CN111547758A - Preparation method of copper oxide nanosheet - Google Patents
Preparation method of copper oxide nanosheet Download PDFInfo
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- CN111547758A CN111547758A CN202010362887.4A CN202010362887A CN111547758A CN 111547758 A CN111547758 A CN 111547758A CN 202010362887 A CN202010362887 A CN 202010362887A CN 111547758 A CN111547758 A CN 111547758A
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- copper
- copper oxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/02—Oxides; Hydroxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
Abstract
The invention discloses a preparation method of copper oxide nanosheets, which is used for obtaining copper oxide nanosheets with uniform thickness, wherein the thickness is about 20 nm. And the used raw material agents are safe and easy to obtain, all preparation processes are safe and reliable, the reaction preparation is carried out under mild conditions, the band gap of the copper oxide nanosheet can be controlled within the range of 1.5-1.86 eV through mild oxidation heat treatment, and the copper oxide nanosheet can be widely used for photocatalysis.
Description
Technical Field
The invention belongs to the field of chemical industry, and relates to a preparation method of a copper oxide nanosheet.
Background
Copper oxide is one of the nano semiconductor materials which are receiving much attention in recent years, belongs to a typical P-type metal semiconductor, has a bottom-centered monoclinic structure, and is an important material for high-temperature superconductivity and giant magnetoresistance. Based on its photosensitivity and photochemical performance, copper oxide is also a potential anode material of solar cells and lithium ion batteries, and is widely applied in the fields of gas sensors, catalytic photosensitive devices, gas sensors, magnetic storage devices and the like. In order to improve material properties, copper oxide materials and devices of nanometer scale have received much attention in recent years, and copper oxide materials having a regular structure such as: nanowires, nanorods, nanoplates, nanospheres, and the like.
According to the traditional preparation method of the copper oxide two-dimensional nanosheet, an atomic deposition method (ALD) is used, copper atoms are gasified at high temperature, then are deposited on a template layer by layer, and finally the template is removed to obtain the copper oxide two-dimensional nanosheet. The improved hydrothermal method has the reaction temperature higher than 120 ℃, needs pressure preparation in a reaction kettle, and has the disadvantages of mild reaction conditions and difficult control of reaction results.
Disclosure of Invention
In order to overcome the defects, the invention aims to provide the preparation method of the copper oxide nanosheet, the preparation method is simple in preparation process, mild in reaction conditions, uniform in thickness of the prepared copper oxide nanosheet and stable in chemical characteristics.
In order to realize the purpose of the invention, the technical scheme adopted by the invention is as follows:
a preparation method of copper oxide nanosheets is characterized by comprising the following steps:
1. taking sodium hydroxide NaOH and cetyl trimethyl ammonium bromide CTAB, wherein the mass ratio of NaOH to CTAB is 7: 1-4: 1, dissolving the mixture in excessive deionized water, and heating to 60-85 ℃ at a stirring speed of 30-60r/min to form an alkaline solution;
2. copper (II) nitrate trihydrate Cu (NO)3)2Adding the mixture into excessive deionized water, and uniformly stirring to form a copper nitrate solution;
3. gradually adding the solution containing copper nitrate in the step 2 into the alkaline solution in the step 1, and finally controlling the final concentration of NaOH to be 2.5-4mol/L, the final concentration of CTAB to be 50-80mmol/L and Cu (NO)3)2The final concentration of (A) is 10-15 mmol/L;
4. keeping the mixed solution at the constant temperature of 30-70 ℃ for 0.5-2h, adsorbing copper nitrate and sodium hydroxide on CTAB, and carrying out the following reaction:
Cu(NO3)2+2NaOH→2NaNO3+Cu(OH)2
the copper hydroxide precipitate is gradually deposited on the template CTAB, so that the thickness of the copper hydroxide precipitate is uniform; then filtering and taking out the precipitate, washing the black precipitate by using excessive deionized water and ethanol, and washing CTAB;
5. and calcining the cleaned precipitate at the temperature of 220-280 ℃, and converting the copper hydroxide into copper oxide to form copper oxide nanosheets with uniform thickness.
In the step 1, the excessive deionized water is more than 10 times of the mass of the mixture.
In the step 2, the excessive deionized water is copper (II) nitrate trihydrate Cu (NO)3)2More than 300% of the mass.
The method can obtain the following beneficial effects: obtaining the copper oxide nano-sheet with uniform thickness, wherein the thickness is about 20 nm. And the used raw material agents are safe and easy to obtain, all preparation processes are safe and reliable, the reaction preparation is carried out under mild conditions, the band gap of the copper oxide nanosheet can be controlled within the range of 1.5-1.86 eV through mild oxidation heat treatment, and the copper oxide nanosheet can be widely used for photocatalysis.
Detailed Description
The following description is given with reference to specific examples:
example 1
1. 120g of sodium hydroxide (NaOH) and 21g of cetyltrimethylammonium bromide (CTAB) were taken and the mixture was dissolved in 900ml of deionized water and warmed to 60 ℃ with stirring at 30r/min to form an alkaline solution.
2. 3.4g of copper (II) nitrate trihydrate (Cu (NO)3)2) The mixture was added to 100mL of deionized water and stirred well to form a copper nitrate solution.
3. Gradually adding the solution containing copper nitrate in the step 2 into the alkaline solution in the step one, wherein the final concentration of the final prepared NaOH is 3mol/L, the final concentration of CTAB is 60mmol/L, and Cu (NO)3)2The final concentration of (2) was 14 mmol/L.
4. The mixed solution was kept at a constant temperature of 50 ℃ for 1 hour, and copper nitrate and sodium hydroxide were adsorbed on CTAB, and the following reaction occurred:
Cu(NO3)2+2NaOH→2NaNO3+Cu(OH)2
the copper hydroxide precipitate was gradually deposited on the template CTAB, and thus the copper hydroxide precipitate was uniform in thickness. The precipitate was then removed by filtration, the black precipitate washed with excess deionized water and ethanol, and CTAB washed away to form 1.12g of a black powder.
5. And calcining the cleaned precipitate at 250 ℃, converting copper hydroxide into copper oxide, and forming 1.06g of copper oxide nanosheets with uniform thickness, wherein the thickness of the copper oxide nanosheets is 22nm, and the band gaps of the copper oxide nanosheets are 1.56-1.62 eV.
Example 2
1. 100g of sodium hydroxide (NaOH) and 18g of cetyltrimethylammonium bromide (CTAB) were taken and the mixture was dissolved in 800ml of deionized water and warmed to 70 ℃ with stirring at 40r/min to form an alkaline solution.
2. 2g of copper (II) nitrate trihydrate (Cu (NO)3)2) The mixture is added into 200mL of deionized water and stirred uniformly to form a copper nitrate solution.
3. Gradually adding the solution containing copper nitrate in the step 2 into the alkaline solution in the step one, wherein the final concentration of the final prepared NaOH is 2.5mol/L, the final concentration of CTAB is 50mmol/L, and Cu (NO)3)2The final concentration of (2) was 10 mmol/L.
4. The mixed solution was kept at a constant temperature of 30 ℃ for 0.5h, and copper nitrate and sodium hydroxide were adsorbed on CTAB, and the following reaction occurred:
Cu(NO3)2+2NaOH→2NaNO3+Cu(OH)2
the copper hydroxide precipitate was gradually deposited on the template CTAB, and thus the copper hydroxide precipitate was uniform in thickness. The precipitate was then removed by filtration, and the black precipitate was washed with excess deionized water and ethanol, and CTAB was washed away to form 0.74g of a black powder.
5. And calcining the cleaned precipitate at 250 ℃, converting copper hydroxide into copper oxide, and forming 0.63g of copper oxide nanosheet with uniform thickness, wherein the thickness of the copper oxide nanosheet is 18nm, and the band gap of the copper oxide nanosheet is 1.52-1.55 eV.
Example 3
1. 160g of sodium hydroxide (NaOH) and 29g of cetyltrimethylammonium bromide (CTAB) were taken and the mixture was dissolved in 950ml of deionized water and heated to 85 ℃ with stirring at 60r/min to form an alkaline solution.
2. 2.8g of copper (II) nitrate trihydrate (Cu (NO)3)2) The mixture was added to 50mL of deionized water and stirred well to form a copper nitrate solution.
3. Gradually adding the solution containing copper nitrate in the step 2 into the alkaline solution in the step one, wherein the final concentration of the final prepared NaOH is 4mol/L, the final concentration of CTAB is 80mmol/L, and Cu (NO)3)2The final concentration of (2) was 15 mmol/L.
4. The mixed solution was kept at a constant temperature of 70 ℃ for 2 hours, and copper nitrate and sodium hydroxide were adsorbed on CTAB, and the following reaction occurred:
Cu(NO3)2+2NaOH→2NaNO3+Cu(OH)2
the copper hydroxide precipitate was gradually deposited on the template CTAB, and thus the copper hydroxide precipitate was uniform in thickness. The precipitate was then removed by filtration, the black precipitate washed with excess deionized water and ethanol, and CTAB washed away to form 1.18g of a black powder.
5. And calcining the cleaned precipitate at 250 ℃, converting copper hydroxide into copper oxide, and forming 1.12g of copper oxide nanosheets with uniform thickness, wherein the thickness of the copper oxide nanosheets is 22nm, and the band gaps of the copper oxide nanosheets are 1.64-1.68 eV.
Claims (3)
1. A preparation method of copper oxide nanosheets is characterized by comprising the following steps:
1) taking sodium hydroxide NaOH and cetyl trimethyl ammonium bromide CTAB, wherein the mass ratio of NaOH to CTAB is 7: 1-4: 1, dissolving the mixture in excessive deionized water, and heating to 60-85 ℃ at a stirring speed of 30-60r/min to form an alkaline solution;
2) copper (II) nitrate trihydrate Cu (NO)3)2Adding the mixture into deionized water, and uniformly stirring to form a copper nitrate solution;
3) gradually adding the solution containing copper nitrate in the step 2 into the alkaline solution in the step 1, and finally controlling the final concentration of NaOH to be 2.5-4mol/L, the final concentration of CTAB to be 50-80mmol/L and Cu (NO)3)2At a final concentration of 10-15mmol/L；
4) Keeping the mixed solution at the constant temperature of 30-70 ℃ for 0.5-2h, adsorbing copper nitrate and sodium hydroxide on CTAB, and carrying out the following reaction:
Cu(NO3)2+2NaOH→2NaNO3+Cu(OH)2
the copper hydroxide precipitate is gradually deposited on the template CTAB, so that the thickness of the copper hydroxide precipitate is uniform; then filtering and taking out the precipitate, washing the black precipitate by using excessive deionized water and ethanol, and washing CTAB;
5) and calcining the cleaned precipitate at the temperature of 220-280 ℃, and converting the copper hydroxide into copper oxide to form copper oxide nanosheets with uniform thickness.
2. A method for producing copper oxide nanoplates as claimed in claim 1, characterized in that: in the step 1, the excessive deionized water is more than 10 times of the mass of the mixture.
3. A method for producing copper oxide nanoplates as claimed in claim 1, characterized in that: in the step 2, the deionized water is copper (II) nitrate trihydrate Cu (NO)3)2More than 300% of the mass.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010362887.4A CN111547758A (en) | 2020-04-30 | 2020-04-30 | Preparation method of copper oxide nanosheet |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101792172A (en) * | 2010-03-03 | 2010-08-04 | 天津理工大学 | Method for preparing copper hydroxide and copper oxide nano material and application |
| CN102328949A (en) * | 2011-06-22 | 2012-01-25 | 哈尔滨工程大学 | Preparation method for copper oxide nanoribbon with high hydrogen storage capacity |
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2020
- 2020-04-30 CN CN202010362887.4A patent/CN111547758A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101792172A (en) * | 2010-03-03 | 2010-08-04 | 天津理工大学 | Method for preparing copper hydroxide and copper oxide nano material and application |
| CN102328949A (en) * | 2011-06-22 | 2012-01-25 | 哈尔滨工程大学 | Preparation method for copper oxide nanoribbon with high hydrogen storage capacity |
Non-Patent Citations (1)
| Title |
|---|
| HAFSA SIDDIQUI ET AL.: ""Surfactant assisted wet chemical synthesis of copper oxide (CuO)nanostructures and their spectroscopic analysis"", 《OPTIK》 * |
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Application publication date: 20200818 |