CN117585649B - Preparation method of cadmium telluride target with excellent photoelectric property and cadmium telluride film - Google Patents
Preparation method of cadmium telluride target with excellent photoelectric property and cadmium telluride film Download PDFInfo
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- MARUHZGHZWCEQU-UHFFFAOYSA-N 5-phenyl-2h-tetrazole Chemical compound C1=CC=CC=C1C1=NNN=N1 MARUHZGHZWCEQU-UHFFFAOYSA-N 0.000 title claims abstract description 109
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000000843 powder Substances 0.000 claims abstract description 109
- YKYOUMDCQGMQQO-UHFFFAOYSA-L cadmium dichloride Chemical compound Cl[Cd]Cl YKYOUMDCQGMQQO-UHFFFAOYSA-L 0.000 claims abstract description 64
- 239000002048 multi walled nanotube Substances 0.000 claims abstract description 61
- 239000011812 mixed powder Substances 0.000 claims abstract description 51
- 239000007788 liquid Substances 0.000 claims abstract description 50
- 239000012298 atmosphere Substances 0.000 claims abstract description 45
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 claims abstract description 44
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims abstract description 38
- 229920003082 Povidone K 90 Polymers 0.000 claims abstract description 36
- 238000003756 stirring Methods 0.000 claims abstract description 33
- 239000002243 precursor Substances 0.000 claims abstract description 32
- 238000002156 mixing Methods 0.000 claims abstract description 29
- 238000010438 heat treatment Methods 0.000 claims abstract description 26
- 238000001816 cooling Methods 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 16
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000012986 modification Methods 0.000 claims abstract description 9
- 230000004048 modification Effects 0.000 claims abstract description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 66
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 claims description 66
- 239000007864 aqueous solution Substances 0.000 claims description 19
- 239000000243 solution Substances 0.000 claims description 19
- 229910052757 nitrogen Inorganic materials 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 17
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000010409 thin film Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 3
- 239000004065 semiconductor Substances 0.000 abstract description 3
- 239000013077 target material Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 30
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 26
- 229910002804 graphite Inorganic materials 0.000 description 26
- 239000010439 graphite Substances 0.000 description 26
- 238000006243 chemical reaction Methods 0.000 description 16
- 238000011068 loading method Methods 0.000 description 13
- 230000001276 controlling effect Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
- 239000013543 active substance Substances 0.000 description 2
- 239000002156 adsorbate Substances 0.000 description 2
- WLZRMCYVCSSEQC-UHFFFAOYSA-N cadmium(2+) Chemical compound [Cd+2] WLZRMCYVCSSEQC-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000010117 shenhua Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 238000009832 plasma treatment Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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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
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0623—Sulfides, selenides or tellurides
- C23C14/0629—Sulfides, selenides or tellurides of zinc, cadmium or mercury
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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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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- 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
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention belongs to the technical field of semiconductor materials, and particularly discloses a preparation method of a cadmium telluride target with excellent photoelectric performance and a cadmium telluride film, wherein the preparation method comprises the following steps: (1) Uniformly mixing tellurium powder, cadmium powder and cadmium telluride powder to obtain mixed powder; (2) Dispersing the multiwall carbon nanotube and cadmium chloride in PVP-K90 water solution, and uniformly stirring to obtain a modified liquid; (3) Adding the mixed powder into the modified liquid, uniformly stirring, carrying out ultrasonic treatment, and drying to obtain precursor powder; (4) Carrying out plasma modification treatment on the precursor powder to obtain plasma modified powder; (5) And carrying out heat treatment and cooling on the plasma modified treatment powder in a mixed atmosphere to obtain the cadmium telluride target material with excellent stability and photoelectric property.
Description
Technical Field
The invention relates to the technical field of semiconductor materials, in particular to a preparation method of a cadmium telluride target with excellent photoelectric properties and a cadmium telluride film.
Background
Cadmium telluride (CdTe) is a semiconductor material with excellent photoelectric properties, and is widely applied to the fields of solar cells, photoelectric detectors, photoelectric devices and the like. In recent years, with increasing importance on renewable energy sources and environmental protection technologies, cadmium telluride targets are increasingly widely applied to the field of solar cells.
However, the existing cadmium telluride target has some technical problems in the preparation process, such as complex preparation process, poor stability, poor photoelectric performance and the like, and the problems limit the further application and development of the cadmium telluride target. Therefore, developing a preparation method with high stability and excellent photoelectric performance has important significance for the application of the cadmium telluride target.
In view of this, the present application is presented.
Disclosure of Invention
The invention provides a preparation method of a cadmium telluride target with excellent photoelectric performance and a cadmium telluride film, which have excellent stability and photoelectric performance.
The invention solves the technical problems by adopting the following technical scheme:
a preparation method of a cadmium telluride target with excellent photoelectric properties comprises the following steps:
(1) Uniformly mixing tellurium powder, cadmium powder and cadmium telluride powder to obtain mixed powder;
(2) Dispersing the multiwall carbon nanotube and cadmium chloride in PVP-K90 water solution, and uniformly stirring to obtain a modified liquid;
(3) Adding the mixed powder into the modified liquid, uniformly stirring, carrying out ultrasonic treatment, and drying to obtain precursor powder;
(4) Carrying out plasma modification treatment on the precursor powder to obtain plasma modified powder;
(5) And carrying out heat treatment on the plasma modified treatment powder in a mixed atmosphere, and cooling to obtain the cadmium telluride target.
The invention creatively blends tellurium powder, cadmium powder and cadmium telluride powder, wherein the tellurium powder and the cadmium powder can be used as active agents, the activity of the cadmium telluride powder is regulated, the density of the cadmium telluride powder is improved, then the mixed powder is placed in a modified liquid containing multi-wall carbon nano tubes and cadmium chloride for modification treatment, the energy band structure and carrier transport property of the cadmium telluride can be changed, the influence of surface defects and adsorbates can be eliminated, the surface quality is improved, the multi-wall carbon nano tubes can be doped into pores, the density of a system is improved, the conductivity is improved, chloride ions and cadmium ions can be doped, the photoelectric performance and the stability are greatly improved, the plasma modification treatment is carried out, the stability and the density of the system can be further improved, finally the mixed powder is subjected to heat treatment, sulfide can be formed on the surface of the cadmium telluride, the surface energy band structure and the electronic state are changed, and the photoelectric performance and the stability are improved.
As a preferred embodiment of the invention, the mass ratio of the tellurium powder to the cadmium telluride powder is (10-20): (8-15): (65-80).
As a preferred embodiment of the present invention, at least one of the following (a) to (f) is satisfied:
(a) The grain size of the tellurium powder is 100-400 meshes;
(b) The purity of the tellurium powder is more than or equal to 3N;
(c) The particle size of the cadmium powder is 100-400 meshes;
(d) The purity of the cadmium powder is more than or equal to 3N;
(e) The particle size of the cadmium telluride powder is 100-400 meshes;
(f) The purity of the cadmium telluride powder is more than or equal to 3N.
As a preferred embodiment of the present invention, the mass ratio of the multi-walled carbon nanotube, cadmium chloride and PVP-K90 aqueous solution is 1: (0.5-2): (4-10).
The PVP-K90 aqueous solution contains 20-30wt% (namely solid content), and the typical PVP-K90 aqueous solution is from the high polymer material limited company of Shenhua in Huzhou, and the solid content is 25%.
As a preferred embodiment of the present invention, the multi-walled carbon nanotubes have an outer diameter of 4 to 8nm and a length of 10 to 20 μm.
As a preferred embodiment of the present invention, the mass ratio of the mixed powder to the modifying liquid is 1: (20-50).
As a preferred embodiment of the invention, the voltage of the plasma modification treatment is 220V, the power is 600-1000W, and the time is 1-5 min.
The plasma treatment is performed in a conventional plasma reaction vessel.
As a preferred embodiment of the invention, the mixed atmosphere comprises nitrogen and sulfur dioxide, and the volume ratio of the nitrogen to the sulfur dioxide is (4-8): (0.5-1).
As a preferred embodiment of the invention, the temperature of the heat treatment is 480-520 ℃ and the heat treatment time is 2-5 h.
The invention also provides a cadmium telluride film which is prepared by adopting the cadmium telluride target, and the cadmium telluride target is prepared by adopting the preparation method.
The invention has the beneficial effects that: (1) The invention creatively blends tellurium powder, cadmium powder and cadmium telluride powder, wherein the tellurium powder and the cadmium powder can be used as active agents, the activity of the cadmium telluride powder is regulated, the density of the cadmium telluride powder is improved, then the mixed powder is placed in a modified liquid containing multi-wall carbon nano tubes and cadmium chloride for modification treatment, the energy band structure and carrier transport property of the cadmium telluride can be changed, the influence of surface defects and adsorbates can be eliminated, the surface quality is improved, the multi-wall carbon nano tubes can be doped into pores, the density of a system is improved, the conductivity is improved, chloride ions and cadmium ions can be doped, the photoelectric performance and the stability are greatly improved, the plasma modification treatment is carried out, the stability and the density of the system can be further improved, finally the mixed powder is subjected to heat treatment, sulfide can be formed on the surface of the cadmium telluride, the surface energy band structure and the electronic state are changed, and the photoelectric performance and the stability are improved.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the invention, the technical characteristics described in an open mode comprise a closed technical scheme composed of the listed characteristics and also comprise an open technical scheme comprising the listed characteristics.
In the present invention, the numerical ranges are referred to as continuous, and include the minimum and maximum values of the ranges, and each value between the minimum and maximum values, unless otherwise specified. Further, when a range refers to an integer, each integer between the minimum and maximum values of the range is included. Further, when multiple range description features or characteristics are provided, the ranges may be combined. In other words, unless otherwise indicated, all ranges disclosed herein are to be understood to include any and all subranges subsumed therein.
In the present invention, the specific dispersing and stirring treatment method is not particularly limited.
The raw materials or instruments for the components used in each example and comparative example of the present invention were all commercially available raw materials or instruments unless otherwise specified, and the raw materials for the components used in each parallel experiment were all the same.
The PVP-K90 aqueous solutions of the examples and comparative examples of the present invention were derived from the high molecular materials Co., ltd. In Shenhua, huzhou, and had a solids content of 25%.
Example 1
A preparation method of a cadmium telluride target with excellent photoelectric properties comprises the following steps:
(1) The method comprises the steps of (1) mixing tellurium powder with the purity of 4N, cadmium powder with the purity of 4N and cadmium telluride powder with the purity of 4N according to the mass ratio of 15:12:73, uniformly mixing to obtain mixed powder;
wherein the grain sizes of the tellurium powder, the cadmium powder and the cadmium telluride powder are 325 meshes.
(2) Dispersing the multiwall carbon nanotube and cadmium chloride in PVP-K90 water solution, and uniformly stirring to obtain a modified liquid;
the mass ratio of the multi-wall carbon nano tube to the cadmium chloride to the PVP-K90 aqueous solution is 1:1:8, the outer diameter of the multi-wall carbon nano tube is 4-8 nm, and the length of the multi-wall carbon nano tube is 10-20 mu m;
(3) Adding the mixed powder into the modified liquid, stirring for 2 hours at 500rpm, performing ultrasonic treatment at 500W for 30 minutes, and drying to obtain precursor powder;
the mass ratio of the mixed powder to the modified liquid is 1:40.
(4) Placing the precursor powder into a plasma reaction container, treating for 3min under the plasma with the power of 800W at the voltage of 220V and the normal temperature and the normal pressure (one atmosphere pressure), and taking out to obtain plasma modified treatment powder;
(5) And (3) loading the plasma modified treatment powder into a graphite boat, then putting the graphite boat into a tube furnace, performing heat treatment for 4 hours at 500 ℃ under a mixed atmosphere, and cooling to obtain the cadmium telluride target.
The mixed atmosphere comprises nitrogen and sulfur dioxide, and the volume ratio of the nitrogen to the sulfur dioxide is 7:0.5.
example 2
A preparation method of a cadmium telluride target with excellent photoelectric properties comprises the following steps:
(1) The method comprises the steps of (1) mixing tellurium powder with the purity of 4N, cadmium powder with the purity of 4N and cadmium telluride powder with the purity of 4N according to the mass ratio of 20:15:65, uniformly mixing to obtain mixed powder;
wherein the grain sizes of the tellurium powder, the cadmium powder and the cadmium telluride powder are all 100 meshes.
(2) Dispersing the multiwall carbon nanotube and cadmium chloride in PVP-K90 water solution, and uniformly stirring to obtain a modified liquid;
the mass ratio of the multi-wall carbon nano tube to the cadmium chloride to the PVP-K90 aqueous solution is 1:1:8, the outer diameter of the multi-wall carbon nano tube is 4-8 nm, and the length of the multi-wall carbon nano tube is 10-20 mu m;
(3) Adding the mixed powder into the modified liquid, stirring for 2 hours at 500rpm, performing ultrasonic treatment at 500W for 30 minutes, and drying to obtain precursor powder;
the mass ratio of the mixed powder to the modified liquid is 1:40.
(4) Placing the precursor powder into a plasma reaction container, treating for 3min under the plasma with the power of 800W at the voltage of 220V and the normal temperature and the normal pressure (one atmosphere pressure), and taking out to obtain plasma modified treatment powder;
(5) And (3) loading the plasma modified treatment powder into a graphite boat, then putting the graphite boat into a tube furnace, performing heat treatment for 4 hours at 500 ℃ under a mixed atmosphere, and cooling to obtain the cadmium telluride target.
The mixed atmosphere comprises nitrogen and sulfur dioxide, and the volume ratio of the nitrogen to the sulfur dioxide is 7:0.5.
example 3
A preparation method of a cadmium telluride target with excellent photoelectric properties comprises the following steps:
(1) The method comprises the steps of (1) mixing tellurium powder with the purity of 4N, cadmium powder with the purity of 4N and cadmium telluride powder with the purity of 4N according to the mass ratio of 10:10:80, uniformly mixing to obtain mixed powder;
wherein the grain sizes of the tellurium powder, the cadmium powder and the cadmium telluride powder are 400 meshes.
(2) Dispersing the multiwall carbon nanotube and cadmium chloride in PVP-K90 water solution, and uniformly stirring to obtain a modified liquid;
the mass ratio of the multi-wall carbon nano tube to the cadmium chloride to the PVP-K90 aqueous solution is 1:1:8, the outer diameter of the multi-wall carbon nano tube is 4-8 nm, and the length of the multi-wall carbon nano tube is 10-20 mu m;
(3) Adding the mixed powder into the modified liquid, stirring for 2 hours at 500rpm, performing ultrasonic treatment at 500W for 30 minutes, and drying to obtain precursor powder;
the mass ratio of the mixed powder to the modified liquid is 1:40.
(4) Placing the precursor powder into a plasma reaction container, treating for 3min under the plasma with the power of 800W at the voltage of 220V and the normal temperature and the normal pressure (one atmosphere pressure), and taking out to obtain plasma modified treatment powder;
(5) And (3) loading the plasma modified treatment powder into a graphite boat, then putting the graphite boat into a tube furnace, performing heat treatment for 4 hours at 500 ℃ under a mixed atmosphere, and cooling to obtain the cadmium telluride target.
The mixed atmosphere comprises nitrogen and sulfur dioxide, and the volume ratio of the nitrogen to the sulfur dioxide is 7:0.5.
example 4
A preparation method of a cadmium telluride target with excellent photoelectric properties comprises the following steps:
(1) The method comprises the steps of (1) mixing tellurium powder with the purity of 4N, cadmium powder with the purity of 4N and cadmium telluride powder with the purity of 4N according to the mass ratio of 15:12:73, uniformly mixing to obtain mixed powder;
wherein the grain sizes of the tellurium powder, the cadmium powder and the cadmium telluride powder are 325 meshes.
(2) Dispersing the multiwall carbon nanotube and cadmium chloride in PVP-K90 water solution, and uniformly stirring to obtain a modified liquid;
the mass ratio of the multi-wall carbon nano tube to the cadmium chloride to the PVP-K90 aqueous solution is 1:0.5:4, the outer diameter of the multi-wall carbon nano tube is 4-8 nm, and the length of the multi-wall carbon nano tube is 10-20 mu m;
(3) Adding the mixed powder into the modified liquid, stirring for 2 hours at 500rpm, performing ultrasonic treatment at 500W for 30 minutes, and drying to obtain precursor powder;
the mass ratio of the mixed powder to the modified liquid is 1:40.
(4) Placing the precursor powder into a plasma reaction container, treating for 3min under the plasma with the power of 800W at the voltage of 220V and the normal temperature and the normal pressure (one atmosphere pressure), and taking out to obtain plasma modified treatment powder;
(5) And (3) loading the plasma modified treatment powder into a graphite boat, then putting the graphite boat into a tube furnace, performing heat treatment for 4 hours at 500 ℃ under a mixed atmosphere, and cooling to obtain the cadmium telluride target.
The mixed atmosphere comprises nitrogen and sulfur dioxide, and the volume ratio of the nitrogen to the sulfur dioxide is 7:0.5.
example 5
A preparation method of a cadmium telluride target with excellent photoelectric properties comprises the following steps:
(1) The method comprises the steps of (1) mixing tellurium powder with the purity of 4N, cadmium powder with the purity of 4N and cadmium telluride powder with the purity of 4N according to the mass ratio of 15:12:73, uniformly mixing to obtain mixed powder;
wherein the grain sizes of the tellurium powder, the cadmium powder and the cadmium telluride powder are 325 meshes.
(2) Dispersing the multiwall carbon nanotube and cadmium chloride in PVP-K90 water solution, and uniformly stirring to obtain a modified liquid;
the mass ratio of the multi-wall carbon nano tube to the cadmium chloride to the PVP-K90 aqueous solution is 1:2:10, wherein the outer diameter of the multi-wall carbon nano tube is 4-8 nm, and the length is 10-20 mu m;
(3) Adding the mixed powder into the modified liquid, stirring for 2 hours at 500rpm, performing ultrasonic treatment at 500W for 30 minutes, and drying to obtain precursor powder;
the mass ratio of the mixed powder to the modified liquid is 1:40.
(4) Placing the precursor powder into a plasma reaction container, treating for 3min under the plasma with the power of 800W at the voltage of 220V and the normal temperature and the normal pressure (one atmosphere pressure), and taking out to obtain plasma modified treatment powder;
(5) And (3) loading the plasma modified treatment powder into a graphite boat, then putting the graphite boat into a tube furnace, performing heat treatment for 4 hours at 500 ℃ under a mixed atmosphere, and cooling to obtain the cadmium telluride target.
The mixed atmosphere comprises nitrogen and sulfur dioxide, and the volume ratio of the nitrogen to the sulfur dioxide is 7:0.5.
example 6
A preparation method of a cadmium telluride target with excellent photoelectric properties comprises the following steps:
(1) The method comprises the steps of (1) mixing tellurium powder with the purity of 4N, cadmium powder with the purity of 4N and cadmium telluride powder with the purity of 4N according to the mass ratio of 15:12:73, uniformly mixing to obtain mixed powder;
wherein the grain sizes of the tellurium powder, the cadmium powder and the cadmium telluride powder are 325 meshes.
(2) Dispersing the multiwall carbon nanotube and cadmium chloride in PVP-K90 water solution, and uniformly stirring to obtain a modified liquid;
the mass ratio of the multi-wall carbon nano tube to the cadmium chloride to the PVP-K90 aqueous solution is 1:1:8, the outer diameter of the multi-wall carbon nano tube is 4-8 nm, and the length of the multi-wall carbon nano tube is 10-20 mu m;
(3) Adding the mixed powder into the modified liquid, stirring for 2 hours at 500rpm, performing ultrasonic treatment at 500W for 30 minutes, and drying to obtain precursor powder;
the mass ratio of the mixed powder to the modified liquid is 1:20.
(4) Placing the precursor powder into a plasma reaction container, treating for 3min under the plasma with the power of 800W at the voltage of 220V and the normal temperature and the normal pressure (one atmosphere pressure), and taking out to obtain plasma modified treatment powder;
(5) And (3) loading the plasma modified treatment powder into a graphite boat, then putting the graphite boat into a tube furnace, performing heat treatment for 4 hours at 500 ℃ under a mixed atmosphere, and cooling to obtain the cadmium telluride target.
The mixed atmosphere comprises nitrogen and sulfur dioxide, and the volume ratio of the nitrogen to the sulfur dioxide is 7:0.5.
example 7
A preparation method of a cadmium telluride target with excellent photoelectric properties comprises the following steps:
(1) The method comprises the steps of (1) mixing tellurium powder with the purity of 4N, cadmium powder with the purity of 4N and cadmium telluride powder with the purity of 4N according to the mass ratio of 15:12:73, uniformly mixing to obtain mixed powder;
wherein the grain sizes of the tellurium powder, the cadmium powder and the cadmium telluride powder are 325 meshes.
(2) Dispersing the multiwall carbon nanotube and cadmium chloride in PVP-K90 water solution, and uniformly stirring to obtain a modified liquid;
the mass ratio of the multi-wall carbon nano tube to the cadmium chloride to the PVP-K90 aqueous solution is 1:1:8, the outer diameter of the multi-wall carbon nano tube is 4-8 nm, and the length of the multi-wall carbon nano tube is 10-20 mu m;
(3) Adding the mixed powder into the modified liquid, stirring for 2 hours at 500rpm, performing ultrasonic treatment at 500W for 30 minutes, and drying to obtain precursor powder;
the mass ratio of the mixed powder to the modified liquid is 1:50.
(4) Placing the precursor powder into a plasma reaction container, treating for 3min under the plasma with the power of 800W at the voltage of 220V and the normal temperature and the normal pressure (one atmosphere pressure), and taking out to obtain plasma modified treatment powder;
(5) And (3) loading the plasma modified treatment powder into a graphite boat, then putting the graphite boat into a tube furnace, performing heat treatment for 4 hours at 500 ℃ under a mixed atmosphere, and cooling to obtain the cadmium telluride target.
The mixed atmosphere comprises nitrogen and sulfur dioxide, and the volume ratio of the nitrogen to the sulfur dioxide is 7:0.5.
example 8
A preparation method of a cadmium telluride target with excellent photoelectric properties comprises the following steps:
(1) The method comprises the steps of (1) mixing tellurium powder with the purity of 4N, cadmium powder with the purity of 4N and cadmium telluride powder with the purity of 4N according to the mass ratio of 15:12:73, uniformly mixing to obtain mixed powder;
wherein the grain sizes of the tellurium powder, the cadmium powder and the cadmium telluride powder are 325 meshes.
(2) Dispersing the multiwall carbon nanotube and cadmium chloride in PVP-K90 water solution, and uniformly stirring to obtain a modified liquid;
the mass ratio of the multi-wall carbon nano tube to the cadmium chloride to the PVP-K90 aqueous solution is 1:1:8, the outer diameter of the multi-wall carbon nano tube is 4-8 nm, and the length of the multi-wall carbon nano tube is 10-20 mu m;
(3) Adding the mixed powder into the modified liquid, stirring for 2 hours at 500rpm, performing ultrasonic treatment at 500W for 30 minutes, and drying to obtain precursor powder;
the mass ratio of the mixed powder to the modified liquid is 1:40.
(4) Placing the precursor powder into a plasma reaction container, treating for 3min under the plasma with the power of 800W at the voltage of 220V and the normal temperature and the normal pressure (one atmosphere pressure), and taking out to obtain plasma modified treatment powder;
(5) And (3) loading the plasma modified treatment powder into a graphite boat, then putting the graphite boat into a tube furnace, performing heat treatment for 5 hours at 480 ℃ in a mixed atmosphere, and cooling to obtain the cadmium telluride target.
The mixed atmosphere comprises nitrogen and sulfur dioxide, and the volume ratio of the nitrogen to the sulfur dioxide is 7:0.5.
example 9
A preparation method of a cadmium telluride target with excellent photoelectric properties comprises the following steps:
(1) The method comprises the steps of (1) mixing tellurium powder with the purity of 4N, cadmium powder with the purity of 4N and cadmium telluride powder with the purity of 4N according to the mass ratio of 15:12:73, uniformly mixing to obtain mixed powder;
wherein the grain sizes of the tellurium powder, the cadmium powder and the cadmium telluride powder are 325 meshes.
(2) Dispersing the multiwall carbon nanotube and cadmium chloride in PVP-K90 water solution, and uniformly stirring to obtain a modified liquid;
the mass ratio of the multi-wall carbon nano tube to the cadmium chloride to the PVP-K90 aqueous solution is 1:1:8, the outer diameter of the multi-wall carbon nano tube is 4-8 nm, and the length of the multi-wall carbon nano tube is 10-20 mu m;
(3) Adding the mixed powder into the modified liquid, stirring for 2 hours at 500rpm, performing ultrasonic treatment at 500W for 30 minutes, and drying to obtain precursor powder;
the mass ratio of the mixed powder to the modified liquid is 1:40.
(4) Placing the precursor powder into a plasma reaction container, treating for 3min under the plasma with the power of 800W at the voltage of 220V and the normal temperature and the normal pressure (one atmosphere pressure), and taking out to obtain plasma modified treatment powder;
(5) And (3) loading the plasma modified treatment powder into a graphite boat, then putting the graphite boat into a tube furnace, performing heat treatment for 2 hours at 520 ℃ in a mixed atmosphere, and cooling to obtain the cadmium telluride target.
The mixed atmosphere comprises nitrogen and sulfur dioxide, and the volume ratio of the nitrogen to the sulfur dioxide is 7:0.5.
example 10
A preparation method of a cadmium telluride target with excellent photoelectric properties comprises the following steps:
(1) The method comprises the steps of (1) mixing tellurium powder with the purity of 4N, cadmium powder with the purity of 4N and cadmium telluride powder with the purity of 4N according to the mass ratio of 15:12:73, uniformly mixing to obtain mixed powder;
wherein the grain sizes of the tellurium powder, the cadmium powder and the cadmium telluride powder are 325 meshes.
(2) Dispersing the multiwall carbon nanotube and cadmium chloride in PVP-K90 water solution, and uniformly stirring to obtain a modified liquid;
the mass ratio of the multi-wall carbon nano tube to the cadmium chloride to the PVP-K90 aqueous solution is 1:1:8, the outer diameter of the multi-wall carbon nano tube is 4-8 nm, and the length of the multi-wall carbon nano tube is 10-20 mu m;
(3) Adding the mixed powder into the modified liquid, stirring for 2 hours at 500rpm, performing ultrasonic treatment at 500W for 30 minutes, and drying to obtain precursor powder;
the mass ratio of the mixed powder to the modified liquid is 1:40.
(4) Placing the precursor powder into a plasma reaction container, treating for 3min under the plasma with the power of 800W at the voltage of 220V and the normal temperature and the normal pressure (one atmosphere pressure), and taking out to obtain plasma modified treatment powder;
(5) And (3) loading the plasma modified treatment powder into a graphite boat, then putting the graphite boat into a tube furnace, performing heat treatment for 4 hours at 500 ℃ under a mixed atmosphere, and cooling to obtain the cadmium telluride target.
The mixed atmosphere comprises nitrogen and sulfur dioxide, and the volume ratio of the nitrogen to the sulfur dioxide is 4:1.
example 11
A preparation method of a cadmium telluride target with excellent photoelectric properties comprises the following steps:
(1) The method comprises the steps of (1) mixing tellurium powder with the purity of 4N, cadmium powder with the purity of 4N and cadmium telluride powder with the purity of 4N according to the mass ratio of 15:12:73, uniformly mixing to obtain mixed powder;
wherein the grain sizes of the tellurium powder, the cadmium powder and the cadmium telluride powder are 325 meshes.
(2) Dispersing the multiwall carbon nanotube and cadmium chloride in PVP-K90 water solution, and uniformly stirring to obtain a modified liquid;
the mass ratio of the multi-wall carbon nano tube to the cadmium chloride to the PVP-K90 aqueous solution is 1:1:8, the outer diameter of the multi-wall carbon nano tube is 4-8 nm, and the length of the multi-wall carbon nano tube is 10-20 mu m;
(3) Adding the mixed powder into the modified liquid, stirring for 2 hours at 500rpm, performing ultrasonic treatment at 500W for 30 minutes, and drying to obtain precursor powder;
the mass ratio of the mixed powder to the modified liquid is 1:40.
(4) Placing the precursor powder into a plasma reaction container, treating for 3min under the plasma with the power of 800W at the voltage of 220V and the normal temperature and the normal pressure (one atmosphere pressure), and taking out to obtain plasma modified treatment powder;
(5) And (3) loading the plasma modified treatment powder into a graphite boat, then putting the graphite boat into a tube furnace, performing heat treatment for 4 hours at 500 ℃ under a mixed atmosphere, and cooling to obtain the cadmium telluride target.
The mixed atmosphere comprises nitrogen and sulfur dioxide, and the volume ratio of the nitrogen to the sulfur dioxide is 8:0.5.
comparative example 1
Comparative example 1 is different from example 1 in that the mass ratio of tellurium powder having a purity of 4N, cadmium telluride powder having a purity of 4N is different, and the other are the same.
The mass ratio of the tellurium powder with the purity of 4N to the cadmium telluride powder with the purity of 4N is 5:5:90.
comparative example 2
Comparative example 2 is different from example 1 in that the mass ratio of tellurium powder having a purity of 4N, cadmium telluride powder having a purity of 4N is different, and the other are the same.
The mass ratio of the tellurium powder with the purity of 4N to the cadmium telluride powder with the purity of 4N is 30:20:50.
comparative example 3
A preparation method of a cadmium telluride target with excellent photoelectric properties comprises the following steps:
(1) The method comprises the steps of (1) mixing tellurium powder with the purity of 4N, cadmium powder with the purity of 4N and cadmium telluride powder with the purity of 4N according to the mass ratio of 15:12:73, uniformly mixing to obtain mixed powder;
wherein the grain sizes of the tellurium powder, the cadmium powder and the cadmium telluride powder are 325 meshes.
(2) Dispersing cadmium chloride in PVP-K90 water solution, and uniformly stirring to obtain modified liquid;
the mass ratio of the cadmium chloride to the PVP-K90 aqueous solution is 1:8, the outer diameter of the multi-wall carbon nano tube is 4-8 nm, and the length of the multi-wall carbon nano tube is 10-20 mu m;
(3) Adding the mixed powder into the modified liquid, stirring for 2 hours at 500rpm, performing ultrasonic treatment at 500W for 30 minutes, and drying to obtain precursor powder;
the mass ratio of the mixed powder to the modified liquid is 1:40.
(4) Placing the precursor powder into a plasma reaction container, treating for 3min under the plasma with the power of 800W at the voltage of 220V and the normal temperature and the normal pressure (one atmosphere pressure), and taking out to obtain plasma modified treatment powder;
(5) And (3) loading the plasma modified treatment powder into a graphite boat, then putting the graphite boat into a tube furnace, performing heat treatment for 4 hours at 500 ℃ under a mixed atmosphere, and cooling to obtain the cadmium telluride target.
The mixed atmosphere comprises nitrogen and sulfur dioxide, and the volume ratio of the nitrogen to the sulfur dioxide is 7:0.5.
comparative example 4
A preparation method of a cadmium telluride target with excellent photoelectric properties comprises the following steps:
(1) The method comprises the steps of (1) mixing tellurium powder with the purity of 4N, cadmium powder with the purity of 4N and cadmium telluride powder with the purity of 4N according to the mass ratio of 15:12:73, uniformly mixing to obtain mixed powder;
wherein the grain sizes of the tellurium powder, the cadmium powder and the cadmium telluride powder are 325 meshes.
(2) Dispersing the multi-wall carbon nano tube in PVP-K90 water solution, and uniformly stirring to obtain modified liquid;
the mass ratio of the multi-wall carbon nano tube to the PVP-K90 aqueous solution is 1:8, the outer diameter of the multi-wall carbon nano tube is 4-8 nm, and the length of the multi-wall carbon nano tube is 10-20 mu m;
(3) Adding the mixed powder into the modified liquid, stirring for 2 hours at 500rpm, performing ultrasonic treatment at 500W for 30 minutes, and drying to obtain precursor powder;
the mass ratio of the mixed powder to the modified liquid is 1:40.
(4) Placing the precursor powder into a plasma reaction container, treating for 3min under the plasma with the power of 800W at the voltage of 220V and the normal temperature and the normal pressure (one atmosphere pressure), and taking out to obtain plasma modified treatment powder;
(5) And (3) loading the plasma modified treatment powder into a graphite boat, then putting the graphite boat into a tube furnace, performing heat treatment for 4 hours at 500 ℃ under a mixed atmosphere, and cooling to obtain the cadmium telluride target.
The mixed atmosphere comprises nitrogen and sulfur dioxide, and the volume ratio of the nitrogen to the sulfur dioxide is 7:0.5.
comparative example 5
Comparative example 5 is different from example 1 in that the heat treatment temperature of comparative example 5 is 400 deg.c, and the other are the same.
Comparative example 6
Comparative example 6 is different from example 1 in that the heat treatment temperature of comparative example 6 is 600 c, and the other are the same.
Comparative example 7
Comparative example 7 is different from example 1 in that comparative example 7 uses nitrogen instead of the mixed atmosphere, i.e., this comparative example is subjected to heat treatment under nitrogen atmosphere, and all other things are the same.
Comparative example 8
Comparative example 8 differs from example 1 in that the volume ratio of nitrogen to sulfur dioxide of comparative example 8 is 2:1, all others being identical.
Comparative example 9
Comparative example 9 differs from example 1 in that the volume ratio of nitrogen to sulfur dioxide of comparative example 9 is 4:0.2, all others being identical.
Test case
The photoelectric output performance of the solar cell with the FTO glass/cadmium telluride/Au structure is tested.
Wherein cadmium telluride is respectively prepared in examples and comparative examples, and 100mW/cm is adopted in the experimental process 2 The solar simulator (Newport) am1.5g was run under light and the solar cell was left at 45 ℃ for 2 weeks, again detecting the photoelectric conversion.
TABLE 1
As can be seen from Table 1, the cadmium telluride target material has excellent stability and photoelectric properties.
As can be seen from comparative examples 1 to 11, example 1 is the best mode for carrying out the present invention, and has the best stability and photoelectric conversion performance.
As can be seen from comparative examples 1 and 1-2, the stability and the photoelectric performance of the invention are obviously improved by controlling the mass ratio of tellurium powder, cadmium powder and cadmium telluride.
As can be seen from comparative examples 1 and 3-4, the stability and the photoelectric performance of the invention are remarkably improved by adding the multiwall carbon nanotube and the cadmium chloride into the modified liquid.
As can be seen from comparative examples 1 and 5-6, the stability and photoelectric properties of the invention are remarkably improved by controlling the heat treatment temperature.
As can be seen from comparative examples 1 and 7-9, the invention remarkably improves the stability and the photoelectric performance by adding sulfur dioxide gas and controlling the addition amount thereof.
Finally, it should be noted that the above-mentioned embodiments illustrate rather than limit the scope of the invention, and that those skilled in the art will understand that changes can be made to the technical solutions of the invention or equivalents thereof without departing from the spirit and scope of the technical solutions of the invention.
Claims (5)
1. The preparation method of the cadmium telluride target with excellent photoelectric performance is characterized by comprising the following steps of:
(1) Uniformly mixing tellurium powder, cadmium powder and cadmium telluride powder to obtain mixed powder;
(2) Dispersing the multiwall carbon nanotube and cadmium chloride in PVP-K90 water solution, and uniformly stirring to obtain a modified liquid;
(3) Adding the mixed powder into the modified liquid, uniformly stirring, carrying out ultrasonic treatment, and drying to obtain precursor powder;
(4) Carrying out plasma modification treatment on the precursor powder to obtain plasma modified powder;
(5) Carrying out heat treatment on the plasma modified treatment powder in a mixed atmosphere, and cooling to obtain a cadmium telluride target;
the mass ratio of the tellurium powder to the cadmium telluride powder is (10-20): (8-15): (65-80);
the mass ratio of the multi-wall carbon nano tube to the cadmium chloride to the PVP-K90 aqueous solution is 1: (0.5-2): (4-10);
the PVP-K90 content in the PVP-K90 aqueous solution is 20-30wt%;
the mass ratio of the mixed powder to the modified liquid is 1: (20-50);
the mixed atmosphere comprises nitrogen and sulfur dioxide, wherein the volume ratio of the nitrogen to the sulfur dioxide is (4-8): (0.5-1);
the temperature of the heat treatment is 480-520 ℃, and the heat treatment time is 2-5 h.
2. The method for producing a cadmium telluride target having excellent photoelectric properties according to claim 1, wherein at least one of the following (a) to (f) is satisfied:
(a) The grain size of the tellurium powder is 100-400 meshes;
(b) The purity of the tellurium powder is more than or equal to 3N;
(c) The particle size of the cadmium powder is 100-400 meshes;
(d) The purity of the cadmium powder is more than or equal to 3N;
(e) The particle size of the cadmium telluride powder is 100-400 meshes;
(f) The purity of the cadmium telluride powder is more than or equal to 3N.
3. The method for preparing the cadmium telluride target with excellent photoelectric properties according to claim 1, wherein the multi-wall carbon nanotubes have an outer diameter of 4-8 nm and a length of 10-20 μm.
4. The method for preparing the cadmium telluride target with excellent photoelectric properties according to claim 1, wherein the voltage of the plasma modification treatment is 220V, the power is 600-1000W, and the time is 1-5 min.
5. The cadmium telluride thin film is characterized by being prepared from a cadmium telluride target, and the cadmium telluride target is prepared by the preparation method of any one of claims 1-4.
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| KR20120050279A (en) * | 2010-11-10 | 2012-05-18 | 동의대학교 산학협력단 | Multi-walled carbon nanotubes composites with cadmium telluride nanoparticles and preparation method thereof |
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| CN114956823A (en) * | 2022-05-27 | 2022-08-30 | 先导薄膜材料（广东）有限公司 | Preparation method of conductive cadmium telluride target |
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| KR20120050279A (en) * | 2010-11-10 | 2012-05-18 | 동의대학교 산학협력단 | Multi-walled carbon nanotubes composites with cadmium telluride nanoparticles and preparation method thereof |
| CN107104158A (en) * | 2017-06-15 | 2017-08-29 | 绍兴文理学院 | A kind of preparation method of doping CdTe nano photovoltaic materials |
| CN109065665A (en) * | 2018-06-28 | 2018-12-21 | 华南理工大学 | A kind of miniature carving etching method of cadmium telluride nano-crystal film |
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