CN112456539A - Method for regulating and controlling morphology of p-type semiconductor material - Google Patents
Method for regulating and controlling morphology of p-type semiconductor material Download PDFInfo
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- CN112456539A CN112456539A CN202011635527.3A CN202011635527A CN112456539A CN 112456539 A CN112456539 A CN 112456539A CN 202011635527 A CN202011635527 A CN 202011635527A CN 112456539 A CN112456539 A CN 112456539A
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- 238000000034 method Methods 0.000 title claims abstract description 13
- 230000001105 regulatory effect Effects 0.000 title claims abstract description 13
- 239000004065 semiconductor Substances 0.000 title claims abstract description 12
- 239000000463 material Substances 0.000 title claims abstract description 11
- 230000001276 controlling effect Effects 0.000 title abstract description 3
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 claims abstract description 24
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229940112669 cuprous oxide Drugs 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 239000013078 crystal Substances 0.000 claims abstract description 15
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 13
- 239000008103 glucose Substances 0.000 claims abstract description 13
- 230000009467 reduction Effects 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 28
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 239000012071 phase Substances 0.000 abstract description 6
- 239000003638 chemical reducing agent Substances 0.000 abstract description 4
- 239000007791 liquid phase Substances 0.000 abstract description 4
- 230000001699 photocatalysis Effects 0.000 abstract description 3
- 230000002194 synthesizing effect Effects 0.000 abstract description 3
- 230000008859 change Effects 0.000 abstract description 2
- 230000003287 optical effect Effects 0.000 abstract description 2
- 230000005855 radiation Effects 0.000 abstract description 2
- 238000007146 photocatalysis Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 9
- 239000002245 particle Substances 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- -1 halogen anions Chemical class 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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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
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/72—Copper
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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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
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/30—Particle morphology extending in three dimensions
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- C01—INORGANIC CHEMISTRY
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- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/41—Particle morphology extending in three dimensions octahedron-like
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/51—Particles with a specific particle size distribution
- C01P2004/52—Particles with a specific particle size distribution highly monodisperse size distribution
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Abstract
The invention relates to a method for regulating and controlling the appearance of a p-type semiconductor material, which is characterized in that the p-type semiconductor material is reacted in a closed reaction kettle, so that reactions which are difficult to occur at normal temperature and normal pressure are caused to occur at high temperature and high pressure to form a gas-phase CO-liquid-phase (PVP and glucose) two-phase reduction system, the PVP is firstly used for synthesizing cuprous oxide, the growth of crystals can be inhibited by the PVP, the change of the appearance of the crystals from an octahedron to a strip shape is regulated and controlled by changing the relative dosage of a gas-phase reducing agent CO and a liquid-phase reducing agent glucose under an alkaline condition, the appearance and the size of the product are uniform, and the characteristic that the photocatalysis reaction is initiated under the radiation of sunlight based on the unique optical property of a.
Description
Technical Field
The invention belongs to the technical field of semiconductor material synthesis, and particularly relates to a cuprous oxide morphology regulating and synthesizing method.
Background
Cuprous oxide is a typical P-type semiconductor and can be applied to the fields of solar energy conversion, magnetic storage, catalysis, gas sensitivity and the like. After reaching the micro-nanometer level, the nano-composite material has a great potential application in the aspects of solar cells, gas catalysis, gas sensors and the like due to the large specific surface area and excellent surface physical and chemical properties. The Cu2O has the most obvious advantage of being used as a photocatalyst that visible light can be directly utilized to decompose water into hydrogen and oxygen, has good application prospect in the aspect of photocatalytic degradation of organic pollutants, and is expected to become a new generation of semiconductor photocatalyst.
The shape and size of the particles are closely related to the macroscopic physical and chemical properties of the particles, for example, the regular octahedral structure of cuprous oxide has better adsorption capacity and photocatalytic activity than the cubic structure, so the application field of the particles can be determined according to the shape of the cuprous oxide, at present, the control of the nano shape of the particles at home and abroad has many research reports, Chinese patent CN109761263A discloses that the shape of a cuprous oxide crystal is regulated and controlled from a cube to an octahedron through halogen anions, Chinese patent CN104261457A discloses that the shape of the cuprous oxide crystal is regulated and controlled through the compounding reduction of glucose and sodium citrate, and Chinese patent CN102583499A discloses that the shape of a cuprous oxide micro-nano crystal is regulated and controlled through lactic acid reduction and the change of pH. However, the existing cuprous oxide morphology is mainly cubic and cubic, the exposed crystal planes of the cuprous oxide are mostly {111} and {110} crystal planes, and a rod-shaped morphology with a surface atomic arrangement of {100} is rarely reported.
Disclosure of Invention
In order to synthesize more cuprous oxide crystal morphologies and further explore a new synthesis method, the invention provides a morphology regulation method for a P-type semiconductor material; in order to achieve the purpose, the technical scheme adopted by the invention is as follows: a method for regulating the appearance of a P-type semiconductor material comprises the following steps:
1. step one, adding 1.5g of PVP into 100mLCuCl2(0.01mol/L) solution, stirring and dissolving for 15min to form solution 1;
2. step two, dripping 10.0mL of NaOH (2mol/L) aqueous solution into the solution 1, and continuously stirring for 10min to form a solution 2;
3. step three, (5-10.0) ml of glucose (0.9mol/L) is dripped into the solution 2, and the solution 3 is obtained after continuous stirring for 10 min;
4. and step four, transferring the solution 3 into a hydrothermal reaction kettle, discharging air in the reaction kettle by using CO reduction gas, introducing (0.05-0.8 MPa) CO gas into the reaction kettle, sealing the reaction kettle, placing the hydrothermal reaction kettle into an oven, preserving the temperature at (80-100) DEG C for 3-6 hours, naturally cooling to room temperature, centrifugally washing, washing with water for three times, washing with ethanol for 1 time, and vacuum-drying at 40 ℃ to obtain cuprous oxide crystals.
5. Preferably, the dosage of the glucose in the third step is 5 ml, and 0.8MPa of CO is introduced into the fourth step to obtain the cuprous oxide with the rod shape.
6. Preferably, the dosage of the glucose in the third step is 10 ml, and 0.05MPa of CO is introduced into the fourth step to obtain the cuprous oxide with the octahedral morphology.
7. Preferably, the temperature of the heat preservation in the fourth step is 90 ℃.
8. Preferably, the heat preservation time in the fourth step is 4 hours.
The invention has the beneficial effects that: the invention carries out reaction in a closed reaction kettle, so that some reactions which are difficult to occur at normal temperature and normal pressure occur at high temperature and high pressure to form a gas-phase CO-liquid-phase (PVP and glucose) two-phase reduction system which is firstly used for synthesizing cuprous oxide, the PVP can inhibit the growth of crystals, the transformation of the appearance of the crystals from an octahedron to a strip shape is regulated and controlled by changing the relative using amount of a gas-phase reducing agent CO and a liquid-phase reducing agent glucose under an alkaline condition, the appearance and the size of the product are uniform, and more efficient photocatalytic performance can be expected to be obtained based on the characteristic that the unique optical property of a Cu2O nano material initiates a photocatalytic reaction under the radiation of sunlight.
Drawings
FIG. 1 is an SEM representation of cuprous oxide crystals obtained in example 1 of the present invention;
FIG. 2 is an SEM representation of cuprous oxide crystals obtained in example 2 of the present invention.
Detailed Description
The invention is described in further detail below with reference to the following figures and detailed description:
example 1:
a method for regulating the appearance of a P-type semiconductor material comprises the following steps:
9. step one, adding 1.5g of PVP into 100mLCuCl2(0.01mol/L) solution, stirring and dissolving for 15min to form solution 1;
10. step two, dripping 10.0mL of NaOH (2mol/L) aqueous solution into the solution 1, and continuously stirring for 10min to form a solution 2;
11. step three, dripping 10.0ml of glucose (0.9mol/L) into the solution 2, and continuously stirring for 10min to obtain a solution 3;
12. and step four, transferring the solution 3 into a hydrothermal reaction kettle, discharging air in the reaction kettle by using CO reduction gas, introducing 0.05MPa of CO gas into the reaction kettle, closing the reaction kettle, putting the hydrothermal reaction kettle into an oven, preserving heat at 90 ℃ for 4 hours, naturally cooling to room temperature, centrifugally washing, washing with water for three times, washing with ethanol for 1 time, and drying in vacuum at 40 ℃ to obtain the cuprous oxide crystal with the octahedral morphology as shown in the figure 1.
Example 2:
a method for regulating the appearance of a P-type semiconductor material comprises the following steps:
14. step one, adding 1.5g of PVP into 100mLCuCl2(0.01mol/L) solution, stirring and dissolving for 15min to form solution 1;
15. step two, dripping 10.0mL of NaOH (2mol/L) aqueous solution into the solution 1, and continuously stirring for 10min to form a solution 2;
16. step three, dripping 5.0 ml of glucose (0.9mol/L) into the solution 2, and continuously stirring for 10min to obtain a solution 3;
17. and step four, transferring the solution 3 into a hydrothermal reaction kettle, discharging air in the reaction kettle by using CO reduction gas, introducing 0.8MPa CO gas into the reaction kettle, sealing the reaction kettle, putting the hydrothermal reaction kettle into an oven, keeping the temperature of 90 ℃ for 4 hours, naturally cooling to room temperature, centrifugally washing, washing with water for three times, washing with ethanol for 1 time, and vacuum-drying at 40 ℃ to obtain the strip-shaped cuprous oxide crystal shown in the figure 2.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and substitutions can be made without departing from the technical principle of the present invention, and these modifications and substitutions should also be regarded as the protection scope of the present invention.
Claims (5)
1. A method for regulating the appearance of a P-type semiconductor material comprises the following steps:
step one, adding 1.5g of PVP into 100mLCuCl2(0.01mol/L) solution, stirring and dissolving for 15min to form solution 1;
step two, dripping 10.0mL of NaOH (2mol/L) aqueous solution into the solution 1, and continuously stirring for 10min to form a solution 2;
step three, (5-10.0) ml of glucose (0.9mol/L) is dripped into the solution 2, and the solution 3 is obtained after continuous stirring for 10 min;
and step four, transferring the solution 3 into a hydrothermal reaction kettle, discharging air in the reaction kettle by using CO reduction gas, introducing (0.05-0.8 MPa) CO gas into the reaction kettle, sealing the reaction kettle, placing the hydrothermal reaction kettle into an oven, preserving the temperature at (80-100) DEG C for 3-6 hours, naturally cooling to room temperature, centrifugally washing, washing with water for three times, washing with ethanol for 1 time, and vacuum-drying at 40 ℃ to obtain cuprous oxide crystals.
2. The method of claim 1, wherein: the dosage of the glucose in the third step is 5 ml, and the CO with the pressure of 0.8MPa is introduced into the fourth step to obtain the cuprous oxide with the rod shape.
3. The method according to claims 1-2, characterized in that: the dosage of the glucose in the third step is 10 ml, and 0.05MPa of CO is introduced into the fourth step to obtain the cuprous oxide with the octahedral morphology.
4. A method according to claims 1-3, characterized in that: in the fourth step, the heat preservation temperature is 90 ℃.
5. The method according to claims 1-4, characterized in that: in the fourth step, the heat preservation time is 4 hours.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113698373A (en) * | 2021-09-09 | 2021-11-26 | 昆明理工大学 | Method for preparing 2, 5-furandicarboxylic acid by high-efficiency photocatalytic oxidation |
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2020
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113698373A (en) * | 2021-09-09 | 2021-11-26 | 昆明理工大学 | Method for preparing 2, 5-furandicarboxylic acid by high-efficiency photocatalytic oxidation |
| CN113698373B (en) * | 2021-09-09 | 2024-03-08 | 昆明理工大学 | Method for preparing 2, 5-furandicarboxylic acid by high-efficiency photocatalytic oxidation |
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