CN107248534B - A kind of semiconducting alloy film of ingredient continuous gradation and its preparation method and application - Google Patents
A kind of semiconducting alloy film of ingredient continuous gradation and its preparation method and application Download PDFInfo
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- CN107248534B CN107248534B CN201710387303.7A CN201710387303A CN107248534B CN 107248534 B CN107248534 B CN 107248534B CN 201710387303 A CN201710387303 A CN 201710387303A CN 107248534 B CN107248534 B CN 107248534B
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- 239000000956 alloy Substances 0.000 title claims abstract description 85
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 81
- 239000004615 ingredient Substances 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 238000001704 evaporation Methods 0.000 claims abstract description 73
- 230000008020 evaporation Effects 0.000 claims abstract description 70
- 239000011669 selenium Substances 0.000 claims abstract description 61
- 239000000758 substrate Substances 0.000 claims abstract description 41
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910052711 selenium Inorganic materials 0.000 claims abstract description 25
- ZQRRBZZVXPVWRB-UHFFFAOYSA-N [S].[Se] Chemical compound [S].[Se] ZQRRBZZVXPVWRB-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229940065287 selenium compound Drugs 0.000 claims abstract description 6
- 230000008021 deposition Effects 0.000 claims abstract description 4
- 239000011521 glass Substances 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 15
- 239000004065 semiconductor Substances 0.000 claims description 14
- 239000005357 flat glass Substances 0.000 claims description 10
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims description 8
- 238000012545 processing Methods 0.000 claims description 8
- 239000000919 ceramic Substances 0.000 claims description 7
- 150000003346 selenoethers Chemical class 0.000 claims description 7
- 238000002207 thermal evaporation Methods 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 6
- 239000010439 graphite Substances 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 5
- 239000005864 Sulphur Substances 0.000 claims description 5
- 229940007424 antimony trisulfide Drugs 0.000 claims description 5
- NVWBARWTDVQPJD-UHFFFAOYSA-N antimony(3+);trisulfide Chemical compound [S-2].[S-2].[S-2].[Sb+3].[Sb+3] NVWBARWTDVQPJD-UHFFFAOYSA-N 0.000 claims description 5
- OQRNKLRIQBVZHK-UHFFFAOYSA-N selanylideneantimony Chemical compound [Sb]=[Se] OQRNKLRIQBVZHK-UHFFFAOYSA-N 0.000 claims description 5
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 3
- 238000000151 deposition Methods 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- IBEWGOCMLWIGCZ-UHFFFAOYSA-N [Bi]=S.[Se] Chemical class [Bi]=S.[Se] IBEWGOCMLWIGCZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 2
- 238000005137 deposition process Methods 0.000 claims description 2
- 238000005070 sampling Methods 0.000 claims description 2
- OMEPJWROJCQMMU-UHFFFAOYSA-N selanylidenebismuth;selenium Chemical compound [Se].[Bi]=[Se].[Bi]=[Se] OMEPJWROJCQMMU-UHFFFAOYSA-N 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 238000012544 monitoring process Methods 0.000 claims 1
- 239000010408 film Substances 0.000 abstract description 62
- 238000000034 method Methods 0.000 abstract description 31
- 239000010409 thin film Substances 0.000 abstract description 5
- 239000000203 mixture Substances 0.000 description 13
- 238000010438 heat treatment Methods 0.000 description 12
- 230000008569 process Effects 0.000 description 12
- 239000010931 gold Substances 0.000 description 10
- 239000000463 material Substances 0.000 description 9
- 239000000523 sample Substances 0.000 description 8
- 238000010586 diagram Methods 0.000 description 7
- 229910052737 gold Inorganic materials 0.000 description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- 230000008859 change Effects 0.000 description 5
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 5
- 238000012546 transfer Methods 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 4
- 229910017083 AlN Inorganic materials 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 238000010025 steaming Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 241001148715 Lamarckia aurea Species 0.000 description 2
- NNLOHLDVJGPUFR-UHFFFAOYSA-L calcium;3,4,5,6-tetrahydroxy-2-oxohexanoate Chemical compound [Ca+2].OCC(O)C(O)C(O)C(=O)C([O-])=O.OCC(O)C(O)C(O)C(=O)C([O-])=O NNLOHLDVJGPUFR-UHFFFAOYSA-L 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- MUYUEDVRJJRNOO-UHFFFAOYSA-N selanylidene(sulfanylidene)antimony Chemical compound S=[Sb]=[Se] MUYUEDVRJJRNOO-UHFFFAOYSA-N 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000005619 thermoelectricity Effects 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 229910001370 Se alloy Inorganic materials 0.000 description 1
- 241000501540 Senegalia interior Species 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910000905 alloy phase Inorganic materials 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 230000000740 bleeding effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005202 decontamination Methods 0.000 description 1
- 230000003588 decontaminative effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 208000021760 high fever Diseases 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005118 spray pyrolysis Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- H01L31/0272—Selenium or tellurium
- H01L31/02725—Selenium or tellurium characterised by the doping material
-
- 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
- H01L31/02—Details
- H01L31/0216—Coatings
-
- 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
- H01L31/02—Details
- H01L31/0216—Coatings
- H01L31/02161—Coatings for devices characterised by at least one potential jump barrier or surface barrier
- H01L31/02167—Coatings for devices characterised by at least one potential jump barrier or surface barrier for solar cells
-
- 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
- H01L31/0296—Inorganic materials including, apart from doping material or other impurities, only AIIBVI compounds, e.g. CdS, ZnS, HgCdTe
- H01L31/02963—Inorganic materials including, apart from doping material or other impurities, only AIIBVI compounds, e.g. CdS, ZnS, HgCdTe characterised by the doping material
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
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- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Computer Hardware Design (AREA)
- Power Engineering (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Electromagnetism (AREA)
- General Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Sustainable Development (AREA)
- Life Sciences & Earth Sciences (AREA)
- Sustainable Energy (AREA)
- Physical Vapour Deposition (AREA)
- Physical Deposition Of Substances That Are Components Of Semiconductor Devices (AREA)
Abstract
The invention discloses a kind of semiconducting alloy films of ingredient continuous gradation and its preparation method and application, and the feature of the wherein film has：Film be ternary sulphur selenium compound alloy, selenium ingredient X-direction can continuous gradation, be basically unchanged in Y direction and Z-direction；The semiconducting alloy film of the ingredient continuous gradation is used for thin-film solar cells array and photodetector as good light absorbing layer.Preparation method includes：(1) deposition substrate is chosen；(2) prepare evaporation source；(3) semiconducting alloy film is prepared.Method proposed by the present invention can deposit the semiconducting alloy film of a wide range of consecutive variations of ingredient under identical conditions, and film speed is fast, and technique is convenient, it is easy to accomplish, it is reliable and stable, it has wide range of applications.
Description
Technical field
The invention belongs to semiconductor film material technical fields, and in particular, to a kind of ingredient continuous gradation semiconductor conjunction
The preparation method and application of gold thin film.
Background technology
Semiconducting alloy thin-film material is rapidly progressed and is widely used in photodetector and solar-electricity
Chi Zhong.This kind of material is (such as：Antimony sulphur selenium, bismuth sulphur selenium etc.) major advantage be that there is controllable optical band gap and electric property, energy
Enough good match spectrum characteristics.Such as antimony sulphur selenium alloy (Sb2(SexS1-x)3) the advantages of combining monomer material while also gram
The deficiency of band gap is taken, it has big absorption coefficient, and band gap can be adjusted from 1.1eV to 1.7eV by changing its ingredient.However half
Influence of the composition transfer of conductor alloy to device performance is huge, and the preparation method of the alloy of heterogeneity needs to continue to develop.
Currently, the preparation method of semiconducting alloy based on solwution method, adjusts a kind of ingredient, workload is heavy, and is easy out every time
Existing accidental error.Therefore, being with the semiconducting alloy film for preparing continuous component continuous gradation of condition simultaneously disposably must
It wants.In order to probe into influence of the alloying component variation to physical characteristic and device performance, high-throughput preparation method is development
Trend.
Invention content
Present invention seek to address that the technical problems existing in the prior art, it is proposed that a kind of semiconductor of ingredient continuous gradation
Alloy firm and its preparation method and application.
Purpose according to the invention provides a kind of semiconducting alloy film of ingredient continuous gradation, the semiconducting alloy
The ingredient of film is ternary sulphur selenium compound；Note is located on the semiconducting alloy film surface and semiconductor closes in the direction
The direction that the selenium element content on gold thin film surface remains unchanged is Y direction, remembers that the thickness direction of the semiconducting alloy film is Z
Axis direction, and note is located on the semiconducting alloy film surface and the direction being respectively perpendicular with the Y-axis, the Z axis is X
Axis direction；
The atom number of selenium element accounts for the ratio between the total atom number of selenium and sulphur in alloy firm in the semiconducting alloy film
Continuous gradation in the X-axis direction remains unchanged in Y-axis and Z-direction.
The content of selenium element is in the raw material i.e. sulfide and selenium for preparing the sulphur selenium compound in the semiconducting alloy film
The two evaporation source center line connecting direction, that is, X direction continuous gradations of compound, in the two vertical evaporation source center line connecting directions
I.e. y direction is constant, constant to bottom direction, that is, depth direction in film surface.
Preferably, the sulphur selenium compound is Sb2(SexS1-x)3Or Bi2(SexS1-x)3, wherein 0<x<1.
Preferably, the sulphur selenium compound Sb2(SexS1-x)3The molar percentage x of middle selenium element is continuous in X-direction
The ranging from 0.09-0.84 of gradual change；The film is 5.5-6.5cm in the length of X-direction, is 2- in the width of Y direction
5cm is 280nm-550nm in the thickness of Z-direction.
Other side according to the invention, the semiconducting alloy film for providing ingredient continuous gradation are answered as absorbed layer
For solar cell and photodetector.
Other side according to the invention provides the preparation method of the semiconducting alloy film of ingredient continuous gradation,
Include the following steps：
(1) select glass, electro-conductive glass or oxide semiconductor film as substrate, in 400-500 DEG C of condition after cleaning
Lower heating；
(2) sulfide powder is uniformly sprinkling upon on one block of sheet glass, selenides powder is uniformly sprinkling upon another block of sheet glass
On, keep the amount of the substance of the powder on unit area not only equal on respective sheet glass, but also the also phase on two blocks of sheet glass
Deng, and be 0.1-0.12mmol/cm2；Obtain two plane evaporation sources；
(3) the two plane evaporation sources obtained in step (2) splicing is placed on aluminum nitride thin on piece, is placed in fast speed heat and steams
Device tray frame bottom is sent out, the substrate described in step (1) is tipped upside down on tray supporter, one piece of heat conduction is added above substrate back
Cover board vacuumizes, and then carries out film deposition；The film deposition process includes warm-up phase and evaporation stage, the preheating
The temperature of the evaporation source in stage is 200-350 DEG C, and the processing time of the warm-up phase is 600-900s；The steaming of the evaporation stage
The temperature to rise is 500-600 DEG C, and the processing time of the evaporation stage is 20-40s；It is 3- that the evaporation stage, which is in vacuum degree,
It is carried out under conditions of 8mTorr, the evaporation stage terminates to obtain the semiconducting alloy film of ingredient continuous gradation.
Preferably, the sulfide described in the step (2) is antimony trisulfide or bismuth sulfide, and selenides is antimony selenide or selenizing
Bismuth；It is 2-3cm to support the length of sulfide rectangle glass piece, supports the length of selenides rectangle glass piece for 3-4cm, two
A sheet glass is of same size, is 2-3cm.
Preferably, substrate is 0.8-1.2cm at a distance from evaporation source in the step (3), and the temperature of evaporation source is by thermoelectricity
It is monitored in real time when even；Heat conducting cover plate is opaque in the step (3), and fusing point is higher than 600 DEG C.
Preferably, the heat conducting cover plate is that graphite block, metal derby or ceramics are fast.
Preferably, the oxide semiconductor film in the step (1) is TiO2, ZnO, SnO or NiO, substrate ethyl alcohol
Ultrasound is cleaned, and is used in combination UV ozone to handle 20-30 minutes, before evaporation, substrate heats 10-30 minutes in air；The step
(2) sulfide and selenides are spread on substrate using mesh screen in, repeat to sieve powder 2-3 times, the mesh screen aperture is 40-60 mesh.
Preferably, the process of the preheating described in step (3) and evaporation carries out in a vacuum, and vacuum degree is maintained at 3-
12mTorr, temperature is less than 100 DEG C when sampling.
The semiconducting alloy film and preparation method thereof that the present invention provides ingredient continuous gradation is described mainly as short distance
The method of the quick thermal evaporation of biplane evaporation source.This method realizes in a rapid thermal treatment tube furnace with infrared heating,
Two kinds of materials are used into identical evaporating temperature, wherein simultaneously provided with two processes of insulating process and evaporation, quickly by powder
Last source is evaporated on substrate, has obtained the semiconducting alloy film of an ingredient continuous gradation.Element in the ingredient of the alloy
Just derive from the element in evaporation source material.
Advantageous effect of the invention is：
(1) the semiconducting alloy film of ingredient continuous gradation proposed by the present invention is suitable for a variety of ternary sulphur selenium compounds,
Such semiconducting alloy has good photoelectric characteristic, can be widely used in various photoelectric devices, such as solar cell
And photodetector.
(2) traditional evaporation technology is evaporated using long range high vacuum single-point, and the comparison of ingredients of obtained film is single, with
This is compared, and the area for two evaporation sources that method proposed by the present invention uses can be with sets itself, using the evaporation of different area
The range for the alloy firm composition transfer that source obtains can adjust on demand, convenient and efficient.
(3) extremely high vacuum degree, about 10 are needed in traditional evaporation technology-3Pa, generally use molecular pump realize that price is high
Expensive, and the time is longer, the vacuum degree that method proposed by the present invention needs is 3-12mTorr, only use mechanical pump it is achieved that
It is a large amount of cost-effective, and the present invention uses infrared heating, realizes fast lifting temperature, and film speed is fast, takes few.
(4) it is 0.8-1.2cm at a distance from evaporation source that method provided by the invention, which uses close evaporation distance, substrate, is protected
Card evaporation source does not decompose, and obtains the film of high quality, and there is the film of preparation fabulous crystallinity, crystal grain up and down, to lack
It falls into seldom, is conducive to the transmission of charge, while the film has good stability, can be good at matching subsequent device system
Standby technique.
(5) method proposed by the present invention is capable of the semiconducting alloy film of growth components continuous gradation on different substrates,
Such as glass, electro-conductive glass, oxide semiconductor film, stabilization simple for process, therefore can combine and use with other semi-conducting materials
In the semiconductor devices of different structure, application potential is huge.
(6) the semiconducting alloy film realizes ingredient continuous gradation in one dimension, and not outer two dimensions are constant.This
The large-scale ingredient consecutive variations of kind, the research for follow-up photoelectric device provide material foundation.If using the thin of single component
Film probes into influence of the ingredient to device performance, needs repeat number to can be only achieved purpose ten times, and systematic error is larger, this method
It is disposable to realize composition transfer simultaneously, working efficiency can be not only improved, but also the accuracy of composition Study can be increased.
Description of the drawings
Fig. 1 is the Sb being prepared2(SexS1-x)3In semiconducting alloy selenium ingredient with change in location X-Y scheme；
Fig. 2 is Sb2(SexS1-x)3The tendency chart that the selenium ingredient of alloy changes in X-direction, which show in vertical histogram
To ingredient average value and standard deviation；
Fig. 3 is Sb2(SexS1-x)3The tendency chart that the selenium ingredient of alloy changes in Y-axis, which show X-direction at
The average value and standard deviation divided；
Fig. 4 is Sb2(SexS1-x)3XRD spectra of the alloy under different selenium ingredients；
Fig. 5 is Sb2(SexS1-x)3The transmission electron microscope sectional view of alloy；
Fig. 6 is the overall schematic of the quick thermal evaporation method of biplane evaporation source of short distance；
Evaporation source and substrate temperature variation relation figure when Fig. 7 is device program operation；
Fig. 8 is the Sb of the crystallization obtained using graphite cover board2(SexS1-x)3The scanning electron microscope (SEM) photograph of alloy；
Fig. 9 is the Sb of the amorphous obtained using ceramic cover plate2(SexS1-x)3The scanning electron microscope (SEM) photograph of alloy；
Figure 10 is the structural schematic diagram of the solar battery array of the semiconductor alloy material based on ingredient continuous gradation；
Figure 11 is relational graph of the solar battery efficiency with selenium composition transfer；
Figure 12 is the J-V characteristic curve diagrams of the best device of solar cell；
Figure 13 is the structural schematic diagram of the photoconductive detector of the semiconductor alloy material based on ingredient continuous gradation；
Figure 14 is the Sb of two heterogeneities2(SexS1-x)3The electric current of alloy firm photoconductive detector becomes with periodical light source
The curve graph of change.
In all the appended drawings, identical reference numeral is used for indicating identical element or structure, wherein：1- vacuum cavities；
2- bleeding points；3- tray supporters；4- thermocouples；5- sulfide powder evaporation sources；6- aluminium nitride thermally conductive sheets；7- selenides powder steams
It rises；8- substrate samples；9- heat conducting cover plates；10- infrared heatings；11- gold back electrodes；The Sb of 12- ingredient continuous gradations2
(SexS1-x)3Alloy firm；13-TiO2Film；14- goldentop electrodes；15-FTO；16- glass；17- incident rays；18- wavelength is
The LED light source of 530nm；19- gold electrodes；The Sb of 20- ingredient continuous gradations2(SexS1-x)3Alloy firm；21- glass substrates.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.As long as in addition, technical characteristic involved in the various embodiments of the present invention described below
It does not constitute a conflict with each other and can be combined with each other.
Embodiment 1
The Sb of ingredient continuous gradation2(SexS1-x)3Semiconducting alloy film and preparation method thereof, wherein selenium percent composition
Variation range 0.09-0.84.Specifically include following steps：
(1) selection and processing of substrate：It is 6 × 2.5cm that FTO, which is cut into size,2Pattern, cleaned respectively using go from
Sub- water, acetone, absolute ethyl alcohol ultrasound decontamination, then high pure nitrogen drying, UV ozone processing after twenty minutes, use on FTO
The method of spray pyrolysis prepares the TiO of 60nm2Film, as the substrate of alloy deposition, then 450 DEG C of 10 points of heating in thermal station
Clock.
(2) preparation of evaporation source：The antimony selenide for weighing the antimony trisulfide and 0.45g of 0.23g respectively, will using the sieve of 50 mesh
Two kinds of powder sieve carefully respectively, remove excessive particle, and it is 2.5 × 2.5cm that two kinds of powder, which are uniformly then sprinkling upon size, respectively2With
3.5×2.5cm2Glass planar on so that its be distributed density be 0.107mmol/cm2。
(3) the semiconducting alloy film is prepared：Antimony trisulfide evaporation source 5 and antimony selenide are placed according to the structure diagram of such as Fig. 6
Evaporation source 7 and substrate sample 8, two plane evaporation source splicings are placed on aluminium nitride wafer 6 and are placed in 3 bottom of tray supporter, substrate 8
It tips upside down on tray supporter 3, ensures that substrate is 1cm at a distance from evaporation source, add one piece of graphite heat conducting cover board above substrate back
9, it is above-mentioned it is all be placed in vacuum chamber 1, vacuumized after shutting lid；Evaporating temperature and time such as Fig. 7 are set, was entirely deposited
Journey program setting is preheating and two processes of evaporation stage, and warm-up phase uses temperature to be 900s for 300 DEG C of times and evaporate rank
It is 28s that Duan Caiyong temperature, which is 540 DEG C of times,；When vacuum degree reaches 5.6mTorr, bring into operation evaporation procedure.Entire heat preservation and
The process of evaporation carries out in a vacuum, and heating is completed by infrared heating 10, detects temperature by thermocouple 4, vacuum degree is maintained at
8mTorr or so, temperature take out sample after being cooled to room temperature.
We are to obtained Sb2(SexS1-x)3Alloy firm carries out relevant characterization and analysis.Fig. 1 is surveyed by EDS power spectrums
Try obtained Sb2(SexS1-x)3The X-Y scheme of thin film composition variation, Fig. 2 and Fig. 3 are Sb respectively2(SexS1-x)3The selenium ingredient of alloy
In the tendency chart that X-axis and Y direction change.It can be seen that selenium ingredient is into uniformly connects in the X-axis direction in gained alloy
Continuous linear change, wherein the ingredient x of selenium can taper to 0.84 from 0.09.And ingredient in the Y-axis direction is substantially not
Become.Fig. 4 is the XRD characterization carried out to the alloy firm, therefrom it can be seen that the Sb being prepared2(SexS1-x)3Film is not
Object on congruent is mutually that pure semiconducting alloy phase shows antimony sulphur selenium prepared by this method and close there is no the phase of mixture
Gold utensil has high crystalline quality.Fig. 5 is Sb2(SexS1-x)3The transmission electron microscope sectional view of alloy.Alloy firm as can be seen from Figure
Crystal grain clearly and up and down, thickness is about 300nm.
Fig. 6 is the overall schematic of the quick thermal evaporation method of biplane evaporation source of short distance, whole using at fast speed heat
Equipment is managed, which can reach with vacuum-control(led) system, temperature control system, cooling system, infrared heating system, heating rate
To 20 DEG C/s.Interior room is supported in vacuum cavity with glass frame, the actual temperature of thermocouple detection evaporation source, dotted line institute is used in combination
The interior room of picture is the nucleus of hydatogenesis film.Close distance is kept up and down.Wherein the insulation effect of heat conducting cover plate ensures
Evaporation source and substrate keep opposite temperature difference, the crystallization degree for the semiconducting alloy film that different cover boards obtain in evaporation process
It is different.Evaporation source and substrate temperature variation, 15 minutes warms make evaporation source when Fig. 7 describes device program operation
Consistent with substrate temperature, in evaporation process, there is difference in the two temperature.
Embodiment 2
The Bi of ingredient continuous gradation2(SexS1-x)3Semiconducting alloy film and preparation method thereof, wherein selenium percent composition
Variation range 0.12-0.69.Specifically include following steps：
(1) selection and processing of substrate：The step is identical as step (1) in embodiment 1.
(2) preparation of evaporation source：The bismuth selenide for weighing the bismuth sulfide and 0.66g of 0.26g respectively, will using the sieve of 50 mesh
Two kinds of powder sieve carefully respectively, remove excessive particle, and it is 2 × 2.5cm that two kinds of powder, which are uniformly then sprinkling upon size, respectively2With 4
×2.5cm2Glass planar on so that its be distributed density be 0.10mmol/cm2。
(3) the semiconducting alloy film is prepared：The step is identical as step (3) in embodiment 1.
The variation range of selenium ingredient in the X-axis direction is 0.12-0.69 in gained alloy, since different materials have difference
Molten boiling point, the complexity of evaporation is different, therefore the variation range for the film being prepared is limited, and obtained range is small
Range in embodiment 1, the variation range of Se content can also pass through the area of two evaporation sources in semiconducting alloy film
It adjusts.
Embodiment 3
The Sb of amorphous2(SexS1-x)3Semiconducting alloy film and preparation method thereof.Specifically include following steps：
(1) selection and processing of substrate：The step is identical as step (1) in embodiment 1.
(2) preparation of evaporation source：The step is identical as step (2) in embodiment 1.
(3) the semiconducting alloy film is prepared：Antimony trisulfide evaporation source 5 and antimony selenide are placed according to the structure diagram of such as Fig. 6
Evaporation source 7 and substrate sample 8, two plane evaporation source splicings are placed on aluminium nitride wafer 6 and are placed in 3 bottom of tray supporter, substrate 8
It tips upside down on tray supporter 3, ensures that substrate is 1cm at a distance from evaporation source, add one piece of ceramic cover board 9 above substrate back
(graphite heat conducting cover board is changed to ceramics herein) it is above-mentioned it is all be placed in vacuum chamber 1, vacuumized after shutting lid；Setting is steamed
Temperature and time such as Fig. 7 is sent out, entire deposition process program setting is preheating and two processes of evaporation stage, and warm-up phase is using temperature
Degree be 300 DEG C of times be 900s and evaporation stage to use temperature for 540 DEG C of times be 28s；When vacuum degree reaches 5.6mTorr,
Bring into operation evaporation procedure.The entire process for keeping the temperature and evaporating carries out in a vacuum, and heating is completed by infrared heating 10, by thermoelectricity
Even 4 detect temperature, and vacuum degree is maintained at 8mTorr or so, and temperature takes out sample after being cooled to room temperature.
Quickly due to infrared heating speed, heat conducting cover plate is transmitted to after absorbing heat on substrate so that warm substrate
Consistent with the temperature of evaporation source, the evaporation process time is very short, and heat conducting cover plate temperature is no more than variation, it is ensured that in evaporation process
Middle substrate and source temperature are poor, however the capacity of heat transmission of the cover board of different materials is different, and therefore, high fever cover board can influence thin
The crystallinity of film, the crystalline state that heat conducting cover plate prepares film as needed are chosen, and the film crystallized is needed to be chosen for stone
Ink stick or metal derby, need to obtain noncrystal membrane and are chosen for ceramic block or stone.Fig. 8 is the crystallization obtained using graphite cover board
Sb2(SexS1-x)3The scanning electron microscope (SEM) photograph of alloy, wherein each crystal grain is high-visible；Fig. 9 be obtained using ceramic cover plate it is non-
Brilliant Sb2(SexS1-x)3A kind of noncrystalline state is presented in the scanning electron microscope (SEM) photograph of alloy, film.
Embodiment 4
By the Sb of ingredient continuous gradation2(SexS1-x)3Film is applied to solar cell.It is as follows：(1) exist
glass/FTO/TiO2Using the Sb of the method prepared composition continuous gradation of the quick thermal evaporation of above-mentioned double source on substrate 16/15/132
(SexS1-x)3Film 12.(2) specific mask plate is covered on film, the hole of mask plate is the square that the length of side is 2mm, interval
For 1mm, thermal evaporation steaming degree gold hearth electrode 11 and goldentop electrode 14 are then used, solar battery array is prepared.(3) battery is given
Bottom add the incident ray 17 of a sunlight, then go out the electricity conversion of all devices with probe test respectively.
The Sb of Figure 10 ingredient continuous gradations2(SexS1-x)3The structural schematic diagram of alloy solar battery array, the knot of device
Structure is glass/FTO/TiO2/Sb2(SexS1-x)3/ Au, 114 areas are 0.04cm on the film2Solar battery array is pressed
It arranges and arranges according to 6 rows 19, can be good at work under conditions of illumination.Figure 11 is solar battery efficiency with selenium composition transfer
Relational graph, it can be seen that with the increase of selenium ingredient x in alloy, electricity conversion occurs first increasing the trend reduced afterwards,
Its variation range is 1.9%-5.6%, and when selenium percent composition is 0.68, the efficiency of device, which reaches, is up to 5.6%.Most preferably
The J-V characteristic curves of device are as shown in figure 12.
Embodiment 5
By the Sb of ingredient continuous gradation2(SexS1-x)3Film is applied in photoconductive detector.It is as follows：(1)
Using the above method according to the Sb of 1 prepared composition continuous gradation of embodiment on glass substrates 212(SexS1-x)3Film 20.(2)
Specific mask plate is covered on film, the hole of mask plate is a length of 1.5cm, the rectangle of wide 1mm, space before 0.2mm, so
Thermal evaporation steaming degree gold electrode 19 is used afterwards, prepares photoconductive detector array.(3) add a cycle to the surface of detector
The wavelength of light on and off is 530nm LED light sources 18, and added bias voltage is 5V, then goes out the spy of each device with probe test respectively
Survey ability.
Figure 13 is the structural schematic diagram of the photoconductive detector of the semiconductor alloy material based on ingredient continuous gradation, device
Structure be Au/Sb2(SexS1-x)3/ Au, the wherein active region of individual devices are the upward light of long 1.5cm and width 0.2mm
Area.Figure 14 is the Sb of two heterogeneities2(SexS1-x)3The electric current of alloy firm photoconductive detector changes with periodical light source
Curve graph.It can be seen from the figure that the alloy material has fabulous visible light-responded ability, brightness electric current ratio to reach nearly 50
Times, speed of photoresponse is in 0.3ms or so.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, all within the spirits and principles of the present invention made by all any modification, equivalent and improvement etc., should all include
Within protection scope of the present invention.
Claims (10)
1. a kind of semiconducting alloy film of ingredient continuous gradation, which is characterized in that the ingredient of the semiconducting alloy film is
Ternary sulphur selenium compound；
Note is located on the semiconducting alloy film surface and is remained unchanged along the selenium element content of semiconducting alloy film surface
Direction be Y direction, remember the semiconducting alloy film thickness direction be Z-direction, and remember be located at the semiconducting alloy
The direction being respectively perpendicular on film surface and with the Y-axis, the Z axis is X-direction；
The atom number of selenium element accounts in alloy firm the ratio between total atom number of selenium and sulphur in X-axis in the semiconducting alloy film
Continuous gradation on direction remains unchanged in Y-axis and Z-direction.
2. the semiconducting alloy film of ingredient continuous gradation as described in claim 1, which is characterized in that the sulphur selenizing is closed
Object is Sb2(SexS1-x)3Or Bi2(SexS1-x)3, wherein 0<x<1.
3. the semiconducting alloy film of ingredient continuous gradation as claimed in claim 2, which is characterized in that the sulphur selenizing is closed
Object Sb2(SexS1-x)3Ranging from 0.09-0.84s of the molar percentage x of middle selenium element in X-direction continuous gradation；The film
It is 5.5-6.5cm in the length of X-direction, is 2-5cm in the width of Y direction, is 280nm- in the thickness of Z-direction
550nm。
4. the semiconducting alloy film application of ingredient continuous gradation as described in any one of claims 1-3, which is characterized in that described
Film is applied to solar cell or photodetector as absorbed layer.
5. the preparation method of the semiconducting alloy film of ingredient continuous gradation as described in claim 1, which is characterized in that including
Following steps：
(1) it selects glass, electro-conductive glass or oxide semiconductor film as substrate, adds under the conditions of 400-500 DEG C after cleaning
Heat；
(2) sulfide powder is uniformly sprinkling upon on one block of sheet glass, selenides powder is uniformly sprinkling upon on another block of sheet glass, is made
The amount of the substance of powder on unit area is not only equal on respective sheet glass, but also also equal on two blocks of sheet glass, and
It is 0.1-0.12mmol/cm2；Obtain two plane evaporation sources；
(3) the two plane evaporation sources obtained in step (2) splicing is placed on aluminum nitride thin on piece, is placed in quick thermal evaporation and sets
Standby tray supporter bottom, the substrate described in step (1) is tipped upside down on tray supporter, and one piece of conductive cover is added above substrate back
Plate vacuumizes, and then carries out film deposition；The film deposition process includes warm-up phase and evaporation stage, the preheating rank
The temperature of the evaporation source of section is 200-350 DEG C, and the processing time of the warm-up phase is 600-900s；The evaporation of the evaporation stage
The temperature in source is 500-600 DEG C, and the processing time of the evaporation stage is 20-40s；It is 3- that the evaporation stage, which is in vacuum degree,
It is carried out under conditions of 8mTorr, the evaporation stage terminates to obtain the semiconducting alloy film of ingredient continuous gradation.
6. the preparation method of the semiconducting alloy film of ingredient continuous gradation as claimed in claim 5, which is characterized in that described
Sulfide described in step (2) is that either bismuth sulfide selenides is antimony selenide or bismuth selenide to antimony trisulfide；Support the length of sulfide
The length of square glass piece is 2-3cm, and it is 3-4cm, two sheet glass width to support the length of the rectangle glass piece of selenides
It is identical, it is 2-3cm.
7. the preparation method of the semiconducting alloy film of ingredient continuous gradation as claimed in claim 5, which is characterized in that described
Substrate is 0.8-1.2cm at a distance from evaporation source in step (3), and the temperature of evaporation source by monitoring in real time when thermocouple；The step
Suddenly heat conducting cover plate is opaque in (3), and fusing point is higher than 600 DEG C.
8. the preparation method of the semiconducting alloy film of ingredient continuous gradation according to claim 7, it is characterised in that：Institute
The heat conducting cover plate stated is graphite block, metal derby or ceramic block.
9. the preparation method of the semiconducting alloy film of ingredient continuous gradation according to claim 5, it is characterised in that：Institute
It is TiO to state the oxide semiconductor film in step (1)2, ZnO, SnO or NiO, substrate with EtOH Sonicate clean, be used in combination ultraviolet
Ozone treatment 20-30 minutes, before evaporation, substrate heats 10-30 minutes in air；Use mesh screen by sulphur in the step (2)
Compound and selenides are spread on substrate, repeat to sieve powder 2-3 times, and the mesh screen aperture is 40-60 mesh.
10. the preparation method of the semiconducting alloy film of ingredient continuous gradation according to claim 5, it is characterised in that：
Warm-up phase and evaporation stage described in step (3) carry out in a vacuum, and vacuum degree is maintained at 3-12mTorr, temperature when sampling
Less than 100 DEG C.
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