argentiferous ion solution or colloidal sol are the aqueous solution or the water-sol of various silver salt, for example: the aqueous solution of Silver Nitrate, Trisilver phosphate, Sulfuric acid disilver salt or Silver monochloride or the water-sol.Only contain water and silver salt in the said argentiferous ionic aqueous solution or the water-sol, do not contain other chemical reagent.
Preferable, concentration of silver ions is 100ppm～10000ppm (weight percentage) in described argentiferous ion solution or the colloidal sol, is preferably 500ppm～10000ppm.
Preferable, described constant current is a direct current, size is 0.01mA～0.1A, is preferably 0.1mA～0.1A.
Preferable, described electrochemical reaction temperature is 5～50 ℃, is preferably 10～50 ℃; Reaction times is 0.5～12h, is preferably 1～4h.
Preferable, the process of said separated product is: working electrode is placed the organic solvent for ultrasonic vibration, promptly obtain the dispersion liquid of nano-silver powder, promptly obtain nano-silver powder after the oven dry.Preferably, said organic solvent is an absolute ethyl alcohol.
Adopt aforesaid method through control electrode kind, size of current and electrolytic solution kind; Nano-silver powder uniform, different shape be can prepare, dendritic nano-silver powder, flake nano aluminium powder, stack layer flake nano aluminium powder, fibrous nano aluminium powder, cubes cage-shaped nano aluminium powder, tetrahedron cube cage-shaped nano aluminium powder comprised.
The present invention selects carbon containing/metal electrode for use, is electrolytic solution to contain silver ion solution/colloidal sol, passes to suitable electric current, can prepare the nano-silver powder of different shape through adjusting electrode materials, size of current, bath composition.Compared with prior art have following characteristics:
1, only uses electrochemical method can prepare the specific form nano-silver powder, need not to add other chemical reagent, nontoxic, environmental protection.
2, ME is simple, and low, the high efficiency of cost has vast market prospect.
3, through use different electrode materialss, change bath composition, the control current size, i.e. the form of may command nano-silver powder, compare with the traditional chemical method of reducing more simple and easy, product stable, control shape better effects if.
4, product is polynary, form is regular, powder is even, can be widely used in fields such as electronic industry, biosensor, electrically conducting coating, health care.
Description of drawings
Fig. 1 is product production device figure of the present invention.
1 is galvanostat among the figure, and 2 is counter electrode, and 3 is working electrode, and 4 is lead, and 5 for containing silver ion solution/colloidal sol.
Fig. 2 is for implementing sem (SEM) picture of finished product dendritic nano-silver powder.
Fig. 3 is sem (SEM) picture of embodiment 2 finished product flake nano aluminium powders.
Fig. 4 is for implementing sem (SEM) picture of finished product stack layer flake nano aluminium powder.
Fig. 5 is sem (SEM) picture of embodiment 1 finished fiber shape nano silver powder.
Fig. 6 is sem (SEM) picture of embodiment 3 finished product cubes cage-shaped nano aluminium powders.
Fig. 7 is for implementing sem (SEM) picture of finished product tetrahedron cube cage-shaped nano aluminium powder.
Fig. 8 is for implementing X powder diffraction (XRD) spectrogram of finished product.
Embodiment
Elaborate in the face of embodiments of the invention down, present embodiment provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment being to implement under the prerequisite with technical scheme of the present invention.
Embodiment 1:
Selecting bamboo charcoal for use is negative electrode, and vitreous carbon is an anode, and the 500ppm silver sulfate solution is an electrolytic solution; With lead electrode is linked to each other with galvanostat, under 10 ℃, pass to the galvanic current of 3mA; Stop energising behind the 2h; Working electrode is placed the absolute ethyl alcohol sonic oscillation, promptly obtain the alcohol dispersion liquid of fibrous nano silver powder, oven dry promptly obtains fibrous nano silver powder.
Embodiment 2:
Selecting graphite for use is negative electrode, and platinum filament is an anode, and the 1000ppm silver nitrate solution is an electrolytic solution; With lead electrode is linked to each other with galvanostat, under 20 ℃, pass to the galvanic current of 0.1A; Stop energising behind the 4h; Working electrode is placed the absolute ethyl alcohol sonic oscillation, promptly obtain the alcohol dispersion liquid of flake nano silver powder, oven dry promptly obtains flake nano silver powder.
Embodiment 3:
Selecting platinum guaze for use is negative electrode, and spun gold is an anode, and 10000ppm Silver monochloride colloidal sol is electrolytic solution; With lead electrode is linked to each other with galvanostat, under 50 ℃, pass to the galvanic current of 0.1mA; Stop energising behind the 1h; Working electrode is placed the absolute ethyl alcohol sonic oscillation, promptly obtain the alcohol dispersion liquid of cubes cage-shaped nano silver powder, oven dry promptly obtains cubes cage-shaped nano silver powder.
Claims (9)
1. the method for an electrochemistry aid preparation nano-silver powder comprises step: with carbon-containing electrode or metal electrode as working electrode and counter electrode; With working electrode and counter electrode are ultrasonic clean after, immerse in the argentiferous ion solution or colloidal sol that disposes with ultrapure deionized water; With the working electrode is negative electrode, is anode with the counter electrode, and lucifuge passes to constant current and carries out electrochemical reaction; Reaction obtains nano-silver powder after separated product and the drying after accomplishing.
2. the method for electrochemistry aid preparation nano-silver powder as claimed in claim 1 is characterized in that, said carbon-containing electrode is selected from Graphite Electrodes, glassy carbon electrode, activated carbon electrodes and bamboo charcoal electrode; Said metal electrode is selected from platinum electrode and gold electrode.
3. the method for electrochemistry aid preparation nano-silver powder as claimed in claim 1 is characterized in that, described argentiferous ion solution or colloidal sol are the aqueous solution or the water-sol of various silver salt.
4. the method for electrochemistry aid preparation nano-silver powder as claimed in claim 3 is characterized in that said silver salt is selected from Silver Nitrate, Trisilver phosphate, Sulfuric acid disilver salt and Silver monochloride.
5. the method for electrochemistry aid preparation nano-silver powder as claimed in claim 1 is characterized in that, concentration of silver ions is 100ppm～10000ppm in described argentiferous ion solution or the colloidal sol.
6. the method for electrochemistry aid preparation nano-silver powder as claimed in claim 1 is characterized in that, described constant current is a direct current, and size is 0.01mA～0.1A.
7. the method for electrochemistry aid preparation nano-silver powder as claimed in claim 1 is characterized in that, described electrochemical reaction temperature is 5～50 ℃, and the reaction times is 0.5～12h.
8. the method for electrochemistry aid preparation nano-silver powder as claimed in claim 1 is characterized in that, the process of said separated product is: working electrode is placed the organic solvent for ultrasonic vibration, promptly obtain the dispersion liquid of nano-silver powder, promptly obtain nano-silver powder after the oven dry.
9. like the method for the arbitrary described electrochemistry aid preparation nano-silver powder of claim 1-8; It is characterized in that the form of said nano-silver powder is dendritic nano-silver powder, flake nano aluminium powder, stack layer flake nano aluminium powder, fibrous nano aluminium powder, cubes cage-shaped nano aluminium powder or tetrahedron cube cage-shaped nano aluminium powder.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102719858A (en) * | 2012-06-01 | 2012-10-10 | 西安交通大学 | Preparation method of dendritic nano silver |
| CN103388175A (en) * | 2013-08-15 | 2013-11-13 | 扬州大学 | Method for preparing silver dendritic matter |
| CN106283123A (en) * | 2016-09-30 | 2017-01-04 | 天津宝兴威科技有限公司 | A kind of preparation method of nanometer silver coating |
| CN108531943A (en) * | 2018-04-16 | 2018-09-14 | 沈阳建筑大学 | A kind of electrochemical preparation method of nano silver powder |
| CN108598190A (en) * | 2018-05-31 | 2018-09-28 | 苏州瑞力博新材科技有限公司 | A kind of low-density HIT low temperature silver paste used for solar batteries and preparation method |
| CN109321948A (en) * | 2018-12-17 | 2019-02-12 | 陕西理工大学 | A kind of method that quick Green Electrochemical prepares Silver nanorod |
| CN113005561A (en) * | 2019-12-19 | 2021-06-22 | 财团法人工业技术研究院 | Conductive fiber and method for producing same |
| CN113084190A (en) * | 2021-04-09 | 2021-07-09 | 浙江技嘉材料科技有限公司 | Simple preparation and purification method of dendritic nano-silver material |
| CN113337847A (en) * | 2021-05-11 | 2021-09-03 | 武汉大学 | Preparation method of cubic copper particles with multi-edge structure |
| CN113737223A (en) * | 2021-08-25 | 2021-12-03 | 金川集团股份有限公司 | Preparation method of rod-like silver powder with flaky laminated structure on surface |
| CN114540881A (en) * | 2022-02-24 | 2022-05-27 | 昆明高聚科技有限公司 | Preparation method of micron-sized monodisperse silver powder based on electrochemical deposition method |
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| CN102181885A (en) * | 2011-04-07 | 2011-09-14 | 东南大学 | Method for preparing nano silver solution by electrolysis |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102719858A (en) * | 2012-06-01 | 2012-10-10 | 西安交通大学 | Preparation method of dendritic nano silver |
| CN102719858B (en) * | 2012-06-01 | 2015-04-29 | 西安交通大学 | Preparation method of dendritic nano silver |
| CN103388175A (en) * | 2013-08-15 | 2013-11-13 | 扬州大学 | Method for preparing silver dendritic matter |
| CN106283123A (en) * | 2016-09-30 | 2017-01-04 | 天津宝兴威科技有限公司 | A kind of preparation method of nanometer silver coating |
| CN108531943A (en) * | 2018-04-16 | 2018-09-14 | 沈阳建筑大学 | A kind of electrochemical preparation method of nano silver powder |
| CN108598190A (en) * | 2018-05-31 | 2018-09-28 | 苏州瑞力博新材科技有限公司 | A kind of low-density HIT low temperature silver paste used for solar batteries and preparation method |
| CN109321948A (en) * | 2018-12-17 | 2019-02-12 | 陕西理工大学 | A kind of method that quick Green Electrochemical prepares Silver nanorod |
| CN109321948B (en) * | 2018-12-17 | 2023-10-10 | 陕西理工大学 | Method for preparing silver nanorods by rapid green electrochemical method |
| CN113005561A (en) * | 2019-12-19 | 2021-06-22 | 财团法人工业技术研究院 | Conductive fiber and method for producing same |
| CN113084190A (en) * | 2021-04-09 | 2021-07-09 | 浙江技嘉材料科技有限公司 | Simple preparation and purification method of dendritic nano-silver material |
| CN113337847A (en) * | 2021-05-11 | 2021-09-03 | 武汉大学 | Preparation method of cubic copper particles with multi-edge structure |
| CN113337847B (en) * | 2021-05-11 | 2022-03-04 | 武汉大学 | Preparation method of cubic copper particles with multi-edge structure |
| CN113737223A (en) * | 2021-08-25 | 2021-12-03 | 金川集团股份有限公司 | Preparation method of rod-like silver powder with flaky laminated structure on surface |
| CN113737223B (en) * | 2021-08-25 | 2024-04-09 | 金川集团股份有限公司 | Preparation method of rod-like silver powder with flaky laminated structure on surface |
| CN114540881A (en) * | 2022-02-24 | 2022-05-27 | 昆明高聚科技有限公司 | Preparation method of micron-sized monodisperse silver powder based on electrochemical deposition method |
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Application publication date: 20120418 |