CN104078244A - Metallic-niobium-doping titanium dioxide nanometer sheet, and preparing method and application of metallic-niobium-doping titanium dioxide nanometer sheet - Google Patents
Metallic-niobium-doping titanium dioxide nanometer sheet, and preparing method and application of metallic-niobium-doping titanium dioxide nanometer sheet Download PDFInfo
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- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/542—Dye sensitized solar cells
Abstract
The invention provides a metallic-niobium-doping titanium dioxide nanometer sheet, and a preparing method and application of the metallic-niobium-doping titanium dioxide nanometer sheet. The method comprises the following steps that: niobium pentaethoxide is added into a titanium source according to a doping ratio that Nb/(Ti+Nb)=1 percent to 20 percent; hydrofluoric acid is added under the stirring condition; the stirring is continuously carried out to obtain a clear niobium-doping titanium dioxide solution; the obtained solution is contained into a stainless steel reaction kettle provided with a polyfluortetraethylene inner liner; the stainless steel reaction kettle is sealed and is then placed into a constant-temperature drying box; next, the temperature is reduced to the room temperature through natural cooling, and white precipitates are obtained; the obtained white precipitates are sequentially and repeatedly cleaned by ethanol and deionized water and are then placed into the constant-temperature drying box to be dried; the dried precipitates are taken out to be ground; and finally, the metallic-niobium-doping titanium dioxide nanometer sheet is obtained. The method provided by the invention has the advantages that the preparing process is simple; the raw material cost is low; and the purification is easy. Through the test, dye-sensitized solar batteries prepared by the niobium-doping titanium dioxide nanometer sheet provided by the invention obtain 9.8 percent of battery efficiency.
Description
Technical field
The present invention relates to the fields such as nanometer technology, solar cell, be specifically related to a kind of doping metals niobium titanium dioxide nanoplate and its preparation method and application.
Background technology
World today's energy and environmental problem have become the focus that various countries pay close attention to.Along with the cumulative year after year of the world to energy-output ratio, energy problem has become the bottleneck of restriction socio-economic development.And the exhaustion day by day of the non-renewable energy resources such as coal, oil, natural gas, regenerative resource has become the selection of the novel alternative energy source in the world today.Solar energy has broad application prospects as a kind of green regenerative energy sources, to the efficient utilization of solar energy, is therefore the important channel that solves lack of energy.
Dye-sensitized solar cells is simple with its preparation technology, and the cost of raw material is cheap, and its cost only has 1/5～1/10 of silicon solar cell, has become the focus of various countries' researcher research.At present, the peak efficiency of dye-sensitized solar cells report, in 12% left and right, also has very large gap with its theoretical efficiency.For how improving its battery efficiency, mainly concentrate on novel electrolytes and the preparation aspect with the reactive monoazo dyestuffs of wide spectral response range at present.And for the research of the electrode material poriferous titanium dioxide semiconductor electrode film of dye-sensitized solar cells seldom.Particularly for modulate the conductivity of Fermi level and the material itself of titanium dioxide semiconductor by other metallic element that adulterates, and the material after doping is applied to dye-sensitized solar cells the impact of its battery efficiency is not almost also had to relevant research.
In order effectively to improve the photoelectric conversion efficiency of dye-sensitized solar cells, the present invention has prepared a kind of titanium dioxide nanoplate novel semiconductor material of metal niobium doping, by the doping of niobium, can effectively improve the conductivity of material itself, reduce its conduction level, thereby be conducive to injection and transmission and then the raising battery efficiency of electronics.
Summary of the invention
The object of this invention is to provide a kind of doping metals niobium (Nb) titanium dioxide nanoplate and its preparation method and application.
The invention provides a kind of doping metals niobium titanium dioxide nanoplate (niobium doping titanium dioxide nano sheet), the crystal formation of this nanometer sheet agent structure is Detitanium-ore-type TiO
2, the thin slice that is square, length and width are between 30-100 nanometer, and thickness is 2-7 nanometer, and upper and lower surface is TiO
2(001) crystal face; The molar content of metal niobium in this nanometer sheet (Nb) is between 1%-20%.
The present invention also provides the preparation method of described doping metals niobium titanium dioxide nanoplate, and the concrete steps of the method are as follows:
(1) the doping ratio of pressing Nb/ (Ti+Nb) (mol ratio) 1%～20% is by five ethyoxyl niobiums (Nb (OEt)
5) join in titanium source, under stirring, add 0.5～1.5 milliliter of hydrofluoric acid (crystal morphology controlling agent), continue to stir the niobium adulterated TiOx solution that obtains clarification for 15 minutes;
(2) niobium adulterated TiOx mixed solution step (1) being obtained is put into the stainless steel cauldron of polytetrafluoroethylliner liner;
(3) after the stainless steel cauldron of step (2) is airtight, put into thermostatic drying chamber, at 160～200 ℃, be incubated 12～24 hours, then naturally cool to room temperature, obtain white precipitate;
(4) the resulting white depositions of step (3) is cleaned repeatedly with ethanol and deionized water successively, put into afterwards 60～100 ℃ of thermostatic drying chambers (being preferably 60 ℃) dry 24～48 hours, take out and grind, finally obtain doping metals niobium titanium dioxide nanoplate.
The preparation method of described doping metals niobium titanium dioxide nanoplate provided by the invention, the titanium source in described step (1) is one or more (being preferably tetra-n-butyl titanate) in tetra-n-butyl titanate, isopropyl titanate, titanium tetrachloride.
The preparation method of described doping metals niobium titanium dioxide nanoplate provided by the invention, the structure of the doping metals niobium titanium dioxide nanoplate preparing in described step (4) is that average length and width are 50 nanometers, average thickness is the cuboid thin slice of 5 nanometers, upper bottom surface is highly active (001) crystal face, and crystal formation is Detitanium-ore-type.
The invention provides the application of described doping metals niobium titanium dioxide nanoplate, this nanometer sheet, as battery cathode, is prepared dye-sensitized solar cells.
Detitanium-ore-type niobium doping titanium dioxide nano sheet provided by the invention is as follows for the preparation of the method for dye-sensitized solar cells:
(1) preparation of niobium doping titanium dioxide nano chip semiconductor membrane electrode: take in the ethanol that the niobium doping titanium dioxide nano sheet of 1.0～8.0 grams is dispersed in 40～120 milliliters, add successively afterwards the ethyl cellulose of 0.5～4.0 gram and the saturating alcohol of turpentine oil of 4.0～32 grams, continue agitating solution after 2～4 hours, solution is repeated 3 times in 5 minutes these processes of stirring for ultrasonic 5 minutes, afterwards niobium doping titanium dioxide nano sheet suspension-turbid liquid is rotated to ethanol evaporation at 40 ℃ and within 1～6 hour, obtain niobium doped Ti O
2nanometer sheet slurry.Gained slurry is imprinted on clean fluorine-doped tin oxide (FTO) electro-conductive glass through silk screen printing, and 450～500 ℃ of high temperature sinterings 45～60 minutes, then by the niobium doped Ti O preparing
2nanometer sheet membrane electrode is immersed in (the N719 bipyridyl ruthenium dye solution that acetonitrile/tert-butyl alcohol (volume ratio is 1:1) is 300 micromoles per liter for mixed solvent compound concentration contains the coadsorbent chenodeoxycholic acid (cheno) of 1 mM/l) in the N719 dye solution preparing, and the time is 18～24 hours.
(2) assembling of dye-sensitized solar cells: by chloroplatinic acid (H
2ptCl
6) aqueous isopropanol (1 ml soln containing 4 milligrams of Pt) be added drop-wise on FTO conducting surface by spin coating instrument, its spin coating is even, 450 ℃ of heat treatment afterwards 15 minutes, obtain platinum to electrode.The positive pole and the niobium doping titanium dioxide nano sheet membrane electrode that are covered with Platinum Nanoparticles are passed through to the ring-type heat-sealing film heated sealant of 35 micron thickness, afterwards electrolyte is injected in battery to the dye-sensitized solar cells that to obtain take niobium doping titanium dioxide nano sheet after sealing be negative pole semi-conducting material.
Creative contribution of the present invention is mainly: synthesized first the titanium dioxide nanoplate semi-conducting material of doping metals niobium, its average length and width are 50 nanometers, and average thickness is 5 nanometers, take high activity (001) crystal face as the main crystal face that exposes.Due to the doping of metal niobium, not only improve the conductivity of semi-conducting material but also reduced the photoelectric properties that semi-conductive energy gap has increased material.The niobium doped Ti O preparing with the present invention
2the battery that nanometer sheet semi-conducting material is prepared as the negative pole of dye-sensitized solar cells, through solar simulator test, obtained 9.8% battery efficiency, and take battery that current industrialized P25 nano particle is cell negative electrode material and compare battery efficiency and be significantly improved.
Reaction raw materials of the present invention is with low cost, and synthesis technique is simply easy to preparation and purifying.
Accompanying drawing explanation
Fig. 1 is the XRD collection of illustrative plates of the synthetic niobium doping titanium dioxide nano sheet of embodiment 1;
Fig. 2 is the transmission electron microscope photo of the synthetic niobium doping titanium dioxide nano sheet of embodiment 1;
Fig. 3 is the X ray energy chromatogram (EDS) of the synthetic niobium doping titanium dioxide nano sheet of embodiment 1, the Cu in figure, Fe, Co and C element peak be instrument and equipment with impurity peaks;
Fig. 4 is the high-resolution-ration transmission electric-lens photo of the synthetic niobium doping titanium dioxide nano sheet of embodiment 1;
Fig. 5 is that embodiment 8 be take niobium doping titanium dioxide nano chip semiconductor material and prepared the electric current of dye-sensitized solar cells and the graph of relation of voltage as battery cathode.
Embodiment
The following examples will be further described the present invention, but not thereby limiting the invention.
Embodiment 1: the preparation of niobium doping titanium dioxide nano sheet
(1) get the tetra-n-butyl titanate of 36 mMs, in the ratio of Nb/ (Ti+Nb) (mol ratio) 2.5%, add five ethyoxyl niobiums, under the state of magnetic agitation, add the hydrofluoric acid of 0.75 milliliter, continue to stir the niobium adulterated TiOx solution that obtains clarification for 15 minutes.
(2) the niobium adulterated TiOx mixed solution of step (1) is transferred in the stainless steel cauldron of polytetrafluoroethylliner liner of 50 milliliters.
(3) after the stainless steel cauldron of step (2) is airtight, put into thermostatic drying chamber and be incubated 20 hours at 200 ℃, then take out and naturally cool to room temperature, obtain white precipitate.
(4) the resulting white depositions of step (3) is cleaned respectively 3 times with deionized water and ethanol, then put it in thermostatic drying chamber 60 ℃ dry 24 hours, take out and grind, obtain niobium doping titanium dioxide nano sheet.Fig. 1 is the XRD figure of titanium dioxide nanoplate, can find out that prepared niobium doping titanium dioxide nano sheet is Detitanium-ore-type.Fig. 2 is transmission electron microscope (TEM) photo of prepared niobium doping titanium dioxide nano sheet, can find out that the titania-doped crystalline material of prepared niobium is laminated structure, and average length and width are 50 nanometers, and average thickness is 5 nanometers.Fig. 3 is the X ray energy chromatogram (EDS) of niobium doping titanium dioxide nano sheet, and from figure, we can determine that prepared material has mixed niobium element and can obtain niobium-doped mass fraction.Fig. 4 is high-resolution-ration transmission electric-lens (HRTEM) photo of prepared niobium doping titanium dioxide nano sheet, and the spacing of lattice from figure can determine that the crystal face of prepared niobium doping titanium dioxide nano sheet is (001) crystal face.
Embodiment 2
Repeat the operating procedure of embodiment 1, it is 1% to add five ethyoxyl niobium and isopropyl titanates that difference is by Nb/ (Ti+Nb) (mol ratio), and result and embodiment 1 are similar, but the molar content of metal niobium (Nb) is 1% in this nanometer sheet.The microstructure of sample is consistent with embodiment 1, and crystal structure is consistent with embodiment 1.
Embodiment 3
Repeat the operating procedure of embodiment 1, it is 5% to add five ethyoxyl niobium and tetra-n-butyl titanates that difference is by Nb/ (Ti+Nb) (mol ratio), result and embodiment 1 are similar, but the molar content of metal niobium (Nb) is 5% in this nanometer sheet.The microstructure of sample is consistent with embodiment 1, and crystal structure is consistent with embodiment 1.
Embodiment 4
Repeat the operating procedure of embodiment 1, it is 7.5% to add five ethyoxyl niobium and isopropyl titanates that difference is by Nb/ (Ti+Nb) (mol ratio), result and embodiment 1 are similar, but the molar content of metal niobium (Nb) is 7.5% in this nanometer sheet.The microstructure of sample is consistent with embodiment 1, and crystal structure is consistent with embodiment 1.
Embodiment 5
Repeat the operating procedure of embodiment 1, it is 10% to add five ethyoxyl niobium and tetra-n-butyl titanates that difference is by Nb/ (Ti+Nb) (mol ratio), result and embodiment 1 are similar, but the molar content of metal niobium (Nb) is 10% in this nanometer sheet.The microstructure of sample is consistent with embodiment 1, and crystal structure is consistent with embodiment 1.
Embodiment 6
Repeat the operating procedure of embodiment 1, it is 15% to add five ethyoxyl niobium and tetra-n-butyl titanates that difference is by Nb/ (Ti+Nb) (mol ratio), result and embodiment 1 are similar, but the molar content of metal niobium (Nb) is 15% in this nanometer sheet.The microstructure of sample is consistent with embodiment 1, and crystal structure is consistent with embodiment 1.
Embodiment 7
Repeat the operating procedure of embodiment 1, it is 20% to add five ethyoxyl niobium and tetra-n-butyl titanates that difference is by Nb/ (Ti+Nb) (mol ratio), result and embodiment 1 are similar, but the molar content of metal niobium (Nb) is 20% in this nanometer sheet.The microstructure of sample is consistent with embodiment 1, and crystal structure is consistent with embodiment 1.
Embodiment 8: the preparation of the dye-sensitized solar cells that is battery cathode based on niobium doping titanium dioxide nano chip semiconductor material
(1) preparation of niobium doping titanium dioxide nano sheet membrane electrode: take 4.0 grams of niobium doping titanium dioxide nano sheets and be distributed in 60 milliliters of ethanol, under the state stirring again afterwards, add successively the ethyl cellulose of 2.0 grams and the saturating alcohol of turpentine oil of 16.0 grams, continue agitating solution after 2 hours, by solution after ultrasonic 5 minutes, stirring 5 minutes, this process repeats 3 times, afterwards niobium doping titanium dioxide nano sheet suspension-turbid liquid is rotated to ethanol evaporation at 40 ℃ and within 3 hours, obtains niobium doping titanium dioxide nano sheet slurry.The slurry of preparation is imprinted on the conducting surface of FTO electro-conductive glass through silk screen printing, and on high temperature titanium heating plate with 10 ℃/speed temperature programming to 500 ℃ continuous heating per minute 45 minutes, then by the niobium doped Ti O preparing
2nanometer sheet membrane electrode is immersed in (the N719 dye solution that acetonitrile/tert-butyl alcohol (volume ratio is 1:1) is 300 micromoles per liter for mixed solvent compound concentration contains the coadsorbent cheno of 1 mM/l) in the N719 dye solution preparing, and the time is 18 hours.After sensitization completes, taking-up is cleaned and dries up and obtain the niobium doped Ti O that sensitization is good by nitrogen gun with acetonitrile
2nanometer sheet membrane electrode.
(2) assembling of dye-sensitized solar cells: by chloroplatinic acid (H
2ptCl
6) aqueous isopropanol (1 ml soln containing 4 milligrams of Pt) be added drop-wise on FTO conducting surface with the rotating speed of 2000 revs/min, its spin coating is even by spin coating instrument, 450 ℃ of heat treatment afterwards 15 minutes, make platinum to electrode.The positive pole and the niobium doping titanium dioxide nano sheet membrane electrode that are covered with Platinum Nanoparticles are passed through to the ring-type heat-sealing film heated sealant of 35 micron thickness, afterwards will be with I
-/ I
3 -for the electrolyte solution of oxidation-reduction pair is injected in battery, the dye-sensitized solar cells that to obtain take niobium doping titanium dioxide nano chip semiconductor material after sealing be negative pole.At room temperature by the photoelectric properties of solar simulator test battery.As shown in Figure 5, the open circuit photovoltage of battery is 763mV to test result, and current density is 20.8mA/cm2, has obtained 9.8% battery efficiency.
Claims (7)
1. a doping metals niobium titanium dioxide nanoplate, is characterized in that: the crystal formation of this nanometer sheet is Detitanium-ore-type TiO
2, the thin slice that is square, length and width are between 30-100 nanometer, and thickness is 2-7 nanometer, and upper and lower surface is TiO
2(001) crystal face; The molar content of metal niobium in this nanometer sheet (Nb) is between 1%-20%.
2. the preparation method of doping metals niobium titanium dioxide nanoplate described in claim 1, is characterized in that: the concrete steps of the method are as follows:
(1) doping that is 1%～20% by the mol ratio of Nb/ (Ti+Nb) joins in titanium source than by five ethyoxyl niobiums, under stirring, adds hydrofluoric acid, and lasting stirring obtains the niobium adulterated TiOx solution of clarification;
(2) niobium adulterated TiOx solution step (1) being obtained is put into the stainless steel cauldron of polytetrafluoroethylliner liner;
(3) after the stainless steel cauldron of step (2) is airtight, put into thermostatic drying chamber, at 160～200 ℃, be incubated 12～24 hours, then naturally cool to room temperature, obtain white precipitate;
(4) the resulting white depositions of step (3) is cleaned repeatedly with ethanol and deionized water successively, put into afterwards 60～100 ℃ of thermostatic drying chambers and be dried 24～48 hours, take out and grind, finally obtain doping metals niobium titanium dioxide nanoplate.
3. according to the preparation method of doping metals niobium titanium dioxide nanoplate described in claim 2, it is characterized in that: the titanium source in described step (1) is one or more in tetra-n-butyl titanate, isopropyl titanate, titanium tetrachloride.
4. according to the preparation method of doping metals niobium titanium dioxide nanoplate described in claim 3, it is characterized in that: the titanium source in described step (1) is tetra-n-butyl titanate.
5. according to the preparation method of doping metals niobium titanium dioxide nanoplate described in claim 2, it is characterized in that: in described step (1), the addition of hydrofluoric acid is 0.5～1.5 milliliter.
6. according to the preparation method of doping metals niobium titanium dioxide nanoplate described in claim 2, it is characterized in that: the structure of the doping metals niobium titanium dioxide nanoplate preparing in described step (4) is that average length and width are 50 nanometers, average thickness is the cuboid thin slice of 5 nanometers, upper bottom surface is highly active (001) crystal face, and crystal formation is Detitanium-ore-type.
7. the application of doping metals niobium titanium dioxide nanoplate described in claim 1, is characterized in that: this nanometer sheet, as battery cathode, is prepared dye-sensitized solar cells.
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| CN113380910B (en) * | 2020-03-09 | 2023-01-24 | 中国科学院大连化学物理研究所 | Niobium halide material, preparation and application |
| CN111509063A (en) * | 2020-04-24 | 2020-08-07 | 中国科学院山西煤炭化学研究所 | Preparation method and application of niobium-doped titanium dioxide nano material |
| CN113936926A (en) * | 2021-10-15 | 2022-01-14 | 佛山科学技术学院 | Titanium dioxide composite electrode material and preparation method thereof |
| CN113936926B (en) * | 2021-10-15 | 2022-05-24 | 佛山科学技术学院 | Titanium dioxide composite electrode material and preparation method thereof |
| CN114887651A (en) * | 2022-05-19 | 2022-08-12 | 浙江工业大学 | TiO2 2 Nanosheet @ hydrophobic zeolite composite microsphere photocatalytic material and preparation method and application thereof |
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