CN110451560A - A kind of acanthosphere shape TiO2Environment-friendly preparation method thereof and purposes - Google Patents
A kind of acanthosphere shape TiO2Environment-friendly preparation method thereof and purposes Download PDFInfo
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- CN110451560A CN110451560A CN201910761962.1A CN201910761962A CN110451560A CN 110451560 A CN110451560 A CN 110451560A CN 201910761962 A CN201910761962 A CN 201910761962A CN 110451560 A CN110451560 A CN 110451560A
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
- C01G23/0536—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing chloride-containing salts
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/20—Light-sensitive devices
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- H01G9/2031—Light-sensitive devices comprising an oxide semiconductor electrode comprising titanium oxide, e.g. TiO2
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Abstract
The invention discloses a kind of acanthosphere shape TiO2Environment-friendly preparation method thereof and purposes, this kind of method is with cheap TiCl4Raw material is titanium source, and does not use other any auxiliary reagents.The method of the present invention greatly simplifies preparation process, promotes synthesis quality, reduces process costs, simultaneously synthesizing TiO2Have the characteristics that the diameter of relatively small, the one-dimensional basic structure of particle size is smaller, may make TiO according to the present invention2It can preferably coordinate to require of both Dye Adsorption and charge transmission, there are the potentiality realized and photoelectric conversion performance is substantially improved.
Description
Technical field
The application belongs to dye-sensitized solar cell anode technical field of material, is directed to a kind of acanthosphere
The environment-friendly preparation method thereof and purposes of shape TiO2.
Technical background
Dye-sensitized solar cells (DSCs) is turned with its cheap cost, simple technique and relatively high photoelectricity
It changes efficiency and has attracted worldwide attention, become one of the solar battery of current most potentiality to be exploited.Dyestuff is quick
Change solar battery to consist of three parts: the nanocrystalline porous light anode of dye sensitization and is loaded with catalysis at redox electrolytes liquid
Agent to electrode.Wherein, developing efficient optical anode material is the key that improve such cell photoelectric transformation efficiency.Efficient light anode
Material usually has biggish specific surface area and quick charge transfer performance.Generally, the light being made of nano-crystalline granule
Anode film often has biggish specific surface area, to guarantee sufficiently large Dye Adsorption amount, promotes light utilization ratio.However it receives
The presence of a large amount of granular boundaries greatly reduces the rate of carrier transport in the brilliant film of rice, increases the probability of charge recombination.
In fact, charge transport properties are highly dependent on the pattern of anode material, compared to nano-crystalline granule, one-dimentional structure is such as received
Mitron, nano wire etc. have biggish charge transport rate, thus construct one-dimensional nano structure become reduce charge transfer resistance,
Increase the effective way of transmission speed.However, effectively overcoming electricity based on the dye-sensitized solar cells of one-dimensional nano structure
While lotus transmission performance, but along with the extreme loss of specific surface area.Thus how to balance efficiency of light absorption and charge transmits
Relationship between performance is universal, the crucial problem of the efficient DSCs of exploitation.
Structure by the lesser structural unit composition micron level of partial size is effective coordination and the above-mentioned two necessary item of balance
One important method of part.Based on such a design philosophy, multiple research teams have been prepared with different-grain diameter
TiO2Microballoon.Due to nanocrystalline as basic unit using small particle TiO2, thus can while large specific surface area is provided
The crystal grain boundary and defect inside spherical structure are reduced to a certain extent.Moreover, the TiO of this three-dimensional2Usually have
Micropore or meso-hole structure, thus get enter into light wave inside light anode, greatly increase light utilization ratio.With commercially use TiO2
(P25) and the TiO of small particle2It compares, the incident photon-to-electron conversion efficiency of the structure is remarkably reinforced.However due to mistake inside the three-dimensional structure
Small basic structural unit partial size also will increase inside configuration charge recombination not only bad for Built-in potential is formed, to limit
The further promotion of battery performance.
Increase the draw ratio of basic unit and provides new Research Thinking to promote the performance of dye-sensitized solar cells.
Basic unit for constructing three-dimensional structure can be nanometer rods, nanometer bundle and nano wire etc..In this configuration, because of 1D structure
Presence and so that electron-transport is accelerated;At the same time, specific surface area can be made by adjusting the size with optimization 1D structure
It is maintained, realizes the active balance of electron-transport and Dye Adsorption.Moreover, light scattering in this hierarchy
It will can also get a promotion.It may be speculated that promote the photoelectric conversion performance of such three-dimensional structure, for basic cell structure
It is most important with the regulation of pattern.Kim etc. synthesizes the three-dimensional TiO of a variety of dendritic structures using hydro-thermal method2, but the research is adopted
It is titanium source with the higher butyl titanate of price, thus increases preparation cost;In addition, in the synthesis process also for control pattern
A variety of organic reagents, i.e. ethylene glycol and cetyl trimethylammonium bromide are additionally added to, expenditure is not only increased and also aggravates
Environmental pressure.
Application number 201510740402.X discloses a kind of flower-shaped TiO2It the preparation method of/graphene photo-catalyst and its answers
With specifically with titanium tetrachloride TiCl4As titanium source, bromo N- butyl-pyridinium ionic liquid passes through water as style control agent
Hot microwave method is prepared.But this method in implementation process only by means of style control agent (bromo N- butyl-pyridinium from
Sub- liquid) under the action of can just obtain flower-shaped TiO2, this undoubtedly increases environmental pressure and cost;In addition, to finally obtain flower
Shape TiO2It also needs by hydro-thermal microwave treatment, and the use of relevant device considerably increases the research cost of product.And it is of the invention
The synthesis technology of involved exploitation controls without any shape or regulates and controls reagent, while without High-temperature water heat treatment.It synthesized
Journey is simpler, economical and environmentally protective.
Up to the present cut-off, still rarely has using three-dimensional dendroid or acanthosphere TiO2Report of the structure as optical anode material
Road, one of them important reason may just be the absence of the important method for synthesizing such material.
Summary of the invention
The purpose of this invention is to provide a kind of more mild, economy, environmentally friendly synthesis route, has efficiency light with preparation
The TiO of electrotransformation performance2Optical anode material.
A kind of acanthosphere shape TiO2Environment-friendly preparation method thereof, it is characterised in that: step are as follows:
(1) it takes dehydrated alcohol to be placed in container, obtains solution A, acquired solution A is put into ice-water bath for use;
(2) titanium tetrachloride solution is measured by several times, is added dropwise in solution A, after stirring 5min, secondary water is added and continues to stir
10min obtains the flaxen titanium tetrachloride solution B of color;
(3) it measures solution B to be added into container, reaction is hydrolyzed at 80 DEG C, it is milky uniformly water-soluble for obtaining color
Liquid C;
(4) acquired solution C is placed 4 months in a reservoir, through centrifuge washing, even if dry obtain the TiO that pattern is acanthosphere2。
Further, step (2) titanium tetrachloride solution and the amount ratio of solution A are that 0.6:1 ~ 1:20(is preferred, are used
Amount is than being 1:7.5).
Further, it is 1:1 that the amount ratio of step (2) secondary water and solution A, which is 12:1 ~ 1:1(amount ratio).
Further, the step (3) hydrolysis 0.5 ~ 3 hour.
Further, step (4) drying temperature is 40-100 DEG C.
Further, acanthosphere shape TiO made from the environment-friendly preparation method thereof2In dye sensitization solar battery electrode material
In application.
Further, acanthosphere shape TiO made from the environment-friendly preparation method thereof2Application in wastewater photocatalytic degradation.
Preparation method provided by the invention has the advantage that
1. preparation process can be greatly simplified, promotes synthesis quality, reduces process costs;
2. the TiO for the acanthosphere that the present invention synthesizes2Have the characteristics that particle size is relatively small, one-dimentional structure diameter is smaller, it can
So that TiO according to the present invention2It can preferably coordinate to require of both Dye Adsorption and charge transmission, have realization big
The potentiality of width promotion photoelectric conversion performance.
Detailed description of the invention
Fig. 1 TiO2TEM figure;
Fig. 2 TiO2XRD figure.
Specific embodiment
A kind of embodiment 1: acanthosphere shape TiO2Preparation method, steps are as follows:
(1) 67ml dehydrated alcohol is measured in 200ml beaker, obtains solution A, above-mentioned solution is put into ice-water bath;
(2) 6ml titanium tetrachloride solution is measured, is added dropwise in solution A, 67ml secondary water is added after stirring 5min and continues to stir
10min is mixed, the flaxen titanium tetrachloride solution of color (solution B) may finally be obtained;
(3) solution B is added in 200ml beaker, is reacted at 80 DEG C and obtains within 2 hours color as milky homogeneous aqueous solution
(solution C);
(4) solution C is placed 4 months in beaker, through centrifuge washing, the dry pattern that just obtains for the TiO of acanthosphere2。
A kind of embodiment 2: acanthosphere shape TiO2Environment-friendly preparation method thereof, steps are as follows:
(1) 20ml dehydrated alcohol is measured in 200ml beaker, obtains solution A, above-mentioned solution is put into ice-water bath;
(2) 20ml titanium tetrachloride solution is measured, is added dropwise in solution A, 114ml secondary water is added after stirring 5min and is continued
10min is stirred, may finally obtain color is flaxen titanium tetrachloride solution (solution B);
(3) solution B is added in 200ml beaker, is reacted at 80 DEG C and obtains within 1 hour color as milky homogeneous aqueous solution
(solution C);
(4) solution C is placed 4 months in beaker, through centrifuge washing, the dry pattern that just obtains for the TiO of acanthosphere2。
A kind of embodiment 3: acanthosphere TiO2Environment-friendly preparation method thereof, steps are as follows:
(1) 100ml dehydrated alcohol is measured in 200ml beaker, obtains solution A, above-mentioned solution is put into ice-water bath;
(2) 6ml titanium tetrachloride solution is measured, is added dropwise in solution A, 240ml secondary water is added after stirring 5min and is continued
10min is stirred, the flaxen titanium tetrachloride solution of color (solution B) may finally be obtained;
(3) solution B is added in 200ml beaker, is reacted at 80 DEG C and obtains within 3 hours color as milky homogeneous aqueous solution
(solution C);
(4) solution C is placed 4 months in beaker, through centrifuge washing, the dry pattern that just obtains for the TiO of acanthosphere shape2。
As shown in Figure 1, TiO designed by the present invention2Feature with three-dimensional structure, particle size are about 200-500 nm
Between;In addition, the basic unit for constituting the structure is one-dimensional nanometer rods, and basic unit has lesser diameter, because
Biggish specific surface area can be maintained while effectively facilitating electron-transport as far as possible;
As shown in Figure 2, prepared TiO2 is based on Rutile Type.The composition is neither Ti (OH)4Also different from Detitanium-ore-type
TiO2, illustrate that, during the reaction along with the formation of thorn chondritic, corresponding variation also occurs for composition, this is found to be shape
The Effective Regulation of looks and composition provides important reference.
Claims (7)
1. a kind of acanthosphere shape TiO2Environment-friendly preparation method thereof, it is characterised in that: step are as follows:
(1) it takes dehydrated alcohol to be placed in container, obtains solution A, acquired solution A is put into ice-water bath for use;
(2) titanium tetrachloride solution is measured by several times, is added dropwise in solution A, after stirring 5min, secondary water is added and continues to stir
10min, obtaining color is flaxen titanium tetrachloride solution B;
(3) it measures solution B to be added into container, reaction is hydrolyzed at 80 DEG C, it is milky uniformly water-soluble for obtaining color
Liquid C;
(4) acquired solution C is placed 4 months in a reservoir, through centrifuge washing, drying to obtain pattern is the TiO of acanthosphere shape2。
2. acanthosphere shape TiO according to claim 12Environment-friendly preparation method thereof, it is characterised in that: (2) four chlorination of step
Titanium solution and the amount ratio of solution A are that 0.6:1 ~ 1:20(is preferred, amount ratio 1:7.5).
3. acanthosphere shape TiO according to claim 12Environment-friendly preparation method thereof, it is characterised in that: step (2) secondary water
Amount ratio with solution A is that 12:1 ~ 1:1(is preferred, amount ratio 1:1).
4. acanthosphere shape TiO according to claim 12Environment-friendly preparation method thereof, it is characterised in that: the step (3) hydrolysis is anti-
It answers 0.5 ~ 3 hour.
5. acanthosphere shape TiO according to claim 12Environment-friendly preparation method thereof, it is characterised in that: the dry temperature of the step (4)
Degree is 40 ~ 100 DEG C.
6. acanthosphere shape TiO made from a kind of any one of claim 1-5 environment-friendly preparation method thereof2In dye sensitization of solar electricity
Application in the electrode material of pond.
7. acanthosphere shape TiO made from a kind of any one of claim 1-5 environment-friendly preparation method thereof2In wastewater photocatalytic degradation
Application.
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2019
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