CN101038944A - Method for preparation of FeS2/In2S3 compound film - Google Patents

Method for preparation of FeS2/In2S3 compound film Download PDF

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CN101038944A
CN101038944A CNA2006100498328A CN200610049832A CN101038944A CN 101038944 A CN101038944 A CN 101038944A CN A2006100498328 A CNA2006100498328 A CN A2006100498328A CN 200610049832 A CN200610049832 A CN 200610049832A CN 101038944 A CN101038944 A CN 101038944A
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CN100440549C (en
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孟亮
刘艳辉
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Zhejiang University ZJU
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Abstract

The invention discloses a method for preparing FeS2/In2S3 composite membrane. An ITO membrane conductive glass substrate is electrodeposited with precast membrane by being merged in a water solution whose molar concentration ratio of 1: 5 to 6, and then is oxidized in 130 to 180 DEG C. to obtain porous Fe3O4/In2O3 composite precursor membrane, and then is vulcanized in a condition of 400 DEG C. and 40 to 80 kPa sulphur vapour nominal pressure for 10 to 30 hours to convert the composite precursor membrane into a FeS2/In2S3 composite membrane. The invention adds oxidation process after the electrodeposition process thereby accelerating the FeS2 reaction in heat vulcanization so as to directly form In2S3 by vulcanizing the substrate membrane, in this manner, the process for independently synthesizing In2S3 can be left out, and the bound of FeS2/In2S4 two phase interfaces can be effectively guaranteed, the composite membrane is tightly and reliably adhibited on the substrate.

Description

A kind of FeS 2/ In 2S 3The preparation method of composite membrane
Technical field
The invention belongs to Material Field, relate to the preparation of functional material, be specially a kind of solar cell material FeS 2/ In 2S 3The preparation method of composite membrane.
Background technology
Along with the development of progress of science and technology and human civilization, the disposable energy such as coal, petroleum and natural gas more and more can not be satisfied the demand.And, in the use procedure of the disposable energy, can discharge the gas that in a large number mankind is harmful to, destroy human environment of depending on for existence.Therefore, in various renewable resources, solar energy has become the emphasis of utilization of new energy resources exploitation, and one of mainly exploitation form is to try hard to that solar energy is converted into electric energy effectively promote the well-being of mankind.
Solar cell is the active parts that luminous energy is converted into electric energy, and optoelectronic pole material wherein is the core of solar cell, thereby some new solar cell materials constantly are being developed exploitation.In these materials, metal sulfide has excellent photoelectric properties, wherein FeS 2Mainly as photronic electrode material, has the energy gap and 10 of about 0.95eV 5Cm -1The absorption coefficient of light of the order of magnitude, and the element reserves are abundant, and Environmental compatibility is good, has been subjected to extensive attention.In 2S 3Can be used as photronic cushioning layer material, energy gap is between 2.0～2.9eV, and the absorption coefficient of light also can reach 10 5Cm -1The order of magnitude.If will absorb the FeS of infrared in the sunshine and visible light part 2In with absorbing ultraviolet light part 2S 3Bi-material effectively makes up, and can more effectively utilize solar energy.
As solar cell material, FeS 2And In 2S 3Should use with form of film.Existing multiple technology of preparing can manually be synthesized FeS 2Film.Patent US6635942 proposes a kind of FeS that contains that is used for solar cell 2The rete semiconductor device, monocrystalline wherein or polycrystalline FeS 2Can take from natural minerals, just have suitable carrier concentration but must adopt the multi-region clean technologies to handle.In addition, above-mentioned patent has proposed to adopt vapor transportation, sol gel reaction deposition, FeS 2Target as sputter, metal-organic chemical vapor deposition equipment, the synthetic technologys such as spray pyrolysis and molecular beam epitaxial growth prepare FeS 2Similarly, patent US6630257 has proposed a kind of FeS of containing 2The technology of preparing of membrane electrode, FeS wherein 2Be considered to adopt chemical vapor transportation chemical vapour deposition (CVD), thermal spray deposition, ferriferous oxide sulfuration, reactive sputtering, prepared such as iron film electrodeposition and silk screen printing.Patent US4649227 has announced two kinds of photosensitive FeS that multiple doped chemical is arranged 2Film preparation technology.First kind of technology is by the natural material hot chemical treatment being obtained the FeS of required crystal type, purity and metering composition 2, and rely on chemical vapor transportation to form film.Second kind of technology is to prepare FeS by the synthetic reaction between iron or iron containing compounds and sulphur or the sulfur-containing compound 2, can adopt that reactant directly contacts, temperature gradient conversion and vapor transportation realize crystal growth, also can be by reaction formation FeS again after carbonyl iron or iron halide and sulphur or the hydrogen sulfide thermal decomposition 2Film.Patent ZL02111221.5 has announced the synthetic FeS of a kind of magnetron sputtering iron film of monocrystalline silicon piece substrate 2The preparation method, magnetron sputtering pure iron film on monocrystalline silicon piece carries out the pure iron film heat cure reaction again and forms and have the FeS that standard chemical metering composition there is no transitional face 2Film has higher adhesive force between film and the substrate, can be used for FeS 2The laboratory sample of film growth research.
Except that existing patented technology, many research papers have also been announced FeS 2The technology of preparing of film.Yamamoto etc. (SolarEnergy Materials and Solar Cells, 2003, vol.75, pp.451-456) reported a kind of FeS close with the electrochemical deposition effect 2Film preparing technology is mainly with FeSO 4And (NH 4) 2S xThe aqueous solution is sprayed at glass and Si sheet, and adds the thermosetting prefabricated membrane at 120 ℃, then at H 2Sulfuration annealing forms the FeS of p-type electric-conducting among the S 2Film.Nakamura etc. (SolarEnergy Materials and Solar Cells, 2001, vol.65, pp.79-85) have proposed to use FeSO 4And Na 2S 2O 3The synthetic FeS of method that the aqueous solution vulcanizes behind Ti substrate By Electrolysis deposition FeS prefabricated membrane again 2Film.(MaterialsResearch Bulletin, 2003, vol.38, the pp.1123-1133 such as Gomes; Electrochimica Acta, 2004, vol.49, pp.2155-2165) 1: 3 (NH of employing 4) 2Fe (SO 4) 2The aqueous solution and Na 2S 2O 3Electrodeposition of Fe-S transition compound film, the Fe-S film is annealed in 250～500 ℃ sulphur atmosphere to change into the FeS of N-shaped conduction subsequently 2Film.Smestad etc. (SolarEnergy Materials, 1990, vol.20, pp.149-165) adopt pyrolysis FeCl 2Or FeCl 3Prepared Fe in substrate of glass 3O 4Or Fe 2O 3Prefabricated membrane places prefabricated membrane 350 ℃ of lower vulcanizing treatment to form FeS again 2Film.In addition, prefabricated membrane also can obtain with the method that the pure Fe film of evaporation reoxidizes processing.Raturi etc. (Renewable Energy, 2000, vol.20, pp.37-43) spray FeCl at 370 ℃ of plate glass 3Solution oxide has formed Fe 2O 3, annealing makes prefabricated membrane change FeS in vulcanized gas again 2Film.
About In 2S 3The thin film technology technology also has report.Patent CN200310107202.8 is in a kind of preparation of copper indium gallium sulphur thing semiconductor film material, with Cu, In, the Ga metal preformed layer of vacuum magnetic-control sputtering, heating evaporation or chemical bath electrodeposition process substep sedimentation chemistry formula proportional quantity on soda-lime glass Mo substrate, carry out vulcanization reaction more earlier.Yasaki etc. (Journalof Electroanalytical Chemistry, 1999, vol.469, pp.116-122) are at InCl 3Middle input H 2The S gas aggradation goes out In 2S 3Colloid evenly is applied on the quartz or Ti substrate of High Rotation Speed after adding acetone and the centrifugal dehydration, obtains the In of different-thickness 400 ℃ of heat treatments again 2S 3Film.Barreau etc. (Vacuum, 2000, vol.56,101-106) replace 4 layers of evaporation to glass substrate with In and S, and heating 30min reaction generates In in 523～723K temperature range under the protection of Ar gas 2S 3Film.Lokhande etc. (Thin Solid Films, 1999, vol.340, pp.18-23) adopt properly mixed In 2(SO 4) 3, NH 4Cl and thioacetyl amine aqueous solution and the method for mixing triethanolamine and hydrazine hydrate under constant temperature, chemical deposition goes out In on substrates of different 2S 3Film.(the Journal of Electroanalytical Chemistry such as Tacconi, 1998, vol.444, pp.7-10) the polymorph A u electrode substrates S layer in containing the S solion at first, be transferred to then and contain in the In ion electrolyte at S layer deposition In and form In 2S 3Layer is finally again transferred to and is contained in the S solion the superfluous In of sulfuration and make film become completely In 2S 3Layer.(Thin Solid Films, 1999, vol.353, the pp.100-107 such as Bay ó n; Applied Surface Science, 2000, vol.158 pp.49-57) comprise InCl by variation 3, acetic acid and thioacetamide solution concentration deposit In at the glass substrate of 70 ℃ of constant temperature 2S 3Film, annealing in process in 300～400 ℃ of air is adjusted the In that solution concentration can form mixed-crystal structure again 2S 3
Yet prior art can only prepare single FeS 2Film or In 2S 3Film is for FeS 2/ In 2S 3Composite membrane does not still have relevant technology of preparing and announces.
Summary of the invention
The purpose of this invention is to provide a kind of FeS 2/ In 2S 3The preparation method of composite membrane, technological parameter is controlled easily, FeS 2With In 2S 3Between the interface in conjunction with reliable, adhesion-tight between film body and the substrate.
For achieving the above object the technical solution used in the present invention such as following step:
(1) adopting the film carrier substrate is In 2O 3: SnO 2=9: 1 ITO conductive glass successively behind each 20min of Ultrasonic Cleaning, is used deionized water rinsing again in acetone and ethanolic solution;
(2) do negative electrode with the film carrier substrate, the Pt sheet is done anode, at FeSO 4And Na 2S 2O 3Aqueous solution electrodeposition is produced prefabricated membrane;
(3) prefabricated membrane is carried out oxidation processes in ambiance, obtain the Fe of porous form 3O 4/ In 2O 3The composite precursor film;
(4) be that 99.5% sublimed sulfur powder is packaged in the quartz ampoule with precursor film and purity, by 5 argon filling-vacuum displacement residual gass repeatedly, be evacuated to 0.01Pa during encapsulation before the encapsulation;
(5) the precursor film after will encapsulating carries out vulcanizing treatment in 400 ℃ of constant-temperature ovens, obtains FeS 2/ In 2S 3Composite membrane.
The FeSO that electro-deposition is used in the above step (2) 4And Na 2S 2O 3Aqueous solution molar concentration rate is 1: (5～6), and with the H of dilution 2SO 4Regulate pH value to 3.0～5.0; The electro-deposition electric current of producing prefabricated membrane is 0.75～0.85mA, and sedimentation time is 30～60min.
The prefabricated membrane oxidation temperature is 130～180 ℃ in the step (3), and the oxidation processes temperature retention time is 2～6h.
The sulfur vapor nominal pressure is 40～80kPa in the vulcanizing treatment in the step (5), and cure time is 10～30h.
Advantage of the present invention and beneficial effect are:
1) introduced the oxidation link after electro-deposition, the Fe-S compound that electro-deposition is formed is converted into Fe in advance 3O 4, be conducive to the heat cure reaction and form FeS 2
2) directly utilize In in the electro-conductive glass substrate I TO conducting film 2O 3With Fe 3O 4Simultaneously sulfuration forms FeS 2/ In 2S 3Composite membrane has saved separately synthetic In 2S 3Technical process, preparation technology and equipment are simple, efficient is higher;
3) owing to make In by active S atom diffusion 2O 3With Fe 3O 4Cure simultaneously, thereby FeS 2/ In 2S 3Two-phase interface is in conjunction with accessing effective assurance;
4) FeS 2/ In 2S 3The attachment state of composite film and substrate is equivalent to the attachment state of former ITO conducting film and glass substrate, so film is incrust, and is reliable with the substrate adhesion-tight.
Description of drawings
Fig. 1 is the Fe in the embodiment of the invention 1 3O 4/ In 2O 3Composite precursor film microstructure morphology;
Fig. 2 is the Fe in the embodiment of the invention 1 3O 4/ In 2O 3Composite precursor film crystal structure X-ray diffraction spectrum;
Fig. 3 is the FeS in the embodiment of the invention 1 2/ In 2S 3Composite membrane microstructure morphology;
Fig. 4 is the FeS in the embodiment of the invention 1 2/ In 2S 3Composite membrane crystal structure X-ray diffraction spectrum;
Fig. 5 is the Fe in the embodiment of the invention 2 3O 4/ In 2O 3Composite precursor film microstructure morphology;
Fig. 6 is the Fe in the embodiment of the invention 2 3O 4/ In 2O 3Composite precursor film crystal structure X-ray diffraction spectrum;
Fig. 7 is the FeS in the embodiment of the invention 2 2/ In 2S 3Composite membrane microstructure morphology;
Fig. 8 is the FeS in the embodiment of the invention 2 2/ In 2S 3Composite membrane crystal structure X-ray diffraction spectrum.
Embodiment
Embodiment 1:
Be 20 * 15mm with area 2The ITO electro-conductive glass as the film carrier substrate, the conducting film composition is In 2O 3: SnO 2=9: 1, elder generation Ultrasonic Cleaning 20min, again Ultrasonic Cleaning 20min in ethanolic solution in acetone soln.Ultrasonic waves for cleaning is after the ionized water cleaning down is removed residual organic solution.
The preparation molar concentration rate is 1: 5 FeSO 4And Na 2S 2O 3The aqueous solution is with the H of dilution 2SO 4The pH value to 3.0 of regulator solution.Do negative electrode with the film carrier substrate, the Pt sheet is done anode, adopts the direct current of 0.75mA and the sedimentation time of 60min to deposit prefabricated membrane on substrate.Prefabricated membrane soaks 1h after with deionized water rinsing in absolute ethyl alcohol.
Place the baking oven insulation 6h of 130 ℃ of ambiances to carry out oxidation processes prefabricated membrane, obtain microscopic structure and reach as shown in Figure 1 crystal structure cellular Fe as shown in Figure 2 3O 4/ In 2O 3The composite precursor film.
Press required quality sublimed sulfur powder (purity is 99.5%) and precursor film to be packaged in the quartz ampoule with producing 80kPa name sulphur under 400 ℃ of conditions, pass through repeatedly 5 argon filling-vacuum displacement residual gas before the encapsulation, be evacuated to 0.01Pa during encapsulation.With the sample vulcanizing treatment 10h in 400 ℃ of constant-temperature ovens after the encapsulation.For preventing that film from cracking and peeling off, the control heating rate is not higher than 4 ℃/min before the isothermal, and rate of temperature fall is not higher than 2 ℃/min behind the isothermal.The FeS that obtains after the sulfuration 2/ In 2S 3The composite membrane microscopic structure reaches crystal structure as shown in Figure 4 as shown in Figure 3.
Embodiment 2:
Be 20 * 15mm with area 2The ITO electro-conductive glass as the film carrier substrate, the conducting film composition is In 2O 3: SnO 2=9: 1, elder generation Ultrasonic Cleaning 20min, again Ultrasonic Cleaning 20min in ethanolic solution in acetone soln.Ultrasonic waves for cleaning is after the ionized water cleaning down is removed residual organic solution.
The preparation molar concentration rate is 1: 6 FeSO 4And Na 2S 2O 3The aqueous solution is with the H of dilution 2SO 4The pH value to 5.0 of regulator solution.Do negative electrode with the film carrier substrate, the Pt sheet is done anode, adopts the direct current of 0.85mA and the sedimentation time of 30min to deposit prefabricated membrane on substrate.Prefabricated membrane soaks 1h after with deionized water rinsing in absolute ethyl alcohol.
Place the baking oven insulation 2h of 180 ℃ of ambiances to carry out oxidation processes prefabricated membrane, obtain microscopic structure and reach as shown in Figure 5 crystal structure cellular Fe as shown in Figure 6 3O 4/ In 2O 3The composite precursor film.
Press required quality sublimed sulfur powder (purity is 99.5%) and precursor film to be packaged in the quartz ampoule with producing 40kPa name sulphur under 400 ℃ of conditions, pass through repeatedly 5 argon filling-vacuum displacement residual gas before the encapsulation, be evacuated to 0.01Pa during encapsulation.With the sample vulcanizing treatment 30h in 400 ℃ of constant-temperature ovens after the encapsulation.For preventing that film from cracking and peeling off, the control heating rate is not higher than 4 ℃/min before the isothermal, and rate of temperature fall is not higher than 2 ℃/min behind the isothermal.The FeS that obtains after the sulfuration 2/ In 2S 3The composite membrane microscopic structure reaches crystal structure as shown in Figure 8 as shown in Figure 7.

Claims (5)

1. FeS 2/ In 2S 3The preparation method of composite membrane is characterized in that following step:
(1) adopting the film carrier substrate is In 2O 3: SnO 2=9: 1 ITO conductive glass successively behind each 20min of Ultrasonic Cleaning, is used deionized water rinsing again in acetone and ethanolic solution;
(2) do negative electrode with the film carrier substrate, the Pt sheet is done anode, at FeSO 4And Na 2S 2O 3Aqueous solution electrodeposition is produced prefabricated membrane;
(3) prefabricated membrane is carried out oxidation processes in ambiance, obtain the Fe of porous form 3O 4/ In 2O 3The composite precursor film;
(4) be that 99.5% sublimed sulfur powder is packaged in the quartz ampoule with precursor film and purity, by 5 argon filling-vacuum displacement residual gass repeatedly, be evacuated to 0.01Pa during encapsulation before the encapsulation;
(5) the precursor film after will encapsulating carries out vulcanizing treatment in 400 ℃ of constant-temperature ovens, obtains FeS 2/ In 2S 3Composite membrane.
2. FeS according to claim 1 2/ In 2S 3The composite membrane preparation method is characterized in that: the FeSO that electro-deposition is used in the described step (2) 4And Na 2S 2O 3Aqueous solution molar concentration rate is 1: (5～6), and with the H of dilution 2SO 4Regulate pH value to 3.0～5.0.
3. FeS according to claim 1 2/ In 2S 3The composite membrane preparation method is characterized in that: the electro-deposition electric current of producing prefabricated membrane in the described step (2) is 0.75～0.85mA, and sedimentation time is 30～60min.
4. preparation FeS according to claim 1 2/ In 2S 3The composite membrane method is characterized in that: the prefabricated membrane oxidation temperature is 130～180 ℃ in the described step (3), and the oxidation processes temperature retention time is 2～6h.
5. preparation FeS according to claim 1 2/ In 2S 3The composite membrane method is characterized in that: the sulfur vapor nominal pressure is 40～80kPa in the vulcanizing treatment in the described step (5), and cure time is 10～30h.
CNB2006100498328A 2006-03-14 2006-03-14 Method for preparation of FeS2/In2S3 compound film Expired - Fee Related CN100440549C (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102923790A (en) * 2011-09-15 2013-02-13 华东理工大学 Synthetic method of FeS2 pyrite photoelectric material

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US10181598B2 (en) 2015-01-05 2019-01-15 University Of Florida Resarch Foundation, Inc. Lithium ion battery cathodes, methods of making, and methods of use thereof

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JP2000268969A (en) * 1999-03-17 2000-09-29 Tdk Corp Organic electroluminescent element

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102923790A (en) * 2011-09-15 2013-02-13 华东理工大学 Synthetic method of FeS2 pyrite photoelectric material
CN102923790B (en) * 2011-09-15 2014-06-18 华东理工大学 Synthetic method of FeS2 pyrite photoelectric material

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