CN108878556A - A method of preparation copper and iron selenium conductive film is assisted with selenium powder - Google Patents
A method of preparation copper and iron selenium conductive film is assisted with selenium powder Download PDFInfo
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- CN108878556A CN108878556A CN201810703712.8A CN201810703712A CN108878556A CN 108878556 A CN108878556 A CN 108878556A CN 201810703712 A CN201810703712 A CN 201810703712A CN 108878556 A CN108878556 A CN 108878556A
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 22
- 239000010949 copper Substances 0.000 title claims abstract description 22
- WALCGGIJOOWJIN-UHFFFAOYSA-N iron(ii) selenide Chemical compound [Se]=[Fe] WALCGGIJOOWJIN-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims abstract description 16
- 239000010408 film Substances 0.000 claims abstract description 36
- 239000002243 precursor Substances 0.000 claims abstract description 21
- 239000010409 thin film Substances 0.000 claims abstract description 21
- 239000000758 substrate Substances 0.000 claims abstract description 19
- 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 15
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 239000011669 selenium Substances 0.000 claims abstract description 9
- 238000004140 cleaning Methods 0.000 claims abstract description 7
- 239000005357 flat glass Substances 0.000 claims abstract description 6
- 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
- 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
- 239000000243 solution Substances 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 7
- 229910021591 Copper(I) chloride Inorganic materials 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 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
- 238000004090 dissolution Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 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
- 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
- 238000004506 ultrasonic cleaning Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- MPTQRFCYZCXJFQ-UHFFFAOYSA-L copper(II) chloride dihydrate Chemical compound O.O.[Cl-].[Cl-].[Cu+2] MPTQRFCYZCXJFQ-UHFFFAOYSA-L 0.000 abstract description 3
- 238000002425 crystallisation Methods 0.000 abstract description 2
- 230000008025 crystallization Effects 0.000 abstract description 2
- 230000035484 reaction time Effects 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 4
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 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
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 230000005693 optoelectronics 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
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 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
- 229910052951 chalcopyrite Inorganic materials 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
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
- 238000009776 industrial production Methods 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
- 238000002207 thermal evaporation Methods 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
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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
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/0256—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
- H01L31/0264—Inorganic materials
- H01L31/032—Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312
-
- 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
- H01L31/036—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 their crystalline structure or particular orientation of the crystalline planes
- H01L31/0392—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 their crystalline structure or particular orientation of the crystalline planes including thin films deposited on metallic or insulating substrates ; characterised by specific substrate materials or substrate features or by the presence of intermediate layers, e.g. barrier layers, on the substrate
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Engineering & Computer Science (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Photovoltaic Devices (AREA)
- Chemically Coating (AREA)
Abstract
A kind of preparation method assisting preparation copper and iron selenium conductive film with selenium powder, first cleaning glass substrate, then by CuCl2.2H2O、FeCl3.6H2O and Na2Se2O3.5H2O 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 is put into the middle layer of reaction kettle liner, while being put into selenium powder beside the sheet glass for being coated with precursor solution, the lower layer of reaction kettle liner is put into hydrazine hydrate solution, sample is taken out after closed container equipped with precursor thin-film sample is heated to be dried, and can be improved film quality by increasing reaction times and heat treatment process, be obtained copper and iron selenium conductive film.Uniformity of film made from selenium powder and crystallization, which is relatively not added, in gained copper and iron selenium conductive film to get well, and this new process provides a kind of industrialized production method at low cost, achievable to prepare high performance copper and iron selenium conductive film.
Description
Technical field
The invention belongs to optoelectronic film preparation technical field used for solar batteries more particularly to a kind of selenium powder auxiliary preparations
The preparation method of copper and iron selenium conductive film.
Background technique
Copper and iron selenium 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, imitates without light-induced degradation
The advantages that answering, and because the cheap of copper and iron selenium material, rich reserves and the advantages such as nontoxic receive the extensive concern of scientist.
The preparation method of copper and iron selenium 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, preparation 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 that there are also following documents：
[1] Wen H, Li H, He S, et al. Constructing two-dimensional CuFeSe2@Au
heterostructured nanosheets with an amorphous core and a crystalline shell
for enhanced near-infrared light water oxidation. Nanoscale, 2018.
Mainly have studied CuFeSe2@Au heterogeneous structural nano piece, analyzes CuFeSe2The structure feature of@Au nanometer sheet, and
Their photocatalytic activity and high stability to water oxygen.
[2] Zhang B, Liu Y, Zuo Y, et al. Colloidal Synthesis and
Thermoelectric Properties of CuFeSe2 Nanocrystals. Nanomaterials-Basel, 2018.
It mainly has studied and is prepared for CuFeSe using expansible colloid synthetic method2Nano microcrystalline, while having studied CuFeSe2Material
Ingredient, valence state, size and shape and its photoelectric properties.
[3] Dutkova E, Skorvanek I, Sayagues MJ, Zorkovska A, Kovac J, Balaz
P. Mechanochemically Synthesized CuFeSe2 Nanoparticles and Their Properties.
Acta Phys Pol A, 2017.
It mainly has studied and prepares CuFeSe using mechanochemical reaction2Nano particle has studied CuFeSe2The crystal knot of nano particle
Structure, size, magnetism and photoelectric properties.
[4] Carr WD, Morelli DT. The Thermoelectric Properties and Solubility
Limit of CuFeS2(1-x)Se2x. J Electron Mater, 2016.
Mainly have studied CuFeS2(1-x)Se2xThermoelectric property and solubility limit, with selenium replace CuFeS2Middle sulphur position, has studied
The variation of thermoelectricity capability.
[5] Wang W, Jiang J, Ding T, Wang C, Zuo J, Yang Q. Alternative
Synthesis of CuFeSe2 Nanocrystals with Magnetic and Photoelectric Properties.
Acs Appl Mater Inter, 2015.
It mainly has studied and prepares monodispersed CuFeSe using hot solution injection method2Nanocrystal, and analyze the crystalline substance of sample
Body structure and size, magnetism and photoelectric properties.
[6]Lee PC, Ou MN, Zhong ZW, et al. Nonlinear Thickness and Grain Size
Effects on the Thermal Conductivity of CuFeSe2 Thin Films. Chinese J Phys,
2013.
Mainly film thickness and crystallite dimension are had studied to CuFeSe2The influence of thermal conductivity of thin film.
Summary of the invention
The present invention has invented a kind of with the entirely different copper of existing preparation method to solve the deficiency of existing technology of preparing
The preparation process of iron selenium film.
The present invention prepares copper and iron selenium thin-film material using spin coating-chemistry co-reducing process, uses sheet glass or silicon wafer for substrate,
With CuCl2.2H2O、FeCl3.6H2O、Na2Se2O3.5H2O is raw material, is taken water as a solvent, and CuCl is sequentially added2.2H2O、
FeCl3.6H2O、Na2Se2O3.5H2O reacts it sufficiently.Certain thickness copper and iron selenium precursor thin-film is first prepared with spin-coating method,
It is put into the middle layer of reaction kettle liner, while being put into selenium powder beside the sheet glass for being coated with precursor solution, reaction kettle liner
Lower layer be put into hydrazine hydrate solution, contact precursor thin-film sample directly with hydrazine, using hydrazine hydrate as reducing agent,
It is heated at a lower temperature in closed container, precursor thin-film is made to restore concurrent GCMS computer reaction, it can be by increasing reaction times
Improve prepared film quality with heat treatment after reaction, obtains target product.
Specific preparation method of the invention includes following steps in sequence：
A. the cleaning of substrate is carried out, sheet glass or silicon wafer are switched to by this experimental selection sheet glass or silicon wafer first as substrate
Then 20mm × 20mm × 2mm size is 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 Na2Se2O3.5H2O 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 dissolves it sufficiently, then successively
The FeCl of 0.2702g is added in vial3.6H2The Na of O and 0.2481g2Se2O3.5H2O makes its full and uniform mixed dissolution,
The CuCl being wherein added2.2H2O、FeCl3.6H2O、Na2Se2O3.5H2The amount of O and aqueous solvent can be proportional according to the number of film
Variation.
C. the substrate of the external uniform solution as described in step b of production, and dry, obtain precursor thin-film sample.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 in the middle layer of reaction kettle liner, and is put beside film sample
Enter the selenium powder of 0.078g, the lower layer of reaction kettle liner is put into hydrazine hydrate solution, make precursor thin-film sample not with hydrazine hydrate
Contact；The hydrazine hydrate amount of being put into is 0.5mL.The above-mentioned closed container equipped with precursor thin-film sample is put into baking oven, is heated
To between 160 ~ 220 DEG C, soaking time 2 ~ 40 hours, it is then cooled to room temperature taking-up.
E. it takes out after spontaneously drying, repeats b, c and Step d 2 ~ 6 times, to increase the thickness of prepared film, reduce film
Defect.
F. by step e gains, after spontaneously drying its room temperature, increase heat treatment process, heated in tubular heater
To 200 ~ 400 DEG C, 5 ~ 15 hours are kept the temperature to get copper and iron selenium conductive film is arrived.
The present invention does not need high vacuum condition, low to instrument and equipment requirement, and production cost is low, high production efficiency, is easy to grasp
Make.Uniformity of film made from selenium powder and crystallization, which is relatively not added, in gained copper and iron selenium conductive film to get well, main phase CuFeSe2Phase,
Inexpensive large-scale industrial production may be implemented.
Specific embodiment
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 dissolves it sufficiently, then successively
The FeCl of 0.2702g is added in vial3.6H2The Na of O and 0.321g2Se2O3.5H2O makes its full and uniform mixed dissolution.
C. above-mentioned solution is dripped in 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, make drop on solution coating it is uniform after, 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 in the middle layer of reaction kettle liner, and is put beside film sample
Enter the selenium powder of 0.078g, the lower layer of reaction kettle liner is put into hydrazine hydrate solution, make precursor thin-film sample not with hydrazine hydrate
Contact；The hydrazine hydrate amount of being put into is 0.5mL.The above-mentioned closed container equipped with precursor thin-film sample is put into baking oven, is heated
To 180 DEG C, soaking time 10 hours, it is then cooled to room temperature taking-up.
E. it takes out after spontaneously drying, repeats b, c and Step d 4 times, to increase the thickness of prepared film, reduce film and lack
It falls into.
F. by step e gains, after spontaneously drying its room temperature, increase heat treatment process, heated in tubular heater
To 300 DEG C, 10 hours are kept the temperature to get copper and iron selenium conductive film is arrived.
Claims (5)
1. a kind of method for assisting preparation copper and iron selenium conductive film with selenium powder, 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 dissolves it sufficiently, then successively in vial
The FeCl of 0.2702g is added3.6H2The Na of O and 0.321g2Se2O3.5H2O makes its full and uniform mixed dissolution；
C. the substrate of solution described in surface even spread step b is made, naturally dry obtains precursor thin-film sample；
D. precursor thin-film sample obtained by step c is placed in the middle layer of reaction kettle liner, and is put into beside film sample
The selenium powder of 0.078g, the lower layer of reaction kettle liner are put into hydrazine hydrate solution, connect precursor thin-film sample with hydrazine hydrate
Touching；The hydrazine hydrate amount of being put into is 0.5mL；The above-mentioned closed container equipped with precursor thin-film sample is put into baking oven, is heated to
Between 160 ~ 220 DEG C, soaking time 2 ~ 40 hours, it is then cooled to room temperature taking-up；
E. it takes out after spontaneously drying, repeats the above steps 2 ~ 6 times, to increase the thickness of prepared film；
F. by step e gains, after spontaneously drying its room temperature, increase heat treatment process, 200 are heated in tubular heater
~ 400 DEG C, 5 ~ 15 hours are kept the temperature to get copper and iron selenium conductive film is arrived.
2. a kind of method for assisting preparation copper and iron selenium conductive film with selenium powder as described in claim 1, which is characterized in that step
It is cleaned described in a, sheet glass or silicon wafer is switched to 20mm × 20mm × 2mm size as film substrate, it is then clear with deionized water
It washes 2 ~ 3 times, then passes through dilute sulfuric acid and boil 30 ~ 40min, 40 ~ 50min of heating water bath, deionized water ultrasonic cleaning 20min, this
After three important cleaning steps, saved backup with hydrogen peroxide dipping.
3. a kind of preparation method for assisting preparation copper and iron selenium conductive film with selenium powder as described in claim 1, which is characterized in that
Solvent described in step b is aqueous solution, and the CuCl being wherein added2.2H2O、FeCl3.6H2O、Na2Se2O3.5H2O and aqueous solvent
Amount can be according to how much proportional variations of film.
4. a kind of preparation method for assisting preparation copper and iron selenium conductive film with selenium powder as described in claim 1, which is characterized in that
The substrate uniformly smeared described in step c is by sol evenning machine spin coating, and sol evenning machine is rotated with 200 ~ 3500 revs/min, then to substrate
After being dried, so repeats 2 ~ 8 times again, obtained certain thickness precursor thin-film sample.
5. a kind of preparation method for assisting preparation copper and iron selenium conductive film with selenium powder as described in claim 1, which is characterized in that
The selenium powder of 0.078g is put into described in step d beside film sample, the lower layer of reaction kettle liner is put into hydrazine hydrate solution, makes
Precursor thin-film sample is not contacted with hydrazine hydrate；The hydrazine hydrate amount of being put into is 0.5mL.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810703712.8A CN108878556A (en) | 2018-07-01 | 2018-07-01 | A method of preparation copper and iron selenium conductive film is assisted with selenium powder |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810703712.8A CN108878556A (en) | 2018-07-01 | 2018-07-01 | A method of preparation copper and iron selenium conductive film is assisted with selenium powder |
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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 |
| CN105489672A (en) * | 2015-12-17 | 2016-04-13 | 山东建筑大学 | Method for preparing copper indium diselenide photoelectric thin film by chloride system through two-step method |
| CN105552166A (en) * | 2015-12-16 | 2016-05-04 | 山东建筑大学 | Method for preparing copper-indium-diselenide photoelectric film by two-step method of nitrate system |
-
2018
- 2018-07-01 CN CN201810703712.8A patent/CN108878556A/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 |
| CN105552166A (en) * | 2015-12-16 | 2016-05-04 | 山东建筑大学 | Method for preparing copper-indium-diselenide photoelectric film by two-step method of nitrate system |
| CN105489672A (en) * | 2015-12-17 | 2016-04-13 | 山东建筑大学 | Method for preparing copper indium diselenide photoelectric thin film by chloride system through two-step method |
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