CN117186881A - CuO-Te material with strong ultraviolet luminescence - Google Patents
CuO-Te material with strong ultraviolet luminescence Download PDFInfo
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- CN117186881A CN117186881A CN202311088715.2A CN202311088715A CN117186881A CN 117186881 A CN117186881 A CN 117186881A CN 202311088715 A CN202311088715 A CN 202311088715A CN 117186881 A CN117186881 A CN 117186881A
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- cuo
- annealed
- powder
- strong ultraviolet
- luminescence
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- 239000000463 material Substances 0.000 title claims abstract description 59
- 238000004020 luminiscence type Methods 0.000 title claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 21
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 238000000137 annealing Methods 0.000 claims description 20
- 238000000034 method Methods 0.000 abstract description 7
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 3
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 66
- 239000004065 semiconductor Substances 0.000 description 12
- 238000012360 testing method Methods 0.000 description 9
- 238000005424 photoluminescence Methods 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 238000012512 characterization method Methods 0.000 description 4
- 238000000103 photoluminescence spectrum Methods 0.000 description 4
- 239000005751 Copper oxide Substances 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 229910000431 copper oxide Inorganic materials 0.000 description 3
- 230000001747 exhibiting effect Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002159 nanocrystal Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000000724 energy-dispersive X-ray spectrum Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
The invention discloses a CuO-Te material with strong ultraviolet luminescence, which is prepared by mixing CuO powder and Sb 2 Te 3 The powder is fully mixed and ground according to the mol ratio of 10:1.0-2.0, pressed into tablets, and annealed for 10-15 min at 800-950 ℃ in an air environment. The Te material has the advantages of high luminous intensity, abundant natural reserves, low preparation cost, simple process and the like, the highest ultraviolet luminous intensity of the Te material can reach more than 180000a.u.s, the Te material is 200 times of annealed pure CuO, the photoelectric and electro-optical conversion efficiency of the CuO is greatly improved, and the Te material is hopeful to become a novel material in the field of photoelectric property materials and has potential of commercial application.
Description
Technical Field
The invention belongs to the technical field of semiconductor photoelectric materials, and particularly relates to a CuO: te material with strong ultraviolet luminescence.
Background
Semiconductor materials play a critical role in the optoelectronic field. However, the high-performance monocrystalline semiconductor material has high manufacturing cost and limits the large-scale application thereof. Amorphous and nanocrystalline semiconductor materials are suitable for large-scale applications due to simple production processes and low manufacturing costs.
Copper oxide (CuO) is black powder, has good heat and photo-chemical stability, no toxicity and low cost preparation method, high light absorption coefficient and good photoelectric property, and is an important narrow-bandgap (1.2-1.4 eV) p-type semiconductor material. However, cuO semiconductor materials prepared by using a magnetron sputtering method, a gel method, a hydrothermal method and other methods mostly have nanocrystalline and amorphous structures due to a high melting point (1446 ℃), so that the CuO semiconductor materials have many defects, serious carrier recombination and poor light-emitting characteristics, and the photoelectric application of the CuO semiconductor materials is severely limited.
Patent ZL202110820587.0 by SeS 2 The doping improves the luminescence property of CuO, and compared with pure CuO, the luminescence property of CuO can be improved by about 14 times at maximum, and the luminescence property is required to be further improved. Patent ZL202110820254.8 by doping MoS 2 The luminescence property of CuO is improved by 108 times compared with pure CuO, and the luminescence property is compared with SeS 2 The doping is obviously improved, but the luminescence peak position of the material obtained by the method is 520nm (the intensity is 217411 a.u.), and the material is green light. The light emission peak position of the semiconductor photoelectric material determines the absorption light wavelength range (such as a solar cell and a photoelectric detector, light with a wavelength smaller than the light emission peak position can be absorbed by the device) or the wavelength of emitted light (such as a light emitting diode and a semiconductor laser), and particularly for the laser, the monochromaticity is required to be better, namely, the smaller the half-width of the light emission peak is, the better. On the other hand, the higher the luminous intensity of the semiconductor photoelectric material, the higher the photoelectric and electro-optical conversion efficiency of the material. CuO doped MoS 2 The half-width of the luminescence peak is wider, the monochromaticity is poor for the application of lasers and the like, the photoluminescence intensity is not high, and the application is greatly limited.
Disclosure of Invention
The invention aims to overcome the defects of a CuO semiconductor material and provides a CuO: te material with strong ultraviolet luminescence.
In view of the above, the CuO-Te material with strong ultraviolet light emission of the present invention is prepared by mixing CuO powder with Sb 2 Te 3 The powder is fully mixed and ground according to the mol ratio of 10:1.0-2.0, pressed into tablets, and annealed for 10-15 min at 800-900 ℃ in an air environment.
Among the above materials, cuO powder and Sb are preferable 2 Te 3 The powder is fully mixed and ground according to the mol ratio of 10:1.0-1.2 and then pressed into tablets.
The pressed sheet is kept under the pressure of 10-15 MPa for 8-10 s, and is pressed into a round sheet with the thickness of 0.8-1.2 mm.
Among the above materials, annealing at 900℃for 10 to 15 minutes in an air atmosphere is preferable.
The beneficial effects of the invention are as follows:
1. the invention uses CuO and Sb with different molar ratios 2 Te 3 Mixing the powder, grinding, mechanically pressing and high-temperature annealing to prepare the CuO-Te material with strong ultraviolet luminescence. According to the invention, the Te doping modification is adopted to ensure that the highest ultraviolet luminous intensity of the obtained CuO: te material can reach more than 180000a.u., which is about 209 times of that of annealed pure CuO, and the photoelectric and electro-optical conversion efficiency of the CuO is greatly improved. The material is expected to be a novel material in the field of photoelectric materials.
2. The CuO-Te material has the advantages of high luminous intensity, rich natural reserves, low preparation cost, simple process and the like, and has potential of commercial application.
Drawings
FIG. 1 is an EDS spectrum of a CuO: te material prepared in example 1.
FIG. 2 is annealed CuO, annealed Sb 2 Te 3 And XRD patterns of the CuO: te material prepared in example 1.
FIG. 3 is annealed CuO, annealed Sb 2 Te 3 And PL spectrum of CuO: te material prepared in example 1.
FIG. 4 is annealed CuO, annealed Sb 2 Te 3 And XRD patterns of the CuO: te material prepared in example 2.
FIG. 5 is annealed CuO, annealed Sb 2 Te 3 And PL spectrum of CuO: te material prepared in example 2.
FIG. 6 is annealed CuO, annealed Sb 2 Te 3 And XRD patterns of the CuO: te material prepared in example 3.
FIG. 7 is an annealed CuO, annealed Sb 2 Te 3 And PL spectrum of CuO: te material prepared in example 3.
FIG. 8 is annealed CuO, annealed Sb 2 Te 3 And XRD patterns of the CuO: te material prepared in example 4.
FIG. 9 is an annealed CuO, annealed Sb 2 Te 3 And PL spectrum of CuO: te material prepared in example 4.
Detailed Description
The invention will be further described with reference to the drawings and specific examples, but the scope of the invention is not limited to these examples.
Example 1
Mixing CuO powder with Sb 2 Te 3 The powder is fully ground and mixed according to the mol ratio of 10:1, and then a tablet press is used for tabletting under the pressure of 10MPa for 8-10 s, so that a sample with the thickness of 1mm is prepared. And (3) placing the obtained sample on quartz glass for annealing in an air environment, wherein the annealing temperature is 900 ℃, and the annealing time is 10min, so that the CuO-Te material is obtained.
The annealed samples were first subjected to EDS testing and the elemental content of the annealed samples passing the EDS test is given in fig. 1. The atomic percentages of Cu, O and Te in the annealed sample are 42.9%, 52.1% and 5.0%, respectively, and the content of Sb element is 0.0%, which indicates that the Sb element volatilizes away from the sample in the annealing process at 900 ℃. The results demonstrate that the material prepared is Te doped CuO, i.e., cuO: te.
The resulting material was subjected to XRD and PL characterization, the results of which are shown in fig. 2 and 3. XRD measurements of FIG. 2 show that the major diffraction peaks (110), (11-1), (111) of CuO are at Sb 2 Te 3 Offset occurs after doping annealing, indicating that Te is incorporated into the CuO lattice and appears as CuO: te nanocrystals. The PL test results of fig. 3 show that annealed pure CuO has photoluminescence at around 460nm, with weaker intensity, about 890; annealed pure Sb 2 Te 3 The powder also has weaker luminescence and intensity of about 10000, and the molar ratio of CuO to Sb 2 Te 3 The sample of 10:1 annealed material of CuO: te exhibits strong photoluminescence at 445nm and has an intensity of about 95568, and the reason for the strong photoluminescence is that the incorporation of Te element into CuO lattice improves the luminescence characteristics of CuO. The ultraviolet photoluminescence intensity of the CuO-Te material obtained in the embodiment can reach about 107 times of that of annealed pure CuO.
Example 2
Mixing CuO powder with Sb 2 Te 3 The powder is fully ground and mixed according to the mol ratio of 10:1.2, and then a tablet press is used for tabletting under the pressure of 10MPa for 6-8 s, so that a sample with the thickness of 1mm is prepared. And (3) placing the obtained sample on quartz glass for annealing in an air environment, wherein the annealing temperature is 900 ℃, and the annealing time is 10min, so that the CuO-Te material is obtained.
The resulting composite was subjected to XRD and PL characterization, the results of which are shown in fig. 4 and 5. XRD testing of FIG. 4 shows that the major diffraction peaks (110), (11-1), (111) of copper oxide are at Sb 2 Te 3 The doping anneals were all offset by 0.4 degrees to a small angle direction, indicating that Te was incorporated into the CuO lattice and was shown to be CuO: te nanocrystals. The PL test results of FIG. 5 show that the molar ratio is CuO to Sb 2 Te 3 Sample annealing of =10:1.2 gave CuO: te material exhibiting strong photoluminescence at 445nm with an intensity of about 185534, which was about 209 times higher than the pure annealed CuO.
Example 3
Mixing CuO powder with Sb 2 Te 3 The powder is fully ground and mixed according to the mol ratio of 5:1, and then a tablet press is used for tabletting under the pressure of 10MPa for 6-8 s, so that a sample with the thickness of 1mm is prepared. And (3) placing the obtained sample on quartz glass for annealing in an air environment, wherein the annealing temperature is 800 ℃, and the annealing time is 10min, so that the CuO-Te material is obtained.
The resulting composite was subjected to XRD and PL characterization, the results of which are shown in fig. 6 and 7. XRD testing of FIG. 6 shows that the major diffraction peaks (110), (11-1), (111) of copper oxide are at Sb 2 Te 3 The offset occurs after the doping annealing,te is illustrated to be incorporated into the CuO lattice and is shown as CuO: te nanocrystalline. The PL test results of FIG. 7 show that the molar ratio is CuO to Sb 2 Te 3 The sample =5:1 annealed to give a CuO: te material exhibiting strong photoluminescence at 445nm with an intensity of about 30992, which is about 35 times as strong as the pure annealed CuO.
Example 4
Mixing CuO powder with Sb 2 Te 3 The powder is fully ground and mixed according to the mol ratio of 5:1, and then a tablet press is used for tabletting under the pressure of 10MPa for 6-8 s, so that a sample with the thickness of 1mm is prepared. And (3) placing the obtained sample on quartz glass for annealing in an air environment, wherein the annealing temperature is 900 ℃, and the annealing time is 10min, so that the CuO-Te material is obtained.
The resulting composite was subjected to XRD and PL characterization, the results of which are shown in fig. 8 and 9. XRD testing of FIG. 8 shows that the major diffraction peaks (110), (11-1), (111) of copper oxide are at Sb 2 Te 3 Offset occurs after doping annealing, indicating that Te is incorporated into the CuO lattice and appears as CuO: te nanocrystals. The PL test results of FIG. 9 show that the molar ratio is CuO to Sb 2 Te 3 The sample =5:1 annealed to give a CuO: te material exhibiting strong photoluminescence at 445nm with an intensity of about 78334, which is about 88 times as strong as the pure annealed CuO.
Claims (4)
1. A CuO: te material with strong ultraviolet luminescence is characterized in that: the material is prepared by mixing CuO powder and Sb 2 Te 3 The powder is fully mixed and ground according to the mol ratio of 10:1.0-2.0, pressed into tablets, and annealed for 10-15 min at 800-900 ℃ in an air environment.
2. The CuO: te material having strong ultraviolet light emission according to claim 1, characterized in that: mixing CuO powder with Sb 2 Te 3 The powder is fully mixed and ground according to the mol ratio of 10:1.0-1.2 and then pressed into tablets.
3. The CuO: te material having strong ultraviolet light emission according to claim 1 or 2, characterized in that: the tabletting is carried out for 8-10 s under the pressure of 10-15 MPa, and the thickness of the tablet is 0.8-1.2 mm.
4. The CuO: te material having strong ultraviolet light emission according to claim 1 or 2, characterized in that: annealing for 10-15 min at 900 ℃ in the air environment.
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