CN105803509A - Electrochemical preparation method for nanometer copper oxide - Google Patents
Electrochemical preparation method for nanometer copper oxide Download PDFInfo
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- CN105803509A CN105803509A CN201610119413.0A CN201610119413A CN105803509A CN 105803509 A CN105803509 A CN 105803509A CN 201610119413 A CN201610119413 A CN 201610119413A CN 105803509 A CN105803509 A CN 105803509A
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- cupric oxide
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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
- C25D11/02—Anodisation
- C25D11/34—Anodisation of metals or alloys not provided for in groups C25D11/04 - C25D11/32
Abstract
The invention provides an electrochemical preparation method for nanometer copper oxide and belongs to the technical field of material preparation. A three-electrode system is adopted. In a sodium hydroxide or potassium hydroxide solution, a copper substrate serves as a working electrode, electrochemical cyclic voltammetry polarization is conducted on the copper substrate by setting a specified polarization potential polarization mode, nanometer copper crystal particles directly grow on the copper substrate, and the diameter of the crystal particles is smaller than 50 nm. According to the method, the steps are simple, the cost is low, limit by the shape of the copper substrate is avoided, and the nanometer copper oxide can grow in situ in any position, making contact with the electrolyte solution, of the substrate. The nanometer copper oxide can be obtained at normal temperature, the adhesive force between the nanometer copper oxide and a base is high, and the nanometer copper oxide is not prone to fall off and can be directly used for catalysts, circuit board design, microorganism sterilization and other devices.
Description
Technical field
The invention belongs to technical field of material, particularly relate to the electrochemical preparation method of a kind of nano cupric oxide.
Background technology
The energy gap of copper oxide is 1.2eV, belongs to a kind of indirect band gap p-type semiconductor material, has good electro-chemical activity.And nano cupric oxide also has small-size effect, macro quanta tunnel effect, skin effect and bulk effect, and there is important application in fields such as energy storage material, electrochemistry, catalytic reaction, environmental conservation.
But, chemical method and physical method are mainly taked in a nanometer current copper oxide preparation, wherein physical preparation method technique relative complex, cost is high, chemical method causes bigger environmental pollution, greatly constrains extensive preparation, is also increasingly not suitable for the development of human society.Therefore, developing the nano cupric oxide electrochemical preparation method of a kind of low cost and environmental protection, the performance for copper oxide nano material improves and extension has great importance.
Summary of the invention
For the technical problem of above-mentioned existence, the present invention provides the electrochemical preparation method of a kind of nano cupric oxide.The method processing step is simple, it is possible on copper base, Direct Electrochemistry growth in situ obtains nano cupric oxide.
It is an object of the invention to be achieved through the following technical solutions:
The electrochemical preparation method of a kind of nano cupric oxide of the present invention, comprises the following steps that
(1) copper base deionized water and dehydrated alcohol are respectively washed after totally, with nitrogen, its surface are dried up；
(2) joining in deionized water by sodium hydroxide reagent, stirring makes solid dissolve, and forms sodium hydroxide solution so that it is concentration range is between 0.1mol/L to 2mol/L；
(3) electrolyzer three hole is connected Copper substrate respectively, saturated calomel electrode reference electrode and platinum guaze are to electrode, reference electrode Copper substrate and to electrode between, Copper substrate is working electrode, is connected with three counter electrodes of electrochemical workstation respectively by three electrodes；
(4) scanning speed in activation polarization process, take-off potential, intermediate potential and terminal current potential are set, the solution that step (2) is prepared are inserted in electrolyzer, copper base is carried out activation polarization, obtains nano cupric oxide.
Further, described step (4) carries out activation polarization when electrolyte temperature is 20 DEG C.
Further, in the activation polarization process of described step (4), scanning speed ranges for 5mV/s～80mV/s.
Further, the take-off potential of the cyclic voltammetric polarization process of described step (4) ranges for-1.8V～-0.5V, and termination potential range is 0.2V～0.6V.
Further, step (4) is taken out after preparing nano cupric oxide immediately, after distilled water flushing, dries up with nitrogen.
Further, the sodium hydroxide solution of described step (2) adopts potassium hydroxide solution to replace.
Further, described nano oxidized steel structure is dendrite.
Further, growth in situ is out on copper base for described dendrite.
The invention have the benefit that
Electrochemistry of the present invention prepares nano oxidized copper method not by the restriction of copper base shape.On copper base, the nano cupric oxide of directly preparation may be used for hydrogen-bearing alloy electrode, nickel-hydrogen battery negative pole material or DSSC device.The inventive method is simple, quick, environmental protection, relatively strong with the adhesion of substrate, difficult drop-off.
Accompanying drawing explanation
Fig. 1 is the activation polarization figure of the embodiment of the present invention 1 nano cupric oxide.
Fig. 2 is the scanning electron microscope diagram sheet of nano cupric oxide prepared by the embodiment of the present invention 1 electrochemistry.
Detailed description of the invention
Describe the present invention below in conjunction with drawings and Examples.
Embodiment 1: the present invention specifically comprises the following steps that
Step 1: copper base deionized water and dehydrated alcohol are respectively washed after totally, with nitrogen, its surface are dried up；
Step 2: weigh 40g sodium hydrate particle, it is poured slowly in the beaker equipped with 600mL distilled water, after stirring, pours in the volumetric flask of 1000mL, pouring distilled water in volumetric flask into makes liquid level arrive volumetric flask graduation mark, is mixed into uniform 1mol/L sodium hydroxide solution electrolyte.
Step 3: use electrochemistry three-electrode system, electrolyzer three hole is connected respectively Copper substrate, reference electrode and to electrode, and reference electrode money base sheet and to electrode between, copper base is working electrode, and three electrodes connect three electrodes of electrochemical workstation respectively；
Step 4: electrochemical parameter is set, the solution of preparation is proceeded in electrolyzer, copper base is carried out activation polarization, particularly as follows: polarization take-off potential is-1.8V, termination current potential is 0.2V, and scanning speed is 40mV/s, under 20 DEG C of conditions, copper base is carried out activation polarization, obtaining nano cupric oxide on copper base, polarization process is as shown in Figure 1.
Prepared nano cupric oxide microscopic appearance is as in figure 2 it is shown, show that its structure is nano cupric oxide dendrite, and its length is more than 800nm, and width is 50～100nm.
Embodiment 2: the processing step that this example is different from implementing 1 is:
Step 2: weigh 56.1g potassium hydroxide pellet, it is poured slowly in the beaker equipped with 600mL distilled water, after stirring, pours in the volumetric flask of 1000mL, pouring distilled water in volumetric flask into makes liquid level arrive volumetric flask graduation mark, is mixed into uniform 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, and scanning speed is 40mV/s, under 20 DEG C of conditions, copper base is carried out activation polarization, obtains nano cupric oxide on copper base.
Embodiment 3: the processing step that this example is different from implementing 1 is:
Step 2: weigh 40g sodium hydrate particle, slowly import equipped with, in the beaker equipped with 600mL distilled water, after stirring, importing in the volumetric flask of 1000mL, pouring distilled water in volumetric flask into makes liquid level arrive volumetric flask graduation mark, is mixed into uniform 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, and scanning speed is 40mV/s, under 20 DEG C of conditions, copper base is carried out activation polarization, obtains nano cupric oxide on copper base.
Claims (8)
1. an electrochemical preparation method for nano cupric oxide, is characterized in that, comprises the following steps that
(1) copper base deionized water and dehydrated alcohol are respectively washed after totally, with nitrogen, its surface are dried up；
(2) joining in deionized water by sodium hydroxide reagent, stirring makes solid dissolve, and forms sodium hydroxide solution so that it is concentration range is between 0.1mol/L to 2mol/L；
(3) electrolyzer three hole is connected Copper substrate respectively, saturated calomel electrode reference electrode and platinum guaze are to electrode, reference electrode Copper substrate and to electrode between, Copper substrate is working electrode, is connected with three counter electrodes of electrochemical workstation respectively by three electrodes；
(4) scanning speed in activation polarization process, take-off potential, intermediate potential and terminal current potential are set, the solution that step (2) is prepared are inserted in electrolyzer, copper base is carried out activation polarization, obtains nano cupric oxide.
2. the electrochemical preparation method of nano cupric oxide according to claim 1, is characterized in that: described step (4) carries out activation polarization when electrolyte temperature is 20 DEG C.
3. the electrochemical preparation method of nano cupric oxide according to claim 1, is characterized in that: in the activation polarization process of described step (4), scanning speed ranges for 5mV/s～80mV/s.
4. the electrochemical preparation method of nano cupric oxide according to claim 3, is characterized in that: the take-off potential of the cyclic voltammetric polarization process of described step (4) ranges for-1.8V～-0.5V, and termination potential range is 0.2V～0.6V.
5. the electrochemical preparation method of nano cupric oxide according to claim 3, is characterized in that: step (4) is taken out after preparing nano cupric oxide immediately, after distilled water flushing, dries up with nitrogen.
6. the electrochemical preparation method of nano cupric oxide according to claim 1, is characterized in that: the sodium hydroxide solution of described step (2) adopts potassium hydroxide solution to replace.
7. the electrochemical preparation method of nano cupric oxide according to claim 1, is characterized in that: described nano oxidized steel structure is dendrite.
8. the electrochemical preparation method of nano cupric oxide according to claim 1, is characterized in that: growth in situ is out on copper base for described dendrite.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106591922A (en) * | 2017-02-05 | 2017-04-26 | 桂林理工大学 | Preparation method of Cu2O nano film |
| CN106947995A (en) * | 2017-04-28 | 2017-07-14 | 合肥工业大学 | A kind of single-phase CuO nanometer sheet array film and preparation method thereof |
| CN107265492A (en) * | 2017-07-31 | 2017-10-20 | 王兴利 | A kind of spherical alumina copper nano particles 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 |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109778296B (en) * | 2019-01-15 | 2020-09-22 | 中国航发北京航空材料研究院 | Method for polishing and oxidizing copper surface |
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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 |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106591922A (en) * | 2017-02-05 | 2017-04-26 | 桂林理工大学 | Preparation method of Cu2O nano film |
| CN106591922B (en) * | 2017-02-05 | 2018-05-08 | 桂林理工大学 | Cu2Preparation method of O nano film |
| CN106947995A (en) * | 2017-04-28 | 2017-07-14 | 合肥工业大学 | A kind of single-phase CuO nanometer sheet array film and preparation method thereof |
| 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 |
| CN107265492A (en) * | 2017-07-31 | 2017-10-20 | 王兴利 | A kind of spherical alumina copper nano particles 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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Granted publication date: 20180109 Termination date: 20190302 |