CN103700505B - The method of Fast Sintering large-area dye-sensitized solar battery photo-anode - Google Patents
The method of Fast Sintering large-area dye-sensitized solar battery photo-anode Download PDFInfo
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- Y02E10/542—Dye sensitized solar cells
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Abstract
The present invention relates to a kind of method of Fast Sintering large-area dye-sensitized solar battery photo-anode, comprise: by titania nanoparticles, terpinol and cellulosic binder with (1 ~ 2): (0.2 ~ 0.5): the ratio mixing of (5 ~ 9), and obtain TiO after magnetic agitation, high shear and ultrasonic disperse
2colloid; The TiO that silk screen printing is obtained on the electro-conductive glass cleaned
2colloid is with the light anode of obtained DSSC and dry; And the light anode of oven dry is put into sintering furnace sinter, the program of sintering is: program one: put into light anode in sintering furnace after, within 40 minutes, sintering furnace is risen to 300 ~ 800 DEG C from room temperature and takes out the cooling of light anode after being incubated 0 ~ 100 minute; Or program two: after stove to be sintered rises to 300 ~ 800 DEG C, light anode is put into sintering furnace insulation and take out the cooling of light anode after 0 ~ 100 minute, in program one and/or program two, the instrument of taking when taking out light anode is heated to 100 ~ 400 DEG C in advance.
Description
Technical field
The present invention relates to a kind of preparation method of dye-sensitized solar cell anode, particularly relate to a kind of method of Fast Sintering large-area dye-sensitized solar battery photo-anode.
Background technology
The instead energy of fossil fuel, the solar cell that make use of sunlight receives publicity, and people have carried out various research to it.Solar cell is a kind of is the photoelectric conversion device of electric energy by transform light energy, due to using sunlight as the energy, so minimum on the impact of earth environment, can be popularized widely.
The research and development converting solar energy into luminous energy is in recent years very fast.Apply by the dye-sensitized solar cell (Dye-SensitizedSolarCell of the photoinduction electronics movement of dye sensitization, DSSC), instead the solar cell of future generation of silicon (Si) class solar cell etc. receives publicity in recent years, and is extensively studied.The advantage of DSSC (DSSC) is very outstanding: 1, make simple, cost is low; 2, the dye sensitizing agent used can be issued to saturated in very low light energy, therefore can use under various illumination condition; 3, normally can work in very wide temperature range; 4, transparent product can be made, be applied to door and window, roof and vehicle top.Therefore it becomes rapidly research emphasis and the focus of countries in the world, achieves abundant achievement, has started the upsurge of various countries' research DSSC solar cell.
DSSC is as third generation solar cell, it is current most potential silicon solar cell cheap alternative, it is prepared into the broad-band gap oxide semiconductor of cheapness has loose structure, the nano-crystal film of high-specific surface area, the semiconductive thin film of nanocrystalline structure is the core of work electrode, the feature of its porous and huge specific area ensure that the enough absorption of dye molecule, simultaneously, followed the interface formed between titanium dioxide nano-particle can make the migration of electronic high-effective by the dye molecule adsorbed, and select suitable redox electrolytes matter, utilize dyestuff to capture sunlight.
On the light anode of dye-sensitized cell, light-sensitive coloring agent molecule absorption sunlight transits to excitation state, and the dyestuff being in excitation state injects electronics so as to realizing separation of charge in the conduction band of conductor oxidate.The light anode porosity of dye-sensitized cell is higher, and absorbing dye is more, and the non equilibrium carrier density produced under illumination increases, and can make resistance decreasing, and cell photoelectric conversion efficiency improves.
But in the preparation method of existing dye-sensitized cell, there is large area light anode sintering overlong time, high temperature directly takes out the phenomenon that light anode carrier very easily ftractures, can not meet the requirement that industrialization is produced, its related process also has to be further improved and optimizes.
Summary of the invention
The object of the invention is to overcome above-mentioned deficiency, a kind of method of Fast Sintering large-area dye-sensitized solar battery photo-anode is provided, thus effectively can shorten sintering time, reduce light anode carrier cracking phenomena, form multidimensional network structure after making large area light anode sintering and improve Dye Adsorption amount, thus battery efficiency is reached and sinters the effect compared favourably for a long time.
At this, the invention provides a kind of method of Fast Sintering large-area dye-sensitized solar battery photo-anode, comprising:
(1) by titania nanoparticles, terpinol and cellulosic binder with (1 ~ 2): (0.2 ~ 0.5): the ratio mixing of (5 ~ 9), and obtains TiO after magnetic agitation, high shear and ultrasonic disperse
2colloid;
(2) TiO that screen printing step (1) is obtained on the electro-conductive glass cleaned
2colloid is with the light anode of obtained DSSC and dry; And
(3) the light anode of oven dry is put into sintering furnace to sinter, the program of sintering is:
Program one: put into light anode in sintering furnace after, rose to 300 ~ 800 DEG C by sintering furnace from room temperature and takes out the cooling of light anode after being incubated 0 ~ 100 minute within 40 minutes; Or
Program two: after stove to be sintered rises to 300 ~ 800 DEG C, puts into sintering furnace insulation and takes out the cooling of light anode after 0 ~ 100 minute by light anode,
In program one and/or program two, the instrument of taking when taking out light anode is heated to 100 ~ 400 DEG C in advance.
The present invention is by the Fast Sintering that is rapidly heated, or the Fast Sintering that heats up in advance, and directly from sintering furnace, takes out light anode when high temperature, effectively can shorten sintering time, increase work efficiency, and saves energy consumption, reduces production cost.In addition, in the present invention, the instrument of taking when taking out light anode is heated to 100 ~ 400 DEG C in advance, takes like this and when instrument contacts with high temp glass, to there will not be contact site to cause ftractureing due to temperature shock, again, the TiO in light anode is prepared by use said method
2film, when after can making sintering, high temperature takes out, film is not easy to crack.Like this, sintering after high temperature take out light anode time glass and film all not easy to crack, thus the useful life of the DSSC prepared by this light anode can be increased, and form multidimensional network structure after making large area light anode sintering and improve Dye Adsorption amount, thus battery efficiency is reached and sinters the effect compared favourably for a long time.And the invention provides two kinds of sintering procedures, these two kinds of sintering procedures can reach same sintering result, are convenient to according to circumstances select flexibly.
In one preferred embodiment, in described program one, the heating-up time is preferably less than 20 minutes.Effectively can shorten sintering time like this, increase work efficiency.
Another preferred embodiment in, in described program one, temperature retention time is preferably 0 ~ 15 minute.Effectively can shorten sintering time like this, increase work efficiency.
Another preferred embodiment in, in described program two, temperature retention time is preferably less than 30 minutes.Effectively can shorten sintering time like this, increase work efficiency.
Another preferred embodiment in, described titania nanoparticles comprises and is of a size of the little nano particle of 15 ~ 60nm titanium dioxide and be of a size of the large nano particle of 200 ~ 500nm titanium dioxide, and the mass ratio of the little nano particle of described titanium oxide and the large nano particle of titanium dioxide is 1:(0 ~ 100).
In a preferred execution mode, the mass ratio of the little nano particle of described titanium dioxide and the large nano particle of titanium dioxide is 1:(0.1 ~ 0.4).
In another preferred execution mode, the mass ratio of the little nano particle of described titanium dioxide and the large nano particle of titanium dioxide is (0.01 ~ 0.1): 1.
Another preferred embodiment in, the little nano particle of described titanium dioxide is anatase titanium dioxide nano particle, prepared by sol-gel process, described sol-gel process comprises: be (9 ~ 99) by weight ratio: the titanium precursors of 1 and the mixed solution of acetic acid are added drop-wise in deionized water, acid adding regulates solution ph to be 1 ~ 3,80 DEG C ~ 120 DEG C are reacted 6 ~ 24 hours, then 16 ~ 96 hours are incubated at being placed in reactor 200 DEG C ~ 270 DEG C, collect, after washing, obtain 15 ~ 60 nano crystal anatase titanias.
Another preferred embodiment in, described titanium precursors is butyl titanate and/or tetraisopropyl titanate.
Another preferred embodiment in, for regulating the acid of solution ph to be selected from sulfuric acid, nitric acid, acetic acid, hydrochloric acid, benzoic acid, citric acid, laurate, with at least one in oxalic acid.
The present invention has following beneficial effect:
(1) shorten the sintering time of large area light anode, improve operating efficiency;
(2) light anode can not ftracture, and adds the useful life of battery;
(3) two kinds of sintering procedures can reach same sintering result, are convenient to according to circumstances select flexibly;
(4) for the industrialization production of large-area dye-sensitized solar battery provides technical support.
Accompanying drawing explanation
Fig. 1 is the endurance test result figure of the DSSC prepared by the light anode obtained according to the method for example of the present invention, and a, b, c, d, e, f are wherein respectively open circuit voltage (Voc), short circuit current (Jsc), fill factor, curve factor (FF), conversion efficiency (Eff), resistance (Rs), normalization efficiency (NormalizedEff) time dependent figure;
Fig. 2 is the I-V curve of the DSSC prepared by the light anode obtained according to the method for example of the present invention;
Fig. 3 is the temperature curve of sintering procedure two;
Fig. 4 is the temperature curve of sintering procedure one and sintering procedure two.
Embodiment
Further illustrate the present invention below in conjunction with accompanying drawing and following execution mode, should be understood that accompanying drawing and following execution mode are only for illustration of the present invention, and unrestricted the present invention.Although should understand following with TiO
2as active nanoparticles, but also can adopt ZnO, SnO by similar method
2, ZrO, Fe
2o
3, Nb
2o
5, Al
2o
3, MgO, TiO
2/ PbS, TiO
2/ PbS/CdS, SiO
2/ TiO
2substitute.
The invention provides a kind of method of Fast Sintering large-area dye-sensitized solar battery photo-anode: prepare light anode by the method for silk screen printing, sintering after drying.This sintering can reach same effect by two kinds of programs.Program one: put into light anode, stove rises to sintering temperature from room temperature, insulation a period of time, takes out the rear assembled battery of light anode cooling; Program two: treat that furnace rises to sintering temperature, puts into light anode heat-insulation a period of time, takes out the rear assembled battery of light anode cooling.Particularly, exemplarily, method of the present invention can comprise the following steps.
Step one, TiO
2the preparation of colloid: titania nanoparticles and terpinol and cellulosic binder are with (1 ~ 2): (0.2 ~ 0.5): the ratio of (5 ~ 9) mixes, and obtain after magnetic agitation, high shear and ultrasonic disperse.Thus obtained TiO
2colloid can comprise TiO
2, solvent and binding agent, wherein, TiO
2content is 0 ~ 30%, and solvent is 0 ~ 20%, and binder content is 50 ~ 90%.
In one example, TiO is prepared
2the titania nanoparticles adopted during colloid is anatase titanium dioxide nano particle, and sol-gel process can be adopted to prepare.In one example, sol-gel process can be: be (9 ~ 99) by weight ratio: the titanium precursors of 1 and the mixed solution of acetic acid are added drop-wise in deionized water, acid adding regulates solution ph to be 1 ~ 3,80 DEG C ~ 120 DEG C are reacted 6 ~ 24 hours, then 16 ~ 96 hours are incubated at being placed in reactor 200 DEG C ~ 270 DEG C, collect, after washing, obtain 15 ~ 60 nano crystal anatase titanias.Wherein, the titanium precursors adopted can be butyl titanate and/or tetraisopropyl titanate.For regulating the acid of solution ph optional from sulfuric acid, nitric acid, acetic acid, hydrochloric acid, benzoic acid, citric acid, laurate, and at least one in oxalic acid.
Should understand and can be of a size of the large nano particle of 200 ~ 500nm titanium dioxide and replace that part is above-mentioned is of a size of the little nano particle of 15 ~ 60nm titanium dioxide, the mass ratio of the little nano particle of titanium dioxide and the large nano particle of titanium dioxide can be 1:(0 ~ 100).In one example, the mass ratio of the little nano particle of titanium dioxide and the large nano particle of titanium dioxide is 1:(0.1 ~ 0.4).In another example, the mass ratio of the little nano particle of titanium dioxide and the large nano particle of titanium dioxide can be (0.01 ~ 0.1): 1.
Step 2, clean electro-conductive glass on silk screen printing TiO
2colloid obtains the light anode of DSSC and dries.
Wherein, the oven dry in step 2 can be of short duration oven dry on hot plate, such as, 0 ~ 350 DEG C of heating 0 ~ 100 minute.
Step 3, the light anode of oven dry is put into sintering furnace sinter.
This sintering can adopt following two kinds of programs:
Program one: put into light anode in sintering furnace after, rose to 300 ~ 800 DEG C (sintering temperatures) by sintering furnace from room temperature and takes out the cooling of light anode after being incubated 0 ~ 100 minute within 40 minutes.In a preferred example, the heating-up time is less than 20 minutes.In another preferred example, temperature retention time is 0 ~ 15 minute.By heating-up time and/or temperature retention time are set to shorter, can sintering time be shortened, increase work efficiency;
Program two: after stove to be sintered rises to 300 ~ 800 DEG C (sintering temperatures), puts into sintering furnace insulation and takes out the cooling of light anode after 0 ~ 100 minute by light anode.Put into light anode again sinter by advance furnace temperature being risen to sintering temperature, can sintering time be shortened, increase work efficiency.In a preferred example, temperature retention time is less than 30 minutes.Shorter by temperature retention time is set to, sintering time can be shortened further, increase work efficiency;
The temperature curve of the example of program two can see Fig. 3, and the temperature curve of the example of program one and program two can see Fig. 4.
Again, in program one and/or program two, at the end of sintering, directly from sintering furnace, take out light anode when high temperature.The instrument of taking when taking out light anode can be heated to 100 ~ 400 DEG C in advance.Take like this and when instrument contacts with high temp glass, to there will not be contact site to cause cracking due to temperature shock, thus the useful life of the DSSC prepared by this light anode can be increased, and form multidimensional network structure after making large area light anode sintering and improve Dye Adsorption amount, thus battery efficiency is reached and sinters the effect compared favourably for a long time.
Above two kinds of sintering procedures can reach same sintering effect, are convenient to according to circumstances select flexibly.
The large-area dye-sensitized solar battery photo-anode that method according to the present invention obtains may be used for the preparation of DSSC.Preparation method such as can comprise the following steps.Should be understood that this preparation method only for illustration of effect of the present invention, and unrestricted the present invention.
The light anode cooled after step 4, sintering, puts into dye solution and soaks.Immersion terminates rear taking-up light anode, washes away dye solution with 2 ~ 100mL absolute ethyl alcohol, dry 0.5 ~ 10 minute.
The dye solution adopted such as can comprise dyestuff, solvent and coadsorbent.In one example, dyestuff molar percentage: 0.1mmol/L ~ 5mol/L; Solvent volume is than 1:100 ~ 100:1; Coadsorbent molar percentage: 0.001mmol/L ~ 3mol/L.Wherein adopted dyestuff can be one or more in N3, N719, blackdye, Z907, K8, K19, N945, Z910, K73, K51, Z955, cyanine, cumarin, porphyrin, indoles, perylene flower cyanines and half flower cyanines.The solvent adopted can be acetonitrile, the tert-butyl alcohol, dimethyl formamide and/or dimethyl sulfoxide (DMSO).The coadsorbent adopted can be DPA.
The assembling of step 5, DSSC
To immerse immersing the light anode having dye solution in electrolyte solution 2 ~ 20 minutes, after taking out with encapsulate to form DSSC to electrode.Or immersion there is is the light anode of dye solution with together with electrode assembling, injects electrolyte solution between which, form DSSC.
Wherein, electrolyte solution can be made up of three parts: organic solvent, redox duplet and additive.Organic solvent can be nitrile or carbonates.Redox duplet can be I
3-/ I
-, SCN
-/ (SCN)
2, SeCN
-/ (SeCN)
2.
Wherein, can be the different materials such as graphite, platinum or conducting polymer to electrode.
The performance characterization of DSSC
The photoelectric properties of DSSC such as can be tested under the standard sources of AM1.5, known after tested, and the photoelectric conversion efficiency of obtained DSSC can be more than 6%, is even more than 7%.
Fig. 1 illustrates the endurance test result figure of DSSC prepared by the light anode obtained according to the method for example of the present invention, as shown in the figure, each performance parameter such as open circuit voltage (Voc), short circuit current (Jsc), fill factor, curve factor (FF), conversion efficiency (Eff), resistance (Rs), the normalization efficiency (NormalizedEff) of this battery are coincide very well with standard sample, illustrate that shortening the durability of light anode sintering time on battery does not affect.
Fig. 2 illustrates the I-V curve of the DSSC prepared by the light anode obtained according to the method for example of the present invention, as seen from the figure, shortens the photoelectric properties impact of light anode sintering time on battery very little.
Good effect of the present invention is: the DSSC prepared with the light anode obtained according to the present invention, and (1) shortens the sintering time of large area light anode, improves operating efficiency.(2) light anode can not ftracture, and adds the useful life of battery.(3) two kinds of sintering procedures can reach same sintering result, are convenient to according to circumstances select flexibly.(4) for the industrialization production of large-area dye-sensitized solar battery provides technical support.
Exemplify embodiment below further to describe the present invention in detail.Should understand equally; following examples are only used to further illustrate the present invention; can not be interpreted as limiting the scope of the invention, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention.The technological parameter etc. that following example is concrete is also only an example in OK range, and namely those skilled in the art can be done in suitable scope by explanation herein and select, and do not really want the concrete numerical value being defined in Examples below.
Embodiment 1
TiO
2colloid 1(TSP) preparation:
The titania nanoparticles being of a size of 15 ~ 60nm is mixed with the ratio of 1 ~ 2:0.2 ~ 0.5:5 ~ 9 with terpinol and cellulose thickener, by obtaining TSP after magnetic agitation, high shear and ultrasonic disperse.
Embodiment 2
TiO
2colloid 2(DSP) preparation:
Reference embodiment 1, DSP and TSP difference is the large nano particle of titanium dioxide additionally adding 200 ~ 500nm when titania nanoparticles mixes with terpinol and cellulose thickener, and nanometer granule and nanometer bulky grain ratio are 1:0.1 ~ 0.4.
Embodiment 3
TiO
2colloid 3(Rpaste) preparation:
Be that the oarse-grained ratio of nanometer granule and nanometer is different with reference to embodiment 2, Rpaste and DSP is different, ratio is 0.01 ~ 0.1:1.
Embodiment 4
1 raw material
Dyestuff Z991:3.9g, acetonitrile 500ml, tert-butyl alcohol 500ml, TiO
2colloid 500g, electrolyte 50ml, electro-conductive glass, DPA.
2 preparation methods
The eight pieces of electro-conductive glass cleaned are placed in automatic screen printing machine, with the homemade TiO in laboratory
2jel print obtains four groups of dye-sensitized solar cell anodes, is placed on of short duration oven dry on hot plate.Four groups of light anodes of drying are put into stove sinter, wherein one group of light anode is sintered by temperature programming and programmed cooling as reference light anode 1, and its complete sintering procedure is: room temperature-80 DEG C: 5 minutes; 80-510 DEG C: 15 minutes; 510 DEG C are incubated 15 minutes; 510-460 DEG C: 5 minutes; 460-250 DEG C: 20 minutes; 250-80 DEG C: 20 minutes; Wherein in programmed cooling process, slightly cold (500 DEG C) take out other group of light anode pole (exemplary optical anode 1) and put into dye solution and soak; One group of light anode (exemplary optical anode 2), being cooled to 400 DEG C of taking-ups, being put into dye solution and is soaked; One group of light anode (exemplary optical anode 3) is put into dye solution and is soaked being cooled to 300 DEG C of taking-ups; Cooled see light anode 1, also put into dye solution and soak.
Wash away dye solution with 2-100ml absolute ethyl alcohol, dry 0.5-10 minute after the reference light anode 1 of above-mentioned preparation and exemplary optical anode 1-3 take out, inject electrolyte with note electrolytic solution device, take out encapsulation; The efficiency of obtained battery is see table 1.
The cell photoelectric performance that table 1 is prepared by reference light anode 1 and exemplary optical anode 1-3
As shown in Table 1, the situation of exemplary optical anode 1-3 is compared with the situation of reference light anode 1, and photoelectric properties difference is very little, and even photoelectric properties are more excellent, illustrates that shortening the light anode sintering time affects very little on the photoelectric properties of battery.
Embodiment 5
1 raw material
Dyestuff Z991:3.9g, acetonitrile 500ml, tert-butyl alcohol 500ml, TiO
2colloid 500g, electrolyte 50ml, electro-conductive glass, DPA.
2 preparation methods
The eight pieces of electro-conductive glass cleaned are placed in automatic screen printing machine, with the homemade TiO in laboratory
2jel print obtains four groups of dye-sensitized solar cell anodes, is placed on of short duration oven dry on hot plate.Four groups of light anodes of drying are put into stove sinter, wherein one group of light anode is sintered by temperature programming and programmed cooling as reference light anode 2, and complete sintering procedure is: room temperature-80 DEG C: 5 minutes; 80-510 DEG C: 15 minutes; 510 DEG C are incubated 15 minutes; 510-460 DEG C: 5 minutes; 460-250 DEG C: 20 minutes; 250-80 DEG C: 20 minutes; Wherein in program 510 DEG C of insulating processes, take out after one group of light anode (exemplary optical anode 4) directly puts into 10 minutes when program is incubated and put into dye solution and soak; Take out after one group of light anode (exemplary optical anode 5) directly puts into 20 minutes when program is incubated and put into dye solution and soak; Take out after one group of light anode (exemplary optical anode 6) directly puts into 30 minutes when program is incubated and put into dye solution and soak; The reference light anode 2 cooled, also puts into dye solution and soaks.
Wash away dye solution with 2-100ml absolute ethyl alcohol, dry 0.5-10 minute after the reference light anode 2 of above-mentioned preparation and exemplary optical anode 4-6 take out, inject electrolyte with note electrolytic solution device, take out encapsulation; The efficiency of obtained battery is see table 2.
The cell photoelectric performance that table 2 is prepared by reference light anode 2 and exemplary optical anode 4-6
From Fig. 2 and table 2, the situation of exemplary optical anode 4-6 is compared with the situation of reference light anode 2, and photoelectric properties difference is very little, and even photoelectric properties are more excellent, illustrates that shortening the light anode sintering time affects very little on the photoelectric properties of battery.
Although the test result of the battery efficiency between two groups of light anodes prepared by table 1 and table 2 is different, this causes due to different experiments batch.But table 1(embodiment 4) and show 2(embodiment 5) result that illustrates separately can show fully, it is very little that the exemplary optical anode that the shortening light anode sintering time obtains compares its reference light anode photoelectric properties difference, even photoelectric properties are more excellent, illustrate that shortening the light anode sintering time affects very little on the photoelectric properties of battery.
Industrial applicability: the present invention can shorten the sintering time of large area light anode, increases work efficiency, and light anode can not ftracture, and adds the useful life of battery, can produce provide technical support for the industrialization of large-area dye-sensitized solar battery.
Claims (10)
1. a method for Fast Sintering large-area dye-sensitized solar battery photo-anode, is characterized in that, comprising:
(1) by titania nanoparticles, terpinol and cellulosic binder with (1 ~ 2): (0.2 ~ 0.5): the ratio mixing of (5 ~ 9), and obtains TiO after magnetic agitation, high shear and ultrasonic disperse
2colloid;
(2) TiO that screen printing step (1) is obtained on the electro-conductive glass cleaned
2colloid is with the light anode of obtained DSSC and dry; And
(3) the light anode of oven dry is put into sintering furnace to sinter, the program of sintering is:
Program one: put into light anode in sintering furnace after, rose to 300 ~ 800 DEG C by sintering furnace from room temperature and is incubated the cooling of less than 100 minutes rear taking-up light anodes within 40 minutes; Or
Program two: after stove to be sintered rises to 300 ~ 800 DEG C, puts into sintering furnace and is incubated taking-up light anode cooling after less than 100 minutes by light anode,
In program one and/or program two, the instrument of taking when taking out light anode is heated to 100 ~ 400 DEG C in advance.
2. method according to claim 1, is characterized in that, in described program one, the heating-up time is less than 20 minutes.
3. method according to claim 1 and 2, is characterized in that, in described program one, temperature retention time is less than 15 minutes.
4. method according to claim 1, is characterized in that, in described program two, temperature retention time is less than 30 minutes.
5. method according to claim 1, it is characterized in that, described titania nanoparticles comprises and is of a size of the little nano particle of 15 ~ 60nm titanium dioxide and be of a size of the large nano particle of 200 ~ 500nm titanium dioxide, and the mass ratio of the little nano particle of described titanium dioxide and the large nano particle of titanium dioxide is 1:(0.1 ~ 100).
6. method according to claim 5, is characterized in that, the mass ratio of the little nano particle of described titanium dioxide and the large nano particle of titanium dioxide is 1:(0.1 ~ 0.4).
7. method according to claim 5, is characterized in that, the mass ratio of the little nano particle of described titanium dioxide and the large nano particle of titanium dioxide is (0.01 ~ 0.1): 1.
8. the method according to any one of claim 5 to 7, it is characterized in that, the little nano particle of described titanium dioxide is anatase titanium dioxide nano particle, prepared by sol-gel process, described sol-gel process comprises: be (9 ~ 99) by weight ratio: the titanium precursors of 1 and the mixed solution of acetic acid are added drop-wise in deionized water, acid adding regulates solution ph to be 1 ~ 3, 80 DEG C ~ 120 DEG C are reacted 6 ~ 24 hours, then 16 ~ 96 hours are incubated at being placed in reactor 200 DEG C ~ 270 DEG C, collect, 15 ~ 60 nano crystal anatase titanias are obtained after washing.
9. method according to claim 8, is characterized in that, described titanium precursors is butyl titanate and/or tetraisopropyl titanate.
10. method according to claim 8, is characterized in that, for regulating the acid of solution ph to be selected from sulfuric acid, nitric acid, acetic acid, hydrochloric acid, benzoic acid, citric acid, and at least one in laurate and oxalic acid.
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