CN101127374B - Making method for flexible dye sensitized solar battery nano crystal thin film - Google Patents

Making method for flexible dye sensitized solar battery nano crystal thin film Download PDF

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CN101127374B
CN101127374B CN2007100186392A CN200710018639A CN101127374B CN 101127374 B CN101127374 B CN 101127374B CN 2007100186392 A CN2007100186392 A CN 2007100186392A CN 200710018639 A CN200710018639 A CN 200710018639A CN 101127374 B CN101127374 B CN 101127374B
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tio
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CN101127374A (en
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李长久
杨冠军
范圣强
李成新
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Xian Jiaotong University
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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
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    • 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
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    • 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
    • Y02E10/549—Organic 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
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Abstract

The utility model belongs to field of solar battery, and relates to a manufacturing approach of flexible nanometer-crystalline film of dye sensitizing solar battery, which adopts nanostructured porous TiO2 powder as the material and forms the porous TiO2 film by depositing on a conducting substrate by vacuum deposition. The utility model is characterized in that a porous TiO2 film is made by vacuum cold coating, wherein the nanostructured porous TiO2 powder is accelerated by airflow and impacts on the substrate or the TiO2 coat at a high speed to speed up the combinations of the powder under the pressure of high speed impact at instantaneous high temperature rise; therefore the coat is combined well with the substrate and so are the grains in the coat. The film made by the above approach dose not need to go through high temperature process during manufacturing and after manufacturing, therefore is suitable for manufacture of flexible nanometer-crystalline film of dye sensitizing solarbattery.

Description

The manufacture method of flexible dye sensitized solar battery nano crystal thin film
Technical field
The invention belongs to especially dye-sensitized solar cells technical field of solar cell field, be specifically related to a kind of manufacture method that is used for the nanocrystalline photo-anode film of the flexible dye-sensitized solar cell on flexible organic polymer conductive substrates.
Background technology
Solar cell can directly become electric energy with conversion of solar energy, is main one of form of utilizing of solar energy.The solar cell of being studied at present mainly comprises: silicon solar cell, compound semiconductor battery, polymer film solar cell and dye sensitized nano crystal solar cell.From 1991
Figure G200710018639201D00011
Deng having reported that on Nature (dye-sensitized solar cell, since solar conversion efficiency DSC)＞7%, DSC just has been subjected to widely paying close attention to the dye sensitized nano crystal solar cell.So far, the energy conversion efficiency of DSC has surpassed 11%.According to the state difference of electrolyte, be divided into liquid DSC and solid-state DSC two classes, have solid-state feature on the semisolid DSC macroscopic view of latest developments and have liquid feature on the microcosmic.
At present the DSC of preparation is that the electro-conductive glass with hard is substrate mostly, so battery can not bend.If with the transparent organic material base material of flexibility is substrate, then DSC has characteristics such as the flexible district is bent, and this will significantly expand the scope of application of DSC.Simultaneously, when liquid DSC is substrate with the fragility electro-conductive glass, may occurs owing to hard thing bump or scratch reasons such as the district is excessive and cause cracking, thereby cause the leakage of liquid electrolyte, environment is caused certain destruction.If prepare DSC with flexible substrates, then the probability of battery drain significantly reduces.Simultaneously, in light weight at the bottom of the organic group, can realize that Scroll produces continuously, from and can further reduce manufacturing cost.
Battery is by the light anode, form electrode and electrolyte.The porous TiO that in substrates such as electro-conductive glass, deposits 2Constitute the light anode behind the film absorbing dye.Consider electricity conversion be by dyestuff lighting efficiency, electronics from dyestuff to TiO 2The injection efficiency of film, electronics are at TiO 2Transmission in the film and the collection efficiency, electrolyte ion that reach conducting base are at TiO 2Transmittance process determines in the film.Therefore, to TiO 2The specific requirement of film is:
(1) needle-like or the nearly spherical nanoparticles perforated membrane of being piled into so that bigger surface area to be provided, increases the adsorption density of dyestuff, improves lighting efficiency;
(2) appropriate porosity and pore-size distribution are to guarantee electrolyte transmission in dyestuff absorption and the film.
(3) good connection between the nano particle is to increase electronics at TiO 2Good transmission performance in the film improves collection efficiency; Typical TiO 2Film is the TiO by 10-30nm 2Particle packing forms, thickness 5-30 μ m, coarse factor hundreds of to several thousand, general more than 50%, the aperture of porosity is mainly 5-30nm.Aspect pore structure, spread angle from diffusion absorption, the electrolyte of dyestuff to the infiltration diffusion and the electrolyte charge carrier of film inside to film inside, wish that the duct size can not be too little.
TiO at DSC 2The film preparation aspect, at present broad research and the preparation method commonly used that obtains bigger progress comprise methods such as knife coating, silk screen print method, spin coating method, pyrosol jet deposition.These methods all are difficult to use in flexible substrates, because about 150 ℃ of general organic substance flexible substrates heatproof, and the something in common of said method to be base material must experience 450 ℃～550 ℃ high-temperature process, in order to realize removing residual organic principle in the film, with TiO 2Amorphous component crystallization, removal TiO 2Some crystal defects in the crystal, make TiO 2Has the purpose such as combine between connection status preferably, reinforcing membrane and base material between nano particle.
At the low temperature preparation of the light anode porous nano-crystal thin-film of most critical among the DSC, preceding two ratios are easier to realize in the above-mentioned requirements, but the 3rd has stronger challenge.Existing so far low temperature film-forming method has mechanical pressed film method, hydrothermal reaction at low temperature, film transfer method, chemical deposition, electrophoretic deposition, colloid film direct low-temperature sintering method, hydrothermal method etc.
In recent years, the applicant is based on the vacuum cold spray method, and the porous type nanostructured powders that adopts PEG and P25 preparation to be of a size of sub-micron is a sprayed on material, has prepared TiO 2Film, film is removed PEG and TiCl through 400 ℃～500 ℃ heat treatments 4Can be met the high-performance Na crystal porous membrane that DSC requires after the sintering processes.
Summary of the invention
The objective of the invention is to propose a kind of manufacture method of flexible dye sensitized solar battery nano crystal thin film, this method adopts the process that relates to high-temperature heat treatment to prepare the porous type nanostructure dusty spray of special construction design, has good connection status between primary nanoparticle by every porous type nanostructured powders inside of powder preparation process assurance, adopt the vacuum cold spray method to realize the low temperature film-forming process then, adopt high velocity air that the porous type nanostructured powders is quickened the back high-speed impact and form film in the matrix surface deposition, promote combining between powder by the porous type nanostructured powders jointly with the high-speed impact pressure and the local instantaneous temperature of matrix surface, thereby coating and matrix, has good binding between the coating internal particle.The film of this method preparation, owing to do not relate to traditional pyroprocess in the coating preparation process on flexible substrate, and also can not experience pyroprocess after the film preparation, film is had between internal particle in conjunction with good characteristic, therefore can be used for the preparation of the high performance thin film of high-efficiency soft dye sensitized solar cel electrode.
In order to realize above-mentioned task, the present invention takes following technical solution:
A kind of manufacture method of flexible dye sensitized solar battery nano crystal thin film is characterized in that implementing according to the following steps:
With nano-TiO 2Powder is an original material, connects heat treatment by containing the Ti compound, constitutes powder or blank, obtains porous type nanostructure TiO through break process then 2Powder.
With porous type nanostructure TiO 2Powder is a sprayed on material, adopts the vacuum cold spray method in the spraying of compliant conductive substrate surface, can obtain the dye sensitized solar battery nano crystal thin film of porous nanometer structure.
Described porous type nanostructure TiO 2Powder has loose structure, two essential characteristics of nanostructure.The granularity of this powder is 0.1 μ m～3 μ m, and each porous type nanostructured powders particle is by a plurality of nanocrystalline TiO 2The primary granule single powder particle that links together and constitute, the granularity of these primary granules is 1nm～1000nm, therefore has the nanostructure feature; Contain the duct that the aperture of not exclusively filling between the primary nanoparticle and realizing mainly is distributed in a few nanometer to tens nanometers in this porous type nanostructured powders, therefore have the loose structure feature.In addition, thus having the good binding state between the primary granule in this porous type nanostructured powders guarantees to have electron transport performance preferably between the primary granule of single powder inside.
Described nano-TiO 2Powder is that primary particle size is powder, the TiO of nanoscale 2The attritive powder of amorphous component, or can heat treatment generate nano-TiO 2The mixture that contains two classes in Ti material three classes or three classes of particle.
Described connection heat treatment is that original material and the system that contains the Ti compound-material are heat-treated, and heat treatment temperature is 50 ℃～800 ℃, generates new TiO in connecting heat treatment process 2And make and produce better combination between the powder particle in the original material.
Described connection heat treatment is selected from conventional heat treatment, UV radiation treatment, microwave irradiation processing, electron beam irradiation processing, hydrothermal treatment consists or wherein two or more.
Described powder or blank are through connecting the powder block that the size that obtains after the heat treatment surpasses 0.05～5 μ m, will be less than the powder that is called of 1mm, and will be above the blank that becomes of 1mm.
Described break process is the process that powder or blank is become the small scale powder by the type of action of grinding, impact, pushing or vibrating.
Describedly be selected from UV radiation treatment, microwave irradiation processing, electron beam irradiation processing, hydrothermal treatment consists, steam treatment or two or more processing procedure wherein, with the bonding state between further enhanced granule through described two films that prepare of step of claim 1 and matrix system.
The present invention has realized the low temperature system film on the flexible substrates, is applicable to the film demand of high-efficiency soft DSC, and the positive technique effect that is brought is:
The first, have good connection status between the inner primary nanoparticle of this film of this invention preparation.In porous type nanostructured powders preparation process, guaranteed to have the good binding state between the primary nanoparticle of every porous type nanostructured powders inside by the process that may relate to high temperature, in the depositing of thin film preparation process, promote combining between powder by the porous type nanostructured powders jointly with the high-speed impact pressure and the local instantaneous temperature of matrix surface, thereby have good binding between coating and matrix, coating internal particle.This helps the electrons spread transmission of film inside, thereby has established for improving battery efficiency
The first, have good connection status between the inner primary nanoparticle of this film of this invention preparation.In porous type nanostructured powders preparation process, guaranteed to have the good binding state between the primary nanoparticle of every porous type nanostructured powders inside by the process that may relate to high temperature, in the depositing of thin film preparation process, promote combining between powder by the porous type nanostructured powders jointly with the high-speed impact pressure and the local instantaneous temperature of matrix surface, thereby have good binding between coating and matrix, coating internal particle.This helps the electrons spread transmission of film inside, thereby has established for improving battery efficiency
Important foundation.
Second, the film of this invention preparation has novel multiple dimensioned pore passage structure feature, promptly have reduced size duct and large-size duct simultaneously, be particularly conducive to diffusion and the absorption of dyestuff to film inside, help the transmission of electrolyte charge carrier in film, for the battery of solid or accurate solid electrolyte, this film also is beneficial to electrolyte osmosis and diffuses into film inside.
The 3rd, the method for this invention is suitable for the continuous roll shaft formula of flexible substrates upper film produces, and has significantly easily industrialization feature and low-cost production feature.
The 4th, the thickness of film can be controlled by the spraying parameter of vacuum cold spray, and the two-dimentional geometrical shape of film could move, spray direction by the program of matrix or spray gun mask set designs realization, and it can be designed to lattice-shaped TiO 2Film is used for the series and parallel of dye sensitized nano crystal salar battery, thereby technology simple and flexible, controllability are good, and volume production is with low cost.
Adopt the photo-anode film that can be used for flexible dye-sensitized nano crystal solar cell of this method manufacturing, the battery performance of assembling can be better than the battery that conventional method prepares film at some aspect of performances, be a kind of desirable new method that is used for high-efficiency soft dye sensitized nano crystal solar cell manufacturing field, be expected to positive facilitation is played in the further high efficiency and the industrialization that promote flexible DSC.
Description of drawings
Fig. 1 is porous type nanostructure TiO 2The structural representation of powder
Fig. 2 is this porous TiO according to the present invention's preparation 2The typical section pattern of film;
Fig. 3 is TiO 2The nanoaperture structure of film inside;
Fig. 4 is the representative cells output characteristic;
The present invention is described in further detail below in conjunction with drawings and Examples.
Below be the embodiment that the inventor provides, need to prove that these embodiment are the more excellent examples of the present invention, be used for those skilled in the art and understand the present invention, but the present invention is not limited to these embodiment.
Embodiment 1:
The commercially available P25 nano-TiO that adopts German XX company to produce 2The Detitanium-ore-type TiO of powder 36g, commercially available 200nm 2Powder 4g joins 0.05mol/L, 70 ℃ TiCl 4Carry out ultrasonic vibration 10min among the aqueous solution 1000ml, be heated to 500 ℃ of heat treatment 30min then, TiCl 4The TiO that forms after the hydrolysis 2At initial TiO 2Primary granule better can be linked together between the particle, thereby to TiO 2Connection between primary granule is strengthened.The sintering blank that obtains is obtained the porous type nanostructured powders of micron/submicron order through break process.With this porous type nanostructure TiO 2Powder is that raw material adopts the vacuum cold spray method to prepare the porous nanometer structure film in the spraying of compliant conductive substrate (such as ITO-PET, the conductive polyester plastics) surface.The thin-membrane section structure as shown in Figure 2, film is evenly distributed at matrix surface.Film is carried out obtaining after the research of nitrogen adsorption desorption the hole characteristic of receiving of film inside, and as shown in Figure 3, visible pore mainly is distributed between the 5-40 nanometer, and the porosity is about 47%.Film is heated to 100 ℃ of insulations was immersed in the N719 dyestuff of 30mM the room temperature sensitization behind the 10min 24 hours, be prepared into the light anode.With above-mentioned electrode and Pt to the utmost point, LiI and I 2Acetonitrile solution be assembled into DSSC, at AM1.5 (100mW/cm 2) the xenon source simulated solar irradiation under, the output characteristic that records battery is as shown in Figure 4.Short-circuit current density 8.1mA/cm 2, open circuit voltage 0.65V, energy conversion efficiency 1.9%.
Embodiment 2:
Adopt the Detitanium-ore-type TiO of 15nm 2The colloidal sol 100ml that nanometer powder 50g, the hydrolysis of 5g butyl titanate obtain is heated to 400 ℃ of heat treatment 20min behind the ultrasonic dispersion 5min, contain the Ti material at initial TiO in the colloidal sol 2Particle surface and between crystallization be new TiO 2, primary granule better can be linked together, the sintering blank that obtains is passed through the porous type nanostructured powders that break process obtains micron/submicron order, with this porous type nanostructure TiO 2Powder is that raw material adopts the vacuum cold spray method to prepare the porous nanometer structure film in the spraying of compliant conductive substrate surface.The medium pressure mercury lamp that this film is carried out 125W carries out UV apart from film surface 4cm to be handled 3 hours, made the connection between the nano particle of film inside better.
Embodiment 3:
Further, utilize nano-TiO 2Self sintering interconnect function of particle is directly with nano-TiO 2Powder is heat-treated, at 520 ℃ of heat treatment 4h, with this porous type nanostructure TiO 2Powder is that raw material adopts the vacuum cold spray method to prepare the porous nanometer structure film in the spraying of compliant conductive substrate surface.If film is carried out the hydrothermal treatment consists of 100 ℃ of 10h, adopt the Microwave Treatment 5 minutes of 28GHz then, realize strengthening purpose of connecting between particle.Dry then the taking-up after porous type nanostructured powders broken and screening adopts the vacuum cold spray method to prepare the porous nanometer structure film in the spraying of compliant conductive substrate surface with this powder.
Method of the present invention not only can prepare dye sensitized solar battery nano crystal thin film on flexible substrates, and can prepare the porous nanometer structure film at the conductive glass surface of hard.

Claims (8)

1. the manufacture method of a flexible dye sensitized solar battery nano crystal thin film is characterized in that implementing according to the following steps:
With nano-TiO 2Powder is an original material, connects heat treatment by containing the Ti compound, constitutes powder or blank, obtains porous type nanostructure TiO through break process then 2Powder;
With porous type nanostructure TiO 2Powder is a sprayed on material, adopts the vacuum cold spray method in the spraying of compliant conductive substrate surface, can obtain the dye sensitized solar battery nano crystal thin film of porous nanometer structure.
2. manufacture method as claimed in claim 1 is characterized in that, described porous type nanostructure TiO 2The granularity of powder is 0.1 μ m～3 μ m, each porous type nanostructure TiO 2Powder particle is by a plurality of nanocrystalline TiO 2The primary granule single powder particle that links together and constitute, the granularity of these primary granules is 1nm～1000nm; Contain between the primary nanoparticle aperture of not exclusively filling and realizing in this porous type nanostructured powders and mainly be distributed in the duct of a few nanometer to tens nanometers, guarantee to have electron transport performance preferably between the primary granule of single powder inside thereby have the good binding state between the primary granule in this porous type nanostructured powders.
3. manufacture method as claimed in claim 1 is characterized in that, described nano-TiO 2Powder is that primary particle size is powder, the TiO of nanoscale 2The attritive powder of amorphous component, or can heat treatment generate nano-TiO 2The mixture that contains two classes in Ti material three classes or three classes of particle.
4. manufacture method as claimed in claim 3 is characterized in that, described connection heat treatment is that original material and the system that contains the Ti compound-material are heat-treated, and heat treatment temperature is 50 ℃～800 ℃, generates new TiO in connecting heat treatment process 2And make and produce better combination between the powder particle in the original material.
5. manufacture method as claimed in claim 1 is characterized in that, described connection heat treatment is selected from conventional heat treatment, UV radiation treatment, microwave irradiation processing, electron beam irradiation processing, hydrothermal treatment consists or wherein two or more.
6. manufacture method as claimed in claim 1 is characterized in that, described powder or blank are through connecting the powder block that the size that obtains after the heat treatment surpasses 0.05～5 μ m, will be less than the powder that is called of 1mm, and will be above the blank that is called of 1mm.
7. manufacture method as claimed in claim 1 is characterized in that, described break process is by the type of action of grinding, impact, pushing or vibrating powder or blank to be become the small scale powder.
8. manufacture method as claimed in claim 1, it is characterized in that, describedly be selected from UV radiation treatment, microwave irradiation processing, electron beam irradiation processing, hydrothermal treatment consists, steam treatment or two or more processing procedure wherein, with the bonding state between further enhanced granule through described two films that prepare of step of claim 1 and matrix system.
CN2007100186392A 2007-09-11 2007-09-11 Making method for flexible dye sensitized solar battery nano crystal thin film Expired - Fee Related CN101127374B (en)

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Publication number Priority date Publication date Assignee Title
CN101261901B (en) * 2008-04-29 2010-06-02 四川大学 A dye sensitized solar battery anode and its making method
CN101800130B (en) * 2010-04-19 2011-06-22 西安交通大学 Method for preparing dye-sensitized solar cell compound light anode with zinc oxide nanometer structure
CN102222575B (en) * 2011-03-30 2012-11-28 东南大学 Preparation method for photoanode of dye-sensitized solar cell
CN102231332B (en) * 2011-03-31 2013-06-12 中国科学院安徽光学精密机械研究所 Flexible Dye-sensitized Solar Cells (DSSCs) based on titanium dioxide nanometer rod array film and preparation method thereof
CN102768227B (en) * 2012-06-11 2015-04-22 江苏大学 Production method of dye-sensitized TiO2 film based gas sensor
EP2927980B1 (en) * 2012-11-27 2019-05-22 Sekisui Chemical Co., Ltd. Method for manufacturing solar cell
CN104508183B (en) * 2013-01-22 2017-07-18 积水化学工业株式会社 Film-forming method, multiple aperture plasma membrane, optoelectronic pole and dye-sensitized solar cell
CN103346263B (en) * 2013-05-31 2016-04-27 奇瑞汽车股份有限公司 The flexible carbon of DSSC to the preparation method of electrode, flexible carbon to electrode and battery
CN114953667A (en) * 2022-04-24 2022-08-30 山西阳中新材有限责任公司 Aerogel-containing temperature-sensitive heat-insulating film and preparation method thereof

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