CN105023757A - Tin-doped Sb2S3 thin film material and preparation method thereof - Google Patents

Tin-doped Sb2S3 thin film material and preparation method thereof Download PDF

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CN105023757A
CN105023757A CN201510401342.9A CN201510401342A CN105023757A CN 105023757 A CN105023757 A CN 105023757A CN 201510401342 A CN201510401342 A CN 201510401342A CN 105023757 A CN105023757 A CN 105023757A
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tin
sb2s3
doped
thin film
film material
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CN105023757B (en
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孙盼盼
姚方
孙小华
黄妞
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China Three Gorges University CTGU
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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
    • 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
    • Y02E10/542—Dye sensitized solar 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

The invention provides a tin-doped Sb2S3 thin film material and a preparation method thereof. The preparation method comprises the following steps: successively adding a certain amount of antimony trichloride (Sb2S3), tin tetrachloride (SnCl4-4H2O), thiourea and polyvinylpyrrolidone (PVP) to ethyl alcohol, and carrying out uniform and lasting stirring for a while and then, carrying out still standing; transferring sediment to a certain amount of water solution, uniformly stirring the solution and pouring the solution into a hydrothermal reaction vessel provided with an FTO substrate so as to carry out hydrothermal reaction; and after the hydrothermal reaction is finished, taking the FTO substrate out for cleaning and drying, and placing the FTO substrate in an atmosphere furnace for carrying out annealing treatment to obtain a tin-doped Sb2S3 thin film. The tin-doped Sb2S3 thin film material prepared in the invention has the advantages of good dye-sensitized solar cell counter electrode performance, simple synthetic process and low-cost and pollution-free raw materials; and the obtained tin-doped Sb2S3 thin film has the advantages of good uniformity, stability and transmittance and the like.

Description

A kind of tin dope Sb2S3 thin-film material and preparation method thereof
Technical field
The present invention relates to a kind of tin dope Sb 2s 3thin-film material and preparation method thereof, belongs to DSSC to electrode preparation field.
Background technology
DSSC is a kind of Novel photovoltaic power generating device grown up the nineties in last century, have compared to traditional photovoltaic device that environmental friendliness, preparation technology are simple, photoelectric conversion efficiency advantages of higher, particularly in low cost, there is outstanding advantage, be acknowledged as one of selection of most attraction in low-cost solar utilization in following low-carbon economy.
To the important component part of electrode as DSSC, be mainly used to the light induced electron of collection external circuit and realize teriodide (I in electrolyte 3 -) reducing/regenerating.Because Pt has remarkable electrocatalysis characteristic to iodine electrolyte, current high-performance DSSC mainly adopts the electro-conductive glass of plating Pt as to electrode, but because the reserves of Pt are low, cost is high, significantly limit large-scale production and the application of DSSC.Therefore, research and develop low cost, high efficiency novel be one of the study hotspot in this field to electrode material always.In recent years, inorganic compound material comprises metal carbides (see Electra. Acta magazine, 2015,157th volume, 225th page), nitride is (see J. Mater. Chem. A magazine, 2013,1st volume, 14350th page), sulfide (see Chem. Eur. J. magazine, 2014, the 20th volume, 8670th page) and selenides (see Chem. Comm. magazine, 2014, the 50th volume, the 4475th page) show excellent in DSSC to electrode field and become study hotspot.Wherein, Sb 2s 3to demonstrating good electrocatalysis characteristic and application prospect in electrode (see J. Phys. Chem. C magazine, 2013,117th volume, 10285th page), but its conductivity is poor, and the material of synthesis is at present generally powder, there is the shortcoming that later stage thin film preparation process is more complicated, consumption of materials is large, limits its large-scale production and application.Therefore, Sb is improved 2s 3the conductivity of film also simplifies thin film preparation process, is to improve its DSSC to electrode performance and then realize large-scale application and have aspect to be solved.
Summary of the invention
The object of this invention is to provide a kind of tin dope Sb 2s 3thin-film material and preparation method thereof, this material has good electrocatalysis characteristic to iodine electrolyte, and preparation technology is simply controlled, the Sb of acquisition 2s 3film has good homogeneity, stability and light transmission, can replace Pt as new and effective DSSC to electrode material.
Technical scheme of the present invention comprises the following steps:
Successively add a certain amount of trichloride antimony (SbCl in ethanol 3), butter of tin (SnCl 44H 2o), thiocarbamide and polyvinylpyrrolidone (PVP), consistent leaves standstill after stirring a period of time.Sediment is transferred in the aqueous solution of 40-100mL, stirs and be poured in the hydrothermal reaction kettle being placed with FTO substrate (conducting surface down), 120 ~ 180 oc insulation reaction 2 ~ 24 hours.After reaction terminates, washing, drying are taken out in FTO substrate, put it in atmosphere furnace at heating rate 2 ~ 8 oc/min, 400 ~ 500 oannealing in process 1 ~ 3 hour under C, waits for nature cooling, namely obtains tin dope Sb 2s 3film.
In such scheme:
SbCl 3concentration be 30-50mM, SnCl 44H 2the concentration of O is 1-4mM, and the concentration of thiocarbamide is the quality of 0.1-0.2M, PVP is 0.2-0.5g, and sintering atmosphere is N 2atmosphere.
Advantage of the present invention is:
1, Sb is improved by tin dope 2s 3the conductivity of film, realizes Sb 2s 3film DSSC is to the improvement of electrode performance.This film has that electrocatalysis characteristic is high, the advantage of good conductivity.Under the optical excitation of AM1.5 simulated solar, with tin dope Sb 2s 3film is 5% as the most high-photoelectric transformation efficiency realized electrode, and this is than with the Sb that do not adulterate 2s 3film wants high as the photoelectric conversion efficiency 3.93% realized electrode.Therefore, tin dope Sb 2s 3film has preferably to electrode performance, can replace Pt as new and effective DSSC to electrode material.
2, hydrothermal method hydrothermal growth tin dope Sb on electrically conducting transparent substrate FTO is adopted 2s 3film, this preparation technology is simple, avoid complicated later stage film-forming process, and the prices of raw and semifnished materials is cheap, pollution-free.The Sb prepared 2s 3film has good homogeneity, stability and light transmission.
Accompanying drawing explanation
Fig. 1 is Sb prepared by example 1 2s 3film XRD collection of illustrative plates and standard stibnite PDF card comparison diagram.
Fig. 2 is tin dope Sb prepared by example 2 2s 3the SEM photo of film.
Fig. 3 is tin dope Sb prepared by example 2 2s 3film through spectrum.
Fig. 4 is the tin dope Sb prepared with example 2 2s 3film is as the J-V curve of the device obtained electrode test.
embodiment:
example 1configuration SbCl 3concentration is 35mM, thiourea concentration is the ethanolic solution of 0.15M, then adds 0.4gPVP, and consistent leaves standstill after stirring a period of time.Sediment is transferred in the aqueous solution of 80mL, stirs and be poured in the hydrothermal reaction kettle being placed with FTO substrate (conducting surface down), 120 ~ 180 oc insulation reaction 24 hours.After reaction terminates, washing, drying are taken out in FTO substrate, put it into N 2at heating rate 2 ~ 8 in atmosphere furnace oc/min, 450 osinter 1 ~ 3 hour under C, naturally obtain crystallization Sb after cooling 2s 3film.
Fig. 1 is Sb prepared by this example 2s 3the XRD collection of illustrative plates of film and standard stibnite PDF card comparison diagram, comparing result shows to successfully pass hydrothermal method fabricated in situ stibnite Sb in FTO substrate 2s 3film (wherein * position represents FTO substrate diffraction maximum).
example 2configuration SbCl 3concentration is 33mM, SnCl 44H 2the concentration of O is 2mM, thiourea concentration is the ethanolic solution of 0.2M, then adds 0.4gPVP, and consistent leaves standstill after stirring a period of time.Sediment is transferred in the aqueous solution of 60mL, stirs and be poured in the hydrothermal reaction kettle being placed with FTO substrate (conducting surface down), 120 ~ 180 oc insulation reaction 24 hours.After reaction terminates, washing, drying are taken out in FTO substrate, put it into N 2at heating rate 2 ~ 8 in atmosphere furnace oc/min, 450 osinter 1 ~ 3 hour under C, naturally obtain tin dope Sb after cooling 2s 3film.
Fig. 2 is the tin dope Sb prepared under this example 2s 3the SEM photo of film, as can be seen from this picture, Sb 2s 3film surface is made up of loose structure.
Fig. 3 is the tin dope Sb to prepare under this example 2s 3film through spectrum, can Sb be found out 2s 3film is thinner, has the light transmittance of 40-50% at visible-range, is suitable for large-scale production and application.
Fig. 4 is the tin dope Sb to prepare under this example 2s 3film to electrode, tests the J-V curve of the device obtained as DSSC under AM1.5 simulated solar irradiation irradiates.Can calculate from figure, tin dope Sb 2s 3thin-film device photoelectric conversion efficiency is 5.0%, compares, demonstrate tin dope Sb with the device that do not adulterate (3.93%) with Pt device (5.28%) 2s 3film excellence to electrode performance, be expected to replace Pt as new and effective DSSC to electrode material.
example 3configuration SbCl 3concentration is 31mM, SnCl 44H 2the concentration of O is 4mM, thiourea concentration is the ethanolic solution of 0.15M, then adds 0.5gPVP, and consistent leaves standstill after stirring a period of time.Sediment is transferred in the aqueous solution of 60mL, stirs and be poured in the hydrothermal reaction kettle being placed with FTO substrate (conducting surface down), 120 ~ 180 oc insulation reaction 12 hours.After reaction terminates, washing, drying are taken out in FTO substrate, put it into N 2at heating rate 2 ~ 8 in atmosphere furnace oc/min, 500 osinter 1 ~ 3 hour under C, naturally obtain tin dope Sb after cooling 2s 3film.

Claims (2)

1. a tin dope Sb 2s 3thin-film material, is characterized in that: tin dope Sb 2s 3the surface of thin-film material is loose structure composition, this tin dope Sb 2s 3the preparation method of thin-film material is as follows:
1) successively add trichloride antimony, butter of tin, thiocarbamide and polyvinylpyrrolidone in ethanol, leave standstill after consistent stirs, be precipitated thing;
2) sediment in above-mentioned steps is transferred in the aqueous solution of 40-100mL, stirs and be poured in the hydrothermal reaction kettle being placed with FTO substrate, wherein, the conducting surface of FTO substrate down, 120 ~ 180 DEG C of insulation reaction 2 ~ 24 hours;
3) FTO substrate is taken out washing, drying after terminating by reaction, puts it in atmosphere furnace at heating rate 2 ~ 8 oc/min, 400 ~ 500 oannealing in process 1 ~ 3 hour under C, obtains tin dope Sb after cooling naturally 2s 3film.
2. tin dope Sb according to claim 1 2s 3thin-film material and preparation method thereof, is characterized in that the mol ratio of trichloride antimony, butter of tin, thiocarbamide and polyvinylpyrrolidone is 30-50:1-4:100-200:0.005-0.0125.
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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105489384A (en) * 2016-01-11 2016-04-13 三峡大学 Preparation method of C/Sb<2>S<3> composite thin-film counter electrode material
CN105632771A (en) * 2016-03-16 2016-06-01 三峡大学 Preparation method of Sb<2>Se<3> film counter electrode material
CN105762207A (en) * 2016-03-30 2016-07-13 北京化工大学 Hydrothermal preparation method of Sb2S3 semiconductor film with narrow band gap
CN105932114A (en) * 2016-07-19 2016-09-07 福建师范大学 Method for preparing solar cell absorbing layer film based on water bath and post-selenization
CN107068797A (en) * 2017-04-11 2017-08-18 重庆文理学院 Thin-film solar cells and preparation method thereof
CN108711608A (en) * 2018-09-07 2018-10-26 中南大学 Three-dimensional leader shape all-solid lithium-ion battery cathode, preparation method and battery
CN109545659A (en) * 2018-10-31 2019-03-29 金陵科技学院 A kind of chemical bath preparation method of tin antimony sulphur film
CN109802010A (en) * 2019-01-23 2019-05-24 福建师范大学 A kind of recyclable chemical baths prepare solar battery obsorbing layer Sb2S3The method of film

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CN102543477A (en) * 2012-02-29 2012-07-04 中国科学院等离子体物理研究所 Preparation method for metal sulfide catalytic electrode and application thereof
CN103354273A (en) * 2013-06-17 2013-10-16 华侨大学 Embedded large-area flexible sensitized solar cell and preparation method thereof

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105489384A (en) * 2016-01-11 2016-04-13 三峡大学 Preparation method of C/Sb<2>S<3> composite thin-film counter electrode material
CN105489384B (en) * 2016-01-11 2018-04-10 三峡大学 A kind of C/Sb2S3Preparation method of the laminated film to electrode material
CN105632771A (en) * 2016-03-16 2016-06-01 三峡大学 Preparation method of Sb<2>Se<3> film counter electrode material
CN105762207A (en) * 2016-03-30 2016-07-13 北京化工大学 Hydrothermal preparation method of Sb2S3 semiconductor film with narrow band gap
CN105932114A (en) * 2016-07-19 2016-09-07 福建师范大学 Method for preparing solar cell absorbing layer film based on water bath and post-selenization
CN107068797A (en) * 2017-04-11 2017-08-18 重庆文理学院 Thin-film solar cells and preparation method thereof
CN108711608A (en) * 2018-09-07 2018-10-26 中南大学 Three-dimensional leader shape all-solid lithium-ion battery cathode, preparation method and battery
CN109545659A (en) * 2018-10-31 2019-03-29 金陵科技学院 A kind of chemical bath preparation method of tin antimony sulphur film
CN109545659B (en) * 2018-10-31 2021-09-10 金陵科技学院 Chemical bath preparation method of tin-antimony-sulfur film
CN109802010A (en) * 2019-01-23 2019-05-24 福建师范大学 A kind of recyclable chemical baths prepare solar battery obsorbing layer Sb2S3The method of film
CN109802010B (en) * 2019-01-23 2020-11-03 福建师范大学 Solar cell absorption layer Sb prepared by recyclable chemical bath method2S3Method for making thin film

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