CN108831963A - A method of copper and iron selenium conductive film is prepared with sulfate - Google Patents

A method of copper and iron selenium conductive film is prepared with sulfate Download PDF

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Publication number
CN108831963A
CN108831963A CN201810705112.5A CN201810705112A CN108831963A CN 108831963 A CN108831963 A CN 108831963A CN 201810705112 A CN201810705112 A CN 201810705112A CN 108831963 A CN108831963 A CN 108831963A
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film
conductive film
copper
iron selenium
precursor thin
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刘科高
孙齐磊
荆明星
姬明
石磊
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Shandong Jianzhu University
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Shandong Jianzhu University
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    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES; ELECTRIC SOLID STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H01L31/00Semiconductor devices sensitive to infra-red 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
    • H01L31/18Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES; ELECTRIC SOLID STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104Forming layers
    • H01L21/02365Forming inorganic semiconducting materials on a substrate
    • H01L21/02367Substrates
    • H01L21/0237Materials
    • H01L21/02373Group 14 semiconducting materials
    • H01L21/02381Silicon, silicon germanium, germanium
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES; ELECTRIC SOLID STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104Forming layers
    • H01L21/02365Forming inorganic semiconducting materials on a substrate
    • H01L21/02367Substrates
    • H01L21/0237Materials
    • H01L21/02422Non-crystalline insulating materials, e.g. glass, polymers
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES; ELECTRIC SOLID STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104Forming layers
    • H01L21/02365Forming inorganic semiconducting materials on a substrate
    • H01L21/02518Deposited layers
    • H01L21/02521Materials
    • H01L21/02568Chalcogenide semiconducting materials not being oxides, e.g. ternary compounds
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES; ELECTRIC SOLID STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104Forming layers
    • H01L21/02365Forming inorganic semiconducting materials on a substrate
    • H01L21/02612Formation types
    • H01L21/02617Deposition types
    • H01L21/02623Liquid deposition
    • H01L21/02628Liquid deposition using solutions
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES; ELECTRIC SOLID STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104Forming layers
    • H01L21/02365Forming inorganic semiconducting materials on a substrate
    • H01L21/02656Special treatments
    • H01L21/02664Aftertreatments
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES; ELECTRIC SOLID STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H01L31/00Semiconductor devices sensitive to infra-red 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
    • H01L31/0248Semiconductor devices sensitive to infra-red 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
    • H01L31/0256Semiconductor devices sensitive to infra-red 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
    • H01L31/0264Inorganic materials
    • H01L31/032Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product

Abstract

A method of copper and iron selenium conductive film being prepared with sulfate, belongs to optoelectronic film preparation technical field, the present invention obtains as follows, first cleaning glass substrate, then by CuSO4·5H2O、FeSO4·7H2O and SeO2It is sequentially placed into aqueous solvent, a small amount of salt sour solvent is added after being sufficiently mixed uniformly, prepare clear transparent solutions, precursor thin-film is obtained on the glass sheet with spin-coating method, and naturally dry, be put into hydrazine hydrate can closed container, contact precursor thin-film sample directly with hydrazine, 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.The present invention does not need high temperature high vacuum condition, low to instrument and equipment requirement, and production cost is low, high production efficiency, easily operated.Gained copper and iron selenium conductive film has preferable continuity and uniformity, 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

A method of copper and iron selenium conductive film is prepared with sulfate
Technical field
The invention belongs to optoelectronic film preparation technical field used for solar batteries more particularly to a kind of copper is prepared with sulfate The method of iron selenium conductive film.
Background technique
Copper and iron selenium is a kind of ternary I-III-VI2Compound semiconductor has eskebornite tetragonal crystal structure, The band gap of copper and iron selenium block materials is 0.16 eV, and it is that a kind of p-type of low band gaps is partly led that the band gap of nanoparticle, which is 0.95 eV, Body has good application prospect in terms of photoelectricity and solar energy conversion.
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 thin-film material.
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 CuSO4·5H2O、FeSO4·7H2O、SeO2CuSO is sequentially added using water and hydrochloric acid as solvent for raw material4·5H2O、 FeSO4·7H2O、SeO2, react it sufficiently.Certain thickness copper and iron selenium precursor thin-film is first prepared with spin-coating method, with hydration Hydrazine is reducing agent, is heated at a lower temperature in closed container, so that precursor thin-film is restored concurrent GCMS computer reaction, can lead to Heat treatment improves prepared film quality after crossing increase reaction times and 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 CuSO4·5H2O、FeSO4·7H2O and SeO2It is sequentially placed into solvent, mixes the substance in solution uniformly It closes.Specifically, by the CuSO of 0.250g4·5H2The water that 1mL is added in O in vial dissolves it sufficiently, then successively toward glass The FeSO of 0.278g is added in glass bottle4·7H2The SeO of O and 0.221g2Make its full and uniform mixed dissolution, the salt of 0.5mL is added Acid solution is to clear, wherein the CuSO being added4·5H2O、FeSO4·7H2O、SeO2, aqueous solvent and hydrochloric acid amount can basis The proportional variation of number of film.
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 on bracket, 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, be 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.Gained copper and iron selenium conductive film has preferable continuity and uniformity, main phase CuFeSe2Phase may be implemented inexpensive big The industrialized production of scale.
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 CuSO of 0.250g4·5H2The water that 1mL is added in O in vial dissolves it sufficiently, then successively The FeSO of 0.278g is added in vial4·7H2The SeO of O and 0.221g2Make its full and uniform mixed dissolution, 0.5mL is added Hydrochloric acid solution to clear.
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 on bracket, 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 200 DEG C, soaking time 10 hours, be 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 with sulfate preparation copper and iron selenium conductive film, including it is following steps in sequence:
A. the cleaning of glass substrate or silicon chip;
B. by the CuSO of 0.250g4·5H2The water that 1mL is added in O in vial dissolves it sufficiently, then successively in vial The FeSO of 0.278g is added4·7H2The SeO of O and 0.221g2Make its full and uniform mixed dissolution, the hydrochloric acid solution of 0.5mL is added To clear;
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 on bracket, 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, 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, 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 with sulfate preparation copper and iron selenium conductive film as described in claim 1, which is characterized in that step a Sheet glass or silicon wafer are switched to 20mm × 20mm × 2mm size 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 with sulfate preparation copper and iron selenium conductive film as described in claim 1, which is characterized in that step b The solvent is aqueous solution, and the CuSO being wherein added4·5H2O、FeSO4·7H2O、SeO2, aqueous solvent and hydrochloric acid amount can root According to the proportional variation of number of film.
4. a kind of method with sulfate preparation copper and iron selenium conductive film 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 with sulfate preparation copper and iron selenium conductive film as described in claim 1, which is characterized in that step d 0.5mL hydrazine hydrate is put into the closed container.
CN201810705112.5A 2018-07-01 2018-07-01 A method of copper and iron selenium conductive film is prepared with sulfate Withdrawn CN108831963A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
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
CN105529243A (en) * 2015-12-16 2016-04-27 山东建筑大学 Method for copper indium diselenide optoelectronic film by sulphate system in two-step process
CN105914246A (en) * 2016-06-15 2016-08-31 山东建筑大学 Method for using copper sulphate and gallium nitrate to prepare copper gallium selenide photoelectric film

Patent Citations (4)

* Cited by examiner, † Cited by third party
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
CN105529243A (en) * 2015-12-16 2016-04-27 山东建筑大学 Method for copper indium diselenide optoelectronic film by sulphate system in two-step process
CN105914246A (en) * 2016-06-15 2016-08-31 山东建筑大学 Method for using copper sulphate and gallium nitrate to prepare copper gallium selenide photoelectric film

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Application publication date: 20181116