CN101872655B - Method for preparing nanocrystalline porous thick film by one-time sintering - Google Patents
Method for preparing nanocrystalline porous thick film by one-time sintering Download PDFInfo
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- CN101872655B CN101872655B CN2010101849116A CN201010184911A CN101872655B CN 101872655 B CN101872655 B CN 101872655B CN 2010101849116 A CN2010101849116 A CN 2010101849116A CN 201010184911 A CN201010184911 A CN 201010184911A CN 101872655 B CN101872655 B CN 101872655B
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- Y02E10/542—Dye sensitized solar cells
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Abstract
The invention discloses a method for preparing a nanocrystalline porous thick film by one-time sintering. The method comprises a slurry preparation step, a coating step, a sintering step and the like, wherein the slurry mainly comprises nanoparticles, ethylene glycol and citric acid in a weight ratio of 1/(1.5-4)/(1-3); and the method comprises the following steps of: fully and uniformly mixing the nanoparticles and the ethylene glycol; adding the citric acid into the mixture for dissolving; and fully and uniformly mixing the citric acid and the mixture. Different modifiers are added into the slurry based on different nanoparticles, the mixture is adjusted simply and coating and sintering are performed. Due to the adoption of the method, the problems of poor nano particle dispersibility and easy agglomeration and sedimentation are solved, thick films can be prepared and the film thickness of a film prepared by one-time coating and sintering is up to 40mu m and continuous coating can be performed. A TiO2 film is prepared from commercially-available P25 nano powder without any other modification and the assembling efficiency of a dye-sensitized solar cell is up to 8.9 percent. The method has the advantages of simple process, low cost, wide application and good application prospect.
Description
Technical field
The invention belongs to technical field of nano material application.Be particularly related to a kind of preparation method of nanocrystalline porous film.
Background technology
The TiO2 slurry that is used for preparing the dye sensibilization solar cell nanometer semiconductive thin film is that the TiO2 nano particle is dispersed in the solvent that contains additive, and solvent adopts water, ethanol, terpinol usually.Water is most popular as nonpoisonous and tasteless green solvent, but contains the slurry of big water gaging, is difficult to prepare thicker film and large area uniform film.Just as: on the one hand, contain the film that 20wt%PEG20000 makes the TiO2 aqueous systems slurry primary coating sintering of pore creating material, its thickness is generally the thickest can only to reach 6 μ m, because of not applying continuously, under the situation of need than thick film, for example the optimum thickness of TiO2 film is 8 μ m～16 μ m in the DSSC, can only be coated with the second layer or the second layer again and reburn knot for the second time or for the third time; On the other hand, because the surface tension of water is big, the normal TX-100 of adding is to increase the wetability of slurry on electro-conductive glass FTO, though there is improvement also to be difficult to prepare large area uniform film in the aqueous systems TiO2 slurry.Ethanol system has solved the shortcoming that aqueous systems can not apply continuously, yet because of its viscosity is low, the sedimentation of very easily reuniting of the nano particle in the ethanol system slurry causes the of low quality of film.Terpinol has viscosity higher, and adds ethyl cellulose and make the TiO2 slurry of pore creating material and be used for DSSC and obtained good effect, and it has overcome the shortcoming of aqueous systems and ethanol system, however do not see yet its once property do thick report.
The 16 μ m TiO2 films (Thin Solid Films magazine, 516 phases, 4613-4619 page or leaf, (2008)) that group is used for DSSC often need to be coated with continuously 8～9 times, whenever are coated with one deck and need dry cooling more just can be coated with one deck down near 135 ℃.
Summary of the invention
Purpose of the present invention is exactly to provide a kind of by the once sintered method for preparing nanocrystalline porous thick film at the situation of above-mentioned prior art.Once sintered preparation thick film after both can disposable coating slurry, but continuous several times applies once sintered preparation thick film behind the slurry again.
Technical solution of the present invention comprises steps such as preparation slurry, coating and sintering.In the pulp preparation: its slurry major ingredient is nano particle, ethylene glycol and citric acid, and weight ratio is: nano particle/ethylene glycol/citric acid=1/ (1.5～4)/(1～3); The step of its preparation is: after nano particle and ethylene glycol are fully mixed, add the citric acid dissolving again and fully mix.
Nano particle in the such scheme can be the single component of titanium dioxide, graphite, carbon black, zirconia, zinc oxide, aluminium oxide or the blending constituent that two is above.
In order to increase the quality of slurry, can in slurry, add corresponding dressing agent according to the performance of nano particle, include in the following reagent one or more in its dressing agent:
1, strengthens the chelating agent of nanoparticulate dispersed;
2, regulate the slurry pH value to prevent the reagent of nanoparticle agglomerates;
3, regulate the reagent of slurry viscosity.
Above-mentioned chelating agent comprises polyhydroxy-alcohol, acetylacetone,2,4-pentanedione, ethyl acetate, diethanol amine; The reagent of above-mentioned adjusting pH value comprises water, glacial acetic acid, hydrochloric acid, nitric acid, ammoniacal liquor; The reagent of above-mentioned adjusting slurry viscosity comprises water, ethanol.
In the practical application, the present invention can be in the weight proportion scope, and the first step earlier mixes nano particle and ethylene glycol and adds citric acid again and dissolve and mix.Second step added different modifying agent simple adjustment at different nano particles.The 3rd step applied slurry and the sintering that the first two step makes.
Advantage of the present invention is:
One, a kind of method of simple efficient production high-quality film is provided.1. adopt viscosity higher intercalating agent ethylene glycol and citric acid to come the dispersing nanometer particle, solved the difficult problem of difficult dispersion of nano particle and easy reunion sedimentation.2. citric acid has three carboxyls can generate three-dimensional network shape ester 70 ℃～160 ℃ reaction dehydrations with ethylene glycol, and in sintering process, three-dimensional net structure can suppress collapsing fast of nano particle and reunite, and the uniformity of film is improved greatly.3. in sintering process, three-dimensional network shape ester slowly decomposes, volatilizees and can suppress stress and concentrate, and has prevented micro-crack even cracking, also can be as pore creating material, and make and can prepare the adjustable high-quality film of hole that once can do thick (can reach 40 μ m does not ftracture).The slurry of 4. this method preparation also can be coated with continuously, for example behind spin coating collosol and gel on the FTO electro-conductive glass, need not sintering and just can directly apply slurry, also can be after 50 ℃～160 ℃ dry coolings with the slurry that applies, continue to apply other or slurry of the same race again, for example on the nanometer crystal layer, apply scattering layer.
Two, the commercial P25 nano particle of buying adopts the TiO2 film of this method primary coating preparation, and under without other modification situations, the assembling DSSC has obtained 8.9% efficient.
Three, not only simple, the easy row of the present invention, efficient can effectively promote the commercial application of DSSC, and can be used for preparing the electro-catalysis carbon film and the photocatalysis aspect of DSSC.
Description of drawings
Accompanying drawing 1, accompanying drawing 2, accompanying drawing 3 are the surface and the cross-section structure of different samples of preparation in the embodiment of the present invention one under the field emission microscope.Wherein: accompanying drawing 1 counter sample 1; Accompanying drawing 2 counter samples 2; Accompanying drawing 3 counter samples 4.
Embodiment
Embodiment one
One, preparation nanocrystalline porous thick film:
1, preparation P25 slurry: with P25 (Degussa, particle diameter is 36nm, contains 83% anatase, 5g) mixes with ethylene glycol, add citric acid again and continue to be mixed to evenly, add the 3ml deionized water again and be mixed to evenly (mass ratio of P25/ ethylene glycol/citric acid is 1/2/2).
2, preparation titanium dioxide nanocrystalline wet film: will go up the slurry that the step makes and directly be coated to (to set the parallel electro-conductive glass edge that adheres to of adhesive tape of thickness, with the thickness of control titanium deoxid film) on the conductive glass plate by the thickness of setting.
3, obtained wet film is directly put into Muffle furnace, is incubated 1h under 500 ℃ the condition.Get final product the electrode of titanium dioxide nanocrystalline porous thick film.
Two, the prepared electrode of usefulness N719 dye sensitization the present invention, and dropping proportioning is 0.1M 1-propy-3-methylimidazoliumiodide (1-propyl group-3-methylimidazole iodine), 0.05M LiI, 0.1M GNCS, 0.03M I
2, 0.5M 4-tert-butylpridine (4-tert .-butylpyridine), solvent be the redox electrolytes matter of mixed solution (volume ratio is 1: 1) of propene carbonate and acetonitrile on this electrode, add a cover platinum electrode be assembled into DSSC.
1,500W simulated solar radiant xenon lamp (Oriel 91192, USA), Keithly 2400 source meter, irradiation intensity is 100W/cm
2, it is 0.25cm that battery is subjected to illuminating area
2Measuring light electric energy conversion efficient under the condition, and utilize platform valency instrument (TalyForm S4C-3D profilometer (UK)) MEASUREMENTS OF THIN thickness, its test result is as follows: (in first hurdle 1,2,3, the 4 expression adhesive tape numbers of plies, A represents that thin adhesive tape thickness is 40 μ m, B represents that thin adhesive tape thickness is 60 μ m).
| The adhesive tape sticking mode | Sample number into spectrum | Open circuit voltage (mV) | Short circuit current (mA/cm 2) | Transformation efficiency (%) | Fill factor, curve factor | Thickness μ m |
| 1(A) | 1 | 765 | 16.06 | 8.08 | 0.66 | 7.97 |
| 2(A) | 2 | 735 | 17.79 | 8.6 | 0.66 | 14.3 |
| 3(A) | 3 | 725 | 17.04 | 8.18 | 0.66 | 19.4 |
| 2(A)+1(B) | 4 | 715 | 19.3 | 8.86 | 0.64 | 21.9 |
| 4(A) | 5 | 725 | 17.34 | 7.79 | 0.62 | 24.4 |
Above-mentioned test result shows: utilize P25 film that the present invention prepares just to obtain very high efficient under the situation of any other modification not adding, the efficient of four kinds of film assembled batteries of 8 μ m-22 μ m has all surpassed 8%.
2, (USA) testing film surface and cross-section morphology the results are shown in accompanying drawing for SEM, Sirion FEG to utilize field emission microscope.The surface of sample 1 and section such as accompanying drawing 1, the surface of sample 2 and section such as accompanying drawing 2, the surface of sample 4 and section such as accompanying drawing 3.The i-v curve of five kinds of samples such as Fig. 4.As can be seen, the film that present embodiment makes has favorable uniformity from above-mentioned accompanying drawing, and 3 tensile fracture SEM figure show that film is that primary coating is once sintered and makes, and the interface is not arranged and this is very common in the film of sintering repeatedly because see in the sectional drawing.
Embodiment two
One, preparation nanocrystalline porous thick film:
1, pulp preparation:
A, preparation P25 slurry: with P25 (Degussa, particle diameter is 36nm, contain 83% anatase, 5g) mix with ethylene glycol, add citric acid again and continue to be mixed to even, add the 3ml deionized water again and be mixed to evenly (mass ratio of P25/ ethylene glycol/citric acid is 1/2/2), promptly get slurry 1;
B, preparation are used for the slurry of dye-sensitized solar cell anode scattering layer: with P25 (Degussa, particle diameter is 36nm, contain 83% anatase, 2.5g) and TiO2 (rutile, 500nm, 7.5g) mix with ethylene glycol, add citric acid again and continue to be mixed to evenly, add 1ml TX-100 again and be mixed to evenly (mass ratio of nano particle/ethylene glycol/citric acid is 1/4/3).
2, preparation titanium dioxide nanocrystalline wet film:
A, will go up the step slurry 1 that makes of a and directly be coated to conductive glass plate (with the parallel electro-conductive glass edge that adheres to of the thick adhesive tape of one deck 40 μ m by the 40 μ m thickness of setting, thickness with control titanium dioxide wet film) on, again with 65 ℃ of wet films, after 5h dries again natural cooling promptly get dry wet film;
B, continue to apply the scattering layer slurry that step b makes on one deck on the wet film of drying again.
3, will go up prepared film of step (comprising the wet film of drying film and adding scattering layer that does not add scattering layer) and put into Muffle furnace, be incubated 1h under 500 ℃ the condition.Can obtain the electrode of titanium dioxide nanocrystalline porous thick film.
Two, usefulness N719 dye sensitization TiO2 electrode, and dropping proportioning is 0.1M 1-propy-3-methylimidazolium iodide (1-propyl group-3-methylimidazole iodine), 0.05M LiI, 0.1M GNCS, 0.03M I
2, 0.5M 4-tert-butylpridine (4-tert .-butylpyridine), solvent be the redox electrolytes matter of mixed solution (volume ratio is 1: 1) of propene carbonate and acetonitrile on this electrode, add a cover platinum electrode be assembled into DSSC.(Oriel 91192, and USA), Keithly 2400source meter, irradiation intensity are 100W/cm at 500W simulated solar radiant xenon lamp
2, it is 0.25cm that battery is subjected to illuminating area
2Measuring light electric energy conversion efficient under the condition, and utilize platform valency instrument (TalyForm S4C-3D profilometer (UK)) MEASUREMENTS OF THIN thickness, its test result is as follows:
| Have or not scattering layer | Sample number into spectrum | Open circuit voltage (mV) | Short circuit current (mA/cm 2) | Transformation efficiency (%) | Fill factor, curve factor | Thickness μ m |
| Do not have | 1 | 645 | 12.44 | 4.96 | 0.62 | 7.07 |
| Have | 2 | 675 | 14.24 | 6.18 | 0.64 | 10.3 |
Above-mentioned test result shows: scattering layer can be raised the efficiency nearly 20%, and this slurry that has illustrated also that on the other hand the present invention makes can be used for the continuous coating between the difference in functionality layer, and only needs sintering once.
Embodiment three
One, preparation nanocrystalline porous thick film:
1, preparation is used for the slurry of dye sensitizing solar battery carbon catalysis electrode: (average grain diameter is 80nm with carbon black, 2.5g), (average grain diameter is 4 μ m to graphite, 7.5g), (average grain diameter is 20nm to zirconia, 1.5g) mix with ethylene glycol, add citric acid again and continue to be mixed to evenly, add 3ml absolute ethyl alcohol and 0.5ml red fuming nitric acid (RFNA) again and be mixed to evenly (mass ratio of nano particle/ethylene glycol/citric acid is 1/1.5/1).
2, preparation electro-catalysis nanocrystalline carbon wet film: will go up the slurry that the step makes and directly be coated to (to set the parallel slide edge that adheres to of adhesive tape of thickness, to control nanocrystalline carbon film thickness) on the slide surface by the thickness of setting.
3, will go up the wet film that makes of step and put into Muffle furnace, be incubated 1h under 500 ℃ the condition.Get final product the carbon of carbon nano-crystal porous thick film to electrode.
Two, with N719 dye sensitization 7 μ m TiO2 electrodes (the above-mentioned embodiment one of reference, but the TiO2 electrode is at 65 ℃ herein, 5h just removes sintering after drying natural cooling again), and to drip proportioning be 0.1M 1-propy-3-methylimidazolium iodide (1-propyl group-3-methylimidazole iodine), 0.05M LiI, 0.1M GNCS, 0.03M I
20.5M 4-tert-butylpridine (4-tert .-butylpyridine), solvent be the redox electrolytes matter of mixed solution (volume ratio is 1: 1) of propene carbonate and acetonitrile on this electrode, add a cover carbon that the present embodiment makes to electrode be assembled into DSSC and with Pt electrode pair ratio commonly used.500W simulated solar radiant xenon lamp (Oriel 91192, USA), Keithly 2400 source meter, irradiation intensity is 100W/cm
2, it is 0.25cm that battery is subjected to illuminating area
2Measuring light electric energy conversion efficient under the condition; And utilize platform valency instrument (TalyForm S4C-3D profilometer (UK)) MEASUREMENTS OF THIN thickness (the corresponding sintering carbon film of one deck 40 μ m thick tapes thickness is about 20 μ m, and the corresponding sintering carbon film of two-layer 40 μ m thick tapes thickness is about 40 μ m).Test result is as follows: (carbon C is μ m to the electrode thickness, and platinum Pt is nm to the electrode thickness)
| To type of electrodes | Sample number into spectrum | Open circuit voltage (mV) | Short circuit current (mA/cm 2) | Transformation efficiency (%) | Fill factor, curve | Thickness |
| C | ||||||
| 1 | 705 | 3.95 | 1.77 | 0.64 | 21.1 | |
| |
1 | 635 | 12.71 | 5.04 | 0.62 | 200 |
| |
2 | 695 | 9.15 | 3.87 | 0.61 | 40.3 |
| |
2 | 635 | 12.79 | 5.20 | 0.64 | 200 |
Above-mentioned test result shows: the present invention can be used for preparing the electro-catalysis carbon film.Answer 5.2% efficient with respect to the Pt electrode pair, the C electrode has only 3.87%.But with respect to the equipment of the price and the magnetic control costliness of Pt and FTO costliness, the C electrode that is coated on the slide only needs simple preparation again, and this has just shown its competitive and dominance of the present invention.
Claims (3)
1. one kind by the once sintered method for preparing nanocrystalline porous thick film, comprises pulp preparation, coating and sintering, it is characterized in that described pulp preparation:
1) the slurry major ingredient is nano particle, ethylene glycol and citric acid, and the weight ratio of its major ingredient is: nano particle/ethylene glycol/citric acid=1/ (1.5～4)/(1～3); Described nano particle is the single component of titanium dioxide, graphite, carbon black, zirconia, zinc oxide, aluminium oxide or the blending constituent that two is above;
2) preparation process is: after nano particle and ethylene glycol are fully mixed, add the citric acid dissolving again and fully mix.
2. according to claim 1 a kind of by the once sintered method for preparing nanocrystalline porous thick film, it is characterized in that: contain in the described slurry and the corresponding dressing agent of slurry, and include in the following reagent one or more in its dressing agent:
1) chelating agent of reinforcement nanoparticulate dispersed;
2) regulate the slurry pH value to prevent the reagent of nanoparticle agglomerates;
3) reagent of adjusting slurry viscosity.
3. according to claim 2 a kind of by the once sintered method for preparing nanocrystalline porous thick film, it is characterized in that:
1) described chelating agent comprises polyhydroxy-alcohol, acetylacetone,2,4-pentanedione, ethyl acetate, diethanol amine;
2) reagent of described adjusting pH value comprises water, glacial acetic acid, hydrochloric acid, nitric acid, ammoniacal liquor;
3) reagent of described adjusting slurry viscosity comprises water, ethanol.
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| CN102522213B (en) * | 2011-12-03 | 2013-11-13 | 三峡大学 | Preparation method for dye sensitization solar cell carbon counter electrodes |
| CN102723213B (en) * | 2012-06-23 | 2015-11-11 | 三峡大学 | A kind of preparation method of dye-sensitized solar cell anode |
| CN103794377B (en) * | 2014-02-21 | 2017-01-25 | 南京大学昆山创新研究院 | Dye-sensitized solar cell (DSSC) photo-anode and manufacturing method and application thereof |
| CN105582931B (en) * | 2014-10-22 | 2020-03-06 | 中国科学院上海高等研究院 | Cobalt-based Fischer-Tropsch synthesis catalyst loaded by mixed oxide carrier and preparation method thereof |
| CN115504780A (en) * | 2021-01-09 | 2022-12-23 | 浙江大学台州研究院 | Method for uniformly doping nano particles in high-temperature superconducting material |
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| CN100358162C (en) * | 2004-09-13 | 2007-12-26 | 武汉大学 | Method for preparing nano crystal thin film from nano particles |
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