CN107248534A - A kind of semiconducting alloy film of composition continuous gradation and its preparation method and application - Google Patents
A kind of semiconducting alloy film of composition continuous gradation and its preparation method and application Download PDFInfo
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- CN107248534A CN107248534A CN201710387303.7A CN201710387303A CN107248534A CN 107248534 A CN107248534 A CN 107248534A CN 201710387303 A CN201710387303 A CN 201710387303A CN 107248534 A CN107248534 A CN 107248534A
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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
- 239000000203 mixture Substances 0.000 title claims abstract description 68
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000010408 film Substances 0.000 claims abstract description 82
- 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
- 238000000034 method Methods 0.000 claims abstract description 32
- 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
- 239000011521 glass Substances 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 15
- 239000004065 semiconductor Substances 0.000 claims description 14
- 230000008569 process Effects 0.000 claims description 12
- 230000008859 change Effects 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 11
- 239000005357 flat glass Substances 0.000 claims description 10
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 9
- 238000012545 processing Methods 0.000 claims description 8
- 150000003346 selenoethers Chemical class 0.000 claims description 8
- 239000000919 ceramic Substances 0.000 claims description 7
- 238000002207 thermal evaporation Methods 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 6
- 239000010439 graphite Substances 0.000 claims description 6
- 229910017083 AlN Inorganic materials 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
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 claims description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 4
- 239000005864 Sulphur Substances 0.000 claims description 4
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 3
- 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 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 238000004140 cleaning Methods 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
- 238000000427 thin-film deposition Methods 0.000 claims description 2
- 239000010409 thin film Substances 0.000 abstract description 5
- 230000008021 deposition Effects 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 description 11
- 239000010931 gold Substances 0.000 description 9
- 239000000523 sample Substances 0.000 description 8
- 229910052737 gold Inorganic materials 0.000 description 6
- 238000012546 transfer Methods 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 4
- 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
- 238000010586 diagram Methods 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
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 241001148715 Lamarckia aurea Species 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000009413 insulation 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
- 206010020741 Hyperpyrexia Diseases 0.000 description 1
- 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
- IBEWGOCMLWIGCZ-UHFFFAOYSA-N [Bi]=S.[Se] Chemical compound [Bi]=S.[Se] IBEWGOCMLWIGCZ-UHFFFAOYSA-N 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
- 230000009286 beneficial effect Effects 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
- 238000012512 characterization method Methods 0.000 description 1
- 150000001875 compounds Chemical class 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
- 238000000151 deposition Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000004615 ingredient Substances 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
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005118 spray pyrolysis Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- 238000007669 thermal treatment Methods 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/0256—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
- H01L31/0264—Inorganic materials
- H01L31/0296—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
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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
- 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 film of composition continuous gradation and its preparation method and application, the feature of the wherein film has：Film be ternary sulphur selenium compound alloy, selenium composition X-direction can continuous gradation, be basically unchanged in Y direction and Z-direction；The semiconducting alloy film of the composition continuous gradation is used for thin-film solar cells array and photodetector as good light absorbing layer.Its preparation method includes：(1) deposition substrate is chosen；(2) evaporation source is prepared；(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 composition under identical conditions, and film speed is fast, and technique is convenient, it is easy to accomplish, it is reliable and stable, have wide range of applications.
Description
Technical field
The invention belongs to semiconductor film material technical field, in particular it relates to which a kind of composition continuous gradation semiconductor is closed
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 with controllable optical band gap and electric property, energy
Enough good match spectrum characteristics.Such as antimony sulphur selenium alloy (Sb2(SexS1-x)3) advantage of monomer material is combined while also gram
The deficiency of band gap is taken, it has big absorption coefficient, band gap can be adjusted from 1.1eV to 1.7eV by changing its composition.But 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.
At present, the preparation method of semiconducting alloy adjusts a kind of composition based on solwution method, every time, and workload is heavy, and easily goes out
Existing accidental error.Therefore, it is disposable simultaneously with condition the semiconducting alloy film for preparing continuous component continuous gradation be must
Want.In order to probe into influence of the alloying component change to physical characteristic and device performance, high-throughout preparation method is development
Trend.
The content of the invention
Present invention seek to address that technical problem present in prior art, it is proposed that a kind of semiconductor of composition continuous gradation
Alloy firm and its preparation method and application.
According to the purpose of the present invention, there is provided a kind of semiconducting alloy film of composition continuous gradation, the semiconducting alloy
The composition of film is ternary sulphur selenium compound；Note is located on the semiconducting alloy film surface and semiconductor is closed in the direction
The direction that the selenium element content on gold thin film surface keeps constant is Y direction, and the thickness direction for remembering the semiconducting alloy film is Z
Direction of principal axis, and remember that the direction for being located on the semiconducting alloy film surface and being respectively perpendicular with the Y-axis, the Z axis is X
Direction of principal axis；
The atom number of selenium element accounts for the ratio between total atom number of selenium and sulphur in alloy firm in the semiconducting alloy film
Continuous gradation in the X-axis direction, keeps constant in Y-axis and Z-direction.
The content of selenium element is preparing the raw material i.e. sulfide and selenium of the sulphur selenium compound in the semiconducting alloy film
The two evaporation source center line connecting directions of compound are X direction continuous gradation, in the two vertical evaporation source center line connecting directions
I.e. y direction is constant, is that depth direction is constant in film surface to bottom direction.
Preferably, described sulphur selenium compound is Sb2(SexS1-x)3Or Bi2(SexS1-x)3, wherein 0<x<1.
Preferably, described sulphur selenium compound Sb2(SexS1-x)3The molar percentage x of middle selenium element is continuous in X-direction
The scope of gradual change is 0.09-0.84；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.
Should as absorbed layer there is provided the semiconducting alloy film of composition continuous gradation according to another aspect of the present invention
For solar cell and photodetector.
According to another aspect of the present invention there is provided the preparation method of the semiconducting alloy film of composition continuous gradation,
Comprise the following steps：
(1) from 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, make the amount of the material of powder in unit area not only equal on respective sheet glass, and 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 aluminium nitride wafer, 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 plate, is vacuumized, and then carries out thin 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 risen is 500-600 DEG C, and the processing time of the evaporation stage is 20-40s；The evaporation stage be vacuum be 3-
Carried out under conditions of 8mTorr, the evaporation stage terminates to obtain the semiconducting alloy film of composition continuous gradation.
Preferably, the sulfide described in the step (2) is antimony trisulfide or bismuth sulfide, and selenides is antimony selenide or selenizing
Bismuth；The length for supporting sulfide rectangle glass piece is 2-3cm, and the length of support selenides rectangle glass piece is 3-4cm, two
Individual sheet glass width is identical, is 2-3cm.
Preferably, the distance of substrate and evaporation source is 0.8-1.2cm in the step (3), and the temperature of evaporation source is by thermoelectricity
Monitored in real time when even；Heat conducting cover plate is opaque in the step (3), and its fusing point is higher than 600 DEG C.
Preferably, described 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 ethanol
Ultrasound is cleaned, and is handled 20-30 minutes with UV ozone, and before evaporation, substrate is heated 10-30 minutes in atmosphere；The step
(2) sulfide and selenides are sprinkling upon on substrate using mesh screen in, sieve powder is repeated 2-3 times, the mesh screen aperture is 40-60 mesh.
Preferably, described in step (3) preheating and the process of evaporation is carried out in a vacuum, and vacuum is maintained at 3-
12mTorr, temperature is less than 100 DEG C during sampling.
The present invention provides semiconducting alloy film of composition continuous gradation and preparation method thereof and is described mainly as closely
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 two processes of insulating process and evaporation are provided with simultaneously, quickly by powder
Last source is evaporated on substrate, has obtained the semiconducting alloy film of a composition continuous gradation.Element in the composition of the alloy
Just derive from the element in evaporation source material.
The beneficial effect of invention is：
(1) the semiconducting alloy film of composition continuous gradation proposed by the present invention, it is adaptable to 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 is used can be with sets itself, using the evaporation of different area
The scope for the alloy firm composition transfer that source is obtained can be adjusted on demand, convenient and swift.
(3) XHV degree, about 10 are needed in traditional evaporation technology-3Pa, generally realizes, price is held high using molecular pump
Expensive, and the time is longer, the vacuum that method proposed by the present invention needs is 3-12mTorr, only with 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) method that provides of the present invention uses near evaporation distance, and the distance of substrate and evaporation source is 0.8-1.2cm, is protected
Card evaporation source is not decomposed, and obtains high-quality film, the film of preparation has fabulous crystallinity, its crystal grain up/down perforation, is lacked
Fall into seldom, be conducive to the transmission of electric charge, while the film has good stability, can be good at matching follow-up 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, technique simple and stable is used therefore, it is possible to be combined with other semi-conducting materials
In the semiconductor devices of different structure, application potential is huge.
(6) the semiconducting alloy film realizes composition continuous gradation in a dimension, and not outer two dimensions are constant.This
Large-scale composition consecutive variations are planted, the research for follow-up photoelectric device provides material foundation.If using the thin of single component
Film probes into influence of the composition to device performance, it is necessary to which repeat number can be only achieved purpose ten times, and systematic error is larger, this method
Disposable to realize composition transfer simultaneously, it can not only improve operating efficiency, and can increase the accuracy of composition Study.
Brief description of the drawings
Fig. 1 is the Sb prepared2(SexS1-x)3In semiconducting alloy selenium composition with change in location X-Y scheme；
Fig. 2 is Sb2(SexS1-x)3The tendency chart that the selenium composition of alloy changes in X-direction, which show in vertical Nogata
To composition average value and standard deviation；
Fig. 3 is Sb2(SexS1-x)3The tendency chart that the selenium composition of alloy changes in Y-axis, which show X-direction into
The average value and standard deviation divided；
Fig. 4 is Sb2(SexS1-x)3XRD spectra of the alloy under different selenium compositions；
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 closely；
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 plate2(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 representation of the solar battery array of the semiconductor alloy material based on composition continuous gradation；
Figure 11 is graph of a relation of the solar battery efficiency with selenium composition transfer；
Figure 12 is the J-V characteristic curve diagrams of the optimal device of solar cell；
Figure 13 is the structural representation of the photoconductive detector of the semiconductor alloy material based on composition continuous gradation；
Figure 14 is the Sb of two heterogeneities2(SexS1-x)3The electric current of alloy firm photoconductive detector becomes with periodicity light source
The curve map of change.
In all of the figs, identical reference is used for representing 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
Rise；8- substrate samples；9- heat conducting cover plates；10- infrared heatings；11- gold back electrodes；The Sb of 12- composition continuous gradations2
(SexS1-x)3Alloy firm；13-TiO2Film；14- goldentop electrodes；15-FTO；16- glass；17- incident rays；18- wavelength is
530nm LED/light source；19- gold electrodes；The Sb of 20- composition continuous gradations2(SexS1-x)3Alloy firm；21- glass substrates.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples
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 each embodiment of invention described below
Not constituting conflict each other can just be mutually combined.
Embodiment 1
The Sb of composition continuous gradation2(SexS1-x)3Semiconducting alloy film and preparation method thereof, wherein selenium percent composition
Excursion 0.09-0.84.Specifically include following steps：
(1) selection and processing of substrate：FTO is cut into size for 6 × 2.5cm2Pattern, cleaned respectively using go from
Sub- water, acetone, absolute ethyl alcohol ultrasound decontamination, then high pure nitrogen drying after UV ozone is handled 20 minutes, is used on FTO
The method of spray pyrolysis prepares 60nm TiO2Film, is used as the substrate of alloy deposition, then 450 DEG C of 10 points of heating in thermal station
Clock.
(2) preparation of evaporation source：0.23g antimony trisulfide and 0.45g antimony selenide are weighed respectively, will using the sieve of 50 mesh
Two kinds of powder are sieved carefully respectively, remove excessive particle, and two kinds of powder are uniformly then sprinkling upon into size for 2.5 × 2.5cm 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 such as Fig. 6 structure diagram
Evaporation source 7 and substrate sample 8, two plane evaporation source splicings are placed on aluminium nitride wafer 6 and are placed in the bottom of tray supporter 3, substrate 8
Tip upside down on tray supporter 3, it is ensured that the distance of substrate and evaporation source is above 1cm, substrate back plus one piece of graphite heat conducting cover plate
9, it is above-mentioned it is all be placed in vacuum chamber 1, shut after lid and vacuumize；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 evaporation rank
Duan Caiyong temperature be 540 DEG C of times be 28s；When vacuum reaches 5.6mTorr, bring into operation evaporation procedure.Whole insulation and
The process of evaporation is carried out in a vacuum, and heating is completed by infrared heating 10, and by the detection temperature of thermocouple 4, vacuum is maintained at
8mTorr or so, temperature, which is cooled to after normal temperature, takes out sample.
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 change, Fig. 2 and Fig. 3 are Sb respectively2(SexS1-x)3The selenium composition of alloy
The tendency chart changed in X-axis and Y direction.It can be seen that selenium composition is into uniformly connects in the X-axis direction in gained alloy
Continuous linear change, the composition x of wherein selenium can taper to 0.84 from 0.09.And composition in the Y-axis direction is substantially not
Become.Fig. 4 is that the XRD that the alloy firm is carried out is characterized, therefrom it can be seen that the Sb prepared2(SexS1-x)3Film is not
Thing on congruent is mutually pure semiconducting alloy phase, and in the absence of the phase of mixture, the antimony sulphur selenium for indicating this method preparation is closed
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 is clear and up/down perforation, its thickness is about 300nm.
Fig. 6 is the overall schematic of the quick thermal evaporation method of biplane evaporation source closely, overall using at fast speed heat
Equipment is managed, the equipment has vacuum-control(led) system, and temperature control system, cooling system, infrared heating system, programming rate can reach
To 20 DEG C/s.Interior room is supported in vacuum cavity with glass frame, and with thermocouple detect evaporation source actual temperature, dotted line institute
The interior room of picture is the nucleus of hydatogenesis film.Near distance is kept up and down.Wherein the insulation effect of heat conducting cover plate ensures
Evaporation source and substrate keep relative temperature difference, the crystallization degree for the semiconducting alloy film that different cover plates are obtained in evaporation process
It is different.Evaporation source and substrate temperature change when Fig. 7 describes device program operation, the warm of 15 minutes cause evaporation source
Consistent with substrate temperature, in evaporation process, there is difference at temperature in both.
Embodiment 2
The Bi of composition continuous gradation2(SexS1-x)3Semiconducting alloy film and preparation method thereof, wherein selenium percent composition
Excursion 0.12-0.69.Specifically include following steps：
(1) selection and processing of substrate：The step is identical with the step (1) in embodiment 1.
(2) preparation of evaporation source：0.26g bismuth sulfide and 0.66g bismuth selenide are weighed respectively, will using the sieve of 50 mesh
Two kinds of powder are sieved carefully respectively, remove excessive particle, and two kinds of powder are uniformly then sprinkling upon into size for 2 × 2.5cm 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 with step (3) in embodiment 1.
The excursion of selenium composition in the X-axis direction is 0.12-0.69 in gained alloy, because different materials have difference
Molten boiling point, complexity that it evaporates is different, therefore the excursion of the film prepared is limited, and the scope that it is obtained is small
The excursion of Se content can also be by the areas of two evaporation sources in scope in embodiment 1, semiconducting alloy film
Regulation.
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 with the step (1) in embodiment 1.
(2) preparation of evaporation source：The step is identical with the step (2) in embodiment 1.
(3) the semiconducting alloy film is prepared：Antimony trisulfide evaporation source 5 and antimony selenide are placed according to such as Fig. 6 structure diagram
Evaporation source 7 and substrate sample 8, two plane evaporation source splicings are placed on aluminium nitride wafer 6 and are placed in the bottom of tray supporter 3, substrate 8
Tip upside down on tray supporter 3, it is ensured that the distance of substrate and evaporation source is above 1cm, substrate back plus one piece of ceramic cover plate 9
(graphite heat conducting cover plate is replaced by ceramics herein) it is above-mentioned it is all be placed in vacuum chamber 1, shut after lid and vacuumize；Setting is steamed
Temperature and time such as Fig. 7 is sent out, whole deposition process program setting is preheating and two processes of evaporation stage, and warm-up phase is using temperature
Degree is that 300 DEG C of times are 900s and evaporation stage uses temperature to be 28s for 540 DEG C of times；When vacuum reaches 5.6mTorr,
Bring into operation evaporation procedure.The whole process for being incubated and evaporating is carried out in a vacuum, and heating is completed by infrared heating 10, by thermoelectricity
Even 4 detection temperatures, vacuum is maintained at 8mTorr or so, and temperature, which is cooled to after normal temperature, takes out sample.
Due to infrared heating speed quickly, heat conducting cover plate is delivered on substrate after absorbing heat 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 change, it is ensured that in evaporation process
Middle substrate and source temperature are poor, but the capacity of heat transmission of the cover plate of different materials is different, and therefore, hyperpyrexia cover plate can influence thin
The crystallinity of film, the crystalline state that heat conducting cover plate prepares film as needed is chosen, it is necessary to which the film crystallized is chosen for stone
Ink stick or metal derby are chosen for ceramic block or stone, it is necessary to obtain noncrystal membrane.Fig. 8 is the crystallization obtained using graphite cover plate
Sb2(SexS1-x)3The scanning electron microscope (SEM) photograph of alloy, each of which crystal grain is high-visible；Fig. 9 be using ceramic cover plate obtain 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 composition continuous gradation2(SexS1-x)3Film is applied to solar cell.Comprise the following steps that：(1) exist
glass/FTO/TiO2The Sb of the method prepared composition continuous gradation of the quick thermal evaporation of above-mentioned double source is used 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, be spaced
For 1mm, then using the golden hearth electrode 11 of thermal evaporation steaming degree and goldentop electrode 14, solar battery array is prepared.(3) battery is given
Bottom add the incident ray 17 of a sunshine, then go out the electricity conversion of all devices with probe test respectively.
The Sb of Figure 10 composition continuous gradations2(SexS1-x)3The structural representation of alloy solar battery array, the knot of device
Structure is glass/FTO/TiO2/Sb2(SexS1-x)3114 areas are 0.04cm on/Au, the film2Solar battery array, is pressed
Arrange and arrange according to 6 rows 19, can be good at work under conditions of illumination.Figure 11 is solar battery efficiency with selenium composition transfer
Graph of a relation, it can be seen that with the increase of selenium composition x in alloy, electricity conversion, which is occurred in that, first increases the trend reduced afterwards,
Its excursion is 1.9%-5.6%, and when selenium percent composition is 0.68, the efficiency of device, which reaches, is 5.6% to the maximum.Most preferably
The J-V characteristic curves of device are as shown in figure 12.
Embodiment 5
By the Sb of composition continuous gradation2(SexS1-x)3Film is applied in photoconductive detector.Comprise the following steps that：(1)
Using Sb of the above method according to the prepared composition continuous gradation of embodiment 1 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, and wide 1mm rectangle, space before is 0.2mm, so
Afterwards using thermal evaporation steaming degree gold electrode 19, photoconductive detector array is prepared.(3) surface to detector adds a cycle
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 representation of the photoconductive detector of the semiconductor alloy material based on composition continuous gradation, device
Structure be Au/Sb2(SexS1-x)3/ Au, wherein individual devices active region are long 1.5cm and width 0.2mm upward light
Area.Figure 14 is the Sb of two heterogeneities2(SexS1-x)3The electric current of alloy firm photoconductive detector changes with periodicity light source
Curve map.It can be seen that the alloy material has fabulous visible light-responded ability, brightness electric current ratio reaches 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, it is not used to
The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the invention etc., it all should include
Within protection scope of the present invention.
Claims (10)
1. a kind of semiconducting alloy film of composition continuous gradation, it is characterised in that the composition of the semiconducting alloy film is
Ternary sulphur selenium compound；
Note is located on the semiconducting alloy film surface and the selenium element content of semiconducting alloy film surface is protected in the direction
Constant direction is held for Y direction, the thickness direction of the semiconducting alloy film is remembered for Z-direction, and note is partly led positioned at this
The direction being respectively perpendicular on body alloy firm 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, keeps constant in Y-axis and Z-direction.
2. the semiconducting alloy film of composition continuous gradation as claimed in claim 1, it is characterised in that described sulphur selenizing is closed
Thing is Sb2(SexS1-x)3Or Bi2(SexS1-x)3, wherein 0<x<1.
3. the semiconducting alloy film of composition continuous gradation as claimed in claim 2, it is characterised in that described sulphur selenizing is closed
Thing Sb2(SexS1-x)3The molar percentage x of middle selenium element is 0.09-0.84 in the scope of 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 the composition continuous gradation as described in claim 1-3 is any, it is characterised in that described
Film is applied to solar cell and photodetector as absorbed layer.
5. the preparation method of the semiconducting alloy film of composition continuous gradation as claimed in claim 1, it is characterised in that including
Following steps：
(1) from glass, electro-conductive glass or oxide semiconductor film as substrate, add after cleaning under the conditions of 400-500 DEG C
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, made
The amount of the material of powder in unit area is not only equal on respective sheet glass, and 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 aluminium nitride wafer, 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, is vacuumized, and then carries out thin 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；The evaporation stage be vacuum be 3-
Carried out under conditions of 8mTorr, the evaporation stage terminates to obtain the semiconducting alloy film of composition continuous gradation.
6. the preparation method of the semiconducting alloy film of composition continuous gradation as claimed in claim 5, it is characterised in that described
Sulfide described in step (2) is antimony trisulfide or bismuth sulfide, and selenides is antimony selenide or bismuth selenide；Support the length of sulfide
The length of square glass piece is 2-3cm, and the length for supporting the rectangle glass piece of selenides is 3-4cm, two sheet glass width
It is identical, it is 2-3cm.
7. the preparation method of the semiconducting alloy film of composition continuous gradation as claimed in claim 5, it is characterised in that described
The distance of substrate and evaporation source is 0.8-1.2cm in step (3), the temperature of evaporation source by thermocouple when monitor in real time；The step
Suddenly heat conducting cover plate is opaque in (3), and its fusing point is higher than 600 DEG C.
8. the preparation method of the semiconducting alloy film of composition gradual change according to claim 7, it is characterised in that：Described
Heat conducting cover plate is graphite block, metal derby or ceramic block.
9. the preparation method of the semiconducting alloy film of composition gradual change according to claim 5, it is characterised in that：The step
Suddenly the oxide semiconductor film in (1) is TiO2, ZnO, SnO or NiO, substrate cleaned with EtOH Sonicate, and uses UV ozone
Processing 20-30 minutes, before evaporation, substrate is heated 10-30 minutes in atmosphere；Mesh screen is used in the step (2) by sulfide
It is sprinkling upon with selenides on substrate, repeats sieve powder 2-3 times, the mesh screen aperture is 40-60 mesh.
10. the preparation method of the semiconducting alloy film of composition gradual change according to claim 5, it is characterised in that：Step
(3) process of preheating and evaporation described in is carried out in a vacuum, and vacuum is maintained at 3-12mTorr, and temperature is less than 100 during sampling
℃。
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| CN109652762A (en) * | 2018-11-29 | 2019-04-19 | 华中科技大学 | A kind of preparation method of antimony sulphur selenium alloy film |
| CN109904059A (en) * | 2019-01-16 | 2019-06-18 | 清华大学 | The preparation method and applications of precious metal chemical complex |
| CN113410321A (en) * | 2021-06-21 | 2021-09-17 | 吉林师范大学 | Preparation method of solar cell with gradient hole collection layer |
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