CN105097989A - Method for preparing zinc sulfide photoelectric film - Google Patents
Method for preparing zinc sulfide photoelectric film Download PDFInfo
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- CN105097989A CN105097989A CN201410261270.8A CN201410261270A CN105097989A CN 105097989 A CN105097989 A CN 105097989A CN 201410261270 A CN201410261270 A CN 201410261270A CN 105097989 A CN105097989 A CN 105097989A
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- zinc sulfide
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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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
A method for preparing a zinc sulfide photoelectric film belongs to the field of the photoelectric film preparation technology. The method includes the following steps of: firstly cleaning a substrate; then putting ZnO and CH4N2S into a solvent; obtaining a precursor film on the substrate by using a spin coating method, and drying the precursor film; putting the precursor film into a container capable of being sealed and having hydrazine hydrate; enabling the precursor film sample to be not in contact with the hydrazine hydrate; finally performing drying; and obtaining the zinc sulfide photoelectric film. The method for preparing the zinc sulfide photoelectric film does not need high temperature or high vacuum conditions, and has advantages of low requirement to apparatuses, low production cost, high production efficiency and easy operation. The obtained zinc sulfide photoelectric film has good continuity and uniformity. In the new technology, it is easy to control components and structure of object products. The preparation method for preparing the zinc sulfide photoelectric film with the high performance is low in cost and can be industrialized.
Description
Technical field
The invention belongs to optoelectronic film preparing technical field, particularly relate to a kind of method preparing zinc sulfide optoelectronic film.
Background technology
The world today, people more and more pay close attention to the problem such as consumption and environmental pollution of non-regeneration energy.Solar energy, as the free of contamination new forms of energy of a kind of high-efficiency cleaning, has become an important component part in new energy resource structure.Thin-film solar cells causes more concerns as the high efficiency solar cell of one, and the mankind constantly probe into and research and develop cheap, that material environment friendly is nontoxic solar cell.
In film photovoltaic material, resilient coating ZnS is group Ⅱ-Ⅵ compound semiconductor, has zincblende and buergerite two kinds of crystal structures.The theoretical energy gap of ZnS is about 3.7eV, is widely used in the fields such as two pole luminous tubes, device for non-linear optical, transducer, laser, the same with CdS, and ZnS can be used for semi-conductor cell and photoelectric device as solar cell and photodetector.But ZnS and CdS compares has that price is low, toxicity is little, energy gap is wider mates more with CIS lattice.CdS is replaced in the CIS battery of preparation, to obtain good result as cushioning layer material using ZnS.Therefore, the preparation of ZnS film and characteristic research will play positive impetus to the development and application of solar-electricity device.
At present, the preparation method of ZnS film is a lot, can be divided into wet method and dry method synthetic reaction type; Chemical vapour deposition technique, gas-phase reaction method, liquid phase synthesizing method, elemental direct reaction method, chemical bath deposition method, electrochemical deposition method, molecular beam epitaxy and photochemical precipitation method etc. can be divided into from the technical characterstic of synthesis.This experiment adopts spin coating-chemical co-reducing process to prepare zinc sulfide optoelectronic film.
Method is the same as previously described, and other method also has different defects.Related to the present invention also has as Publication about Document:
[1]ZhangR,WangB,WeiL,etal.GrowthandpropertiesofZnSthinfilmsbysulfidationofsputterdepositedZn[J].Vacuum,2012,86(8):1210-1214.
Article is mainly described through sulfuration and prepares ZnS film, have studied the impact of sulfuration on ZnS of different temperatures.400 DEG C time, part Zn cures, and 500 DEG C time, Zn all cures and along C axle preferrel orientation, band gap is 3.64eV
[2]ZhouL,TangN,WuS.InfluenceofdepositiontemperatureonZnSthinfilmperformancewithchemicalbathdeposition[J].SurfaceandCoatingsTechnology,2013,228:S146-S149.
With ZnSO
4, ammoniacal liquor and SC (NH
2)
2deng being raw material, adopt chemical bath legal system for ZnS, research temperature is on the impact of deposit film.Zinc sulfide film thickness is about 73-200 nanometer, and the transmissivity of zinc sulfide film is high by 78%, can reduce transmissivity by annealing.
[3]?zkanM,EkemN,PatS,etal.ZnSthinfilmdepositiononSiliconandglasssubstratesbyThermionicvacuumArc[J].MaterialsScienceinSemiconductorProcessing,2012,15(2):113-119.
Hot cathode Abstract The vacuum arc technique is adopted to be coated with ZnS film on silicon chip and sheet glass, on silicon chip and sheet glass, the surface roughness of film is respectively 1.17 and 1.54nm, all along (0114) preferred orientation, mean refractive index value is 2.05, and band-gap energy is about 3.7eV.
[4]XuX,WangF,LiuJ,etal.StructuralandopticalstudiesofZnSnanocrystalfilmspreparedbysulfosalicylicacid(C
7H
6O
6S)-assistedgalvanostaticdepositionwithsubsequentannealing[J].ThinSolidFilms,2012,520(23):6864-6868.
Essentially describing by adding auxiliary constant current current potential at deposition on glass ZnS, then heat-treating.Obtain wurtzite structure energy gap product on the low side by deposition, can energy gap be improved by heat treatment.
[5]DhanyaAC,MuraliKV,PreethaKC,etal.EffectofdepositiontimeonopticalandluminescencepropertiesofZnSthinfilmspreparedbyphotoassistedchemicaldepositiontechnique[J].MaterialsScienceinSemiconductorProcessing,2013,16(3):955-962.
By the method for PCD at deposition on glass ZnS, the product band-gap energy obtained all and theoretical calculation.Photoluminescence spectra observes two continuous print emission bands about 450 and 470nm, and intensity is found the thickness depending on film.
summary of the invention
The present invention for solving the deficiencies in the prior art, and invents a kind of diverse with the preparation method of prior art, the preparation technology of zinc sulphide solar cell optoelectronic thin film material.
The present invention adopts spin coating-chemical co-reducing process to prepare zinc sulfide optoelectronic film material, adopts soda-lime glass sheet or silicon chip to be substrate, with ZnO and CH
4n
2s is raw material, one or more mixture in deionized water, ethanol, ethylene glycol, hydrochloric acid is solvent, the precursor thin-film of certain thickness zinc sulphide is first prepared with spin-coating method, element metering is than being ZnS, take hydrazine hydrate as reducing agent, heat at a lower temperature in closed container, make precursor thin-film reduce concurrent GCMS computer and be obtained by reacting target product.
Concrete preparation method of the present invention comprises the step of following order:
A. carrying out the cleaning of substrate, is that volume ratio HCl put into by 2mm × 2mm glass substrate or silicon chip: the solution of distilled water=1:50 by size, and 30min is boiled in heating; Again substrate is put into volume ratio hydrogen peroxide: the solution of HCl=1:1, heating water bath 90 DEG C insulation 30min; Again in distilled water by substrate supersonic oscillations 10min; Substrate obtained above is emitted in glass dish send in baking oven and dries for masking.
B. by ZnO and CH
4n
2s puts into solvent, makes the material Homogeneous phase mixing in solution.Specifically, can by 1.06 ~ 2.13 parts of ZnO, 1.0 ~ 2.0 parts of CH
4n
2s puts into the solvent of 60 ~ 240 parts, makes the material Homogeneous phase mixing in solution, and wherein solvent is one or more the mixture in deionized water, ethanol, ethylene glycol, hydrochloric acid.
C. make the substrate of solution described in the rapid b of outside uniform application, and dry, obtain precursor thin-film sample.Above-mentioned solution can be dripped on the substrate that is placed on sol evenning machine, restart sol evenning machine and rotate certain hour with 200 ~ 3500 revs/min, after making the solution coat on dripping even, and after substrate is dried, dry again after again repeating to drip upper previous solu and spin coating, repetition like this 4 ~ 8 times, so obtain certain thickness precursor thin-film sample on substrate.
D. be placed on support by step c gained precursor thin-film sample, what be placed with hydrazine hydrate can closed container, and precursor thin-film sample is not contacted with hydrazine.The hydrazine hydrate amount of putting into is 60.0 ~ 105.0 parts.The above-mentioned closed container that precursor thin-film sample is housed is put into baking oven, is heated between 160 ~ 220 DEG C, temperature retention time 20 ~ 40 hours, then cool to room temperature takes out.
E. by steps d products therefrom, after carrying out natural drying, namely zinc sulfide optoelectronic film is obtained.
The present invention does not need high temperature high vacuum condition, and require low to instrument and equipment, production cost is low, and production efficiency is high, is easy to operation.Gained zinc sulfide optoelectronic film has good continuity and uniformity, the composition and structure of the easy control objectives product of this new technology, providing a kind of low cost, can realize the method for large-scale industrial production for preparing high performance zinc sulfide optoelectronic film.
Accompanying drawing explanation
Fig. 1 is the XRD collection of illustrative plates being heated to 180 DEG C of temperature retention times, 20 hours gained zinc sulfide optoelectronic film.
Embodiment
embodiment 1
A. the cleaning of substrate: carry out cleaning glass substrate (size is 2mm × 2mm) as previously mentioned.
B. by 1.06 parts of ZnO and 1 part CH
4n
2s puts into vial, adds 77.037 parts of ethanol, utilizes more than ultrasonic vibration 30min, makes the material Homogeneous phase mixing in solution.
C. above-mentioned solution is dripped on the glass substrate be placed on sol evenning machine, restart sol evenning machine, sol evenning machine rotates 5 seconds with 200 revs/min, rotate 15 seconds with 3000 revs/min, after making the solution coat on dripping even, after substrate is dried, dry again after again repeating to drip upper previous solu and spin coating, repetition like this 8 times, so obtain certain thickness precursor thin-film sample on substrate.
D. the precursor thin-film sample of above-mentioned technique gained is put into sealable container, and put into 77.037 parts of hydrazine hydrates, precursor thin-film sample is placed on support and makes it not contact with hydrazine, the closed container that precursor thin-film sample is housed is put into baking oven, be heated to 180 DEG C, temperature retention time 20 hours, then cool to room temperature takes out.
E. by above-mentioned steps d products therefrom, after carrying out natural drying, namely zinc sulfide optoelectronic film is obtained.
Claims (5)
1. prepare a method for zinc sulfide optoelectronic film, comprise the step of following order: the cleaning of a. glass substrate or silicon chip;
B. by 1.06 ~ 2.13 parts of ZnO, 1.0 ~ 2.0 parts of CH
4n
2s puts into the solvent of 60 ~ 240 parts, makes the material Homogeneous phase mixing in solution; C. make the substrate of solution described in outside uniform application step b, and dry, obtain precursor thin-film sample;
D. step c gained precursor thin-film sample is placed on support, what be placed with hydrazine hydrate can closed container, precursor thin-film sample is not contacted with hydrazine, the closed container that precursor thin-film sample is housed is put into baking oven, be heated between 160 ~ 220 DEG C, temperature retention time 20 ~ 40 hours, then cool to room temperature takes out; E. by steps d products therefrom, carry out natural drying, obtain zinc sulfide optoelectronic film.
2. a kind of method preparing zinc sulfide optoelectronic film as claimed in claim 1, it is characterized in that, clean described in step a, be 2mm × 2mm glass substrate or silicon chip by size, first put into volume ratio HCl: 30min is boiled in the solution heating of distilled water=1:50; Again substrate is put into volume ratio hydrogen peroxide: the solution of HCl=1:1, heating water bath 90 DEG C insulation 30min; Again in distilled water by substrate supersonic oscillations; Substrate obtained above is emitted in glass dish send in baking oven and dries for masking.
3. a kind of method preparing zinc sulfide optoelectronic film as claimed in claim 1, it is characterized in that, solvent described in step b is at least one in deionized water, ethanol, ethylene glycol, hydrochloric acid.
4. a kind of method preparing zinc sulfide optoelectronic film as claimed in claim 1, it is characterized in that, the substrate of even spread described in step c, by sol evenning machine spin coating, sol evenning machine is with 200 ~ 3500 revs/min of rotations, then after substrate being dried, again so repeat 2 ~ 15 times, obtain certain thickness precursor thin-film sample.
5. a kind of method preparing zinc sulfide optoelectronic film as claimed in claim 1, is characterized in that, put into 60.0 ~ 105.0 parts of hydrazine hydrates in closed container described in steps d.
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| CN201410261270.8A CN105097989A (en) | 2014-06-13 | 2014-06-13 | Method for preparing zinc sulfide photoelectric film |
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| CN201410261270.8A CN105097989A (en) | 2014-06-13 | 2014-06-13 | Method for preparing zinc sulfide photoelectric film |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105514215A (en) * | 2015-12-16 | 2016-04-20 | 山东建筑大学 | Method for preparing zinc sulfide photoelectric film through zinc oxide |
| CN106558476A (en) * | 2016-12-01 | 2017-04-05 | 梁结平 | A kind of method for preparing zinc oxide/sulfide composite photoelectric film |
| CN107354448A (en) * | 2017-08-07 | 2017-11-17 | 旭科新能源股份有限公司 | A kind of CBD reactive deposition device and methods of continuous production ZnS films |
| CN109037642A (en) * | 2018-08-07 | 2018-12-18 | 河源广工大协同创新研究院 | The preparation method of lithium ion battery negative material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102603202A (en) * | 2012-03-12 | 2012-07-25 | 山东建筑大学 | Method for preparing tin selenide photoelectric thin film |
| CN103400894A (en) * | 2013-07-09 | 2013-11-20 | 山东建筑大学 | Method for preparing zinc sulfide optoelectronic film |
| CN103474575A (en) * | 2013-09-26 | 2013-12-25 | 天津理工大学 | Hybrid solar cell with zinc oxysulfide serving as electron transfer layer and preparation method thereof |
-
2014
- 2014-06-13 CN CN201410261270.8A patent/CN105097989A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102603202A (en) * | 2012-03-12 | 2012-07-25 | 山东建筑大学 | Method for preparing tin selenide photoelectric thin film |
| CN103400894A (en) * | 2013-07-09 | 2013-11-20 | 山东建筑大学 | Method for preparing zinc sulfide optoelectronic film |
| CN103474575A (en) * | 2013-09-26 | 2013-12-25 | 天津理工大学 | Hybrid solar cell with zinc oxysulfide serving as electron transfer layer and preparation method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105514215A (en) * | 2015-12-16 | 2016-04-20 | 山东建筑大学 | Method for preparing zinc sulfide photoelectric film through zinc oxide |
| CN106558476A (en) * | 2016-12-01 | 2017-04-05 | 梁结平 | A kind of method for preparing zinc oxide/sulfide composite photoelectric film |
| CN107354448A (en) * | 2017-08-07 | 2017-11-17 | 旭科新能源股份有限公司 | A kind of CBD reactive deposition device and methods of continuous production ZnS films |
| CN109037642A (en) * | 2018-08-07 | 2018-12-18 | 河源广工大协同创新研究院 | The preparation method of lithium ion battery negative material |
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Application publication date: 20151125 |