CN101412531A - Hydrothermal preparation capable of realizing controllability of morphology of cuprous oxide crystal - Google Patents
Hydrothermal preparation capable of realizing controllability of morphology of cuprous oxide crystal Download PDFInfo
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- CN101412531A CN101412531A CNA2008101220732A CN200810122073A CN101412531A CN 101412531 A CN101412531 A CN 101412531A CN A2008101220732 A CNA2008101220732 A CN A2008101220732A CN 200810122073 A CN200810122073 A CN 200810122073A CN 101412531 A CN101412531 A CN 101412531A
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Abstract
The invention discloses a hydrothermal preparation method for realizing controllable crystal habit of cuprous oxide. The method is as follows: bluestone is dissolved in water and stirred; sodium lactate the molar number of which is 8 to 10 times of that of the bluestone is added into the solution and continuously stirred; the pH value of the solution is adjusted by utilizing sodium hydroxide the molar concentration of which is 4.0 m/L, and is finally controlled to between 7.0 and 12.0; the finally prepared solution is put into an autoclave, and subjected to hydrothermal treatment for 4 to 8 hours at a temperature of between 150 and 180 DEG C; and finally the treated solution is centrifugated and dried to obtain cuprous oxide powder with different forms. The hydrothermal synthesis technology for controlling the external form of a cuprous oxide crystal controls the relative growth rate of a surface (100) and a surface (111) in the cuprous oxide cubic crystal by controlling the pH value of the solution, so as to prepare the cuprous oxide powder with different forms.
Description
Technical field
The present invention relates to a kind of hydrothermal preparing process of realizing that the cuprous oxide crystal form is controlled.
Background technology
Red copper oxide (Cu
2O) be a kind of very important oxide semiconductor material, its energy gap is 2.1eV, can by wavelength the excited by visible light of 400～800nm, and low, the theoretical utilising efficiency of preparation cost is higher, in fields such as solar cell, catalyzer, fuel cell, gas sensor and superconducting materials important use is arranged all.In recent years, along with the widespread use of Red copper oxide at scientific research and production field, the growth mechanism of cuprous oxide crystal has obtained increasing concern.Cuprous oxide crystal belongs to isometric system, and its crystalline structure and inner point defect constitute performances such as mechanics for material, electricity, calorifics, magnetics, optics material impact.Therefore realize that the crystalline structure of Red copper oxide and formalness are controlled, not only have great importance for research cuprous oxide crystal growth mechanism, and can regulate the various performances of crystalline to satisfy the specific requirement of different components, reach the optimized purpose of device performance.
Hydrothermal method is the important method (Ming-Guo Ma, et al., Journal ofAlloys and Compounds, 455, L15-L18, (2008)) of preparation cuprous oxide crystal.Hydrothermal method is characterized in reacting in closed container (reactor), and some difficult at normal temperatures and pressures being reflected under the High Temperature High Pressure of taking place are taken place.Hydrothermal method can directly be disperseed and well-crystallized's powder, avoided the powder hard aggregation that may form, and in the water-heat process, crystalline structure, particle diameter, crystal habit and the crystal grain purity of product is controlled in the adjusting of condition by experiment.The present invention comes different crystal faces in the cuprous crystal of controlled oxidation by the pH value (concentration of hydroxide ion in the solution) of control solution: the relative growth rate of (100) face and (111) face reaches the purpose of the cuprous crystal formalness of controlled oxidation.Utilize complexing agent and the reductive agent of Sodium.alpha.-hydroxypropionate as mantoquita, adopt ethylenediamine tetraacetic acid (EDTA) (EDTA) and the hydro-thermal synthesis process of glucose as the synthetic cuprous oxide crystal of complexing agent than tradition, the time is significantly shortened.
Summary of the invention
The object of the present invention is to provide a kind of hydrothermal preparing process of realizing that the cuprous oxide crystal form is controlled, utilize Sodium.alpha.-hydroxypropionate and mantoquita (copper sulfate) to form complex compound, use the pH value of sodium hydroxide solution regulator solution, after hydrothermal treatment consists, obtain the controlled cuprous oxide crystal of form.
The technical solution used in the present invention step is as follows:
1) soluble copper salt is soluble in water, the volumetric molar concentration of cupric ion is 0.02～0.04 mol in the control solution, stirs;
2) in above-mentioned solution, add the Sodium.alpha.-hydroxypropionate that volumetric molar concentration is 8～10 times of cupric ion volumetric molar concentrations in the solution again, continue to stir;
3) utilize the pH value of the sodium hydrate regulator solution of 4.0 mol, the pH value of solution is controlled between 7.0～12.0;
4) solution for preparing is put into autoclave, hydrothermal treatment consists is 4～8 hours in 150～180 ℃ of degree scopes;
5), just obtained the cuprous powder of cubic phase oxygenization with the solution centrifugal after the hydrothermal treatment consists, drying.
Described employing copper sulfate is soluble copper salt, Sodium.alpha.-hydroxypropionate is complexing agent and reductive agent, by the pH value of control solution, the relative growth rate of (100) face and (111) face in the cuprous cubic system of controlled oxidation under hydrothermal condition, thus prepare Red copper oxide powder with different outer shape.
The beneficial effect that the present invention has is:
The present invention proposes to utilize complexing agent and the reductive agent of Sodium.alpha.-hydroxypropionate as mantoquita, adopts ethylenediamine tetraacetic acid (EDTA) (EDTA) and the hydro-thermal synthesis process of glucose as the synthetic cuprous oxide crystal of complexing agent than tradition, and the time is significantly shortened.Utilize to adjust the simple method of pH value of solution value, come the relative growth rate of (100) face and (111) face in the cuprous crystal of controlled oxidation, realize that the form of cuprous oxide crystal is controlled.
Description of drawings
Fig. 1 is the XRD figure spectrum of embodiment 1 gained cuprous oxide crystal.
Fig. 2 is the stereoscan photograph of embodiment 1 gained cuprous oxide crystal.
Fig. 3 is the XRD figure spectrum of embodiment 2 gained cuprous oxide crystals.
Fig. 4 is the stereoscan photograph of embodiment 2 gained cuprous oxide crystals.
Fig. 5 be embodiment 3 gained cuprous oxide crystals XRD figure spectrum.
Fig. 6 is the stereoscan photograph of embodiment 3 gained cuprous oxide crystals.
Embodiment
Embodiment 1:
With 0.3995 gram copper sulfate (CuSO
45H
2O) be dissolved in 75.0 ml deionized water, stir after 5 minutes, add 2.5 ml concns and be 60% Sodium.alpha.-hydroxypropionate (C
3H
5NaO
3), the Sodium.alpha.-hydroxypropionate volumetric molar concentration is 0.2 mol, stirs after 5 minutes, the pH value of utilizing the sodium hydrate regulator solution of 4.0 mol is 7.0.Regulating final solution amount with deionized water is 80.0 milliliters, cupric ion volumetric molar concentration 0.02 mol in the solution.The above-mentioned solution for preparing is put in the polytetrafluoroethyllining lining of autoclave.This solution was handled 8 hours down at 180 ℃, solution centrifugal of handling well and drying, obtained the Red copper oxide powder.Fig. 1 is the XRD figure spectrum of this cuprous oxide crystal, and the cuprous standard card (JCPDS No.65-3288) of this collection of illustrative plates and cubic phase oxygenization fits like a glove.Fig. 2 is the stereoscan photograph of this Red copper oxide powder, and as can be seen from the figure the formalness of Jue Daduoshuo cuprous oxide crystal is a branched structure.
Embodiment 2:
With 0.7990 gram copper sulfate (CuSO
45H
2O) be dissolved in 72.5 ml deionized water, stir after 5 minutes, add 5.0 ml concns and be 60% Sodium.alpha.-hydroxypropionate (C
3H
5NaO
3), the Sodium.alpha.-hydroxypropionate volumetric molar concentration is 0.4 mol, stirs after 5 minutes, the pH value of utilizing the sodium hydrate regulator solution of 4.0 mol is 9.0.Regulating final solution amount with deionized water is 80.0 milliliters, cupric ion volumetric molar concentration 0.04 mol in the solution.The above-mentioned solution for preparing is put in the polytetrafluoroethyllining lining of autoclave.This solution was handled 8 hours down at 150 ℃, solution centrifugal of handling well and drying, obtained the Red copper oxide powder.Fig. 3 is the XRD figure spectrum of this cuprous oxide crystal, and the cuprous standard card (JCPDS No.65-3288) of this collection of illustrative plates and cubic phase oxygenization fits like a glove.Fig. 4 is the stereoscan photograph of this Red copper oxide powder, and as can be seen from the figure the formalness of Jue Daduoshuo cuprous oxide crystal is the regular octahedron structure.
Embodiment 3:
With 0.7990 gram copper sulfate (CuSO
45H
2O) be dissolved in 72.5 ml deionized water, stir after 5 minutes, add 4.0 ml concns again and be 60% Sodium.alpha.-hydroxypropionate (C
3H
5NaO
3), the Sodium.alpha.-hydroxypropionate volumetric molar concentration is 0.32 mol, stirs after 5 minutes, the pH value of utilizing the sodium hydrate regulator solution of 4.0 mol is 12.0.Regulating final solution amount with deionized water is 80.0 milliliters, cupric ion volumetric molar concentration 0.04 mol in the solution.The above-mentioned solution for preparing is put in the polytetrafluoroethyllining lining of autoclave.This solution was handled 4 hours down at 180 ℃, solution centrifugal of handling well and drying, obtained the Red copper oxide powder.Fig. 5 is the XRD figure spectrum of this cuprous oxide crystal, and the cuprous standard card (JCPDS No.65-3288) of this collection of illustrative plates and cubic phase oxygenization fits like a glove.Fig. 6 is the stereoscan photograph of this Red copper oxide powder, and as can be seen from the figure the formalness of Jue Daduoshuo cuprous oxide crystal is a cubic structure.
Claims (2)
1, a kind of hydrothermal preparing process of realizing that the cuprous oxide crystal form is controlled is characterized in that the step of this method is as follows:
1) soluble copper salt is soluble in water, the volumetric molar concentration of cupric ion is 0.02～0.04 mol in the control solution, stirs;
2) in above-mentioned solution, add the Sodium.alpha.-hydroxypropionate that volumetric molar concentration is 8～10 times of cupric ion volumetric molar concentrations in the solution again, continue to stir;
3) utilize the pH value of the sodium hydrate regulator solution of 4.0 mol, the pH value of solution is controlled between 7.0～12.0;
4) solution for preparing is put into autoclave, hydrothermal treatment consists is 4～8 hours in 150～180 ℃ of degree scopes;
5), just obtained the cuprous powder of cubic phase oxygenization with the solution centrifugal after the hydrothermal treatment consists, drying.
2, a kind of hydrothermal preparing process of realizing that the cuprous oxide crystal form is controlled according to claim 1, it is characterized in that: described employing copper sulfate is soluble copper salt, Sodium.alpha.-hydroxypropionate is complexing agent and reductive agent, pH value by control solution, the relative growth rate of (100) face and (111) face in the cuprous cubic system of controlled oxidation under hydrothermal condition, thereby the Red copper oxide powder that preparation has different outer shape.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101913645A (en) * | 2010-08-16 | 2010-12-15 | 南京大学 | Cu2O nanocrystalline, preparation method and application thereof and alcohol sensor |
| CN101914804A (en) * | 2010-09-03 | 2010-12-15 | 西安交通大学 | Method for preparing cuprous oxide single crystal powder containing high-index crystal face envelope surface |
| CN102618925A (en) * | 2012-04-13 | 2012-08-01 | 青岛大学 | Preparation method of cuprous oxide (CU2O) nano octahedral materials |
| CN107699885A (en) * | 2017-08-22 | 2018-02-16 | 山东科技大学 | A kind of preparation method of the magnesium hydroxide calcium phosphate composite coating of magnesium/magnesium alloy |
| CN109225219A (en) * | 2018-08-31 | 2019-01-18 | 武汉工程大学 | Copper with schottky junction structure-porous silica titanium composite material preparation method and application |
| CN109485084A (en) * | 2018-12-29 | 2019-03-19 | 合肥学院 | A kind of method and application of form controlledly synthesis cuprous oxide powder |
| CN111118601A (en) * | 2019-12-23 | 2020-05-08 | 山东大学 | Catalyst, electrode and method for preparing ethylene by carbon dioxide reduction |
| CN112093817A (en) * | 2020-10-29 | 2020-12-18 | 广西师范大学 | Preparation method of cuprous oxide dendritic crystal |
-
2008
- 2008-10-31 CN CNA2008101220732A patent/CN101412531A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101913645A (en) * | 2010-08-16 | 2010-12-15 | 南京大学 | Cu2O nanocrystalline, preparation method and application thereof and alcohol sensor |
| CN101914804A (en) * | 2010-09-03 | 2010-12-15 | 西安交通大学 | Method for preparing cuprous oxide single crystal powder containing high-index crystal face envelope surface |
| CN101914804B (en) * | 2010-09-03 | 2012-05-23 | 西安交通大学 | Method for preparing cuprous oxide single crystal powder containing high-index crystal face envelope surface |
| CN102618925A (en) * | 2012-04-13 | 2012-08-01 | 青岛大学 | Preparation method of cuprous oxide (CU2O) nano octahedral materials |
| CN102618925B (en) * | 2012-04-13 | 2014-08-13 | 青岛大学 | Preparation method of cuprous oxide (CU2O) nano octahedral materials |
| CN107699885A (en) * | 2017-08-22 | 2018-02-16 | 山东科技大学 | A kind of preparation method of the magnesium hydroxide calcium phosphate composite coating of magnesium/magnesium alloy |
| CN109225219A (en) * | 2018-08-31 | 2019-01-18 | 武汉工程大学 | Copper with schottky junction structure-porous silica titanium composite material preparation method and application |
| CN109225219B (en) * | 2018-08-31 | 2021-06-01 | 武汉工程大学 | Preparation method and application of copper-porous titanium dioxide composite material with Schottky junction structure |
| CN109485084A (en) * | 2018-12-29 | 2019-03-19 | 合肥学院 | A kind of method and application of form controlledly synthesis cuprous oxide powder |
| CN111118601A (en) * | 2019-12-23 | 2020-05-08 | 山东大学 | Catalyst, electrode and method for preparing ethylene by carbon dioxide reduction |
| CN112093817A (en) * | 2020-10-29 | 2020-12-18 | 广西师范大学 | Preparation method of cuprous oxide dendritic crystal |
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Open date: 20090422 |