CN105803509B - A kind of electrochemical preparation method of nano cupric oxide - Google Patents
A kind of electrochemical preparation method of nano cupric oxide Download PDFInfo
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- CN105803509B CN105803509B CN201610119413.0A CN201610119413A CN105803509B CN 105803509 B CN105803509 B CN 105803509B CN 201610119413 A CN201610119413 A CN 201610119413A CN 105803509 B CN105803509 B CN 105803509B
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
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Abstract
A kind of electrochemical preparation method of nano cupric oxide, belongs to technical field of material.The present invention uses three-electrode system, in sodium hydroxide or potassium hydroxide solution, Copper substrate is working electrode, sets specific polarization potential polarization mode and carries out electrochemistry cyclic voltammetric polarization to copper base, direct growth goes out a nanometer copper crystal particle on copper base, and size of microcrystal is less than 50nm.This method step is simple, and cost is cheap, is not limited by copper-based plate shape, can go out nano cupric oxide with growth in situ with the substrate optional position of electrolyte contacts.The present invention just can obtain nano cupric oxide at normal temperatures, and the adhesive force between the structure and substrate is strong, difficult for drop-off, can be directly used for the devices such as catalyst, board design, microbial disinfection.
Description
Technical field
The invention belongs to technical field of material, more particularly to a kind of electrochemical preparation method of nano cupric oxide.
Background technology
The energy gap of cupric oxide is 1.2eV, belongs to a kind of indirect band gap p-type semiconductor material, has good electrification
Learn activity.And nano cupric oxide also has small-size effect, macro quanta tunnel effect, skin effect and a bulk effect, and
There is important application in the fields such as energy storage material, electrochemistry, catalytic reaction, environmental protection.
However, the current cupric oxide of nanometer prepares and mainly takes chemical method and physical method, wherein physical preparation method work
Skill is relative complex, and cost is high, and chemical method causes larger environmental pollution, greatly constrains extensive preparation, also increasingly
It is not suitable for the development of human society.Therefore, the nano cupric oxide electrochemical preparation method of a kind of low cost and environmental protection is developed, it is right
Improved in the performance of copper oxide nano material and extension has great importance.
The content of the invention
For above-mentioned technical problem, the present invention provides a kind of electrochemical preparation method of nano cupric oxide.The party
Method processing step is simple, can obtain nano cupric oxide by Direct Electrochemistry growth in situ on copper base.
The purpose of the present invention is achieved through the following technical solutions：
A kind of electrochemical preparation method of nano cupric oxide of the present invention, including step are as follows：
(1) after copper base is respectively washed totally with deionized water and absolute ethyl alcohol, its surface is dried up with nitrogen；
(2) sodium hydroxide reagent is added in deionized water, stirring makes solid dissolving, forms sodium hydroxide solution, makes
Its concentration range is between 0.1mol/L to 2mol/L；
(3) hole of electrolytic cell three is connected into Copper substrate, saturated calomel electrode reference electrode and platinum guaze to electrode, reference electricity respectively
Pole is located at Copper substrate and between electrode, Copper substrate is working electrode, by three electrodes, three with electrochemical workstation respectively
Counter electrode connects；
(4) sweep speed, take-off potential, intermediate potential and the terminal current potential during activation polarization are set, by step
(2) solution prepared is inserted in electrolytic cell, is carried out activation polarization to copper base, is obtained nano cupric oxide.
Further, the step (4) carries out activation polarization under conditions of being 20 DEG C in electrolyte temperature.
Further, sweep speed scope is 5mV/s~80mV/s during the activation polarization of the step (4).
Further, the take-off potential scope of the cyclic voltammetric polarization process of the step (4) is -1.8V~-0.5V, eventually
Only potential range is 0.2V~0.6V.
Further, after nano cupric oxide is prepared in step (4), take out, after distilled water flushing, blown with nitrogen immediately
It is dry.
Further, the sodium hydroxide solution of the step (2) is replaced using potassium hydroxide solution.
Further, the nano oxidized steel structure is dendrite.
Further, described dendrite is that growth in situ comes out on copper base.
Beneficial effects of the present invention are：
Electrochemistry of the present invention prepares nano oxidized copper method and not limited by copper-based plate shape.Directly prepared on copper base
Nano cupric oxide can be used for hydrogen-bearing alloy electrode, nickel-hydrogen battery negative pole material or DSSC device.This
Inventive method is simple, quick, environmental protection, stronger with the adhesion of substrate, difficult for drop-off.
Brief description of the drawings
Fig. 1 is the activation polarization figure of the nano cupric oxide of the embodiment of the present invention 1.
Fig. 2 is the scanning electron microscope diagram piece of nano cupric oxide prepared by the electrochemistry of the embodiment of the present invention 1.
Embodiment
The present invention will be described in detail with reference to the accompanying drawings and examples.
Embodiment 1：The present invention comprises the following steps that：
Step 1：After copper base is respectively washed totally with deionized water and absolute ethyl alcohol, its surface is dried up with nitrogen；
Step 2：40g sodium hydrate particles are weighed, are poured slowly into the beaker equipped with 600mL distilled water, after stirring,
Pour into 1000mL volumetric flask, distilled water is poured into volumetric flask makes liquid level reach volumetric flask graduation mark, is mixed into uniform
1mol/L sodium hydroxide solution electrolyte.
Step 3：Using electrochemistry three-electrode system, the hole of electrolytic cell three is connected into Copper substrate, reference electrode and to electricity respectively
Pole, and reference electrode is located at silver-based piece and between electrode, copper base is working electrode, and three electrodes are connected into electrochemistry respectively
Three electrodes of work station；
Step 4：Electrochemical parameter is set, the solution of preparation is transferred in electrolytic cell, activation polarization is carried out to copper base,
Specially：Polarization take-off potential is -1.8V, and termination current potential is 0.2V, sweep speed 40mV/s, to copper-based under the conditions of 20 DEG C
Plate carries out activation polarization, nano cupric oxide is obtained on copper base, polarization process is as shown in Figure 1.
Prepared nano cupric oxide microscopic appearance is as shown in Fig. 2 show that its structure is nano cupric oxide dendrite, its length
More than 800nm, width is 50~100nm.
Embodiment 2：This example from implement 1 different processing step be：
Step 2：56.1g potassium hydroxide pellets are weighed, is poured slowly into the beaker equipped with 600mL distilled water, stirs
Afterwards, pour into 1000mL volumetric flask, distilled water is poured into volumetric flask makes liquid level reach volumetric flask graduation mark, is mixed into uniformly
1mol/L potassium hydroxide solution electrolyte.
Step 4：Using electrochemistry three-electrode system, polarization take-off potential is -1.5V, and termination current potential is 0.4V, scanning speed
Spend for 40mV/s, activation polarization is carried out to copper base under the conditions of 20 DEG C, nano cupric oxide is obtained on copper base.
Embodiment 3：This example from implement 1 different processing step be：
Step 2：40g sodium hydrate particles are weighed, slowly imports and is equipped with the beaker equipped with 600mL distilled water, stirring is equal
After even, import in 1000mL volumetric flask, distilled water is poured into volumetric flask makes liquid level reach volumetric flask graduation mark, is mixed into
Even 1mol/L sodium hydroxide solution electrolyte.
Step 4：Using electrochemistry three-electrode system, polarization take-off potential is -1.5V, and termination current potential is 0.4V, scanning speed
Spend for 40mV/s, activation polarization is carried out to copper base under the conditions of 20 DEG C, nano cupric oxide is obtained on copper base.
Claims (6)
1. a kind of electrochemical preparation method of nano cupric oxide, it is characterized in that, including step is as follows：
（1）After copper base is respectively washed totally with deionized water and absolute ethyl alcohol, its surface is dried up with nitrogen；
（2）Sodium hydroxide reagent is added in deionized water, stirring makes solid dissolving, forms sodium hydroxide solution, makes its dense
Scope is spent between 0.1mol/L to 2mol/L；
（3）The hole of electrolytic cell three is connected into Copper substrate, saturated calomel electrode reference electrode and platinum guaze to electrode, reference electrode position respectively
It is in Copper substrate and between electrode, Copper substrate is working electrode, three electrodes are corresponding with three of electrochemical workstation respectively
Electrode connects；
（4）Sweep speed, take-off potential, intermediate potential and termination current potential during activation polarization, take-off potential model are set
It is 0.2V~0.6V to enclose for -1.8V~-0.5V, termination potential range；By step（2）The solution of preparation is inserted in electrolytic cell,
Activation polarization is carried out to copper base, obtains nano cupric oxide, the nano oxidized steel structure is dendrite.
2. the electrochemical preparation method of nano cupric oxide according to claim 1, it is characterized in that：The step（4）In electricity
Solution liquid temperature degree carries out activation polarization under conditions of being 20 °C.
3. the electrochemical preparation method of nano cupric oxide according to claim 1, it is characterized in that：The step（4）Electricity
Sweep speed scope is 5mV/s~80mV/s during chemical polarization.
4. the electrochemical preparation method of nano cupric oxide according to claim 3, it is characterized in that：Step（4）It is prepared
After nano cupric oxide, take out, after distilled water flushing, dried up with nitrogen immediately.
5. the electrochemical preparation method of nano cupric oxide according to claim 1, it is characterized in that：The step（2）Hydrogen
Sodium hydroxide solution is replaced using potassium hydroxide solution.
6. the electrochemical preparation method of nano cupric oxide according to claim 1, it is characterized in that：Described dendrite is in copper
Growth in situ comes out on substrate.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109778296A (en) * | 2019-01-15 | 2019-05-21 | 中国航发北京航空材料研究院 | A method of polishing and CuO surface |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106591922B (en) * | 2017-02-05 | 2018-05-08 | 桂林理工大学 | Cu2Preparation method of O nano film |
| CN106947995B (en) * | 2017-04-28 | 2018-12-21 | 合肥工业大学 | A kind of single-phase CuO nanometer sheet array film and preparation method thereof |
| CN107265492B (en) * | 2017-07-31 | 2019-07-02 | 王兴利 | A kind of spherical shape copper oxide nanometer particle and preparation method thereof |
| CN108456910A (en) * | 2018-02-02 | 2018-08-28 | 沈阳建筑大学 | The in-situ electrochemistry preparation of nanometer copper coating on a kind of copper carrier |
| CN110342563A (en) * | 2019-07-17 | 2019-10-18 | 湖北大学 | A kind of cupric oxide nano line and its preparation method and application |
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| CN102445468A (en) * | 2011-09-29 | 2012-05-09 | 重庆大学 | Electrode for determining nitrate concentration in solution and manufacturing method thereof |
| RU2466515C1 (en) * | 2011-10-11 | 2012-11-10 | Леонид Геннадьевич Менчиков | Method for laser deposition of copper on dielectric surface |
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| CN103913493B (en) * | 2014-04-24 | 2015-07-08 | 青岛大学 | Keggin type heteropoly acid functionalized graphene loaded nano copper particle modified electrode and application thereof |
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|---|---|---|---|---|
| CN102445468A (en) * | 2011-09-29 | 2012-05-09 | 重庆大学 | Electrode for determining nitrate concentration in solution and manufacturing method thereof |
| RU2466515C1 (en) * | 2011-10-11 | 2012-11-10 | Леонид Геннадьевич Менчиков | Method for laser deposition of copper on dielectric surface |
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| "在碱性溶液中铜的腐蚀机理的研究";冉琴等;《四川师范学院学报》;19900702;第11卷(第2期);第147-152页 * |
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| CN109778296A (en) * | 2019-01-15 | 2019-05-21 | 中国航发北京航空材料研究院 | A method of polishing and CuO surface |
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