CN113555459A - Selenium sulfide doped copper oxide with strong luminescence characteristic - Google Patents

Selenium sulfide doped copper oxide with strong luminescence characteristic Download PDF

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CN113555459A
CN113555459A CN202110820587.0A CN202110820587A CN113555459A CN 113555459 A CN113555459 A CN 113555459A CN 202110820587 A CN202110820587 A CN 202110820587A CN 113555459 A CN113555459 A CN 113555459A
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cuo
copper oxide
doped copper
selenium sulfide
ses
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CN113555459B (en
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高斐
石伯男
张超群
李佳辉
李元瑞
刘生忠
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Shaanxi Normal University
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L31/00Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L31/0248Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
    • H01L31/0256Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
    • H01L31/0264Inorganic materials
    • H01L31/032Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312
    • H01L31/0321Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312 characterised by the doping material
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    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B19/00Selenium; Tellurium; Compounds thereof
    • C01B19/04Binary compounds including binary selenium-tellurium compounds
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G3/00Compounds of copper
    • C01G3/02Oxides; Hydroxides
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product

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Abstract

The invention discloses selenium sulfide doped copper oxide with strong luminescence property, which is prepared by firstly utilizing a powder tabletting method to mix CuO powder and SeS2The powder is mixed and tabletted according to the molar ratio of 4: 1-12: 1 to form a wafer, and then the obtained wafer is subjected to rapid thermal annealing treatment at 450-650 ℃ for 2-10 min to prepare the silicon nitride/silicon oxide/silicon. SeS is doped in CuO2Modifying to improve the photoelectric property of CuO and to dope SeS2The photoluminescence intensity of the CuO material can reach about 14 times of the photoelectric property of the pure CuO material, and the material is expected to become a novel material in the field of photoelectric property materials.

Description

Selenium sulfide doped copper oxide with strong luminescence characteristic
Technical Field
The invention belongs to the technical field of semiconductor photoelectric materials, and particularly relates to selenium sulfide doped copper oxide with strong luminescence property.
Background
Semiconductor materials play an increasingly important role in the field of optoelectronics. However, high performance single crystal semiconductor materials are expensive to fabricate, limiting their wide-scale application. The amorphous or nanocrystalline material has low production cost and is suitable for large-scale application.
Copper oxide (CuO) is a p-type semiconductor material, is black, belongs to a monoclinic system, is a typical transition metal oxide, and has rich earth resources and low toxicity. And CuO has a very ideal band gap (1.4eV) and a very high light absorption coefficient. However, CuO has a high melting point (1446 ℃ C.), and decomposes around the melting point. At present, the main preparation methods of CuO semiconductor materials include a magnetron sputtering method, a gel method, a hydrothermal method and the like. CuO prepared by the methods is mostly in an amorphous and nanocrystalline structure, has more defects and serious carrier recombination, and seriously limits the application of the CuO in the photoelectric field. Therefore, there is a need to develop a doping method that can maintain the CuO in an amorphous or nano-crystalline state with good photoelectric properties.
Disclosure of Invention
The invention aims to overcome the problems of a CuO semiconductor material and provide selenium sulfide doped copper oxide with strong luminescence property.
Aiming at the purposes, the selenium sulfide doped copper oxide with strong luminescence property is prepared by the following method: mixing CuO powder with SeS2The powder is fully mixed according to the mol ratio of 4: 1-12: 1, then tabletting is carried out, and annealing is carried out for 2-10 min at the temperature of 450-650 ℃.
In the above production method, CuO powder and SeS are preferably used2And fully mixing the powder according to the molar ratio of 6: 1-10: 1, and tabletting.
In the preparation method, the pressed sheet is kept for 8-10 s under the pressure of 12-15 MPa to form a wafer with the thickness of 0.6-1.0 mm.
In the above preparation method, annealing at 500 to 600 ℃ is further preferably performed for 3 to 5 min.
The invention has the following beneficial effects:
1. the invention is characterized in that a small amount of SeS is doped2The method is simple, convenient, low in cost and applicable to large-scale application. HeadFirstly, CuO and SeS with different molar ratios are mixed2Mixing and tabletting through a simple machine, and then annealing CuO and SeS by adopting an annealing furnace2Fully mixed and reacted to form CuO and SeS2To obtain a new semiconductor composite material. The photoelectric performance of the composite material can reach the highest independently annealed CuO and SeS2About 14 times of the total weight of the product.
2. The CuO semiconductor material adopted by the invention comprises: high light absorption coefficient, stable chemical property, rich earth reserves, low manufacturing cost, non-harsh synthesis conditions, wide temperature window and the like, and is very suitable for large-scale application. And SeS2As a common chemical, the compound also has the advantages of low cost, abundant reserves, non-harsh preparation conditions and the like.
Drawings
Figure 1 is a PL profile of selenium sulfide doped copper oxide prepared in example 1.
Figure 2 is an XRD pattern of selenium sulphide doped copper oxide prepared in example 1.
Figure 3 is a PL profile of the selenium sulfide doped copper oxide prepared in example 2.
Figure 4 is an XRD pattern of selenium sulphide doped copper oxide prepared in example 2.
Figure 5 is a PL profile of selenium sulfide doped copper oxide prepared in example 3.
Figure 6 is an XRD pattern of selenium sulphide doped copper oxide prepared in example 3.
Figure 7 is a PL profile of selenium sulfide doped copper oxide prepared in example 4.
Figure 8 is an XRD pattern of selenium sulphide doped copper oxide prepared in example 4.
Figure 9 is a PL profile of selenium sulfide doped copper oxide prepared in example 5.
Figure 10 is an XRD pattern of selenium sulfide doped copper oxide prepared in example 5.
Detailed Description
The invention will be further described with reference to the following figures and specific examples, but the scope of the invention is not limited to these examples.
Example 1
Mixing CuO powder with SeS2Fully grinding and mixing the powder according to a molar ratio of 4:1, and then tabletting by using a tabletting machine under the pressure of 15MPa for 8-10 s to form a wafer with the thickness of 0.6-0.8 mm. And (3) annealing the wafer on quartz glass in an annealing furnace at the annealing temperature of 500 ℃ for 3min to obtain the selenium sulfide doped copper oxide.
Photoluminescence (PL) and X-ray diffraction (XRD) characterization was performed on this material, and the results are shown in fig. 1 and fig. 2. The PL test results in fig. 1 show that the PL peak intensity of the resulting material is 5.38 times higher than CuO alone at the same annealing temperature and time (the peak intensity increases from 701 to 3772). XRD testing of FIG. 2 shows that a large amount of CuO and newly formed CuSe exist in the obtained material2
Example 2
Mixing CuO powder with SeS2Fully grinding and mixing the powder according to the molar ratio of 6:1, and then tabletting by using a tabletting machine under the pressure of 15MPa for 8-10 s to form a wafer with the thickness of 0.6-0.8 mm. And (3) annealing the wafer on quartz glass in an annealing furnace at the annealing temperature of 500 ℃ for 3min to obtain the selenium sulfide doped copper oxide.
Photoluminescence (PL) and X-ray diffraction (XRD) characterization was performed on this material, and the results are shown in fig. 3 and 4. The PL test results of fig. 3 show that the PL peak intensity of the resulting material is 7.82 times higher than CuO alone at the same annealing temperature and time (the peak intensity increases from 701 to 5483). XRD testing of FIG. 4 shows that a significant amount of CuO and newly formed CuSe are present in the resulting material2
Example 3
Mixing CuO powder with SeS2Fully grinding and mixing the powder according to a molar ratio of 10:1, and then tabletting by using a tabletting machine under the pressure of 15MPa for 8-10 s to form a wafer with the thickness of 0.6-0.8 mm. And (3) annealing the wafer on quartz glass in an annealing furnace at the annealing temperature of 500 ℃ for 3min to obtain the selenium sulfide doped copper oxide.
Photoluminescence (PL) and X-ray diffraction (XRD) characterization was performed on this material, and the results are shown in fig. 5 and 6. The PL test results of FIG. 5 show that the PL peak intensity of the resulting materialIs 8.81 times of that of the single CuO under the same annealing temperature and time (the peak intensity is improved to 6174 from the original 701). XRD testing of FIG. 6 shows that the resulting material contains a significant amount of CuO and newly formed Cu5Se4And Cu7Se4
Example 4
Mixing CuO powder with SeS2Fully grinding and mixing the powder according to the molar ratio of 6:1, and then tabletting by using a tabletting machine under the pressure of 15MPa for 8-10 s to form a wafer with the thickness of 0.6-0.8 mm. And (3) annealing the wafer on quartz glass in an annealing furnace at the annealing temperature of 600 ℃ for 3min to obtain the selenium sulfide doped copper oxide.
Photoluminescence (PL) and X-ray diffraction (XRD) characterization was performed on this material, and the results are shown in fig. 7 and 8. The PL test results of fig. 7 show that the PL peak intensity of the resulting material is 13.91 times higher than CuO alone at the same annealing temperature and time (the peak intensity increases from 1483 to 20633). XRD testing of FIG. 4 shows that a significant amount of CuO and newly formed CuSe are present in the resulting material2And Cu7Se4
Example 5
Mixing CuO powder with SeS2Fully grinding and mixing the powder according to the molar ratio of 12:1, and then tabletting by using a tabletting machine under the pressure of 15MPa for 8-10 s to form a wafer with the thickness of 0.6-0.8 mm. And (3) annealing the wafer on quartz glass in an annealing furnace at the annealing temperature of 500 ℃ for 3min to obtain the selenium sulfide doped copper oxide.
Photoluminescence (PL) and X-ray diffraction (XRD) characterization was performed on this material, and the results are shown in fig. 9 and 10. The PL test results in fig. 9 show that the PL peak intensity of the resulting material is 3.59 times higher than CuO alone at the same annealing temperature and time (the peak intensity increases from 701 to 2517). XRD testing of FIG. 10 shows that the resulting material contains a significant amount of CuO and newly formed Cu2S。
Example 6
Mixing CuO powder with SeS2Fully grinding and mixing the powder according to the molar ratio of 8:1, and then tabletting by using a tabletting machine under the pressure of 15MPa for 8-10 s to form a wafer with the thickness of 0.6-0.8 mm. Obtained byAnd (3) annealing the wafer on quartz glass in an annealing furnace at the annealing temperature of 650 ℃ for 3min to obtain the selenium sulfide doped copper oxide.
Photoluminescence (PL) characterization is carried out on the material, and PL test results show that the PL peak intensity of the obtained material is 2.09 times that of CuO alone at the same annealing temperature and time (the peak intensity is increased to 3241 from 1554 originally).

Claims (4)

1. The selenium sulfide doped copper oxide with strong luminescence property is characterized in that the material is prepared by the following method: mixing CuO powder with SeS2The powder is fully mixed according to the mol ratio of 4: 1-12: 1, then tabletting is carried out, and annealing is carried out for 2-10 min at the temperature of 450-650 ℃.
2. The selenium sulfide doped copper oxide with strong luminescence property of claim 1, wherein: mixing CuO powder with SeS2And fully mixing the powder according to the molar ratio of 6: 1-10: 1, and tabletting.
3. The selenium sulfide doped copper oxide with strong luminescence property of claim 1 or 2, wherein: the tabletting is kept for 8-10 s under the pressure of 12-15 MPa to form a wafer with the thickness of 0.6-1.0 mm.
4. The selenium sulfide doped copper oxide with strong luminescence property of claim 1 or 2, wherein: annealing at 500-600 deg.C for 3-5 min.
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Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5986271A (en) * 1982-11-09 1984-05-18 Matsushita Electric Ind Co Ltd Manufacture of photoconductive thin film
US5731031A (en) * 1995-12-20 1998-03-24 Midwest Research Institute Production of films and powders for semiconductor device applications
CN1998068A (en) * 2004-05-18 2007-07-11 Nm斯平特罗尼克公司 Copper doped magnetic semiconductors
CN101260507A (en) * 2008-04-24 2008-09-10 复旦大学 P-type semiconductor nickel-doping copper oxide target material and preparation method thereof
CN102230212A (en) * 2011-06-22 2011-11-02 泉州师范学院 Method for preparing zinc oxide copper-doped room temperature magnetic semiconductor
CN102603201A (en) * 2011-09-29 2012-07-25 山东建筑大学 Method for preparing cuprous selenide thin film
JP2012206899A (en) * 2011-03-30 2012-10-25 Dowa Electronics Materials Co Ltd Particle powder of copper selenide and method of producing the same
CN109713115A (en) * 2018-12-29 2019-05-03 昆明理工大学 A kind of Cu-Se-S system thermoelectric material and preparation method thereof
CN109913814A (en) * 2019-03-28 2019-06-21 陕西师范大学 A kind of copper oxide/selenium composite material film

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5986271A (en) * 1982-11-09 1984-05-18 Matsushita Electric Ind Co Ltd Manufacture of photoconductive thin film
US5731031A (en) * 1995-12-20 1998-03-24 Midwest Research Institute Production of films and powders for semiconductor device applications
CN1998068A (en) * 2004-05-18 2007-07-11 Nm斯平特罗尼克公司 Copper doped magnetic semiconductors
CN101260507A (en) * 2008-04-24 2008-09-10 复旦大学 P-type semiconductor nickel-doping copper oxide target material and preparation method thereof
JP2012206899A (en) * 2011-03-30 2012-10-25 Dowa Electronics Materials Co Ltd Particle powder of copper selenide and method of producing the same
CN102230212A (en) * 2011-06-22 2011-11-02 泉州师范学院 Method for preparing zinc oxide copper-doped room temperature magnetic semiconductor
CN102603201A (en) * 2011-09-29 2012-07-25 山东建筑大学 Method for preparing cuprous selenide thin film
CN109713115A (en) * 2018-12-29 2019-05-03 昆明理工大学 A kind of Cu-Se-S system thermoelectric material and preparation method thereof
CN109913814A (en) * 2019-03-28 2019-06-21 陕西师范大学 A kind of copper oxide/selenium composite material film
US20200308691A1 (en) * 2019-03-28 2020-10-01 Shaanxi Normal University CuO/Se COMPOSITE FILM

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Title
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V.S. GURIN等: "Incorporation of copper and its oxides and chalcogenides into silica sol-gel materials", 《MATERIALS SCIENCE》 *
XIAODONG HUA等: "Preparation of Cu2Se thin films by vacuum evaporation and hot-pressing", 《VACUUM》 *

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