CN113247943B - Preparation method of cuprous phosphide-cuprous oxide composite material - Google Patents
Preparation method of cuprous phosphide-cuprous oxide composite material Download PDFInfo
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- CN113247943B CN113247943B CN202110593633.8A CN202110593633A CN113247943B CN 113247943 B CN113247943 B CN 113247943B CN 202110593633 A CN202110593633 A CN 202110593633A CN 113247943 B CN113247943 B CN 113247943B
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/08—Other phosphides
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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
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
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Abstract
The invention discloses a preparation method of a cuprous phosphide-cuprous oxide composite material3P@Cu2O) a composite material; the cuprous oxide grows on the surface of the nano cuprous phosphide to form a core-shell structure, and the structure improves the photoluminescence performance of the material. In addition, the method is simple in preparation and low in cost.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a preparation method of a cuprous phosphide-cuprous oxide core-shell structure composite material.
Background
Cuprous phosphide (Cu)3P) are commonly used as brazing filler materials and catalysts, and have not attracted sufficient attention for applications in the optical field. As a P-type semiconductor material, with a P-type semiconductor of cuprous oxide (Cu)2O) can be used as a photoluminescence material after being compounded. The mechanism of the material influences the performance of the material, and the patent designs and prepares the cuprous phosphide-cuprous oxide composite material (Cu) with a core-shell structure3P@Cu2O), which is capable of emitting near infrared light upon excitation by ultraviolet or visible light.
Disclosure of Invention
The invention provides a preparation method of a cuprous phosphide-cuprous oxide composite material according to the defects of the prior art.
The invention firstly synthesizes nano cuprous phosphide, and then a layer of cuprous oxide is wrapped outside the nano cuprous phosphide to form a core-shell structure (Cu)3P@Cu2O) a composite material.
The invention relates to a preparation method of a cuprous phosphide-cuprous oxide composite material, which comprises the following steps:
step (1), putting sodium hypophosphite and spherical copper nanoparticles into a corundum crucible for grinding, and then putting into a corundum boat; the mass ratio of the sodium hypophosphite to the copper nanoparticles is as follows: 6:1-1: 1; the diameter of the copper nanoparticles is 30-50 nm;
step (2), putting the product obtained in the step (1) into a corundum tube, vacuumizing, filling argon gas with 1 atmosphere, and then sealing two ends of the corundum tube;
step (3), heating the product in the step (2) to 280 ℃ and 300 ℃ by a tubular furnace, wherein the heating rate is 10 ℃/min; the temperature is increased to 280-300 ℃, and then the temperature is preserved for 30-60 min; then naturally cooling to room temperature, vacuumizing the corundum tube to remove residual gas in the corundum tube, and taking out a product;
and (4) pouring the product prepared in the step (3) into a beaker, adding deionized water, stirring, performing centrifugal settling separation to obtain a precipitate, repeatedly washing the precipitate with deionized water, and performing centrifugal separation twice to obtain a clean precipitate.
And (5) putting copper nitrate, polyvinyl pyrrolidone and 50ml of water into a beaker, and stirring the substances to dissolve. The product of step (4) was added to a beaker with magnetic stirring. Then, 10. mu.l of hydrazine hydrate was slowly added dropwise to the beaker. Then repeatedly washing with deionized water and centrifugally separating for two times to obtain a precipitate with a core-shell structure, and obtaining the cuprous phosphide-cuprous oxide composite material; the mass ratio of the copper nitrate to the polyvinyl polypyrrolidone to the precipitate is 2:1: 1.
Preferably, the diameter of the corundum tube is 2 cm.
Preferably, the corundum boat has dimensions of 0.8 cm × 0.6 cm × 6 cm.
Preferably, the corundum tube vacuumizing equipment is provided with tail gas purifying equipment.
The invention has the advantages that: cuprous oxide grows on the surface of the nano cuprous phosphide to form a core-shell structure, and the photoluminescence performance of the material is improved by the core-shell structure. In addition, the method is simple in preparation and low in cost.
Detailed Description
The first embodiment is as follows:
step (1), 3g of sodium hypophosphite and 3g of spherical copper nanoparticles with the diameter of 30nm are put into a corundum crucible to be ground, and then the ground spherical copper nanoparticles are put into a corundum boat with the size of 0.8 cm multiplied by 0.6 cm multiplied by 6 cm;
step (2), putting the product obtained in the step (1) into a corundum tube, vacuumizing, filling argon gas with 1 atmosphere, and then sealing two ends of the corundum tube; the diameter of the corundum tube is 2 cm;
step (3), heating the product of the step (2) to 280 ℃ by a tubular furnace, wherein the heating rate is 10 ℃/min; keeping the temperature for 30min after the temperature is raised to 280 ℃; then naturally cooling to room temperature, vacuumizing the corundum tube to remove residual gas in the corundum tube, and taking out a product;
and (4) pouring the product prepared in the step (3) into a 100ml beaker, adding deionized water, stirring, performing centrifugal settling separation to obtain a precipitate, and repeatedly washing the precipitate with deionized water and performing centrifugal separation twice to obtain a clean precipitate.
And (5) putting 2g of copper nitrate, 1g of polyvinylpyrrolidone and 50ml of water into a 100ml beaker, and stirring the substances to dissolve. 1g of the product of step (4) was added to a beaker with magnetic stirring. Then, 10. mu.l of hydrazine hydrate was slowly added dropwise to the beaker. Then washing with deionized water and centrifugal separation are repeated twice to obtain the sediment with the core-shell structure.
Example two:
step (1), putting 4g of sodium hypophosphite and 2g of spherical copper nanoparticles with the diameter of 40nm into a corundum crucible for grinding, and then putting into a corundum boat;
step (2), putting the product obtained in the step (1) into a corundum tube, vacuumizing, filling argon gas with 1 atmosphere, and then sealing two ends of the corundum tube;
step (3), heating the product of the step (2) to 290 ℃ by a tube furnace, wherein the heating rate is 10 ℃/min; keeping the temperature for 50min after the temperature is increased to 290 ℃; then naturally cooling to room temperature, vacuumizing the corundum tube (with tail gas purification equipment) to remove residual gas in the corundum tube, and then taking out a product;
and (4) pouring the product prepared in the step (3) into a 100ml beaker, adding deionized water, stirring, performing centrifugal settling separation to obtain a precipitate, and repeatedly washing the precipitate with deionized water and performing centrifugal separation twice to obtain a clean precipitate.
And (5) putting 2g of copper nitrate, 1g of polyvinylpyrrolidone and 50ml of water into a 100ml beaker, and stirring the substances to dissolve. 1g of the product of step (4) was added to a beaker with magnetic stirring. Then, 10. mu.l of hydrazine hydrate was slowly added dropwise to the beaker. Then washing with deionized water and centrifugal separation are repeated twice to obtain the sediment with the core-shell structure.
Example three:
step (1), putting 6g of sodium hypophosphite and 1g of spherical copper nanoparticles with the diameter of 50nm into a corundum crucible for grinding, and then putting into a corundum boat (0.8 cm multiplied by 0.6 cm multiplied by 6 cm);
step (2), putting the product obtained in the step (1) into a corundum tube, vacuumizing, filling argon gas with 1 atmosphere, and then sealing two ends of the corundum tube;
step (3), heating the product of the step (2) to 300 ℃ through a tube furnace, wherein the heating rate is 10 ℃/min; keeping the temperature for 60min after the temperature is raised to 300 ℃; then naturally cooling to room temperature, vacuumizing the corundum tube (with tail gas purification equipment) to remove residual gas in the corundum tube, and then taking out a product;
and (4) pouring the product prepared in the step (3) into a 100ml beaker, adding deionized water, stirring, performing centrifugal settling separation to obtain a precipitate, and repeatedly washing the precipitate with deionized water and performing centrifugal separation twice to obtain a clean precipitate.
And (5) putting 2g of copper nitrate, 1g of polyvinylpyrrolidone and 50ml of water into a 100ml beaker, and stirring the substances to dissolve. 1g of the product of step (4) was added to a beaker with magnetic stirring. Then, 10. mu.l of hydrazine hydrate was slowly added dropwise to the beaker. Then washing with deionized water and centrifugal separation are repeated twice to obtain the sediment with the core-shell structure.
Claims (4)
1. The preparation method of the cuprous phosphide-cuprous oxide composite material is characterized by comprising the following steps of:
step (1), putting sodium hypophosphite and spherical copper nanoparticles into a corundum crucible for grinding, and then putting into a corundum boat; the mass ratio of the sodium hypophosphite to the copper nanoparticles is as follows: 6:1-1: 1; the diameter of the copper nanoparticles is 30-50 nm;
step (2), putting the product obtained in the step (1) into a corundum tube, vacuumizing, filling argon gas with 1 atmosphere, and then sealing two ends of the corundum tube;
step (3), heating the product in the step (2) to 280 ℃ and 300 ℃ by a tubular furnace, wherein the heating rate is 10 ℃/min; the temperature is increased to 280-300 ℃, and then the temperature is preserved for 30-60 min; then naturally cooling to room temperature, vacuumizing the corundum tube to remove residual gas in the corundum tube, and taking out a product;
step (4), pouring the product prepared in the step (3) into a beaker, adding deionized water, stirring, performing centrifugal settling separation to obtain a precipitate, repeatedly washing the precipitate with deionized water, and performing centrifugal separation twice to obtain a clean precipitate;
step (5), putting copper nitrate, polyvinyl pyrrolidone and 50ml of water into a beaker, and stirring the substances to dissolve; adding the product of the step (4) into a beaker under magnetic stirring; then slowly dripping 10 microliter of hydrazine hydrate into the beaker; then repeatedly washing with deionized water and centrifugally separating for two times to obtain a precipitate with a core-shell structure, and obtaining the cuprous phosphide-cuprous oxide composite material; the mass ratio of the copper nitrate to the polyvinyl polypyrrolidone to the precipitate is 2:1: 1.
2. The preparation method of the cuprous phosphide-cuprous oxide composite material according to claim 1, characterized in that: the diameter of the corundum tube is 2 cm.
3. The preparation method of the cuprous phosphide-cuprous oxide composite material according to claim 1, characterized in that: the corundum boat has the size of 0.8 cm multiplied by 0.6 cm multiplied by 6 cm.
4. The preparation method of the cuprous phosphide-cuprous oxide composite material according to claim 1, characterized in that: the corundum tube vacuumizing equipment is provided with tail gas purifying equipment.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB602814A (en) * | 1941-05-23 | 1948-06-03 | Metallo Chimique Sa | Improvements in and relating to the manufacture of copper phosphide |
| CN109731586A (en) * | 2018-12-29 | 2019-05-10 | 江苏大学 | Based on classifying porous phosphorized copper derived from copper-containing metal organic frame/carbon hydrolysis elctro-catalyst preparation method and applications |
| CN110014160A (en) * | 2019-04-26 | 2019-07-16 | 陕西科技大学 | A kind of ellipsoid Cu2O/Cu/Cu3The preparation method of N composite granule |
| CN112791736A (en) * | 2019-11-14 | 2021-05-14 | 天津理工大学 | WP2/Cu3Application of P composite nano-structure catalyst in aspect of hydrogen production by electrolyzing water |
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- 2021-05-28 CN CN202110593633.8A patent/CN113247943B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB602814A (en) * | 1941-05-23 | 1948-06-03 | Metallo Chimique Sa | Improvements in and relating to the manufacture of copper phosphide |
| CN109731586A (en) * | 2018-12-29 | 2019-05-10 | 江苏大学 | Based on classifying porous phosphorized copper derived from copper-containing metal organic frame/carbon hydrolysis elctro-catalyst preparation method and applications |
| CN110014160A (en) * | 2019-04-26 | 2019-07-16 | 陕西科技大学 | A kind of ellipsoid Cu2O/Cu/Cu3The preparation method of N composite granule |
| CN112791736A (en) * | 2019-11-14 | 2021-05-14 | 天津理工大学 | WP2/Cu3Application of P composite nano-structure catalyst in aspect of hydrogen production by electrolyzing water |
Non-Patent Citations (1)
| Title |
|---|
| 磷化铜/石墨烯锂离子负极材料的制备及其电化学性能研究;孙硕等;《常熟理工学院学报》;20200320(第02期);全文 * |
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