CN102856499B - A kind of SnO 2with the preparation method of P3HT hybrid heterojunctions thin-film solar cells - Google Patents

A kind of SnO 2with the preparation method of P3HT hybrid heterojunctions thin-film solar cells Download PDF

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CN102856499B
CN102856499B CN201210292721.5A CN201210292721A CN102856499B CN 102856499 B CN102856499 B CN 102856499B CN 201210292721 A CN201210292721 A CN 201210292721A CN 102856499 B CN102856499 B CN 102856499B
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film
thin
p3ht
sns
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CN102856499A (en
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张艳鸽
王敏
李品将
白赢赢
李明
郑直
张福捐
杨风岭
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Xuchang University
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Abstract

A kind of SnO 2with the preparation method of P3HT hybrid heterojunctions thin-film solar cells.The method sulphur powder, ammonium persulfate and metal tin target are raw material, with absolute ethyl alcohol, DMF and distillation water as solvent, namely in the substrate of ITO electro-conductive glass, prepare SnO through hydro-thermal and solvent heat heat treatment 2film.First solvent structure SnS, its SnS make preparation SnO 2predecessor, from Sn 2+to Sn 4+oxidation reaction simpler, consume energy low; The SnS pattern of synthesis is sheet interconnection network structure, can be SnO 2growth provides template, prepares the open structure be evenly distributed, and increases SnO 2film specific area, makes there be better contact when forming network interpenetrating with P3HT hydridization, to improve the opto-electronic conversion performance of device.Then at its surperficial spin coating P3HT, 120 DEG C of annealing in process 2h, namely obtain SnO 2with the hetero-junction thin-film of P3HT hydridization.The method step is simple, without the need to using any surfactant and other chemical addition agent.

Description

A kind of SnO 2with the preparation method of P3HT hybrid heterojunctions thin-film solar cells
Technical field
The invention belongs to material chemistry technical field, particularly relate to one and prepare SnO in the substrate of ITO electro-conductive glass 2with the method for the hetero-junction thin-film of P3HT hydridization.
Background technology
Global energy requirements increases year by year, and the exploitation of solar energy have become the hot subject of World Focusing.In the development course of solar cell, the first generation solar cell that can be divided into monocrystalline silicon and polysilicon be material, thin-film material is utilized to complete the second generation solar cell of opto-electronic conversion, the basis of hull cell is introduced the third generation solar cell of organic substance and inorganic nano science and technology, and forth generation battery is mainly sandwich construction.People just constantly find new materials and methods, expect to use simple production technology to prepare the solar cell of low-cost high-efficiency.Organic thin film solar cell receives very big concern, utilizes organic solubility, direct in electrode surface film forming at normal temperatures and pressures, forms active layer.But because the charge mobility of organic substance self is lower, therefore its energy conversion efficiency is unsatisfactory so far.Different from organic substance, most inorganic semiconductor material all has higher charge mobility, so the comprehensive organic substance of people and inorganic matter advantage separately, prepares the solar cell of organic inorganic hybridization film.
The Alivisatos seminar that California, USA founds university's Berkeley reports use CdSe semiconductor nanorods as acceptor, with the conjugated polymer/inorganic semiconductor nano-crystal hybrid thin film solar cell of the blended preparation of P3HT, energy efficiency reaches 1.7%.The polymer of n type inorganic semiconductor and p type semiconductor forms interpenetrating networks, inorganic semiconductor material as electron acceptor has the following advantages: the energy level of (1) nano particle and band gap regulate by the kind and size changing nano particle, it is made to have absorption at whole visible-range, the absorption region of polymer organic layer to solar spectrum can be expanded, improve the matching of battery response spectrum and solar radiation; (2) nano material has higher electron mobility, and chemical stability is better.On this basis, people use other inorganic semiconductor material (ZnO, ZnS, TiO 2deng) and organic substance (P3HT or MEHPPV) hydridization, prepare the solar cell device of a series of similar structures, and efficiency also brings up to 5.06%.This opens a new field for the nanocrystalline application of inorganic semiconductor, attracts wide attention.
SnO 2belong to a kind of broad-band gap n-type semiconductor, its direct band gap is 3.6eV, as a kind of environment-friendly type semi-conducting material, the advantages such as electron-transporting is good, synthesis technique is simple, cost is low, toxicity is low owing to having, good stability, long service life, there is very high using value in photocell field, it is applied in lithium ion battery and dye-sensitized cell mostly at present, and for SnO 2the report doing thin-film solar cells aspect with conjugatd polymers hydridization is little.In addition, with regard to current similar preparation research, the preparation of this kind of material greatly mainly with metallic tin salt as Xi Yuan, adopt water and solvent-thermal method or sol-gel process to prepare SnO 2nano-powder material, then utilizes and scrapes the preparation that the skill in using a kitchen knife in cookery or spin coating technique etc. carry out film; Or planting one deck crystal seed in substrate carries out induced growth formation film.But at assembling solar photovoltaic device, testing photoelectronic conversion performance aspect exists some defects: the first, in preparation process, experimental procedure requires loaded down with trivial details, and condition is harsh, and can use some poisonous reactant or solvents, and health risk, pollutes; The second, in film forming procedure, the technology such as crystal seed induced growth or spin-coating method are difficult to control to the thickness of film and distribution consistency degree; Therefore, carrying out compound tense with organic polymer, directly can affect composite effect, thus affecting photoelectric conversion efficiency.Therefore, for the semi-conducting material having significant application value, no matter commercial Application or laboratory research, all material preparation technology is had higher requirement, namely adopt simple technique, cheap raw material, reduce energy consumption as far as possible, synthesize environmentally safe, highly purified product, to meet the preparation requirement under current shortage of resources, energy deficiency condition.
The present invention adopt under cryogenic water and solvent-thermal method to realize SnO 2the preparation of nano film material, and by itself and P3HT hydridization, the hetero-junction thin-film solar cell photovoltaic device of assembling organic inorganic hybridization, studies its opto-electronic conversion performance.Whole preparation process is easy and simple to handle, environmental protection, and energy consumption is low, uses low raw-material cost, without any murder by poisoning accessory substance.
Summary of the invention
Problem to be solved by this invention is: provide a kind of directly at electro-conductive glass substrates at low temperatures water and solvent-thermal process SnO 2the chemical method of nano film material, and by itself and P3HT hydridization, preparation SnO 2with P3HT(SnO 2/ P3HT) the hetero-junction thin-film solar cell device of hydridization.
the present invention to the technical scheme that the problem that will solve is taked is:
of the present inventiona hetero-junction thin-film solar cell device for inorganic/organic hybrid, it is ITO/SnO 2: P3HT/Al is inorganic/the hetero-junction thin-film solar cell device of organic hybrid.
of the present inventiona kind of inorganic/the hetero-junction thin-film solar cell device of organic hybrid in, SnO 2nano film material at low temperatures original position prepares, and method is with nanometer Sn (0)for Xi Yuan, by hydro-thermal and solvent heat two step wet chemical synthesis SnO in the ITO electro-conductive glass substrate being coated with metallic tin 2nano film material, this thin-film material thickness is regulated and controled by reaction temperature and reaction time condition.
of the present inventiona kind of inorganic/the hetero-junction thin-film solar cell device of organic hybrid in, SnO 2the nano film material method that at low temperatures prepared by original position is, first magnetron sputtering is utilized to sputter layer of metal tin in the substrate of ITO electro-conductive glass, the ITO electro-conductive glass sheet inclined side this having been sputtered layer of metal tin is put in volume 30mL polytetrafluoroethylene reactor, make metal covering upward, add 3mg sulphur powder, then absolute ethyl alcohol and each 10mL of DMF is added, to be placed at 160 DEG C of temperature solvent thermal reaction 4 hours, product distilled water and absolute ethanol washing more than 2 times, be drying to obtain SnS film for subsequent use; Then the SnS film inclined side of preparation is put in 30mL polytetrafluoroethylene reactor, add 3mg ammonium persulfate as oxidant, to distill water as solvent, the volume of distilled water is vessel volume 1/2 ~ 2/3, react 24 hours under temperature is 140 DEG C of temperature, product distilled water and absolute ethanol washing more than 2 times, namely drying at room temperature obtains SnO 2nano film material.
of the present inventiona kind of inorganic/the hetero-junction thin-film solar cell device of organic hybrid in, SnO 2with the preparation method of P3HT hybrid heterojunctions thin-film solar cells be, first magnetron sputtering is utilized to sputter layer of metal tin in the substrate of ITO electro-conductive glass, the ITO electro-conductive glass sheet inclined side this having been sputtered layer of metal tin is put in volume 30mL polytetrafluoroethylene reactor, make metal covering upward, add 3mg sulphur powder, then absolute ethyl alcohol and each 10mL of DMF is added, to be placed at 160 DEG C of temperature solvent thermal reaction 4 hours, product distilled water and absolute ethanol washing more than 2 times, be drying to obtain SnS film for subsequent use; Then the SnS film inclined side of preparation is put in 30mL polytetrafluoroethylene reactor, add 3mg ammonium persulfate as oxidant, to distill water as solvent, the volume of distilled water is vessel volume 1/2-2/3, react 24 hours under temperature is 140 DEG C of temperature, product distilled water and absolute ethanol washing more than 2 times, namely drying at room temperature obtains SnO 2nano thin-film;
Then in vacuum glove box, utilize spin-coating method that the P3HT of the 10mg/mL prepared is spun on obtained SnO 2nano thin-film surface, 120 DEG C of annealing in process 2 hours, obtain SnO 2with P3HT hybrid heterojunctions thin-film solar cells.
Take a certain amount of P3HT and be dissolved in chloroform the solution being configured to 10 mg/mL, 40 oc adds thermal agitation makes it fully dissolve.This composite film material is the SnO being prepared loose structure by solvent-thermal method under low temperature 2thin-film material, through the method for spin-coating at its surperficial spin coating one deck P3HT, the n type inorganic semiconductor of preparation and p type semi-conducting polymer form the hetero-junction thin-film of interpenetrating networks.
of the present inventionthe preparation method of the hetero-junction thin-film solar cell device of inorganic/organic hybrid: first prepare SnO by step described above 2high vacuum ion evaporation instrument is put into, by mode evaporation one deck aluminium electrode (vacuum degree 9.0 × 10 of thermal evaporation with P3HT hybrid heterojunctions thin-film material -5mbar), ITO/SnO is namely assembled to obtain 2: P3HT/Al is inorganic/the hetero-junction thin-film solar cell device of organic hybrid.
in the present inventionfirst utilize solvent structure SnS, it is at preparation SnO 2process in serve as predecessor, from Sn 2+to Sn 4+oxidation reaction simpler, consume energy low; In addition, the SnS pattern of synthesis is the network configuration that sheet connects, and can be SnO 2growth template is provided, prepare the open structure be evenly distributed, increase SnO 2the specific area of film, makes there be better contact when forming network interpenetrating with P3HT hydridization, to improve the opto-electronic conversion performance of its device.
The present invention adopts cheap raw material, sulphur powder, ammonium persulfate, metal tin target, with absolute ethyl alcohol, DMF(N, dinethylformamide), distillation water as solvent, SnO can be prepared in the substrate of ITO electro-conductive glass through simple hydro-thermal and solvent heat heat treatment 2film.The method step is simple, again without the need to using any surfactant and other chemical addition agent, only need by ammonium persulfate, the predecessor film SnS of synthesis adds in reactor, and hydro-thermal reaction is taken out after a few hours, with water and ethanol cyclic washing, natural drying, can white clear be obtained, be evenly distributed, have the SnO of open structure 2film.Then adopt spin coating technique to be coated with P3HT(on its surface and gather 3-hexyl thiophene conjugated polymer), 120 DEG C of annealing in process 2h, namely obtain SnO 2with the hetero-junction thin-film of P3HT hydridization.
advantage of the present invention:
1, the present invention's distilled water, ethanol, DMF are as reaction medium, without the need to using the larger solvent of toxicity, belong to environmentally friendly reaction.
2, the present invention is low-temp reaction, and reaction raw materials only need add in reactor by reaction, just can obtain required product at 140 DEG C, and do not need to use any surfactant, reaction raw materials cost is low, and energy consumption is low, and experimental implementation is simple simultaneously.
3, the present invention is first by SnO 2nano semiconductor material and P3HT hydridization prepare SnO 2with P3HT (SnO 2/ P3HT) hetero-junction thin-film of hydridization is applied to assembling solar battery device.
The present invention has important Research Significance for carrying out synthesizing organic-inorganic bulk-heterojunction composite material.
Accompanying drawing explanation
The SnO of Fig. 1, embodiment 1 preparation 2the scanning electron micrograph of thin-film material
The SnO of Fig. 2, embodiment 2 preparation 2the scanning electron micrograph of thin-film material
The SnO of Fig. 3, embodiment 3 preparation 2the scanning electron micrograph of thin-film material
The SnO of Fig. 4, embodiment 3 preparation 2thin-film material X-ray diffraction pattern (XRD)
Can find out in XRD diffraction patterns, except mark ★ is ITO substrate diffraction maximum, and other diffraction maximums are SnO 2diffraction maximum, corresponding crystal face marks, does not occur other impurity peaks;
The SnO of Fig. 5, embodiment 3 preparation 2the hetero-junction thin-film solar cell device schematic diagram of/P3HT hydridization
In figure: 1-substrate of glass, 2-ITO, 3-SnO 2/ P3HT, 4-Al, 5-insulating barrier;
The SnO of Fig. 6, embodiment 3 preparation 2the I-V curve of the hetero-junction thin-film solar cell device of/P3HT hydridization
The open circuit voltage (Voc) of this battery is 0.405V, and density of photocurrent (Jsc) is 0.321mA/cm 2, fill factor, curve factor (FF) is 15.52%, and the electricity conversion of this battery is 0.02% at present.
Embodiment
The present invention is further illustrated below by embodiment.
embodiment 1
1, preparation: volume 30mL polytetrafluoroethylene reactor is respectively washed 1-3 time with running water, distilled water, absolute ethyl alcohol successively, stand-by after dry; Magnetron sputtering is utilized to sputter in the substrate of ITO electro-conductive glass 100nmthick metal Sn is stand-by.
2, reactions steps: add 3mg sulphur powder in the clean polytetrafluoroethylene of volume 30mL, then add absolute ethyl alcohol and each 10mL of DMF, be uniformly mixed, then use the above-mentioned sputtering of clean tweezers gripping ?the ITO electro-conductive glass sheet inclined side of metal Sn is put in volume 30mL polytetrafluoroethylene reactor, makes metal covering upward, reacts 4 hours at 160 DEG C, product distilled water and absolute ethyl alcohol respectively wash 3 times, constant temperature 60 DEG C of dryings, namely obtained SnS film in the substrate of ITO electro-conductive glass sheet, for subsequent use; In the clean polytetrafluoroethylene reactor of volume 30mL, add 3mg ammonium persulfate as oxidant, add distilled water 20mL, stirring and dissolving, then the SnS film inclined side of preparation is put in its polytetrafluoroethylene reactor, 120 DEG C are reacted 18 hours, product distilled water and absolute ethyl alcohol respectively wash 3 times, and constant temperature 60 DEG C is dry obtains SnO 2film product, product is white clear film.Microstructure is under a scanning electron microscope the equally distributed open structure of nano particle, and scanning electron micrograph is shown in Fig. 1.
embodiment 2
1, preparation: volume 30mL polytetrafluoroethylene reactor is respectively washed 2 times with running water, distilled water, absolute ethyl alcohol successively, stand-by after dry; Magnetron sputtering is utilized to sputter in the substrate of ITO electro-conductive glass 200nmthick metal Sn is stand-by.
2, reactions steps: add 3mg sulphur powder in the clean polytetrafluoroethylene reactor of volume 30mL, add absolute ethyl alcohol and each 10mL of DMF, be uniformly mixed, then use the above-mentioned sputtering of clean tweezers gripping ?the ITO electro-conductive glass sheet inclined side of metal Sn is put in polytetrafluoroethylene reactor, make metal covering upward, react 4 hours at 160 DEG C, product distilled water and absolute ethyl alcohol respectively wash 3 times, constant temperature 60 DEG C of dryings, i.e. obtained SnS film in the substrate of ITO electro-conductive glass sheet; In the clean polytetrafluoroethylene reactor of volume 30mL, add 3mg ammonium persulfate as oxidant, add distilled water 20mL, stirring and dissolving, then the SnS film inclined side of preparation is put in polytetrafluoroethylene reactor, 120 DEG C are reacted 24 hours, product distilled water and absolute ethyl alcohol respectively wash 3 times, and constant temperature 60 DEG C is drying to obtain SnO 2film.Product is white clear film, and the open structure of even particle distribution sized by microstructure under a scanning electron microscope, scanning electron micrograph is shown in Fig. 2.
embodiment 3:
1, preparation: volume 30mL polytetrafluoroethylene reactor is respectively washed 2 times with running water, distilled water, absolute ethyl alcohol successively, stand-by after dry; Magnetron sputtering is utilized to sputter in the substrate of ITO electro-conductive glass 200nmthick metal Sn is stand-by.
2, reactions steps: add 3mg sulphur powder in the clean polytetrafluoroethylene reactor of volume 30mL, add a certain amount of absolute ethyl alcohol and each 10mL of DMF, be uniformly mixed, then use the above-mentioned sputtering of clean tweezers gripping ?the ITO electro-conductive glass sheet inclined side of metal Sn is put in polytetrafluoroethylene reactor, make metal covering upward, react 4 hours at 160 DEG C, product distilled water and absolute ethyl alcohol respectively wash 3 times, constant temperature 60 DEG C of dryings, namely in the substrate of ITO electro-conductive glass sheet, obtained SnS film is for subsequent use; In the clean polytetrafluoroethylene reactor of volume 30mL, add 3mg ammonium persulfate as oxidant, add distilled water 20mL, stirring and dissolving, then the SnS film inclined side of preparation is put in its polytetrafluoroethylene reactor, 140 DEG C are reacted 24 hours, product distilled water and absolute ethyl alcohol respectively wash 3 times, and constant temperature 60 DEG C is drying to obtain SnO 2film product.Product is white clear film, and the open structure of even particle distribution sized by microstructure under a scanning electron microscope, scanning electron micrograph is shown in Fig. 3, and X ray diffracting spectrum is shown in Fig. 4.
3, SnO 2the preparation of the hetero-junction thin-film solar cell device of/P3HT hydridization: utilize spin-coating method that the poly-3-hexyl thiophene conjugated polymer (P3HT) of the 10mg/mL prepared is spun on obtained SnO in vacuum glove box 2film surface, 120 DEG C of annealing in process 2 hours, finally utilize vacuum evaporation instrument to steam and do electrode with Al, namely assemble to obtain ITO/SnO 2: P3HT/Al is inorganic/the hetero-junction thin-film solar cell device of organic hybrid.Fig. 5 is shown in by device assembling schematic diagram.
The photoelectric properties of assembled battery are tested by solar simulator, AM1.5 filter, 100 mW/cm 2xenon source irradiate, obtain the density of photocurrent-voltage curve (I-V curve) of battery and see Fig. 6.The open circuit voltage (Voc) of this battery is 0.405V, and density of photocurrent (Jsc) is 0.321mA/cm 2, fill factor, curve factor (FF) is 15.52%, and the electricity conversion of this battery is 0.02% at present.

Claims (4)

1. a hetero-junction thin-film solar cell device for inorganic/organic hybrid, is characterized in that, it is ITO/SnO 2: P3HT/Al is inorganic/the hetero-junction thin-film solar cell device of organic hybrid; Wherein SnO 2nano film material at low temperatures original position prepares, and method is with nanometer Sn (0)for Xi Yuan, first utilize solvent structure SnS, then be predecessor water heat transfer SnO with SnS 2film, to synthesize SnO by hydro-thermal and solvent heat two step wet chemical in the ITO electro-conductive glass substrate being coated with metallic tin 2nano film material, this thin-film material thickness is regulated and controled by reaction temperature and reaction time condition.
2. as claimed in claim 1 a kind of inorganic/the hetero-junction thin-film solar cell device of organic hybrid, it is characterized in that: wherein SnO 2the nano film material method that at low temperatures prepared by original position is, first magnetron sputtering is utilized to sputter layer of metal tin in the substrate of ITO electro-conductive glass, the ITO electro-conductive glass sheet inclined side this having been sputtered layer of metal tin is put in volume 30mL polytetrafluoroethylene reactor, make metal covering upward, add 3mg sulphur powder, then absolute ethyl alcohol and each 10mL of DMF is added, to be placed at 160 DEG C of temperature solvent thermal reaction 4 hours, product distilled water and absolute ethanol washing more than 2 times, be drying to obtain SnS film for subsequent use; Then the SnS film inclined side of preparation is put in 30mL polytetrafluoroethylene reactor, add 3mg ammonium persulfate as oxidant, to distill water as solvent, the volume of distilled water is vessel volume 1/2 ~ 2/3, react 24 hours under temperature is 140 DEG C of temperature, product distilled water and absolute ethanol washing more than 2 times, namely drying at room temperature obtains SnO 2nano film material.
3. as claimed in claim 1 a kind of inorganic/the hetero-junction thin-film solar cell device of organic hybrid, it is characterized in that: wherein SnO 2with the preparation method of P3HT hybrid heterojunctions thin-film solar cells be, first magnetron sputtering is utilized to sputter layer of metal tin in the substrate of ITO electro-conductive glass, the ITO electro-conductive glass sheet inclined side this having been sputtered layer of metal tin is put in volume 30mL polytetrafluoroethylene reactor, make metal covering upward, add 3mg sulphur powder, then absolute ethyl alcohol and each 10mL of DMF is added, to be placed at 160 DEG C of temperature solvent thermal reaction 4 hours, product distilled water and absolute ethanol washing more than 2 times, be drying to obtain SnS film for subsequent use; Then the SnS film inclined side of preparation is put in 30mL polytetrafluoroethylene reactor, add 3mg ammonium persulfate as oxidant, to distill water as solvent, the volume of distilled water is vessel volume 1/2-2/3, react 24 hours under temperature is 140 DEG C of temperature, product distilled water and absolute ethanol washing more than 2 times, namely drying at room temperature obtains SnO 2nano thin-film;
Then in vacuum glove box, utilize spin-coating method that the P3HT of the 10mg/mL prepared is spun on obtained SnO 2nano thin-film surface, 120 DEG C of annealing in process 2 hours and get final product.
4. as claimed in claim 1 a kind of inorganic/preparation method of the hetero-junction thin-film solar cell device of organic hybrid, it is characterized in that: first prepare SnO by the step described in claim 3 2with P3HT hybrid heterojunctions thin-film solar cells, recycling vacuum evaporation instrument steams and does electrode with Al, namely assembles to obtain ITO/SnO 2: P3HT/Al is inorganic/the hetero-junction thin-film solar cell device of organic hybrid.
CN201210292721.5A 2012-08-17 2012-08-17 A kind of SnO 2with the preparation method of P3HT hybrid heterojunctions thin-film solar cells Expired - Fee Related CN102856499B (en)

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