CN104715928A - Preparing method for Li doped TiO2 nano-rod photo-anode - Google Patents
Preparing method for Li doped TiO2 nano-rod photo-anode Download PDFInfo
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- CN104715928A CN104715928A CN201510082277.8A CN201510082277A CN104715928A CN 104715928 A CN104715928 A CN 104715928A CN 201510082277 A CN201510082277 A CN 201510082277A CN 104715928 A CN104715928 A CN 104715928A
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Abstract
The invention discloses a preparing method for a Li doped TiO2 nano-rod photo-anode. The preparing method comprises the following steps that (1) an electric conduction substrate is taken for conducting ultrasonic cleaning, thoroughly cleaned with deionized water, dried and taken out for standby use; (2) tetra-n-butyl titanate, lithium nitrate, hydrochloric acid and deionized water are mixed to be prepared into a reaction solution, and the reaction solution is fully stirred; (3) the electric conduction substrate is put into a reaction kettle, the reaction solution is slowly poured into the reaction kettle, and a pulse electromagnetic field is applied to the reaction solution for processing; (4) the reaction kettle is put into a constant temperature drying box after processing is conducted, a TiO2 film is formed on the surface of the electric conduction substrate after the reaction, the reaction kettle is taken out and cooled, and then the electric conduction substrate is taken out; (5) the TiO2 film simply needs to be scraped into the needed area. The preparing method has the advantages that the electron-hole combination can be restrained, the transfer speed of electrons can be increased, the probability of the electron-hole combination can be reduced, and the photoelectric conversion efficiency can be improved; the electron transmission speed can be increased, the adsorption area of dye can be increased, and the battery conversion efficiency can be further improved.
Description
Technical field
The invention belongs to the preparation method of dye-sensitized solar cell anode, particularly a kind of Li doped Ti O
2the preparation method of nanometer rods light anode.
Background technology
It is simple that DSSC has cheap, manufacture craft, and advantages of environment protection, is expected to the main body becoming following solar cell.But the problem that dye sensitive solar battery conversion efficiency is lower is the bottleneck of this Technique Popularizing application.Adopt one-dimensional nano-array as the light anode material of solar energy dye-sensitized cell, electronics transmission in perpendicular to the crystal array structure of conductive substrates has high transmission rate and lowest loss, the electric transmission time can be reduced, be conducive to improving cell conversion efficiency.But true really not so, numerous experimental result finds, adopts one-dimensional single crystal nanometer stick array as shown in Figure 1 still lower as the dye-sensitized solar cells photoelectric efficiency obtained by light anode.Analyze its reason as follows: in (1) unit Substrate Area, the surface area of nanometer stick array is relatively little, absorbing dye quantity is less, and it is less that electronics produces quantity, and the array of (2) high-sequential is open array, be unfavorable for light absorption, also affect the generation of electronics.
In numerous oxide semiconductors, titanium dioxide due to its biological and chemical stability, strong oxidizing property, cheap, can maintaining a long-term stability property, anti-light corrosion and chemical corrosivity, and in DSSC, be verified TiO
2it is best semi-conducting material.Current research is except to nano-TiO
2photo-anode film carries out micro-structural regulation and control and improves beyond its photoelectric properties, and metal ion mixing can change TiO
2middle deep energy level structure, deep energy level can form trap center, especially lower than Ti
4+metal ion catch hole, effectively suppress the compound of electron-hole, improve electron transfer speed, reduce the recombination probability of electron-hole, improve photon utilance.
Current synthesis TiO
2the method of nanometer stick array mainly contains hydro thermal method, template, sol-gel method etc.Wherein the shortcoming of template has needed after having prepared chemically to remove template, the method complex process, and chemistry removing template procedure affects to some extent for the form of product and performance.Sol-gel method is a kind of preparation method of nano material that application is more now, and the method reaction time is longer, and the pattern of gained one-dimensional nano-array is wayward.Hydro thermal method is carried out in aqueous due to reaction, and reaction temperature is lower, and equipment is simple, is convenient to automated production, be applicable to large-scale production and attention, but hydro thermal method reaction temperature is lower, is unfavorable for doped with metal elements.Therefore independent hydrothermal synthesis method is difficult to realize TiO
2the Uniform Doped of Li element.
Summary of the invention
Technical problem to be solved by this invention to provide a kind of Li doped Ti O
2the preparation method of nanometer rods light anode, the method can realize TiO
2the Uniform Doped of Li element in nanometer rods, improves the density of nanometer rods, adopts Li doped Ti O prepared by the method
2nanometer rods light anode can improve electronic switch speed, reduces the recombination probability of electron-hole, improves photoelectric conversion efficiency and battery conversion efficiency.
For solving the problem, the present invention adopts following technical scheme:
A kind of Li doped Ti O
2the preparation method of nanometer rods light anode, comprises step as follows:
1, get conductive substrate to put into absolute ethyl alcohol and carry out ultrasonic cleaning, then clean with deionized water rinsing, put into drying box dry after take out for subsequent use;
2, tetra-n-butyl titanate, lithium nitrate, hydrochloric acid and deionized water are hybridly prepared into reaction solution by a certain percentage, the reaction solution glass bar configured fully is stirred until reaction solution become colorless by white transparent till; In described reaction solution, hydrochloric acid and deionized water are as solvent, and its volume ratio is 1:1 ~ 1.2:1, and lithium nitrate and tetra-n-butyl titanate are as solute, and its atomic percent is 0.01:1 ~ 0.05:1; Solution concentration is 1.6 ~ 2.0%;
3, the conductive substrate after cleaning-drying is put into reactor down with conducting surface, the reaction solution prepared slowly is injected reactor; Then apply pulse electromagnetic field process to the reaction solution in reactor, the processing time is 30 ~ 60s, and pulse voltage is 800 ~ 900V, and pulse frequency is 5 ~ 7Hz;
4, after process, the reactor of good seal is put into thermostatic drying chamber, regulate reaction temperature to be 170 ~ 190 DEG C, after reaction 10 ~ 13h, form one deck TiO on conductive substrate surface
2film, takes out reactor, takes out conductive substrate, fall the white precipitate on conductive substrate surface and unnecessary ion with deionized water rinsing after being cooled to room temperature, puts it into dry rear taking-up in baking oven;
5, the TiO will prepared
2film spreads to required size, obtains Li doped Ti O to be prepared
2nanometer rods light anode.
Preferably, described conductive substrate is FTO electro-conductive glass.
Preferably, the mass concentration of described hydrochloric acid is 36% ~ 38%.
Preferably, in described step 1, conductive substrate is put into absolute ethyl alcohol and is carried out ultrasonic cleaning 20-30min.
Preferably, glass bar drainage is used slowly to inject reactor the reaction solution configured in described step 3.
Preferably, in described step 3, compactedness during the reaction solution prepared injection reactor is controlled 60% ~ 70%.
The invention has the beneficial effects as follows:
(1) lithium doping TiO is adopted
2as light sun level, metal-lithium ion doping can change TiO
2middle impurity energy level and deep energy level structure, deep energy level can form trap center, can catch hole, effectively suppresses the compound of electron-hole, improves electron transfer speed, reduces the recombination probability of electron-hole, improves photoelectric conversion efficiency.
(2) fine and close, case type one dimension TiO is utilized
2nanometer stick array, as light anode, not only can improve electron transfer rate, also can improve Dye Adsorption area, increases light absorption, improves battery conversion efficiency further.
(3) by adopting pulse electromagnetic field assisting alcohol-hydrothermal method synthesis Li doping titanium dioxide nano rod, effective Uniform Doped of Li element can be realized, improve the density of nanometer rods, nanometer stick array stacking, increase the scattering of sunlight, be conducive to light absorption, thus improve efficiency of dye-sensitized solar battery.
(4) by adopting pulse electromagnetic field assisting alcohol-hydrothermal method synthesis Li doping titanium dioxide nano rod, the method energy consumption is low, Dynamic System is simple, operating cost is low, occupation area of equipment is little, parameter easily regulates, not polluting the object handled by it and surrounding environment, is a kind of processing method of cleaner environmental protection.
Accompanying drawing explanation
Fig. 1 is the SEM image of non-doped Ti O2 nanometer stick array.
Fig. 2 is Li doped Ti O prepared by the embodiment of the present invention 1
2the SEM image of nanometer stick array.
Fig. 3 is Li doped Ti O prepared by the embodiment of the present invention 2
2the SEM image of nanometer stick array.
Fig. 4 is Li doped Ti O prepared by the embodiment of the present invention 3
2the SEM image of nanometer stick array.
Embodiment
Embodiment 1
A kind of Li doped Ti O that the present invention relates to
2the preparation method of nanometer rods light anode, comprises step as follows:
1, substrate is cleaned
Get conductive substrate to put into absolute ethyl alcohol and carry out ultrasonic cleaning 20min, then clean with deionized water rinsing, put into drying box dry after take out for subsequent use.Described conductive substrate can adopt the materials such as FTO electro-conductive glass, ITO electro-conductive glass, PET conductive plastics, and as preferably, described conductive substrate is FTO electro-conductive glass.
2, reaction solution is configured
By tetra-n-butyl titanate, lithium nitrate, hydrochloric acid and deionized water are hybridly prepared into reaction solution by a certain percentage, the reaction solution glass bar configured fully is stirred until reaction solution become colorless by white transparent till.In described reaction solution, hydrochloric acid and deionized water are as solvent, and its volume ratio is 1:1; Lithium nitrate and tetra-n-butyl titanate are as solute, and its atomic percent is 0.01:1; The solution concentration of reaction solution is 1.6%.The mass concentration of described hydrochloric acid is 36% ~ 38%.
3, pulse electromagnetic field process
Conductive substrate after cleaning-drying is put into reactor down with conducting surface, and use glass bar drainage slowly to inject reactor the reaction solution prepared, compactedness controls 60%; Then apply pulse electromagnetic field process to the reaction solution in reactor, the processing time is 30s, and pulse voltage is 800V, and pulse frequency is 5Hz.
4, after process, the reactor of good seal is put into thermostatic drying chamber, regulate reaction temperature to be 170 DEG C, the reaction time is 10h, forms one deck TiO on conductive substrate surface
2film; Then take out reactor, after being cooled to room temperature, take out conductive substrate, fall the white precipitate on conductive substrate surface and unnecessary ion with deionized water rinsing, put it into dry rear taking-up in baking oven.
5, the TiO finally will prepared
2film spreads to required size, obtains Li doped Ti O to be prepared
2nanometer rods light anode.Gained Li doped Ti O
2the SEM image of nanometer stick array, as shown in Figure 2.Can observe from Fig. 2, by adopting pulse electromagnetic field assisting alcohol-hydrothermal method synthesis Li doping titanium dioxide nano rod, effective Uniform Doped of Li element can be realized, improve the density of nanometer rods, nanometer stick array stacking, increase the scattering of sunlight, be conducive to light absorption, thus improve efficiency of dye-sensitized solar battery.
When preparing solar cell, contaminate in N719 dyestuff by the nanometer rods light anode prepared, sealing is placed in drying box, takes out sample, with the dyestuff that absolute ethyl alcohol treatment surface is unnecessary after insulation 12 ~ 16h.Recycling platinum is as photocathode, and assembling DSSC, drips electrolyte, and encapsulate battery.
Embodiment 2
A kind of Li doped Ti O that the present invention relates to
2the preparation method of nanometer rods light anode, comprises step as follows:
1, substrate is cleaned
Get conductive substrate to put into absolute ethyl alcohol and carry out ultrasonic cleaning 30min, then clean with deionized water rinsing, put into drying box dry after take out for subsequent use.Described conductive substrate can adopt the materials such as FTO electro-conductive glass, ITO electro-conductive glass, PET conductive plastics, and as preferably, described conductive substrate is FTO electro-conductive glass.
2, reaction solution is configured
By tetra-n-butyl titanate, lithium nitrate, hydrochloric acid and deionized water are hybridly prepared into reaction solution by a certain percentage, the reaction solution glass bar configured fully is stirred until reaction solution become colorless by white transparent till.In described reaction solution, hydrochloric acid and deionized water are as solvent, and its volume ratio is 1.2:1; Lithium nitrate and tetra-n-butyl titanate are as solute, and its atomic percent is 0.05:1; The solution concentration of reaction solution is 2.0%.The mass concentration of described hydrochloric acid is 36% ~ 38%.
3, pulse electromagnetic field process
Conductive substrate after cleaning-drying is put into reactor down with conducting surface, and use glass bar drainage slowly to inject reactor the reaction solution prepared, compactedness controls 70%; Then apply pulse electromagnetic field process to the reaction solution in reactor, the processing time is 60s, and pulse voltage is 900V, and pulse frequency is 7Hz.
4, after process, the reactor of good seal is put into thermostatic drying chamber, regulate reaction temperature to be 190 DEG C, the reaction time is 13h, forms one deck TiO on conductive substrate surface
2film; Then take out reactor, after being cooled to room temperature, take out conductive substrate, fall the white precipitate on conductive substrate surface and unnecessary ion with deionized water rinsing, put it into dry rear taking-up in baking oven.
5, the TiO finally will prepared
2film spreads to required size, obtains Li doped Ti O to be prepared
2nanometer rods light anode.Gained Li doped Ti O
2the SEM image of nanometer stick array, as shown in Figure 3.
Can observe from Fig. 3, by adopting pulse electromagnetic field assisting alcohol-hydrothermal method synthesis Li doping titanium dioxide nano rod, effective Uniform Doped of Li element can be realized, improve the density of nanometer rods, nanometer stick array stacking, increase the scattering of sunlight, be conducive to light absorption, thus improve efficiency of dye-sensitized solar battery.
Embodiment 3
A kind of Li doped Ti O that the present invention relates to
2the preparation method of nanometer rods light anode, comprises step as follows:
1, substrate is cleaned
Get conductive substrate to put into absolute ethyl alcohol and carry out ultrasonic cleaning 25min, then clean with deionized water rinsing, put into drying box dry after take out for subsequent use.Described conductive substrate can adopt the materials such as FTO electro-conductive glass, ITO electro-conductive glass, PET conductive plastics, and as preferably, described conductive substrate is FTO electro-conductive glass.
2, reaction solution is configured
By tetra-n-butyl titanate, lithium nitrate, hydrochloric acid and deionized water are hybridly prepared into reaction solution by a certain percentage, the reaction solution glass bar configured fully is stirred until reaction solution become colorless by white transparent till.In described reaction solution, hydrochloric acid and deionized water are as solvent, and its volume ratio is 1.1:1; Lithium nitrate and tetra-n-butyl titanate are as solute, and its atomic percent is 0.03:1; The solution concentration of reaction solution is 1.8%.The mass concentration of described hydrochloric acid is 36% ~ 38%.
3, pulse electromagnetic field process
Conductive substrate after cleaning-drying is put into reactor down with conducting surface, and use glass bar drainage slowly to inject reactor the reaction solution prepared, compactedness controls 65%; Then apply pulse electromagnetic field process to the reaction solution in reactor, the processing time is 50s, and pulse voltage is 850V, and pulse frequency is 6Hz.
4, after process, the reactor of good seal is put into thermostatic drying chamber, regulate reaction temperature to be 180 DEG C, after reaction 12h, form one deck TiO on conductive substrate surface
2film; Then take out reactor, after being cooled to room temperature, take out conductive substrate, fall the white precipitate on conductive substrate surface and unnecessary ion with deionized water rinsing, put it into dry rear taking-up in baking oven.
5, the TiO finally will prepared
2film spreads to required size, obtains Li doped Ti O to be prepared
2nanometer rods light anode.Gained Li doped Ti O
2the SEM image of nanometer stick array, as shown in Figure 4.
Can observe from Fig. 4, by adopting pulse electromagnetic field assisting alcohol-hydrothermal method synthesis Li doping titanium dioxide nano rod, effective Uniform Doped of Li element can be realized, improve the density of nanometer rods, nanometer stick array stacking, increase the scattering of sunlight, be conducive to light absorption, thus improve efficiency of dye-sensitized solar battery.
The Li doped Ti O prepared by above-described embodiment
2the parameter of nanometer rods light anode is in table 1.
| The nanometer rods length of side | Density | |
| Example 1 | 86nm | 71 (root/μm 2) |
| Example 2 | 81nm | 75 (root/μm 2) |
| Example 3 | 84nm | 73 (root/μm 2) |
Table 1
Although embodiment of the present invention are open as above, but it is not restricted to listed in specification and execution mode utilization, it can be applied to various applicable the field of the invention completely, for those skilled in the art, can easily realize other amendment, therefore do not deviating under the universal that claim and equivalency range limit, the present invention is not limited to specific details and illustrates here and the legend described.
Claims (6)
1. a Li doped Ti O
2the preparation method of nanometer rods light anode, is characterized in that, comprise step as follows:
1) get conductive substrate to put into absolute ethyl alcohol and carry out ultrasonic cleaning, then clean with deionized water rinsing, put into drying box dry after take out for subsequent use;
2) tetra-n-butyl titanate, lithium nitrate, hydrochloric acid and deionized water are hybridly prepared into reaction solution by a certain percentage, the reaction solution glass bar configured fully is stirred until reaction solution become colorless by white transparent till; In described reaction solution, hydrochloric acid and deionized water are as solvent, and its volume ratio is 1:1 ~ 1.2:1, and lithium nitrate and tetra-n-butyl titanate are as solute, and its atomic percent is 0.01:1 ~ 0.05:1; Solution concentration is 1.6 ~ 2.0%;
3) conductive substrate after cleaning-drying is put into reactor down with conducting surface, the reaction solution prepared slowly is injected reactor; Then apply pulse electromagnetic field process to the reaction solution in reactor, the processing time is 30 ~ 60s, and pulse voltage is 800 ~ 900V, and pulse frequency is 5 ~ 7Hz;
4) after process, the reactor of good seal is put into thermostatic drying chamber, regulate reaction temperature to be 170 ~ 190 DEG C, after reaction 10 ~ 13h, form one deck TiO on conductive substrate surface
2film, takes out reactor, takes out conductive substrate, fall the white precipitate on conductive substrate surface and unnecessary ion with deionized water rinsing after being cooled to room temperature, puts it into dry rear taking-up in baking oven;
5) TiO will prepared
2film spreads to required size, obtains Li doped Ti O to be prepared
2nanometer rods light anode.
2. a kind of Li doped Ti O according to claim 1
2the preparation method of nanometer rods light anode, is characterized in that: described conductive substrate is FTO electro-conductive glass.
3. a kind of Li doped Ti O according to claim 1
2the preparation method of nanometer rods light anode, is characterized in that: the mass concentration of described hydrochloric acid is 36% ~ 38%.
4. a kind of Li doped Ti O according to claim 1
2the preparation method of nanometer rods light anode, is characterized in that: in described step 1, conductive substrate is put into absolute ethyl alcohol and carried out ultrasonic cleaning 20-30min.
5. a kind of Li doped Ti O according to claim 1
2the preparation method of nanometer rods light anode, is characterized in that: use glass bar drainage slowly to inject reactor the reaction solution configured in described step 3.
6. a kind of Li doped Ti O according to claim 1
2the preparation method of nanometer rods light anode, is characterized in that: in described step 3 control compactedness during the reaction solution prepared injection reactor 60% ~ 70%.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101478035A (en) * | 2009-01-09 | 2009-07-08 | 中国科学院上海硅酸盐研究所 | Electrode material used for organic inorganic composite cell and manufacturing process |
| CN101475213A (en) * | 2009-01-14 | 2009-07-08 | 华东理工大学 | Preparation of lithiation nano titanium oxide and use thereof |
| CN102693844A (en) * | 2012-05-30 | 2012-09-26 | 辽宁工业大学 | Method for preparing Al mixed with ZnO nanosheet array by adopting pulsed electromagnetic field |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101478035A (en) * | 2009-01-09 | 2009-07-08 | 中国科学院上海硅酸盐研究所 | Electrode material used for organic inorganic composite cell and manufacturing process |
| CN101475213A (en) * | 2009-01-14 | 2009-07-08 | 华东理工大学 | Preparation of lithiation nano titanium oxide and use thereof |
| CN102693844A (en) * | 2012-05-30 | 2012-09-26 | 辽宁工业大学 | Method for preparing Al mixed with ZnO nanosheet array by adopting pulsed electromagnetic field |
Non-Patent Citations (1)
| Title |
|---|
| ALAGESAN SUBRAMANIAN等: "The effect of Li+ intercalation on different sized TiO2 nanoparticles and the performance of dye-sensitized solar cells", 《THIN SOLID FILMS》 * |
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