CN103145183A - Three-dimensional TiO2 reticular nano-material, as well as preparation method and application thereof - Google Patents
Three-dimensional TiO2 reticular nano-material, as well as preparation method and application thereof Download PDFInfo
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- CN103145183A CN103145183A CN201310099397XA CN201310099397A CN103145183A CN 103145183 A CN103145183 A CN 103145183A CN 201310099397X A CN201310099397X A CN 201310099397XA CN 201310099397 A CN201310099397 A CN 201310099397A CN 103145183 A CN103145183 A CN 103145183A
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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
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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
- Y02E10/542—Dye sensitized solar cells
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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
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Abstract
The invention relates to a three-dimensional TiO2 reticular nano-material, as well as a preparation method and an application thereof, and belongs to the field of dye-sensitized solar cells. The preparation method comprises the following steps: adding titanium dioxide into a sodium hydroxide solution, performing magnetic stirring, then transferring a mixed solution into a hydrothermal kettle, performing hydrothermal reaction and cooling, then performing centrifugal operation on reactants, and further washing and centrifugalizing centrifugation products with dilute hydrochloric acid and deoxidized water; and sintering powder after drying of the centrifugation products at the temperature of 400-500 DEG C for 2-5 hours, and naturally cooling down to room temperature, thereby getting the three-dimensional TiO2 reticular nano-material. The preparation method has the advantages of high efficiency, low cost, simple method, short experimental cycle, large specific surface area of the prepared titanium dioxide and good connectivity, and can be used for large-batch production of the titanium dioxide with high specific surface area. As the titanium dioxide prepared by the method has ultrahigh specific surface area, the titanium dioxide can be widely applied to photocatalysis, photochemistry, lithium cells, the solar cells and other fields.
Description
Technical field
The invention belongs to field of dye-sensitized solar cells, be specifically related to a kind of three-dimensional TiO
2Mesh nano material, preparation method and the application in photochemical catalysis, photochemistry, lithium cell or solar cell.
Background technology
Energy problem is the matter of utmost importance of the present development of world economy of restriction, and sun power is as a kind of inexhaustible, the natural green energy of pollution-free cleaning and become one of most promising energy.Research and most widely used solar cell are mainly that silicon is solar cell at present, but silicon is that the battery raw material cost is high, complex manufacturing, it is limited that efficient improves potentiality, the theoretical boundary of its photoelectric transformation efficiency is 30%, has limited its civil nature, is badly in need of the solar cell of developing low-cost.
Switzerland scholar in 1991
Publish an article Deng on Nature, a kind of novel solar cell take dye sensitization titanium dioxide nanocrystalline film as the light anode has been proposed, it has makes the advantages such as simple, with low cost, that efficient is high and the life-span is long, photoelectric transformation efficiency can reach more than 11% at present, therefore becomes the main direction of studying of solar cell of new generation.
The titanium dioxide nanocrystalline film is the important component part of dye sensitization solar battery, and it is carrying the absorption of dyestuff, the transmission of electronics and to tasks such as incident scatterings of light.At present, the pattern of titanium dioxide nanocrystalline mainly comprises: nanoparticle, nanometer ball, nanometer rod and nanotube etc.High specific surface area titanic oxide is nanocrystalline is the object that the dye-sensitized solar cell anode material is pursued always.Main preparation method comprises: hydrothermal synthesis method, vapour deposition process, sol-gel processing, hydrolytic precipitation method etc.The specific surface area of the material of preparing is probably at 100m
2/ g left and right.In dye sensitization solar battery, have bigger serface titania light anode material prospect is widely arranged.
Summary of the invention
Technical problem to be solved by this invention is for above shortcomings in prior art, and a kind of titanic oxide material and preparation method thereof is provided.
The invention provides a kind of three-dimensional TiO
2Mesh nano material preparation method comprises the following steps:
Take that 0.05～0.15g titanium dioxide joins 60～80mL, concentration is in the sodium hydroxide solution of 5～10mol/L, then magnetic agitation 5～20 minutes was transferred to mixing solutions in water heating kettle, 120～150 ℃ of Water Under thermal responses 30～300 minutes; Naturally open water heating kettle after cooling to room temperature, pour out reactant and carry out centrifugally operated, centrifugation rate is 10000～15000 rev/mins; Be dilute hydrochloric acid and the deionized water wash and centrifugal of 0.1～0.2mol/L with concentration respectively with centrifugal product, each repeats 3～5 times; Last centrifugal product vacuum drying 8～10 hours under 60～80 ℃ of conditions; With the sintering 2～5 hours under 400～500 ℃ of conditions of the powder after oven dry, temperature rise rate is 2～10 ℃/min, naturally cools to room temperature, thereby obtains three-dimensional TiO of the present invention
2The mesh nano material.
The invention provides a kind of three-dimensional TiO
2The mesh nano material, it is prepared by aforesaid method.
Beneficial effect of the present invention: the specific surface area of the titanium dioxide that this preparation method's efficient is high, cost is low, method is simple, experimental period is short, make is large and connectivity good, can be used for producing in enormous quantities the titanium dioxide of high-specific surface area.The titanium dioxide that makes due to the method has superhigh specific surface area, so can be widely used in the fields such as photochemical catalysis, photochemistry, lithium cell and solar cell.
With three-dimensional TiO of the present invention
2For the preparation of dye sensitization solar battery, it is with above-mentioned three-dimensional TiO to the mesh nano material as the light anode material
2Then the water-soluble slurry that is prepared into of mesh nano material uses the spread coating blade coating on the FTO conductive glass, then in 450～500 ℃ of sintering 30～60 minutes, temperature rise rate 1～3min/ ℃, the thickness that obtains light anode material film after sintering was 12～20 μ m.
Description of drawings
Fig. 1: the three-dimensional TiO of the embodiment of the present invention 1 preparation
2The mesh nano material amplifies the scanning electron microscope picture of 40,000 times;
Fig. 2: the three-dimensional TiO of the embodiment of the present invention 2 preparations
2The mesh nano material amplifies the scanning electron microscope picture of 40,000 times;
Fig. 3: the three-dimensional TiO of the embodiment of the present invention 1 preparation
2The transmission scanning electron microscope picture of mesh nano material;
Fig. 4: the three-dimensional TiO of the embodiment of the present invention 1 preparation
2The XRD figure of mesh nano material;
Fig. 5: the three-dimensional TiO of the embodiment of the present invention 1 preparation
2The nitrogen adsorption desorption curve of mesh nano material;
Fig. 6: the three-dimensional TiO of the embodiment of the present invention 1 preparation
2The pore size distribution curve of mesh nano material.
Fig. 7: the current-voltage curve of the battery that titanic oxide material is assembled into (D.H.Chen, F.Z.Huang, Y.B.Cheng, R.A.Caruso, Adv.Mater.2009,21,2206) of the embodiment of the present invention 1 preparation.
By Fig. 1 and Fig. 2 as can be known, the titanic oxide material of embodiment 1 and embodiment 2 preparations is formed by train of thought link different in size, thereby forms big or small irregular pore space structure, looks that to look like Spider Web equally loose porous, and has good connectivity.
As shown in Figure 3, can see the internal structure of the titanic oxide material of embodiment 1 preparation, further show loose porous these characteristics of titanic oxide material and the good connectivity of embodiment 1 preparation.
As shown in Figure 4, the titanic oxide material of embodiment 1 preparation has sharp-pointed bragg peak, and good crystallinity is described.Shown by the XRD figure picture, 2 θ values meet the brilliant picture of anatase titania at 25.36,37.86,47.96,54.14,55.08,62.73,68.66,70.37 and 75.06 degree, and 2 θ values meet the brilliant picture of rutile titanium dioxide at 27.44,36.04,41.36,53.1 and 56.52 degree.Meanwhile, use the Scherrer formula: D=K λ/β cos θ, the average grain size of the titanic oxide material of calculating embodiment 1 preparation.Wherein, λ is the wavelength (0.15148nm) of X ray, and K Scherrer constant (0.89), θ are the diffraction peak positions of X ray, and last, β is full width at half maximum (FWHM).Thereby the grain-size that calculates is approximately 9nm, proves that further train of thought is very thin and loose.
Photo-anode mould material as dye sensitization solar battery should have higher specific surface area, and as shown in Figure 5, the titanic oxide material specific surface area of embodiment 1 preparation is 424m
2g
-1, have the specific surface area of superelevation.
Fig. 6 shows the big or small intensive 12nm place that is distributed in the titanic oxide material aperture of embodiment 1 preparation.
As shown in Figure 7, the battery that titanic oxide material is assembled into of embodiment 1 preparation has good electricity conversion (η), wherein, and current density: J
sc=13.73 milliamperes/centimetre
2, short-circuit voltage: V
oc=0.75 volt, packing factor: FF=0.71, transformation efficiency: η=7.31%.
Embodiment
Prepare the nano titania net materials with hydrothermal synthesis method, detailed process is as follows
Embodiment 1
(1) 0.1g commercial titanium dioxide (P25, the Degussa of manufacturer, approximately 30 nanometers) joins 60mL, concentration is in the sodium hydroxide solution of 10mol/L;
(2) magnetic agitation after 5 minutes, is transferred to mixing solutions in the 100mL water heating kettle
(3) airtight good water heating kettle is put in the middle of baking oven, with after baking oven for heating to 120 ℃, the beginning timing, baking oven is closed in timing 90 minutes, naturally cools to room temperature.
(4) open water heating kettle, pour out reactant and carry out centrifugally operated, centrifugation rate is 10000 rev/mins.Being taken up in order of priority with concentration is dilute hydrochloric acid and the deionized water of 0.2mol/L, centrifugal after washing, and each 3 times repeatedly.
(5) last centrifugal product is put in 60 ℃ of vacuum drying ovens, dried taking-up in 8 hours.
(6) powder after drying is put into sintering in retort furnace, and sintering temperature is 450 ℃, and temperature rise rate is 10 ℃/min, and sintering time is 2 hours, then naturally is down to room temperature, thereby obtains three-dimensional TiO of the present invention
2Mesh nano material, quality are 60mg.
(1) 0.1g commercial titanium dioxide (P25, the Degussa of manufacturer) joins 60mL, and concentration is in the sodium hydroxide solution of 10mol/L
(2) magnetic agitation after 20 minutes, is transferred to mixing solutions in the 100mL water heating kettle
(3) airtight good water heating kettle is put in the middle of baking oven, with after baking oven for heating to 150 ℃, the beginning timing, baking oven is closed in timing 120 minutes, naturally cools to room temperature.
(4) open water heating kettle, pour out reactant and carry out centrifugally operated, centrifugation rate is 15000 rev/mins.Being taken up in order of priority with concentration is dilute hydrochloric acid and the deionized water of 0.2mol/L, washing-centrifugal, and each 3 times repeatedly.
(5) last centrifugal product is put in 60 ℃ of vacuum drying ovens, dried taking-up in 10 hours.
(6) powder after drying is put into sintering in retort furnace, and sintering temperature is 450 ℃, and temperature rise rate is 10 ℃/min, and sintering time is 5 hours, then naturally is down to room temperature.Thereby obtain three-dimensional TiO of the present invention
2Mesh nano material, quality are 60mg.
Claims (6)
1. three-dimensional TiO
2Mesh nano material preparation method, its step is as follows:
1) take that 0.05～0.15g titanium dioxide joins 60～80mL, concentration is in the sodium hydroxide solution of 5～10mol/L, magnetic agitation 5～20 minutes;
2) then with mixing solutions 120～150 ℃ of Water Under thermal responses 30～300 minutes;
3) open water heating kettle after naturally cooling to room temperature, pour out reactant and carry out centrifugal;
4) be dilute hydrochloric acid and the deionized water wash and centrifugal of 0.1～0.2mol/L with concentration respectively with centrifugal product, each repeats 3～5 times;
5) centrifugal product vacuum drying 8～10 hours under 60～80 ℃ of conditions; Powder after oven dry 400～500 ℃ of lower sintering 2～5 hours, is cooled to room temperature naturally, thus must three-dimensional TiO
2The mesh nano material.
2. a kind of three-dimensional TiO as claimed in claim 1
2Mesh nano material preparation method is characterized in that: centrifugation rate is 10000～15000 rev/mins.
3. a kind of three-dimensional TiO as claimed in claim 1
2Mesh nano material preparation method is characterized in that: the temperature rise rate of sintering is 2～10 ℃/min.
4. the prepared three-dimensional TiO of any one method of claim 1～3
2The mesh nano material.
5. three-dimensional TiO claimed in claim 4
2The application of mesh nano material in photochemical catalysis, photochemistry, lithium cell or solar cell.
6. three-dimensional TiO as claimed in claim 5
2The application of mesh nano material in photochemical catalysis, photochemistry, lithium cell or solar cell is characterized in that: as the light anode material for the preparation of dye sensitization solar battery.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104528810A (en) * | 2015-01-20 | 2015-04-22 | 天津大学 | Preparation method for preparing stannic oxide nanorod cluster by using one-step hydrothermal method |
| CN104752063A (en) * | 2015-04-11 | 2015-07-01 | 吉林大学 | Porous TiO2 nanocrystalline thin film with three-dimensional nanorod film chip structure, preparation method and application |
| CN110040820A (en) * | 2019-05-23 | 2019-07-23 | 天津市大陆制氢设备有限公司 | The tin dioxide coating on titanium antimony electrode and preparation method thereof of titanium dioxide reticular structure modification |
| CN116023936A (en) * | 2022-11-16 | 2023-04-28 | 齐鲁工业大学 | Preparation method of netlike nano aggregate and application of netlike nano aggregate in photocatalysis field |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102275986A (en) * | 2011-05-27 | 2011-12-14 | 吉林大学 | Controllable hydro-thermal preparation method for titanium dioxide nanobelts of different crystal forms |
-
2013
- 2013-03-26 CN CN201310099397XA patent/CN103145183A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102275986A (en) * | 2011-05-27 | 2011-12-14 | 吉林大学 | Controllable hydro-thermal preparation method for titanium dioxide nanobelts of different crystal forms |
Non-Patent Citations (1)
| Title |
|---|
| 董祥等: "水热法制备三维网状TiO2纳米线薄膜及其光电化学性能", 《物理化学学报》, vol. 25, no. 9, 30 September 2009 (2009-09-30), pages 1874 - 1882 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104528810A (en) * | 2015-01-20 | 2015-04-22 | 天津大学 | Preparation method for preparing stannic oxide nanorod cluster by using one-step hydrothermal method |
| CN104752063A (en) * | 2015-04-11 | 2015-07-01 | 吉林大学 | Porous TiO2 nanocrystalline thin film with three-dimensional nanorod film chip structure, preparation method and application |
| CN110040820A (en) * | 2019-05-23 | 2019-07-23 | 天津市大陆制氢设备有限公司 | The tin dioxide coating on titanium antimony electrode and preparation method thereof of titanium dioxide reticular structure modification |
| CN110040820B (en) * | 2019-05-23 | 2021-09-21 | 天津市大陆制氢设备有限公司 | Titanium-based tin antimony oxide electrode modified by titanium dioxide net structure and preparation method thereof |
| CN116023936A (en) * | 2022-11-16 | 2023-04-28 | 齐鲁工业大学 | Preparation method of netlike nano aggregate and application of netlike nano aggregate in photocatalysis field |
| CN116023936B (en) * | 2022-11-16 | 2023-11-10 | 齐鲁工业大学 | Preparation method of netlike nano aggregate and application of netlike nano aggregate in photocatalysis field |
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Application publication date: 20130612 |