CN111863986B - Cu-based semiconductor material and preparation method and application thereof - Google Patents
Cu-based semiconductor material and preparation method and application thereof Download PDFInfo
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- CN111863986B CN111863986B CN201910334093.4A CN201910334093A CN111863986B CN 111863986 B CN111863986 B CN 111863986B CN 201910334093 A CN201910334093 A CN 201910334093A CN 111863986 B CN111863986 B CN 111863986B
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- 239000000463 material Substances 0.000 title claims abstract description 61
- 239000004065 semiconductor Substances 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims description 7
- 238000010521 absorption reaction Methods 0.000 claims abstract description 26
- 239000000203 mixture Substances 0.000 claims abstract description 7
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000000843 powder Substances 0.000 claims description 32
- 238000005245 sintering Methods 0.000 claims description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 14
- 230000008569 process Effects 0.000 claims description 6
- 238000004806 packaging method and process Methods 0.000 claims description 5
- 239000010453 quartz Substances 0.000 claims description 5
- 238000009461 vacuum packaging Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 230000003287 optical effect Effects 0.000 abstract description 30
- 238000000862 absorption spectrum Methods 0.000 abstract description 11
- 239000012535 impurity Substances 0.000 abstract description 8
- 230000007704 transition Effects 0.000 abstract description 7
- 238000002474 experimental method Methods 0.000 abstract description 3
- 239000000758 substrate Substances 0.000 abstract description 3
- 230000002708 enhancing effect Effects 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 239000010949 copper Substances 0.000 description 44
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 238000004364 calculation method Methods 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 241000282414 Homo sapiens Species 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000001420 photoelectron spectroscopy Methods 0.000 description 2
- 238000001778 solid-state sintering Methods 0.000 description 2
- 238000000584 ultraviolet--visible--near infrared spectrum Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- DVRDHUBQLOKMHZ-UHFFFAOYSA-N chalcopyrite Chemical compound [S-2].[S-2].[Fe+2].[Cu+2] DVRDHUBQLOKMHZ-UHFFFAOYSA-N 0.000 description 1
- 229910052951 chalcopyrite Inorganic materials 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 230000008571 general function Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor 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
- H01L31/0248—Semiconductor 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
- H01L31/0256—Semiconductor 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
- H01L31/0264—Inorganic materials
- H01L31/032—Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312
- H01L31/0321—Inorganic 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/006—Compounds containing, besides molybdenum, two or more other elements, with the exception of oxygen or hydrogen
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor 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
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention relates to a Cu-based semiconductor material, which is characterized in thatThe Cu-based semiconductor material has a composition of Cu 3 Nb 1‑x Mo x S 4 Wherein x is more than 0 and less than or equal to 0.1 and is atomic percent, and the Cu-based semiconductor material is ternary mixed sulfide. Compared with the prior art, the invention provides the high-transparency p-type material Cu with excellent performance 3 NbS 4 As a substrate material, the electronic energy band structure of the material is regulated and controlled by doping transition element Mo, so that the purpose of enhancing the optical absorption of the material is achieved. The optical absorption spectrum measured by experiments shows that the intrinsic semiconductor can only absorb partial photons, and the optical absorption is obviously enhanced after Mo is doped. The reason for the optical enhancement is that the impurity band introduced by doping makes an electron have one more transition path, so that a new photon is absorbed. The invention greatly improves Cu 3 NbS 4 The optical absorption of the semiconductor material enables the semiconductor material to have better application prospect in the photovoltaic field.
Description
Technical Field
The invention relates to the field of semiconductor materials, in particular to a Cu-based semiconductor material and a preparation method and application thereof.
Background
With the environmental emphasis in recent years, the demand for new energy is becoming more urgent, and solar energy is becoming a new energy source to be widely used. Nowadays, solar energy has become an important component of human energy, especially the energy crisis and the environmental pollution caused by traditional energy are becoming more serious, and the pace of human solar energy exploration is accelerated. The development of clean and environment-friendly energy becomes a major problem facing human beings, and the research of solar cells is one of the important fields of scientific research in the 21 st century.
At present, the semiconductor has a wide application field, and is most prominent in the aspect of solar cells, which requires that the semiconductor material has strong optical absorption. However, the conventional semiconductor material can only absorb photons near the band gap, and the optical absorption of the semiconductor material is difficult to improve, so that the large-scale popularization and application of the semiconductor material are limited to a certain extent. The existing technology is difficult to meet the market requirement.
At the present stage, the method comprises the following steps of,the absorption layer of the solar cell has low optical absorption efficiency mainly due to the conventional semiconductor material (such as Cu) 3 NbS 4 Material) can only absorb photons near the band gap, while some photons below the band gap energy cannot be absorbed by the semiconductor and photons above the band gap are difficult to utilize. The shortage of impurity-carrying semiconductor materials and the preparation technology are not mature enough, and the development of the impurity-carrying semiconductor is hindered due to a series of problems.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a Cu-based semiconductor material, a preparation method and application thereof.
The purpose of the invention can be realized by the following technical scheme:
in order to obtain such an impurity semiconductor, the choice of the parent material and the choice of the appropriate doping element are of critical importance. Cu 3 NbS 4 The p-type transparent conductive compound is a chalcopyrite-based transparent conductive compound, has the characteristics of strong light absorption capacity, large visible light response range and the like, and is very suitable for serving as a substrate material. Through systematic experimental and theoretical research, the transition element Mo is used for doping Cu 3 NbS 4 The mother body can replace Nb site to obtain a semiconductor material with stronger optical property. Based on the characteristics, the invention obtains an improved Cu 3 NbS 4 The optical absorption method solves the problem of low optical absorption of the traditional semiconductor.
Cu 3 NbS 4 The p-type compound is a highly conductive and transparent p-type compound and has good optical absorption capacity. The invention uses transition element Mo to dope the intrinsic semiconductor Cu 3 NbS 4 So as to form a new impurity intermediate energy band in the parent band gap, and the analysis of experiment and theoretical calculation finds that the Cu can be effectively improved 3 NbS 4 The optical absorption capacity of (1).
The Cu-based semiconductor material of the present invention contains Cu as a component 3 Nb 1-x Mo x S 4 Wherein x is more than 0 and less than or equal to 0.1 and is atomic percent, and the Cu-based semiconductor material is ternary mixed sulfide.
Further onThe component of the Cu-based semiconductor material is Cu 3 Nb 0.9 Mo 0.1 S 4 。
Further, the solar energy absorption capacity of the Cu-based semiconductor material is in direct proportion to the atomic percent of Mo.
Further, the Cu 3 Nb 1-x Mo x S 4 Is a semiconductor material having an isolated half-full intermediate band.
The Cu-based semiconductor material is applied to solar cells, photon up/down converters or photocatalysts.
The preparation method of the Cu-based semiconductor material comprises the following steps:
s1: vacuum packaging Cu powder, Nb powder, S powder and Mo powder in a quartz glass tube according to a stoichiometric ratio;
s2: placing the quartz tube in a muffle furnace for sintering, wherein the sintering temperature is 800-900 ℃;
s3: and grinding the mixture into powder after sintering is finished, packaging the powder in a quartz glass tube in vacuum, and repeating the step S2 once to obtain the final Cu-based semiconductor material.
Furthermore, the sintering process comprises the steps of firstly programming the temperature to 800-900 ℃, then keeping the temperature within the range of 800-900 ℃ for 48 hours, and finally cooling to the room temperature.
Compared with the prior art, the invention firstly provides the high-transparency p-type material Cu with excellent performance 3 NbS 4 As a substrate material, the electronic energy band structure of the material is regulated and controlled by doping transition element Mo, so that the purpose of enhancing the optical absorption of the material is achieved. The optical absorption spectrum measured by experiments shows that the intrinsic semiconductor can only absorb part of photons, and the optical absorption is obviously enhanced after Mo is doped. The reason for the optical enhancement is that the doping introduces an impurity band to increase the electron to have a transition path, so that a new photon is absorbed. The invention greatly improves Cu 3 NbS 4 The optical absorption of the semiconductor material enables the semiconductor material to have better application prospect in the photovoltaic field.
Drawings
FIG. 1: cu (copper) 3 Nb 1-x Mo x S 4 XRDA map;
FIG. 2 is a schematic diagram: cu 3 Nb 1-x Mo x S 4 Ultraviolet-visible-near infrared absorption spectrum of (a);
FIG. 3: mo-doped Cu 3 NbS 4 Electron density of states map;
FIG. 4: theoretical calculated Cu 3 NbS 4 And optical absorption spectrum of Mo-doped system.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
Example 1
The material in this embodiment can be prepared by a vacuum solid state sintering reaction method, and the specific process is as follows:
s1: vacuum packaging Cu powder, Nb powder, S powder and Mo powder in a quartz glass tube according to the stoichiometric ratio of 1:0.95:4: 0.05;
s2: placing the quartz tube in a muffle furnace for sintering, wherein the sintering temperature is 800-900 ℃, the sintering process comprises the steps of firstly, heating to 800-900 ℃ in a programmed mode, then, keeping the temperature in the range of 800-900 ℃ for 48 hours, and finally, cooling to the room temperature;
s3: grinding the mixture into powder after sintering, packaging the powder in a quartz glass tube in vacuum, and repeating the step S2 once to obtain the final Cu-based semiconductor material Cu 3 Nb 0.95 Mo 0.05 S 4 。
The X-ray diffraction pattern of the material is measured by a Bruker D8ADVANCE X-ray diffractometer by using Cu Ka1 rays (0.15405nm), the scanning voltage is 40kV, and the scanning current is 40 mA. Photoelectron spectroscopy was performed on an ESCALAB 250 system and binding energy calibration was performed on a C1 s-284.6 eV basis. The UV-Vis-NIR absorption spectra of the materials were determined on a Hitachi U4100UV-Vis-NIR spectrophotometer.
Cu 3 Nb 0.95 Mo 0.05 S 4 (x ═ 0.05) the XRD pattern of the powder sample was consistent with that of the standard card, indicating that the sample was a single pure phase.
The ultraviolet-visible-near infrared absorption spectrum of the material is determined by light splitting in Hitachi U4100UV-Vis-NIRMeasured on a photometer. From Cu 3 Nb 0.95 Mo 0.05 S 4 It can be seen from the ultraviolet-visible-near infrared absorption spectrum (fig. 2) that the optical absorption after doping Mo element is significantly higher than that of the intrinsic semiconductor, thereby widening the absorption spectrum. The optical absorption capacity of the formed semiconductor is different due to different contents of Mo introduced by doping, and the optical absorption capacity is stronger than that of Cu after Mo is introduced 3 NbS 4 。
Example 2
The material in this embodiment can be prepared by a vacuum solid state sintering reaction method, and the specific process is as follows:
s1: vacuum packaging Cu powder, Nb powder, S powder and Mo powder in a quartz glass tube according to the stoichiometric ratio of 1:0.9:4: 0.1;
s2: placing the quartz tube in a muffle furnace for sintering, wherein the sintering temperature is 800-900 ℃, the sintering process comprises the steps of firstly raising the temperature to 800-900 ℃ by a program, then keeping the temperature in the range of 800-900 ℃ for 48 hours, and finally cooling to the room temperature;
s3: grinding the mixture into powder after sintering, packaging the powder in a quartz glass tube in vacuum, and repeating the step S2 once to obtain the final Cu-based semiconductor material Cu 3 Nb 0.9 Mo 0.1 S 4 。
The X-ray diffraction pattern of the material is measured by a Bruker D8ADVANCE X-ray diffractometer by using Cu Ka1 rays (0.15405nm), the scanning voltage is 40kV, and the scanning current is 40 mA. Photoelectron spectroscopy was performed on an ESCALAB 250 system and binding energy calibration was performed on a C1 s-284.6 eV basis. The UV-Vis-NIR absorption spectra of the materials were determined on a Hitachi U4100UV-Vis-NIR spectrophotometer.
Cu 3 Nb 0.9 Mo 0.1 S 4 (x ═ 0.1) the XRD pattern of the powder sample was consistent with that of the standard card, indicating that the sample was a single pure phase.
From Cu 3 Nb 0.9 Mo 0.1 S 4 It can be seen from the ultraviolet-visible-near infrared absorption spectrum (FIG. 2) that the optical absorption after doping Mo element is significantly higher than that of the intrinsic semiconductorThereby broadening the absorption spectrum. The optical absorption capacity of the formed semiconductor is different due to different contents of Mo introduced by doping, and the optical absorption capacity is stronger than that of Cu after Mo is introduced 3 Nb 0.95 Mo 0.05 S 4 。
FIG. 3 is Mo-doped Cu 3 NbS 4 Electron density of states graph. It can be seen from the figure that an intermediate band of impurities is formed in the band gap, which is mainly contributed by the electronic state of the doping element Mo-4 d.
Example 3
In the embodiment, a first principle method based on a density general function is adopted, and Cu doping of transition element Mo is calculated and simulated 3 NbS 4 Influence of electronic structure and optical absorption property, and the Mo element is found to be capable of inducing impurity energy band generation. Before calculation, a 2 × 2 × 2 super cell structure (containing 64 atoms) was first established based on its cell structure (containing 8 atoms), and Nb atoms in the cells were replaced with doping atoms such as Mo, corresponding to a doping content of 12.5%. In the calculation, GGA-PBE exchange association generic function is selected to describe the electron exchange association. And 6 multiplied by 6 Monkhorst-Pack network is adopted for K point sampling of the Brillouin zone during structure optimization. In all calculations, the plane wave cut energy was set to 400 eV.
FIG. 4 shows Cu calculated according to theory 3 NbS 4 And optical absorption spectrum of Mo-doped system. It can be seen from the absorption spectrum that the doped semiconductor has a stronger optical absorption capacity than the intrinsic semiconductor.
The reason for the enhancement of the visible optical absorption is due to the introduction of impurity bands due to the doping, in combination with example 1, example 2 and example 3. Therefore, by adding Cu 3 NbS 4 The method of doping Mo element to construct new impurity band material to enhance the optical absorption is effective.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make modifications and alterations without departing from the scope of the present invention.
Claims (5)
1. A Cu-based semiconductor material is characterized in that the component of the Cu-based semiconductor material is Cu 3 Nb x1- Mo x S 4 Wherein x is more than 0 and less than or equal to 0.1 and is atomic percent, and the Cu-based semiconductor material is ternary mixed sulfide;
the solar energy absorption capacity of the Cu-based semiconductor material is in direct proportion to the atomic percent of Mo;
the Cu 3 Nb x1- Mo x S 4 A semiconductor material having an isolated half-full intermediate band;
the preparation method of the Cu-based semiconductor material comprises the following steps:
s1: vacuum packaging Cu powder, Nb powder, S powder and Mo powder in a quartz glass tube according to a stoichiometric ratio;
s2: placing the quartz tube in a muffle furnace for sintering, wherein the sintering temperature is 800-900 ℃;
s3: and grinding the mixture into powder after sintering, packaging the powder in a quartz glass tube in vacuum, and repeating the step S2 once to obtain the final Cu-based semiconductor material.
2. The Cu-based semiconductor material according to claim 1, wherein the composition of the Cu-based semiconductor material is Cu 3 Nb 0.9 Mo 0.1 S 4 。
3. Use of a Cu-based semiconductor material as claimed in claim 1 in solar cells, photonic up/down converters.
4. A method for preparing a Cu-based semiconductor material as claimed in claim 1, characterized in that it comprises the following steps:
s1: vacuum packaging Cu powder, Nb powder, S powder and Mo powder in a quartz glass tube according to a stoichiometric ratio;
s2: placing the quartz tube in a muffle furnace for sintering, wherein the sintering temperature is 800-900 ℃;
s3: and grinding the mixture into powder after sintering is finished, packaging the powder in a quartz glass tube in vacuum, and repeating the step S2 once to obtain the final Cu-based semiconductor material.
5. The method for preparing a Cu-based semiconductor material according to claim 4, wherein the sintering process comprises the steps of firstly programming the temperature to 800-900 ℃, then keeping the temperature in the range of 800-900 ℃ for 48 hours, and finally cooling to room temperature.
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