CN108517541A - A kind of electrochemical preparation method of Nanometer Copper powder - Google Patents
A kind of electrochemical preparation method of Nanometer Copper powder Download PDFInfo
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- CN108517541A CN108517541A CN201810337082.7A CN201810337082A CN108517541A CN 108517541 A CN108517541 A CN 108517541A CN 201810337082 A CN201810337082 A CN 201810337082A CN 108517541 A CN108517541 A CN 108517541A
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- electrochemical
- copper powder
- nanometer copper
- copper
- platinum guaze
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C5/00—Electrolytic production, recovery or refining of metal powders or porous metal masses
- C25C5/02—Electrolytic production, recovery or refining of metal powders or porous metal masses from solutions
Abstract
The invention belongs to field of nano material preparation, and in particular to a kind of electrochemical preparation method of Nanometer Copper powder.Technical scheme is as follows：A kind of electrochemical preparation method of Nanometer Copper powder, using copper sulfate solution as electrolyte solution, polyvinylpyrrolidone is as dispersant, red copper matrix is working electrode, and platinum guaze is to electrode, to carrying out constant current reduction after electrolyte solution deoxygenation, then platinum guaze is cleaned by ultrasonic in absolute ethyl alcohol, obtained cleaning solution is filtered to obtain solid powder, is dried in vacuum drying chamber, Nanometer Copper powder is obtained.The electrochemical preparation method of Nanometer Copper powder provided by the invention, simple for process, the grain size for being made copper powder is easy to control, good dispersion, purity are high.
Description
Technical field
The invention belongs to field of nano material preparation, and in particular to a kind of electrochemical preparation method of Nanometer Copper powder.
Background technology
Copper nanoparticle is because its grain size is small, specific surface is big, surface-active is strong, high conductivity, and in electronics and microelectronics, chemical industry
There is important application in the fields such as catalysis, composite material, the energy.
The production method of Nanometer Copper powder can be divided into vapour deposition process, mechanochemical reaction, liquid phase reduction, collosol and gel
Method, supercritical extract etc., however these methods high energy consumption having, the equipment cost that has is high, the grain size that has is big, the purity that has is low,
Some is easy to happen reunion.
Invention content
The present invention provides a kind of electrochemical preparation method of Nanometer Copper powder, simple for process, and the grain size that copper powder is made is easy
Control, good dispersion, purity are high.
Technical scheme is as follows：
A kind of electrochemical preparation method of Nanometer Copper powder, using copper sulfate solution as electrolyte solution, polyethylene
For pyrrolidones as dispersant, red copper matrix is working electrode, and platinum guaze is to electrode, to carrying out permanent electricity after electrolyte solution deoxygenation
Platinum guaze, is then cleaned by ultrasonic in absolute ethyl alcohol, is filtered to obtain solid powder to obtained cleaning solution by stream reduction,
It is dried in vacuum drying chamber, obtains Nanometer Copper powder.
The electrochemical preparation method of the Nanometer Copper powder, specifically includes that steps are as follows：
(1) after using red copper matrix and platinum guaze respectively deionized water and washes of absolute alcohol clean, with nitrogen by red copper base
Body and the drying of platinum guaze surface；
(2) three hole of electrolytic cell is separately connected red copper matrix, platinum guaze and thermometer, red copper matrix is working electrode, platinum guaze
For to electrode, thermometer is located at working electrode and between electrode, by working electrode and to electrode respectively with electrochemical workstation
Counter electrode be connected；
(3) copper sulfate solution is prepared, and a small amount of polyvinylpyrrolidone is added, copper sulfate solution is removed using nitrogen
Oxygen；
(4) electrochemical parameter is set：Reduction current density is set in the electrochemical software of electrochemical workstation, it will be described
Copper sulfate solution moves into electrolytic cell, and constant current reduction is carried out under the conditions of 25 DEG C；
(5) after constant current reduction, platinum guaze is moved into absolute ethyl alcohol, ultrasonic cleaning 10min is carried out, it is clear to what is obtained
Washing lotion is filtered to obtain solid powder, after solid powder washes of absolute alcohol 3 times, is put into vacuum drying chamber and dries,
Obtain Nanometer Copper powder.
The electrochemical preparation method of the Nanometer Copper powder, preferred embodiment be, the reduction current density is 0.1~
5mA/cm2。
The electrochemical preparation method of the Nanometer Copper powder, preferred embodiment are that the copper sulfate solution is a concentration of
0.1~2molL-1, the mass ratio of polyvinylpyrrolidone and Salzburg vitriol solid is 0.1~3：100.
The electrochemical preparation method of the Nanometer Copper powder, preferred embodiment are that the drying temperature of vacuum drying chamber is set
It is set to 65 DEG C.
The electrochemical preparation method of the Nanometer Copper powder, preferred embodiment are that the grain size of the Nanometer Copper powder is
30~60nm.
Beneficial effects of the present invention are：
1, the present invention selects absolute ethyl alcohol to carry out cleaning copper nanoparticle, can not only prevent its oxidation, moreover it is possible to remove remaining
Polyvinylpyrrolidone.
2, step of the present invention is simple, of low cost, and copper nanoparticle body just can be obtained at normal temperatures, can be directly used for being catalyzed
The devices such as agent, board design, battery energy storage are manufactured.
Specific implementation mode
For a further understanding of the present invention, Nanometer Copper raw powder's production technology is done mainly in combination with specific embodiment below
Further detailed description, but it is to be understood that the protection domain of the application is not limited by the actual conditions of these embodiments.
Embodiment 1：
Step 1：16g Salzburg vitriols, 0.016g polyvinylpyrrolidones are weighed respectively, slowly import and 600mL is housed
It in the beaker of deionized water, after stirring evenly, imports in the volumetric flask of 1L, deionized water is poured into volumetric flask keeps liquid level close
Volumetric flask graduation mark, obtains copper sulfate solution, and nitrogen deoxygenation 30min is used to copper sulfate solution；
Step 2：Electrochemical parameter is set：Reduction current density is set in the electrochemical software of electrochemical workstation
0.1mA/cm2, the copper sulfate solution is moved into electrolytic cell, constant current reduction is carried out under the conditions of 25 DEG C；
Step 3：After electrochemical reaction, platinum guaze is moved into absolute ethyl alcohol, after being cleaned by ultrasonic 10min, to what is obtained
Cleaning solution is filtered to obtain solid powder, after powder washes of absolute alcohol 3 times, is put into vacuum drying chamber and dries,
It is 30nm copper nanoparticles to obtain grain size.
Embodiment 2：
Step 1：320g Salzburg vitriols, 9.4g polyvinylpyrrolidones are weighed respectively, are slowly imported and are gone equipped with 600mL
It in the beaker of ionized water, after stirring evenly, imports in the volumetric flask of 1L, deionized water is poured into volumetric flask makes liquid level close to appearance
Measuring bottle graduation mark, obtains copper sulfate solution, and nitrogen deoxygenation 30min is used to the solution；
Step 2：Electrochemical parameter is set：Reduction current density is set in the electrochemical software of electrochemical workstation
0.1mA/cm2, copper sulfate solution is moved into electrolytic cell, constant current reduction is carried out under the conditions of 25 DEG C；
Step 3：After electrochemical reaction, platinum guaze is moved into absolute ethyl alcohol, after being cleaned by ultrasonic 10min, to what is obtained
Cleaning solution is filtered to obtain solid powder, after powder washes of absolute alcohol 3 times, is put into vacuum drying chamber and dries,
It is 48nm copper nanoparticles to obtain grain size.
Embodiment 3：
Step 1：320g Salzburg vitriols, 9.4g polyvinylpyrrolidones are weighed respectively, are slowly imported and are gone equipped with 600mL
It in the beaker of ionized water, after stirring evenly, imports in the volumetric flask of 1L, deionized water is poured into volumetric flask makes liquid level close to appearance
Measuring bottle graduation mark, obtains copper sulfate solution, and nitrogen deoxygenation 30min is used to the solution；
Step 2：Electrochemical parameter is set：Reduction current density 5mA/ is set in the electrochemical software of electrochemical workstation
cm2, copper sulfate solution is moved into electrolytic cell, constant current reduction is carried out under the conditions of 25 DEG C；
Step 3：After electrochemical reaction, platinum guaze is moved into absolute ethyl alcohol, after being cleaned by ultrasonic 10min, to what is obtained
Cleaning solution is filtered to obtain solid powder, after powder washes of absolute alcohol 3 times, is put into vacuum drying chamber and dries,
It is 60nm copper nanoparticles to obtain grain size.
Embodiment 4：
Step 1：16g Salzburg vitriols, 0.016g polyvinylpyrrolidones are weighed respectively, slowly import and 600mL is housed
It in the beaker of deionized water, after stirring evenly, imports in the volumetric flask of 1L, deionized water is poured into volumetric flask keeps liquid level close
Volumetric flask graduation mark, obtains copper sulfate solution, and nitrogen deoxygenation 30min is used to the solution；
Step 2：Electrochemical parameter is set：Reduction current density 5mA/ is set in the electrochemical software of electrochemical workstation
cm2, copper sulfate solution is moved into electrolytic cell, constant current reduction is carried out under the conditions of 25 DEG C；
Step 3：After electrochemical reaction, platinum guaze is moved into absolute ethyl alcohol, after being cleaned by ultrasonic 10min, to what is obtained
Cleaning solution is filtered to obtain solid powder, after powder washes of absolute alcohol 3 times, is put into vacuum drying chamber and dries,
It is 51nm copper nanoparticles to obtain grain size.
Embodiment 5：
Step 1：16g Salzburg vitriols, 0.26g polyvinylpyrrolidones are weighed respectively, are slowly imported and are gone equipped with 600mL
It in the beaker of ionized water, after stirring evenly, imports in the volumetric flask of 1L, deionized water is poured into volumetric flask makes liquid level close to appearance
Measuring bottle graduation mark, obtains copper sulfate solution, and nitrogen deoxygenation 30min is used to the solution；
Step 2：Electrochemical parameter is set：Reduction current density 1mA/ is set in the electrochemical software of electrochemical workstation
cm2, copper sulfate solution is moved into electrolytic cell, constant current reduction is carried out under the conditions of 25 DEG C；
Step 3：After electrochemical reaction, platinum guaze is moved into absolute ethyl alcohol, after being cleaned by ultrasonic 10min, to what is obtained
Cleaning solution is filtered to obtain solid powder, after powder washes of absolute alcohol 3 times, is put into vacuum drying chamber and dries,
It is 46nm copper nanoparticles to obtain grain size.
Claims (6)
1. a kind of electrochemical preparation method of Nanometer Copper powder, which is characterized in that molten as electrolyte using copper sulfate solution
Liquid, for polyvinylpyrrolidone as dispersant, red copper matrix is working electrode, and platinum guaze is to electrode, to electrolyte solution deoxygenation
Constant current reduction is carried out afterwards, and platinum guaze is cleaned by ultrasonic in absolute ethyl alcohol then, obtained cleaning solution is filtered
It to solid powder, is dried in vacuum drying chamber, obtains Nanometer Copper powder.
2. the electrochemical preparation method of Nanometer Copper powder according to claim 1, which is characterized in that specifically include step such as
Under：
(1) after red copper matrix and platinum guaze being used respectively deionized water and washes of absolute alcohol clean, with nitrogen by red copper matrix and
Platinum guaze surface dries up；
(2) three hole of electrolytic cell is separately connected red copper matrix, platinum guaze and thermometer, red copper matrix is working electrode, and platinum guaze is pair
Electrode, thermometer are located at working electrode and between electrodes, by working electrode and to electrode respectively with pair of electrochemical workstation
Electrode is answered to be connected；
(3) copper sulfate solution is prepared, and a small amount of polyvinylpyrrolidone is added, nitrogen deoxygenation is used to copper sulfate solution；
(4) electrochemical parameter is set：Reduction current density is set in the electrochemical software of electrochemical workstation, by the sulfuric acid
Copper liquor moves into electrolytic cell, and constant current reduction is carried out under the conditions of 25 DEG C；
(5) after constant current reduction, platinum guaze is moved into absolute ethyl alcohol, ultrasonic cleaning 10min is carried out, to obtained cleaning solution
It is filtered to obtain solid powder, after solid powder washes of absolute alcohol 3 times, is put into vacuum drying chamber and dries, obtain
Nanometer Copper powder.
3. the electrochemical preparation method of Nanometer Copper powder according to claim 2, which is characterized in that the reduction current is close
Degree is 0.1~5mA/cm2。
4. the electrochemical preparation method of Nanometer Copper powder according to claim 1, which is characterized in that the copper sulphate is water-soluble
A concentration of 0.1~2molL of liquid-1, the mass ratio of polyvinylpyrrolidone and Salzburg vitriol solid is 0.1~3：100.
5. the electrochemical preparation method of Nanometer Copper powder according to claim 1, which is characterized in that vacuum drying chamber is done
Dry temperature setting is 65 DEG C.
6. the electrochemical preparation method of Nanometer Copper powder according to claim 1, which is characterized in that the Nanometer Copper powder
Grain size be 30~60nm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110938846A (en) * | 2018-09-21 | 2020-03-31 | 中国科学院大连化学物理研究所 | CO (carbon monoxide)2Electrode for electrochemical reduction, preparation and application thereof |
| CN111364067A (en) * | 2020-04-11 | 2020-07-03 | 傅嘉英 | Electrolytic cell for preparing nano metal |
| CN111705338A (en) * | 2020-07-03 | 2020-09-25 | 朱义奎 | Preparation method of nano-copper powder |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110938846A (en) * | 2018-09-21 | 2020-03-31 | 中国科学院大连化学物理研究所 | CO (carbon monoxide)2Electrode for electrochemical reduction, preparation and application thereof |
| CN110938846B (en) * | 2018-09-21 | 2021-09-07 | 中国科学院大连化学物理研究所 | CO (carbon monoxide)2Electrode for electrochemical reduction, preparation and application thereof |
| CN111364067A (en) * | 2020-04-11 | 2020-07-03 | 傅嘉英 | Electrolytic cell for preparing nano metal |
| CN111705338A (en) * | 2020-07-03 | 2020-09-25 | 朱义奎 | Preparation method of nano-copper powder |
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