CN108807561A - A method of preparing copper and iron sulphur optoelectronic film with chloride - Google Patents
A method of preparing copper and iron sulphur optoelectronic film with chloride Download PDFInfo
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- CN108807561A CN108807561A CN201810704339.8A CN201810704339A CN108807561A CN 108807561 A CN108807561 A CN 108807561A CN 201810704339 A CN201810704339 A CN 201810704339A CN 108807561 A CN108807561 A CN 108807561A
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- film
- iron sulphur
- copper
- chloride
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- 239000010949 copper Substances 0.000 title claims abstract description 25
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 22
- MBMLMWLHJBBADN-UHFFFAOYSA-N Ferrous sulfide Chemical compound [Fe]=S MBMLMWLHJBBADN-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 20
- 230000005693 optoelectronics Effects 0.000 title claims abstract description 19
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 title claims abstract description 9
- 239000010408 film Substances 0.000 claims abstract description 35
- 239000002243 precursor Substances 0.000 claims abstract description 19
- 239000000758 substrate Substances 0.000 claims abstract description 19
- 239000010409 thin film Substances 0.000 claims abstract description 19
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims abstract description 10
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims abstract description 9
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims abstract description 6
- 230000008569 process Effects 0.000 claims abstract description 6
- 239000011521 glass Substances 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 238000004528 spin coating Methods 0.000 claims abstract description 5
- 239000003125 aqueous solvent Substances 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000004140 cleaning Methods 0.000 claims description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 229910021591 Copper(I) chloride Inorganic materials 0.000 claims description 5
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 239000005357 flat glass Substances 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- 238000004090 dissolution Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 239000008236 heating water Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims 2
- 239000007864 aqueous solution Substances 0.000 claims 1
- 238000007598 dipping method Methods 0.000 claims 1
- 239000000243 solution Substances 0.000 claims 1
- 238000004506 ultrasonic cleaning Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 abstract description 6
- MPTQRFCYZCXJFQ-UHFFFAOYSA-L copper(II) chloride dihydrate Chemical compound O.O.[Cl-].[Cl-].[Cu+2] MPTQRFCYZCXJFQ-UHFFFAOYSA-L 0.000 abstract description 4
- PODWXQQNRWNDGD-UHFFFAOYSA-L sodium thiosulfate pentahydrate Chemical compound O.O.O.O.O.[Na+].[Na+].[O-]S([S-])(=O)=O PODWXQQNRWNDGD-UHFFFAOYSA-L 0.000 abstract description 4
- 230000035484 reaction time Effects 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 229910052951 chalcopyrite Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 208000033962 Fontaine progeroid syndrome Diseases 0.000 description 1
- 102000005298 Iron-Sulfur Proteins Human genes 0.000 description 1
- 108010081409 Iron-Sulfur Proteins Proteins 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- DVRDHUBQLOKMHZ-UHFFFAOYSA-N chalcopyrite Chemical compound [S-2].[S-2].[Fe+2].[Cu+2] DVRDHUBQLOKMHZ-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- YNBADRVTZLEFNH-UHFFFAOYSA-N methyl nicotinate Chemical compound COC(=O)C1=CC=CN=C1 YNBADRVTZLEFNH-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005987 sulfurization reaction Methods 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 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
- H01L31/02—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
- H01L31/02168—Coatings for devices characterised by at least one potential jump barrier or surface barrier for solar cells the coatings being antireflective or having enhancing optical properties for the solar cells
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/28—Other inorganic materials
- C03C2217/287—Chalcogenides
- C03C2217/288—Sulfides
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/116—Deposition methods from solutions or suspensions by spin-coating, centrifugation
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
A method of copper and iron sulphur optoelectronic film being prepared with chloride, belongs to optoelectronic film preparing technical field, the present invention obtains as follows, cleans glass substrate first, then by CuCl2.2H2O、FeCl3.6H2O and Na2S2O3.5H2O is sequentially placed into aqueous solvent, prepare clear transparent solutions, precursor thin-film is obtained on the glass sheet with spin-coating method, naturally dry, be put into hydrazine hydrate can closed container, so that precursor thin-film sample is not in direct contact with hydrazine, after the closed container equipped with precursor thin-film sample is heated take out sample be dried, film quality can be improved by increasing reaction times and heat treatment process, obtain copper and iron sulphur optoelectronic film.The present invention does not need high temperature high vacuum condition, low to instrument and equipment requirement, and production cost is low, and production efficiency is high, easily operated.Gained copper and iron sulphur optoelectronic film has preferable continuity and uniformity, this new process to provide a kind of industrialized production method at low cost, achievable to prepare high performance copper and iron sulphur optoelectronic film.
Description
Technical field
The invention belongs to optoelectronic film preparing technical field used for solar batteries more particularly to a kind of preparing copper with chloride
The method of iron sulphur optoelectronic film.
Background technology
Copper and iron sulphur is a kind of ternary I-III-VI as photoelectric material2Compound semiconductor has chalcopyrite and dodges zinc
The crystal structure of mine, at the same have the high absorption coefficient of light, for direct gap semiconductor, thermal stability is good, is imitated without light-induced degradation
The advantages that answering, and because the cheap of copper and iron sulfur materials, rich reserves and the advantages such as nontoxic receive the extensive concern of scientist.
The preparation method of copper and iron sulphur film has much at present, mainly there is electrochemical deposition method, sputtering method, thermal evaporation, heat
Spray coating method etc..It is a kind of very promising due to raw material rich reserves on earth, cheap and nontoxic
Optoelectronic thin film material, but prior art route is complicated, manufacturing cost is high, thus need to explore the preparation process of low cost.
Method as previously described is the same, and other methods also have different defects.It is related to the present invention to also have following document：
[1] Xiankuan Meng, Hongmei Deng, Investigate the growth mechanism of
Cu2FeSnS4 thin films by sulfurization of metallic precursor. Materials
Letters, 2017.
Main have studied prepares Cu by metal precursor vulcanization2FeSnS4Film, and analyze Cu2FeSnS4The life of film
Long mechanism.
[2] Erika Dutková, Zdenka Bujnáková, Mechanochemical synthesis,
structural, magnetic, optical and electrooptical properties of CuFeS2
nanoparticles. Advanced Powder Technology, 2018.
Main have studied prepares CuFeS by mechanical milling method2Nano-particle has studied CuFeS2The structure of nano-particle, magnetic
Property, electrical and optical properties.
[3] Sugathan A, B Bhattacharyya, et al. Why Does CuFeS2 Resemble
Gold. Journal of Physical Chemistary Letters, 2018.
Mainly have studied CuFeS2The physical property of quantum dot.It is combined, is had studied in class using structure and optical characterisation methods
It is similar to the collision phenomenon observed in the spectrum of the quantum dot of 500 nm.
[4] Aliyev YI, TM Ilyasli, et al. The structural and vibrational
properties of Ni-doped chalcopyrite CuFeS2. Journal of Ovonic Research, 2018.
It is main to have studied nickel doping chalcopyrite CuFeS2Structure and oscillatory property, and analyze doping nickel CuFe0.99Ni0.01S2
To CuFeS2The influence of crystal structure.
[5] Rouchdi M, E Salmani, et al. Spray pyrolysis synthesis of CuxFe1- xS2 and their structural, electronic and optical properties: Experimental and
first-principles study. Materials Science and Engineering B-advanced
Functional Solid-state Materials, 2018.
Mainly using chemical spray pyrolysis (CSP) technology synthesis pyrite, FeS2(FS) and chalcopyrite copper and iron sulfide CuxFe1- xS2(CFS) film mainly has studied the influence that Cu concentration grows film.
[6] Xiong X, X Hua, et al. Oxidation mechanism of chalcopyrite
revealed by X-ray photoelectron spectroscopy and first principles studies.
Applied Surface Science, 2018.
Mainly have studied chalcopyrite（CuFeS2）The oxidation mechanism and first-principles calculations on surface.
Invention content
The present invention has invented a kind of and entirely different copper of existing preparation method to solve the deficiency of existing technology of preparing
The preparation process of iron sulphur film.
The present invention prepares copper and iron sulphur film using spin coating-chemistry co-reducing process, uses sheet glass or silicon chip for substrate, with
CuCl2.2H2O、FeCl3.6H2O、Na2S2O3.5H2O is raw material, using water as solvent, sequentially adds CuCl2.2H2O、
FeCl3.6H2O、Na2S2O3.5H2O makes it fully react.Certain thickness copper and iron sulphur precursor thin-film is first prepared with spin-coating method,
It using hydrazine hydrate as reducing agent, is heated at a lower temperature in closed container, so that precursor thin-film is restored concurrent GCMS computer anti-
It answers, prepared film quality can be improved by heat treatment after increasing reaction times and reaction, obtain target product.
The specific preparation method of the present invention includes following steps in sequence：
A. the cleaning of substrate is carried out, sheet glass or silicon chip are switched to by this experimental selection sheet glass or silicon chip first as substrate
Then 20mm × 20mm × 2mm sizes are cleaned 2 ~ 3 times as film substrate with deionized water, then pass through dilute sulfuric acid boil 30 ~
40min, 40 ~ 50min of heating water bath, deionized water are cleaned by ultrasonic 20min, after these three important cleaning steps, with dioxygen water logging
Bubble saves backup.
B. by CuCl2.2H2O、FeCl3.6H2O and Na2S2O3.5H2O is sequentially placed into solvent, keeps the substance in solution equal
Even mixing.Specifically, by the CuCl of 0.1705g2.2H2The water that 1mL is added in O in vial makes it fully dissolve, then successively
The FeCl of 0.2702g is added in vial3.6H2The Na of O and 0.2481g2S2O3.5H2O makes its full and uniform mixed dissolution,
The CuCl of middle addition2.2H2O、FeCl3.6H2O、Na2S2O3.5H2The amount of O and aqueous solvent can be according to the proportional change of number of film
Change.
C. the substrate of the external uniform solution as described in step b is made, and is dried, precursor thin-film sample is obtained.It can incite somebody to action
Above-mentioned solution drips on the substrate being placed on sol evenning machine, restarts sol evenning machine with 200 ~ 3500 revs/min of rotation certain times, makes
After solution coating in drop is uniform, and substrate is carried out after natural drying, repeat to drip again after upper previous solu and spin coating again from
It so dries, so repeatedly 2 ~ 8 times, certain thickness precursor thin-film sample has then been obtained on substrate.
D. precursor thin-film sample obtained by step c is placed on holder, be put into hydrazine hydrate can closed container, make
Precursor thin-film sample is not contacted with hydrazine.The hydrazine hydrate amount of being put into is 0.5mL.It will be above-mentioned close equipped with precursor thin-film sample
It closes container to be put into baking oven, be heated between 160 ~ 220 DEG C, soaking time 2 ~ 40 hours is then cooled to room temperature taking-up.
E. it takes out after spontaneously drying, repeats b, c and Step d 2 ~ 6 times, with the thickness of film prepared by increase, reduce film
Defect.
F. by step e gains, after so that its room temperature is spontaneously dried, increase heat treatment process, heated in tubular heater
To 200 ~ 400 DEG C, heat preservation 5 ~ 15 hours is to get to copper and iron sulphur optoelectronic film.
The present invention does not need high vacuum condition, low to instrument and equipment requirement, and production cost is low, and production efficiency is high, is easy to grasp
Make.Gained copper and iron sulphur optoelectronic film has preferable continuity and uniformity, main phase CuFeS2Inexpensive big rule may be implemented in phase
The industrialized production of mould.
Description of the drawings
Fig. 1 is 140 ~ 220 DEG C of heat preservations, 10 hours XRD comparison diagrams for preparing sample.
Specific implementation mode
Embodiment 1
A. the cleaning of glass substrate or silicon chip：Cleaning substrate is carried out as previously described, and size is 20mm × 20mm × 2mm.
It b. can be first by the CuCl of 0.1705g2.2H2The water that 1mL is added in O in vial makes it fully dissolve, then successively
The FeCl of 0.2702g is added in vial3.6H2The Na of O and 0.2481g2S2O3.5H2O makes its full and uniform mixed dissolution.
C. above-mentioned solution is dripped on the glass substrate being placed on sol evenning machine, restarts sol evenning machine, sol evenning machine is with 200
Rev/min rotation 5 seconds, with 3000 revs/min rotate 15 seconds, after keeping the solution coating in drop uniform, after being dried to substrate, again
It repeats to dry again after dripping upper previous solu and spin coating, is so repeated 6 times, certain thickness presoma has then been obtained on substrate
Film sample.
D. precursor thin-film sample obtained by step c is placed on holder, be put into hydrazine hydrate can closed container, make
Precursor thin-film sample is not contacted with hydrazine.The hydrazine hydrate amount of being put into is 0.5mL.It will be above-mentioned close equipped with precursor thin-film sample
It closes container to be put into baking oven, is heated to 180 DEG C, soaking time 10 hours is then cooled to room temperature taking-up.
E. it takes out after spontaneously drying, repeats b, c and Step d 4 times, with the thickness of film prepared by increase, reduce film and lack
It falls into.
F. by step e gains, after so that its room temperature is spontaneously dried, increase heat treatment process, heated in tubular heater
To 300 DEG C, heat preservation 10 hours is to get to copper and iron sulphur optoelectronic film.
Claims (5)
1. a kind of method preparing copper and iron sulphur optoelectronic film with chloride, including it is following steps in sequence：
A. the cleaning of glass substrate or silicon chip；
B. by the CuCl of 0.1705g2.2H2The water that 1mL is added in O in vial makes it fully dissolve, then successively in vial
The FeCl of 0.2702g is added3.6H2The Na of O and 0.2481g2S2O3.5H2O makes its full and uniform mixed dissolution；
C. the substrate of solution described in the even spread step b of surface is made, naturally dry obtains precursor thin-film sample；
D. precursor thin-film sample obtained by step c is placed on holder, be put into hydrazine hydrate can closed container, make presoma
Film sample is not contacted with hydrazine hydrate；The hydrazine hydrate amount of being put into is 0.5mL；It will be above-mentioned closed equipped with precursor thin-film sample
Container is put into baking oven, is heated between 160 ~ 220 DEG C, and soaking time 2 ~ 40 hours is then cooled to room temperature taking-up；
E. it takes out after spontaneously drying, repeats the above steps 2 ~ 6 times, with the thickness of film prepared by increase；
F. by step e gains, after so that its room temperature is spontaneously dried, increase heat treatment process, 200 are heated in tubular heater
~ 400 DEG C, heat preservation 5 ~ 15 hours is to get to copper and iron sulphur optoelectronic film.
2. a kind of method preparing copper and iron sulphur optoelectronic film with chloride as described in claim 1, which is characterized in that step a
Sheet glass or silicon chip are switched to 20mm × 20mm × 2mm sizes as film substrate, are then cleaned with deionized water by the cleaning
It 2 ~ 3 times, then passes through dilute sulfuric acid and boils 30 ~ 40min, 40 ~ 50min of heating water bath, deionized water ultrasonic cleaning 20min, this three
After a important cleaning step, saved backup with hydrogen peroxide dipping.
3. a kind of method preparing copper and iron sulphur optoelectronic film with chloride as described in claim 1, which is characterized in that step b
The solvent is aqueous solution, and the CuCl being wherein added2.2H2O、FeCl3.6H2O、Na2S2O3.5H2The amount of O and aqueous solvent can root
According to the proportional variation of number of film.
4. a kind of method preparing copper and iron sulphur optoelectronic film with chloride as described in claim 1, which is characterized in that step c
The substrate uniformly smeared is by sol evenning machine spin coating, and sol evenning machine is rotated with 200 ~ 3500 revs/min, is then carried out to substrate
After drying, so repeats 2 ~ 8 times again, obtained certain thickness precursor thin-film sample.
5. a kind of method preparing copper and iron sulphur optoelectronic film with chloride as described in claim 1, which is characterized in that step d
0.5mL hydrazine hydrates are put into the closed container.
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| CN201810704339.8A CN108807561A (en) | 2018-07-01 | 2018-07-01 | A method of preparing copper and iron sulphur optoelectronic film with chloride |
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| CN201810704339.8A CN108807561A (en) | 2018-07-01 | 2018-07-01 | A method of preparing copper and iron sulphur optoelectronic film with chloride |
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|---|---|---|---|---|
| CN103396009A (en) * | 2013-07-09 | 2013-11-20 | 山东建筑大学 | Method for preparing copper-aluminum-tellurium film |
| WO2015004666A1 (en) * | 2013-07-11 | 2015-01-15 | Yissum Research Development Company Of The Hebrew University Of Jerusalem Ltd. | Thermal doping by vacancy formation in nanocrystals |
| CN105489673A (en) * | 2015-12-17 | 2016-04-13 | 山东建筑大学 | Method for preparing copper-indium sulfide photoelectric thin film by chloride system through two-step method |
| CN105932081A (en) * | 2016-06-15 | 2016-09-07 | 山东建筑大学 | Method for preparing copper indium sulfide photoelectric thin film from copper chloride |
-
2018
- 2018-07-01 CN CN201810704339.8A patent/CN108807561A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103396009A (en) * | 2013-07-09 | 2013-11-20 | 山东建筑大学 | Method for preparing copper-aluminum-tellurium film |
| WO2015004666A1 (en) * | 2013-07-11 | 2015-01-15 | Yissum Research Development Company Of The Hebrew University Of Jerusalem Ltd. | Thermal doping by vacancy formation in nanocrystals |
| CN105489673A (en) * | 2015-12-17 | 2016-04-13 | 山东建筑大学 | Method for preparing copper-indium sulfide photoelectric thin film by chloride system through two-step method |
| CN105932081A (en) * | 2016-06-15 | 2016-09-07 | 山东建筑大学 | Method for preparing copper indium sulfide photoelectric thin film from copper chloride |
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Application publication date: 20181113 |