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CN105789373A - Method for preparing copper-based sulfoselenide semiconductor thin film - Google Patents

Method for preparing copper-based sulfoselenide semiconductor thin film Download PDF

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Publication number
CN105789373A
CN105789373A CN201610008801.1A CN201610008801A CN105789373A CN 105789373 A CN105789373 A CN 105789373A CN 201610008801 A CN201610008801 A CN 201610008801A CN 105789373 A CN105789373 A CN 105789373A
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copper
sulfoselenide
thin film
sulfur
spin
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罗文俊
关中杰
温鑫
张川
邹志刚
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Nanjing University
Kunshan Innovation Institute of Nanjing University
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Nanjing University
Kunshan Innovation Institute of Nanjing University
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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10F—INORGANIC SEMICONDUCTOR DEVICES SENSITIVE TO INFRARED RADIATION, LIGHT, ELECTROMAGNETIC RADIATION OF SHORTER WAVELENGTH OR CORPUSCULAR RADIATION
    • H10F71/00—Manufacture or treatment of devices covered by this subclass
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10F—INORGANIC SEMICONDUCTOR DEVICES SENSITIVE TO INFRARED RADIATION, LIGHT, ELECTROMAGNETIC RADIATION OF SHORTER WAVELENGTH OR CORPUSCULAR RADIATION
    • H10F77/00—Constructional details of devices covered by this subclass
    • H10F77/10—Semiconductor bodies
    • H10F77/12—Active materials
    • H10F77/126—Active materials comprising only Group I-III-VI chalcopyrite materials, e.g. CuInSe2, CuGaSe2 or CuInGaSe2 [CIGS]
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10F—INORGANIC SEMICONDUCTOR DEVICES SENSITIVE TO INFRARED RADIATION, LIGHT, ELECTROMAGNETIC RADIATION OF SHORTER WAVELENGTH OR CORPUSCULAR RADIATION
    • H10F77/00—Constructional details of devices covered by this subclass
    • H10F77/10—Semiconductor bodies
    • H10F77/12—Active materials
    • H10F77/128—Active materials comprising only Group I-II-IV-VI kesterite materials, e.g. Cu2ZnSnSe4 or Cu2ZnSnS4
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy
    • Y02E10/541—CuInSe2 material PV cells
    • 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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Abstract

本发明涉及一种高效光电性能铜基硫硒化物半导体薄膜，为多元铜基硫硒化物材料，化学通式为Cux1M1x2M2x3(SSe)x4，M1和M2为不同的金属元素，且分别为Zn、Sn、Ge、Si、In、Ga、Al中的一种；多元铜基硫硒化物为铜锌锡硫或CuGaS2薄膜；制备方法采用溶液‑旋涂法，简单的湿度调控方法制备高效光电性能的多元铜基硫硒化物半导体薄膜。通过调控前驱体溶液所处的环境湿度使多元铜基硫硒化物的光电性能得到显著提升。此湿度调控方法操作简单，且具有通用性。

The invention relates to a copper-based sulfur selenide semiconductor thin film with high photoelectric performance, which is a multi-component copper-based sulfur selenide material, the general chemical formula is Cu x1 M1 x2 M2 x3 (SSe) x4 , M1 and M2 are different metal elements, and They are one of Zn, Sn, Ge, Si, In, Ga, Al respectively; the multi-component copper-based sulfoselenide is copper zinc tin sulfur or CuGaS 2 film; the preparation method adopts solution-spin coating method, simple humidity control method Preparation of multi-component copper-based sulfoselenide semiconductor thin films with high photoelectric performance. The photoelectric performance of the multi-component copper-based sulfoselenide is significantly improved by adjusting the ambient humidity of the precursor solution. This humidity control method is simple to operate and has universality.

Description

One prepares cuprio sulfoselenide semiconductor film film method
Technical field
The present invention relates to the preparation method of a kind of photoelectric properties improving multi-element Cu-base sulfoselenide semiconductive thin film
Background technology
Along with sustainable growth and the rapid development of economy of world population, energy resource consumption can be increasing.And the energy in modern times Carrier remains traditional non-renewable fossil energy-coal, oil, natural gas etc..On the one hand, fossil energy is a large amount of Consume and make it exhausted at last.On the other hand, fossil energy in use can produce substantial amounts of greenhouse gases and pollution Property gas, and then bring serious environmental problem.Therefore, develop reproducible clean energy resource to gradually reduce until finally taking It is to realize the only way of human economic society sustainable development for fossil energy.Solar energy is that the mankind are available the richest Rich regenerative resource, is also most important basic power source.But, although solar energy have total amount abundant, renewable, The advantages such as cleaning, but there is also the shortcomings such as energy density is low, illumination is discontinuous and limit its large-scale actual application.Cause How this, facilitate the capture of economy and storage solar energy to remain the difficult problem utilizing solar energy to be faced on a large scale.Thin film Solar-energy photo-voltaic cell and water decomposition battery are two kinds and can utilize solar energy on a large scale and have the technology of application prospect. Multi-element Cu-base sulfoselenide such as CuIn1-xGaxSe2, Cu2ZnSn(SSe)4(CZTSSe) having suitable band gap, light absorbs High (> 10 of coefficient4cm-1) etc. advantage, be subject in fields such as solar-energy photo-voltaic cell and water decomposition batteries as light absorbing material Arrive the extensive concern of people.But, performance preferably CuIn1-xGaxSe2Or CZTSSe solar energy conversion device It is all to utilize high vacuum method or hydrazine method to prepare.Hydrazine toxicity is relatively big, to bad environmental.Solution-spin-coating method becomes This is cheap, and technique is simple, and environmental friendliness, is one of a kind of Perfected process preparing multi-element Cu-base sulfoselenide thin film.So And, utilize the performance of the multi-element Cu-base sulfoselenide solar energy conversion device that solution-spin-coating method prepares to need further Improve.Therefore, solution-spin-coating method is utilized to prepare high performance multi-element Cu-base sulfoselenide semiconductor film membrane module still It it is a huge challenge.
Summary of the invention
It is an object of the invention to, it is provided that a kind of simple low cost is prepared (especially by humidity regulation) and improved polynary copper The method of base sulfoselenide semiconductor light electrical property, is applied to solar photovoltaic the multi-element Cu-base sulfoselenide prepared Pond or hydrogen production by water decomposition.
Technical scheme: prepare cuprio sulfoselenide semiconductor film film method, described multi-element Cu-base sulfoselenide Chemical general formula is Cux1M1x2M2x3(SSe)x4, M1 and M2 is different metallic elements, and respectively Zn, Sn, Ge, One or two kinds of in Si, In, Ga, Al；Multi-element Cu-base sulfoselenide is copper-zinc-tin-sulfur or CuGaS2Thin film；Tool Body step is:
1) by Schweinfurt green, copper chloride, Cu-lyt., the one or more kinds of arbitrary proportion mixture in copper nitrate With one or any two in the nitrate of M1 and M2 metal ion, chlorate or the acetate described in right 1 Kind arbitrary proportion mixture and thiourea add and be added separately in solvent to be stirred mixing, the presoma obtaining clarification is molten Liquid；Described solvent is ethylene glycol monomethyl ether, and diformazan Asia is mocked, methanol, more than the one or two kinds of in ethanol and ethylene glycol Arbitrary proportion mixture；
2) by step 1) the clarification precursor solution prepared in the environment that relative humidity is 5%-95% aging 0.5-200 hour. On conductive substrates, in the air of 200-550 DEG C, calcining obtains one layer for 1-60 minute in precursor solution spin coating after aging Thin film, repeats above spin coating and the optimal thickness sample of calcining step acquisition 0.05-3 micron；After spin coating and calcining complete, Sample is carried out sulfur selenizing at a temperature of 450-600 DEG C, and the sulfur selenizing time is 20-120 minute, and sulfur selenizing is elemental sulfur Carry out in hydrogen selenide gas with selenium steam atmosphere or hydrogen sulfide；After sulfuration or selenizing complete, obtain about 0.05-3 micron Thick multi-element Cu-base sulfoselenide thin film.
3) by step 1) the transparent precursor solution of gained utilizes step 2) same method is prepared as thin film；Transparent forerunner Do not carry out aging before liquid solution spin coating, but during spin coating, Regulate Environment relative humidity enters between 5%-95% Row spin coating operation.
Described clarification precursor solution, to its aging or different humidity condition backspin under the humidity atmosphere of regulation and control It is coated with the raising each contributing to multi-element Cu-base sulfoselenide film photoelectric performance.
Under the conditions of the relative ambient humidity of 20-30% aging or spin coating operation effect is more preferable.
Described multi-element Cu-base sulfoselenide thin film, may apply to thin-film solar cells, it is also possible to for light emitting diode etc. On electrooptical device.
The method have the benefit that the present invention makes multi-element Cu-base sulfoselenide by the ambient humidity residing for regulation and control precursor solution Photoelectric properties obtain the lifting of about three times.
The inventive method is simple, with low cost, it is easy to large-scale production.It is applicable to solar energy conversion device, such as photovoltaic electric Pond and decomposing water with solar energy etc..
Accompanying drawing explanation
The precursor solution that Fig. 1 is the embodiment of the present invention 1 and comparative example 1 is configured is old under the conditions of high humidity environment The photo figure of (a) (b) afterwards before change.
Fig. 2 be the embodiment of the present invention 1 and comparative example 1 aging before and the CZTS for preparing of aging rear precursor solution thin Film surface and cross section SEM figure.A () and (c) is the surface of the CZTS thin film utilizing aging rear precursor solution to prepare and cuts Face SEM schemes；B () and (d) is surface and the cross section SEM figure of the CZTS thin film utilizing unaged precursor solution to prepare.
Fig. 3 be the embodiment of the present invention 1 and comparative example 1 aging before and the CZTS for preparing of aging rear precursor solution thin The XRD figure of film.
Fig. 4 be the embodiment of the present invention 1 and comparative example 1 aging before and the CZTS for preparing of aging rear precursor solution thin The Raman spectrogram of film.A () is visible Raman spectrogram, (b) is uv raman spectroscopy figure.
Fig. 5 is the embodiment of the present invention 1 and the aging front CZTS light prepared with aging rear precursor solution of comparative example 1 The photoelectric current of negative electrode-potential curve figure.
Fig. 6 is the CuGaS that under the embodiment of the present invention 2 and comparative example 2 different humidity environment prepared by spin coating operation2Thin The XRD figure of film.
Fig. 7 is the CuGaS that under this method embodiment 2 and comparative example 2 different humidity environment prepared by spin coating operation2Light The photoelectric current of negative electrode-potential curve figure.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention will be further described:
Embodiment 1:
Step 1 is by 1.5224g sulfur selenourea, 0.4513g SnCl2·2H2O, 0.7187g Cu (CH3COO)2·H2O with And 0.3271g ZnCl2It is dissolved into successively in the ethylene glycol monomethyl ether solution of 20ml, is sufficiently stirred for being configured to the forerunner of clarification Liquid solution.The precursor solution of clarification is placed in the air of 20 DEG C and 60% humidity and is carried out aging in 12 hours, makes The precursor solution that standby one-tenth is aging.
Precursor solution after step 2 is aging is prepared as CZTS thin film by the way of spin coating on molybdenum glass substrate.Rotation Being coated with rotating speed is 3000 revs/min, and the time is 30 seconds.Every spin coating one layer, calcines 5 minutes in the air of 400 DEG C. In order to obtain the film thickness of optimum, spin coating is from multiple 6 times.After spin coating completes, sulfur under the atmosphere of 580 DEG C of sulfur steam Change 60 minutes.With flow for 130ml min during sulfuration-1Nitrogen be carrier gas.1.3 μ m-thick are obtained after having vulcanized Copper-zinc-tin-sulfur i.e. CZTS thin film.
Comparative example 1:
Utilize clarification precursor solution (but not carrying out aging) system by the way of embodiment 1 is identical that embodiment 1 configures Standby one-tenth CZTS thin film.Owing to the viscosity of clarification precursor solution is less, to obtain and prepare with aging precursor solution The thickness that CZTS thin film is identical, spin coating repeats 28 times.
Embodiment 2:
Step 1 is by the Cu (NO of 0.5843g3)2˙3H2Ga (the NO of O and 0.619g3)3˙H2O is dissolved into 4ml successively Methanol solution in.Then it is stirred being sufficiently mixed with the 3.5ml methanol solution dissolving 0.375g polyvinyl acetate, After stirring 30 minutes, it is thus achieved that the transparent precursor solution of 7.5ml.
The transparent precursor solution of step 2 is prepared as CuGaS by the way of spin coating on molybdenum glass substrate2Thin film.Rotating speed Being 1500 revs/min, the time is 30 seconds.Spin coating calcines 3 points after completing in the air of 150 DEG C and 250 DEG C respectively Clock and 7 minutes.In order to obtain optimum film thickness, spin coating is repeated 6 times.It is spin-coated on the relative ambient humidity condition of 20% Lower operation.After spin coating completes, thin film is calcined 1 hour in the air of 350 DEG C, then at the hydrogen sulfide of 500 DEG C (1%) nitrogen mixed gas and vulcanizes 30 minutes acquisition CuGaS2Thin film.
Comparative example 2:
The transparent precursor solution utilizing embodiment 2 to configure is prepared as CZTS thin film by the way of embodiment 2 is identical. Except for the difference that operate under the conditions of being spin-coated on the relative ambient humidity of 60%.
We have carried out every sign to the multi-element Cu-base sulfide optoelectronic pole obtained through above-mentioned steps, and Fig. 1 to Fig. 7 is Characterization result to multi-element Cu-base sulfide film optoelectronic pole.Wherein, Shanghai occasion China CHI633C type electrochemistry work is utilized Make the photoelectric current-potential curve of station test multi-element Cu-base sulfide optoelectronic pole.Test uses three-electrode system, cuprio sulfur selenium Compound is as negative electrode, and platinum is as anode, and SCE electrode is as reference electrode.AM 1.5G(100mW cm-2) sun Optical simulator is as light source.
It will be seen from figure 1 that become gel after the transparent precursor solution of CZTS is aging.Fig. 2 be aging before (b and D) the CZTS film surface prepared with aging rear (a and c) precursor solution and cross section SEM figure.From CZTS surface and The SEM in cross section schemes it can be seen that CZTS crystal grain prepared by aging rear precursor solution significantly increases, and number of grain boundaries drops Low.Fig. 3 be aging before and the XRD figure of CZTS thin film prepared of aging rear precursor solution.From figure 3, it can be seen that The thin film diffraction peak prepared meets the characteristic diffraction peak of CZTS, the diffraction maximum of other dephasign does not occur.Fig. 4 is old Visible (a) and ultraviolet (b) the Raman spectrogram of the CZTS thin film prepared with aging rear precursor solution before changing.From Fig. 4 (a) It can be seen that all of vibration peak is classified as the characteristic peak of CZTS.From Fig. 4 (b) it can be seen that before aging and aging after before Drive in CZTS thin film prepared by liquid solution and there is ZnS dephasign.Fig. 5 is aging front and prepared by aging rear precursor solution The photoelectric current of CZTS photocathode-potential curve figure.From fig. 5, it can be seen that pass through the aging of precursor solution, compare not Aging sample, the photoelectric current of CZTS photocathode prepared by aging rear precursor solution is had to obtain the lifting of about three times. Fig. 6 is the CuGaS that under different humidity environment prepared by spin coating operation2The XRD figure of thin film.From fig. 6, it can be seen that it is different The thin film that under relative humidity conditions, spin coating operation is prepared is CuGaS2.Fig. 7 is spin coating operation under different humidity environment The CuGaS of preparation2The photoelectric current of photocathode-potential curve figure.By humidity regulation, spin coating operation system under low-humidity environment For the CuGaS gone out2The photoelectric current of photocathode is significantly improved.

Claims (4)

1.一种高效光电性能铜基硫硒化物半导体薄膜，其特征是所述多元铜基硫硒化物的化学通式为Cux1M1x2M2x3(SSe)x4，M1和M2为不同的金属元素，且分别为Zn、Sn、Ge、Si、In、Ga、Al中的一种；多元铜基硫硒化物为铜锌锡硫或CuGaS2薄膜；制备方法采用溶液-旋涂法，具体步骤为：1. A copper-based sulfoselenide semiconductor thin film with high-efficiency photoelectric performance is characterized in that the chemical general formula of the multi-component copper-based sulfoselenide is Cu x1 M1 x2 M2 x3 (SSe) x4 , and M1 and M2 are different metal elements , and are respectively one of Zn, Sn, Ge, Si, In, Ga, Al; the multi-component copper-based sulfoselenide is copper zinc tin sulfur or CuGaS 2 film; the preparation method adopts the solution-spin coating method, and the specific steps are as follows: : 1)将醋酸铜，氯化铜，氯化亚铜，硝酸铜中的一种或者两种以上的任意比例混合物与权利1所述的M1和M2金属离子的硝酸盐、氯化盐或者醋酸盐中的一种或者任意两种的任意比例混合物以及硫脲加分别加入到溶剂中进行搅拌混合，得到澄清的前驱体溶液；所述的溶剂为乙二醇甲醚，二甲亚讽，甲醇，乙醇和乙二醇中的一种或者两种以上的任意比例混合物；1) Copper acetate, cupric chloride, cuprous chloride, one or more mixtures in arbitrary proportions of copper nitrate and nitrate, chloride or acetic acid of M1 and M2 metal ions described in right 1 One of the salts or a mixture of any two in any proportion and thiourea are added to the solvent for stirring and mixing to obtain a clear precursor solution; the solvent is ethylene glycol methyl ether, dimethyl sulfoxide, methanol , one of ethanol and ethylene glycol or a mixture of two or more in any proportion; 2)将步骤1)配制的澄清前驱体溶液在相对湿度为5％-95％的环境中老化0.5-200小时。老化后的前驱体溶液旋涂在导电衬底上，在200-550℃的空气中煅烧1-60分钟得到一层薄膜，重复以上旋涂和煅烧步骤获得0.05-3微米的最优厚度样品；旋涂和煅烧完成后，把样品在450-600℃的温度下进行硫硒化，硫硒化时间为20-120分钟，硫硒化是单质硫与硒蒸汽气氛或者硫化氢与硒化氢气体中进行；硫化或硒化完成后，得到约0.05-3微米厚的多元铜基硫硒化物薄膜。2) Aging the clarified precursor solution prepared in step 1) for 0.5-200 hours in an environment with a relative humidity of 5%-95%. The aged precursor solution is spin-coated on a conductive substrate, and calcined in air at 200-550°C for 1-60 minutes to obtain a thin film, and the above spin-coating and calcining steps are repeated to obtain a sample with an optimal thickness of 0.05-3 microns; After the spin coating and calcination are completed, the sample is subjected to sulfur selenization at a temperature of 450-600 ° C. The sulfur selenization time is 20-120 minutes. The sulfur selenization is an elemental sulfur and selenium vapor atmosphere or hydrogen sulfide and hydrogen selenide gas Carried out in; after sulfuration or selenization is completed, a multi-component copper-based sulfoselenide film with a thickness of about 0.05-3 microns is obtained. 3)将步骤1)所得的透明的前驱体溶液利用步骤2)同样的方法制备成薄膜。不同的是透明前驱体溶液旋涂前不进行老化，而是在旋涂的过程中，调控环境相对湿度在5％-95％之间进行旋涂操作。3) The transparent precursor solution obtained in step 1) is prepared into a thin film by the same method as step 2). The difference is that the transparent precursor solution is not aged before spin-coating, but during the spin-coating process, the relative humidity of the environment is controlled between 5% and 95% to perform the spin-coating operation. 2.根据权利要求1所述的铜基硫硒化物半导体薄膜，其特征是所述澄清前驱体溶液，对其在调控的湿度环境条件下老化或者不同湿度条件下旋涂均有助于多元铜基硫硒化物薄膜光电性能的提高。2. copper-based sulfur selenide semiconductor thin film according to claim 1, it is characterized in that described clarification precursor solution, all contributes to multi-element copper under the humidity environment condition of regulation or spin-coating to it under the different humidity conditions. Improvement of optoelectronic properties of sulfur-based selenide thin films. 3.根据权利要求1所述的铜基硫硒化物半导体薄膜，其特征是在20-30％的相对环境湿度条件下老化或旋涂。3. The copper-based sulfur selenide semiconductor thin film according to claim 1, characterized in that it is aged or spin-coated at a relative humidity of 20-30%. 4.根据权利要求1-3之一所述的铜基硫硒化物半导体薄膜，其特征是所述的多元铜基硫硒化物薄膜，应用到薄膜太阳能电池或用于发光二极管光电转换器件上。4. The copper-based sulfoselenide semiconductor thin film according to any one of claims 1-3, characterized in that the multi-component copper-based sulfoselenide thin film is applied to thin-film solar cells or light-emitting diode photoelectric conversion devices.
CN201610008801.1A 2016-01-07 2016-01-07 Method for preparing copper-based sulfoselenide semiconductor thin film Pending CN105789373A (en)

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CN107364836A (en) * 2017-07-31 2017-11-21 南京大学 Tin germanium sulfoselenide film and preparation method thereof, electrooptical device
CN107968041A (en) * 2017-11-22 2018-04-27 杨晓艳 A kind of preparation method of copper-zinc-tin-sulfur film
CN109087967A (en) * 2018-08-10 2018-12-25 暨南大学 A kind of cuprous oxide film and the preparation method and application thereof

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CN107364836A (en) * 2017-07-31 2017-11-21 南京大学 Tin germanium sulfoselenide film and preparation method thereof, electrooptical device
CN107364836B (en) * 2017-07-31 2020-07-31 南京大学 Tin-germanium-sulfur selenide thin film, preparation method thereof and photoelectric conversion device
CN107968041A (en) * 2017-11-22 2018-04-27 杨晓艳 A kind of preparation method of copper-zinc-tin-sulfur film
CN109087967A (en) * 2018-08-10 2018-12-25 暨南大学 A kind of cuprous oxide film and the preparation method and application thereof

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Application publication date: 20160720