CN103014829A - Method of preparing anatase TiO2 mono-crystalline containing {001} / {010} / {101} crystal face - Google Patents
Method of preparing anatase TiO2 mono-crystalline containing {001} / {010} / {101} crystal face Download PDFInfo
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Abstract
The invention relates to the field of anatase TiO2 mono-crystalline, in particular relates to a method of preparing the anatase TiO2 mono-crystalline containing {001} / {010} / {101} crystal face. The method opens up a brand new synthetic method of anatase containing one or more than two type of {001} / {010} / {101} crystal face, and the high-activity crystal face can be obtained under a simpler and milder condition, the problem of difficult for preparation is solved, so that the anatase TiO2 mono-crystalline produce containing high-activity crystal face can be used in photocatalyst to degrade contaminant, photo splitting of water to hydrogen, dye-sensitized solar cell and photoreduction of carbon dioxide. The method in the invention comprises the following steps: putting presoma into a solution containing specific reaction solute ions, heating for 2-240 hours under 50-300 DEG C to obtain TiO2 mono-crystalline particles with different size distribution which contain three crystal face predominant respectively. The product has the advantages of large superficial area, high reactivity, high reaction selectivity and the like, and can be hopefully used in all types of photocatalytic applications extensively and effectively.
Description
Technical field
The present invention relates to anatase titania monocrystalline field, be specially and a kind ofly be rich in { 001}/{ 010}/{ the method for one or more crystal face anatase titania single crystal particles of 101} by Hydrothermal Growth, utilize the laminate structure alkali metal titanate of heterogeneity as precursor, the anatase titania single crystal particle that is rich in particular crystal plane of preparation different-grain diameter.
Background technology
1972, but finding titanium dioxide photoelectrode water of decomposition under illumination condition, Japanese Fujishima etc. produce hydrogen, titanium dioxide and other conductor photocatalysis material are widely studied subsequently, transform in the hope of the sun power of realizing the based semiconductor photocatalytic process.Titanium dioxide has high stability, nontoxic, environmental friendliness, and the remarkable advantage such as cheap, not only be widely used in the photocatalytic hydrogen production by water decomposition process, also be used to the fields such as photolysis pollutent, dye sensitization solar battery, photoelectrochemistry, biological chemistry and automatically cleaning, but the solar conversion efficiency of current titanium dioxide based photocatalytic material is generally very low, can not satisfy the needs of practical application.Be to improve transformation efficiency, doping, finishing, morphology control, heterojunction structure are compound etc., and means are widely used in modifying titanium dioxide.
Light-catalyzed reaction occurs in the surface of photocatalyst, different crystal faces are because the difference of surface atom arrangement difference and the Electronic Structure that causes thereof shows different photocatalytic activities and selectivity, the crystal face that control photocatalyst material surface exposes is the important means that changes photocatalysis performance, be subject in recent years extensive concern, particularly Australian Lu in 2008 etc. have realized having at high proportion high-energy surface { the controlled preparation of the anatase titania monocrystalline of 001} first.Recently, our research work find first the low index face of three of anatase titania 101}, 001} and the photocatalytic activity obvious difference of 010}, and in photolysis water hydrogen is used photocatalytic activity sequentially satisfy 010}〉and 101}〉{ 001}.Meanwhile, the lot of domestic and foreign research work goes out conclusion again, and in the middle of different light-catalyzed reactions, above-mentioned three kinds of crystal face activity and selectivity again can be different.Therefore, the anatase titania single crystal particle that is rich in respectively above-mentioned crystal face can be according to the different properties of each crystal face, obtain optimized performance performance thereby use in different light-catalyzed reactions targetedly.Yet most titanium body hydrolysis reaction is rapid, and nucleation, process of growth are difficult to control, particularly in industrialization, batch production pattern.Therefore, development low cost, environmental friendliness, be easy to mass-producing synthetic method significant for the photocatalysis material of titanium dioxide that different crystal faces are rich in promotion.
Summary of the invention
The object of the present invention is to provide a kind of take difficult solvability titanate solid as precursor, { 001}/{ 010}/{ the method for the titanium dioxide single crystalline particle of one or more crystal faces of 101} is rich in a large amount of preparations, solved the difficult problem of extensive preparation anatase titania monocrystalline, thereby { 001}, { 010}, { the 101} crystal face can be widely used in different solar energy photocatalytic fields so that highly active anatase octahedrite.
Technical scheme of the present invention is:
Be rich in { 001}/{ 010}/{ 101} crystal face anatase octahedrite TiO a kind of the preparation
2The method of monocrystalline at first, is chosen the titanate with laminate structure of heterogeneity, as the precursor of Hydrothermal Synthesis; Then, presoma is evenly spread in the solution that contains specific reactive solute ion, the volumetric molar concentration of specific reactive solute ion is 0.5mM ~ 3M, and titanate and the ratio that contains between the mass/volume of specific reactive solute solion are 2g/20mL～1g/8000mL; With it with after the reactor sealing, putting into the baking oven Hydrothermal Synthesis processes, Heating temperature is 50 ~ 300 ℃, be 2h ~ 240h heat-up time, collect white depositions after the cooling, with washed with de-ionized water, centrifugal, oven dry, bake out temperature is 50 ~ 120 ℃, obtains being rich in the anatase titania single crystal particle of high reactivity crystal face; Resulting titanium dioxide single crystalline particle, size is controlled, and particle size is 20nm ~ 6 μ m, and { 001}, { 010}, { one or more crystal face ratios of 101} are more than 80%; Wherein, specific reactive solute ion is hydrazine or its hydrate, fluorine-containing acid group salt or oxygen acid root, and the oxygen acid root is the Asia of chlorate anions, sulfate radical, nitrate radical, carbonate, phosphate radical, iodate, borate, oxalate, above-mentioned element, inferior or high acid ion or peroxide acid group.
The selected titanate as precursor has good laminate structure, and the chemical formula of titanate is M
xTi
yO
z, M=H, Li, Na, K, Rb, Cs or Fr; 0＜x, y, z≤15.
In the described solution that contains specific reactive solute ion, the concentration of ammoniacal liquor is 0 ~ 60wt%, and volume grade of alcohol is 0% ~ 95%.
In the described solution that contains specific reactive solute ion, the volumetric molar concentration of specific reactive solute ion is preferably 2mM ~ 100mM, and the concentration of ammoniacal liquor is preferably 10 ~ 30wt%, and volume grade of alcohol is preferably 20% ~ 40%.
During described Hydrothermal Synthesis was processed, Heating temperature was preferably 100 ~ 200 ℃, is preferably 10h ~ 50h heat-up time.
{ 001}/{ 010}/{ 101} crystal face anatase octahedrite TiO is rich in described preparation
2The method of monocrystalline, resulting titanium dioxide single crystalline particle size are preferably 80nm～1 μ m.
The inventive method proposes with the deliquescent titanate of difficulty as precursor, need not any morphology control agent, and { 001}/{ 010}/{ the anatase octahedrite TiO of one or more crystal faces of 101} is rich in preparation
2Single crystal particle, its advantage and beneficial effect are:
1, precursor used in the present invention is easy to preparation, storage, with low cost.
2, the inventive method synthesis window is wide, and equipment is simple, can accomplish scale production.
3, the synthetic high reactivity crystal face gained ratio of the inventive method is large, and quality product is high, and product can be used widely.
4, product of the present invention has the advantages such as surface-area is large, high reaction activity, high reaction preference, is expected extensively and effectively to be applied in the middle of the various photocatalytic applications.
Description of drawings
Fig. 1. particle diameter is at 2 ~ 3 microns { SEM, the TEM of the anatase titania monocrystalline of 010} crystal face and the HRTEM photo of being rich in; Wherein, (a) figure is the SEM photo; (b) figure is the TEM photo.
Fig. 2. particle diameter is at { SEM, the TEM of the anatase titania monocrystalline of 010} crystal face and the HRTEM photo of being rich in of 100 ~ 300 nanometers; Wherein, (a) figure is the SEM photo; (b) figure is the TEM photo.
Fig. 3. particle diameter is at { the SEM photo of the anatase titania monocrystalline of 101} crystal face that is rich in of 100-300 nanometer.
Fig. 4. particle diameter is at { 101} and { the SEM photo of the anatase titania monocrystalline of 010} crystal face of being rich in of 100-300 nanometer.
Fig. 5. particle diameter is at { the TEM photo of the anatase titania monocrystalline of 101} crystal face that is rich in of 30-50 nanometer.
Fig. 6. particle diameter is at { the SEM photo of the anatase titania monocrystalline of 001} crystal face that is rich in of 50 nanometers.
Fig. 7. particle diameter is at { the TEM photo of the anatase titania monocrystalline of 101} crystal face that is rich in of 200 nanometers.
Embodiment
Describe the present invention in detail below in conjunction with embodiment.
Embodiment 1
With 100mg layered titanic acid sodium (Na
2Ti
6O
13) put into the 80mL stainless steel cauldron 40mL deionized water, take tetrafluoroethylene as liner is housed.After the reactor sealing, putting into the baking oven Hydrothermal Synthesis processes, at 160 ℃ of heat treated 24h, collect white depositions, centrifugal and 80 ℃ of oven dry with washed with de-ionized water, be rich in { the anatase titania monocrystalline micron bar of 010} crystal face, the crystal face ratio is higher than 90%, the specification of micron bar is as follows: be about 3 microns, wide about 100-200 nanometer is seen Fig. 1.
Can find out that from Fig. 1 a the gained sample is bar-shaped product, big or small homogeneous; Can analyze from the high-resolution-ration transmission electric-lens photo of Fig. 1 b, this excellent radial side is { 010} crystal face.
Embodiment 2
With 50mg layered titanic acid (H
2Ti
6O
13) put into the 0.6mM Cs that 40mL is housed
2CO
3In the 80mL stainless steel cauldron aqueous solution, take tetrafluoroethylene as liner.After the reactor sealing, putting into the baking oven Hydrothermal Synthesis processes, at 180 ℃ of heat treated 36h, collect white depositions, centrifugal and 80 ℃ of oven dry with washed with de-ionized water, be rich in { the anatase titania monocrystal nano rod of 010} crystal face, the crystal face ratio is higher than 90%, the specification of nanometer rod is as follows: be about 500 nanometers, wide about 20-35 nanometer is seen Fig. 2.
Can find out that from Fig. 2 a the gained sample is bar-shaped product, big or small homogeneous; Can analyze this excellent radial side from the high-resolution-ration transmission electric-lens photo of Fig. 2 b and be { 010} crystal face.
Embodiment 3
With 100mg layered titanic acid (H
2Ti
6O
13) put into the 2.5mM Na that 40mL is housed
3PO
4In the 80mL stainless steel cauldron aqueous solution, take tetrafluoroethylene as liner.After the reactor sealing, putting into the baking oven Hydrothermal Synthesis processes, at 180 ℃ of heat treated 36h, collect white depositions, centrifugal and 80 ℃ of oven dry with washed with de-ionized water, be rich in that { the anatase titania nanometer monocrystalline of 101} crystal face is octahedra, and the crystal face ratio surpasses 90%, the octahedral specification of nanometer is as follows: be about the 400-700 nanometer, see Fig. 3.
As can be seen from Figure 3, sample topography and particle size than homogeneous, long axis direction size 400-700 nanometer, by the anatase titania crystal symmetry as can be known octahedral exposure be { 101} crystal face.
Embodiment 4
With 200mg layered titanic acid (H
2Ti
6O
13) put into the Na that 40mL is housed
2SO
4-ammoniacal liquor-ethanol-water solution (Na
2SO
4Volumetric molar concentration be 10mM, ammoniacal liquor is 20w%, ethanol is 25vol%), in the 80mL stainless steel cauldron take tetrafluoroethylene as liner.After the reactor sealing, putting into the baking oven Hydrothermal Synthesis processes, at 180 ℃ of heat treated 20h, collect white depositions, centrifugal and 80 ℃ of oven dry with washed with de-ionized water, be rich in { 101} and { nanometer that the anatase titania monocrystalline of 010} crystal face elongates is octahedra, and { 101}, { 010} crystal face ratio is about respectively 70% and 30%, the octahedral specification of nanometer is as follows: be about the 200-400 nanometer, see Fig. 4.
As can be seen from Figure 4, sample topography and particle size than homogeneous, long axis direction size 200-400 nanometer, by the anatase titania crystal symmetry as can be known the exposure of monocrystalline be { 101} and { 010} crystal face.
With 500mg layered titanic acid (H
2Ti
6O
13) put into the 20mM N that 40mL is housed
2H
4In the 80mL stainless steel cauldron aqueous solution, take tetrafluoroethylene as liner.After the reactor sealing, putting into the baking oven Hydrothermal Synthesis processes, at 180 ℃ of heat treated 20h, collect white depositions, centrifugal and 80 ℃ of oven dry with washed with de-ionized water, be rich in that { the anatase titania monocrystalline of 101} crystal face is octahedra, and { 101} crystal face ratio is about 90%, the octahedral specification of nanometer is as follows: be about the 30-50 nanometer, see Fig. 5.
As can be seen from Figure 5, sample topography and particle size than homogeneous, long axis direction size 30-50 nanometer, by the anatase titania crystal symmetry as can be known the exposure of monocrystalline be { 101} crystal face.
Embodiment 6
With 500mg layered titanic acid (H
2Ti
6O
13) put into the 80mL stainless steel cauldron 30mM HF aqueous solution, take tetrafluoroethylene as liner that 40mL is housed.After the reactor sealing, putting into the baking oven Hydrothermal Synthesis processes, at 180 ℃ of heat treated 20h, collect white depositions, centrifugal and 80 ℃ of oven dry with washed with de-ionized water, be rich in { the anatase titania single crystal nanoplate of 001} crystal face, { 001} crystal face ratio is about 90%, the about 30-50 nanometer of the nanometer sheet length of side, thickness is seen Fig. 6 less than 20nm.
As can be seen from Figure 6, sample become square laminar, the about 30-50nm of the length of side, thickness is less than 20nm.Its main exposure is { 001} crystal face.
Embodiment 7
With 500mg layered titanic acid (H
2Ti
6O
13) put into the 5mM H that 40mL is housed
2O
2In the 80mL stainless steel cauldron 10mM HCl aqueous solution, take tetrafluoroethylene as liner.After the reactor sealing, putting into the baking oven Hydrothermal Synthesis processes, at 180 ℃ of heat treated 20h, collect white depositions, centrifugal and 80 ℃ of oven dry with washed with de-ionized water, be rich in that { nanometer that the anatase titania monocrystalline of 101} crystal face elongates is octahedra, and { 101} crystal face ratio is about 95%, about 200 nanometers of particle diameter are seen Fig. 7.
As can be seen from Figure 7, sample become square laminar, the about 30-50nm of the length of side, thickness is less than 20nm.Its main exposure is { 101} crystal face.
The result shows, the present invention by Hydrothermal Synthesis wet-chemical process so that layered titanate in solution, decompose, again forming core, be grown to serve as { 001}/{ 010}/{ the anatase titania single crystal particle that one or more crystal faces of 101} are dominant.The method has been opened up the brand-new being rich in { 001}/{ 010}/{ synthetic method of one or more crystal face anatase octahedrites of 101}, { 001}/{ 010}/{ one or more crystal faces of 101} can obtain under more simple condition in a large number so that high reactivity, solved the preparation hard problem, thus can { 001}/{ 010}/{ the anatase titania monocrystalline product of one or more crystal faces of 101} be widely used in the application of photocatalytic degradation pollutent, photolysis water hydrogen, the quick magnificent solar cell of dyestuff and photoreduction carbonic acid gas with being rich in high reactivity.The method is packed precursor into and is contained in the reactor of oxygen acid root solution, through 50 ~ 300 ℃ of heat treated 2h ~ 240h, can obtain { the 001}/{ 010}/{ the titanium dioxide single crystalline particle that one or more crystal faces of 101} are dominant that different-grain diameter distributes.Particle size is 50nm ~ 6 μ m, and { 001}/{ 010}/{ one or more crystal face ratios of 101} are more than 80%.It is large that this product has a surface-area, and the reactive behavior advantages of higher is expected extensively and effectively to be applied in the middle of the various photocatalytic applications.
Claims (6)
1. one kind prepares and is rich in { 001}/{ 010}/{ 101} crystal face anatase octahedrite TiO
2The method of monocrystalline is characterized in that: at first, choose the titanate with laminate structure of heterogeneity, as the precursor of Hydrothermal Synthesis; Then, presoma is evenly spread in the solution that contains specific reactive solute ion, the volumetric molar concentration of specific reactive solute ion is 0.5mM ~ 3M, and titanate and the ratio that contains between the mass/volume of specific reactive solute solion are 2g/20mL ~ 1g/8000mL; With it with after the reactor sealing, putting into the baking oven Hydrothermal Synthesis processes, Heating temperature is 50 ~ 300 ℃, be 2h ~ 240h heat-up time, collect white depositions after the cooling, with washed with de-ionized water, centrifugal, oven dry, bake out temperature is 50 ~ 120 ℃, obtains being rich in the anatase titania single crystal particle of high reactivity crystal face; Resulting titanium dioxide single crystalline particle, size is controlled, and particle size is 20nm ~ 6 μ m, and { 001}, { 010}, { one or more crystal face ratios of 101} are more than 80%; Wherein, specific reactive solute ion is hydrazine or its hydrate, fluorine-containing acid group salt or oxygen acid root, and the oxygen acid root is the Asia of chlorate anions, sulfate radical, nitrate radical, carbonate, phosphate radical, iodate, borate, oxalate, above-mentioned element, inferior or high acid ion or peroxide acid group.
2. be rich in { 001}/{ 010}/{ 101} crystal face anatase octahedrite TiO according to preparation claimed in claim 1
2The method of monocrystalline is characterized in that: the selected titanate as precursor has good laminate structure, and the chemical formula of titanate is M
xTi
yO
z, M=H, Li, Na, K, Rb, Cs or Fr; 0＜x, y, z≤15.
3. be rich in { 001}/{ 010}/{ 101} crystal face anatase octahedrite TiO according to preparation claimed in claim 1
2The method of monocrystalline is characterized in that: in the described solution that contains specific reactive solute ion, the concentration of ammoniacal liquor is 0 ~ 60wt%, and volume grade of alcohol is 0% ~ 95%.
4. be rich in { 010}/{ 101} crystal face anatase octahedrite TiO according to preparation claimed in claim 1
2The method of monocrystalline is characterized in that: in the described solution that contains specific reactive solute ion, the volumetric molar concentration of specific reactive solute ion is preferably 2mM ~ 100mM, and the concentration of ammoniacal liquor is preferably 10 ~ 30w%, and volume grade of alcohol is preferably 20%～40%.
5. be rich in { 001}/{ 010}/{ 101} crystal face anatase octahedrite TiO according to preparation claimed in claim 1
2The method of monocrystalline is characterized in that: during described Hydrothermal Synthesis was processed, Heating temperature was preferably 100 ~ 200 ℃, is preferably 10h ~ 50h heat-up time.
6. be rich in { 001}/{ 010}/{ 101} crystal face anatase octahedrite TiO according to preparation claimed in claim 1
2The method of monocrystalline is characterized in that: resulting titanium dioxide single crystalline particle size is preferably 80nm ~ 1 μ m.
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Cited By (9)
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| CN103626225A (en) * | 2013-10-25 | 2014-03-12 | 河南大学 | Anatase titanium dioxide nanocrystal containing single-electron-trapped oxygen vacancies and with exposed {001} face and preparation method thereof |
| CN104478656B (en) * | 2014-11-26 | 2016-02-10 | 广西大学 | A kind of method of carbon dioxide reduction |
| WO2016026340A1 (en) * | 2014-08-20 | 2016-02-25 | 北京师范大学 | Tio2 nanocrystal and synthesis method therefor |
| WO2016026339A1 (en) * | 2014-08-20 | 2016-02-25 | 北京师范大学 | Synthesis method for tio2 nanocrystal |
| WO2018040685A1 (en) * | 2016-09-05 | 2018-03-08 | 中国科学院金属研究所 | Method for directionally constructing heterostructure by selectively etching ferroelectric-based photocatalytic material |
| CN107889471A (en) * | 2015-06-12 | 2018-04-06 | 朱马国际公司 | A kind of photocatalytic particle comprising TiO2 and preparation method thereof |
| CN111850653A (en) * | 2020-06-23 | 2020-10-30 | 清华大学 | Method and system for preparing titanium dioxide with exposed high-activity surface by using femtosecond laser |
| CN115814785A (en) * | 2022-11-18 | 2023-03-21 | 同济大学 | TiO heterojunction with visible light response nano Au modified crystal face 2 Photoelectrode, construction and application thereof |
| CN115814785B (en) * | 2022-11-18 | 2024-04-26 | 同济大学 | TiO (TiO) with visible light response nano Au modified crystal face heterojunction2Photoelectrode, construction and application thereof |
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| CN103626225A (en) * | 2013-10-25 | 2014-03-12 | 河南大学 | Anatase titanium dioxide nanocrystal containing single-electron-trapped oxygen vacancies and with exposed {001} face and preparation method thereof |
| CN103626225B (en) * | 2013-10-25 | 2015-08-26 | 河南大学 | A kind of expose that { 001} face anatase titania is nanocrystalline and preparation method thereof containing constraint single electron Lacking oxygen |
| WO2016026340A1 (en) * | 2014-08-20 | 2016-02-25 | 北京师范大学 | Tio2 nanocrystal and synthesis method therefor |
| WO2016026339A1 (en) * | 2014-08-20 | 2016-02-25 | 北京师范大学 | Synthesis method for tio2 nanocrystal |
| CN104478656B (en) * | 2014-11-26 | 2016-02-10 | 广西大学 | A kind of method of carbon dioxide reduction |
| CN107889471A (en) * | 2015-06-12 | 2018-04-06 | 朱马国际公司 | A kind of photocatalytic particle comprising TiO2 and preparation method thereof |
| CN107889471B (en) * | 2015-06-12 | 2021-04-16 | 蒂奥泰克公司 | Photocatalytic particle containing TiO2 and preparation method thereof |
| WO2018040685A1 (en) * | 2016-09-05 | 2018-03-08 | 中国科学院金属研究所 | Method for directionally constructing heterostructure by selectively etching ferroelectric-based photocatalytic material |
| CN111850653A (en) * | 2020-06-23 | 2020-10-30 | 清华大学 | Method and system for preparing titanium dioxide with exposed high-activity surface by using femtosecond laser |
| CN115814785A (en) * | 2022-11-18 | 2023-03-21 | 同济大学 | TiO heterojunction with visible light response nano Au modified crystal face 2 Photoelectrode, construction and application thereof |
| CN115814785B (en) * | 2022-11-18 | 2024-04-26 | 同济大学 | TiO (TiO) with visible light response nano Au modified crystal face heterojunction2Photoelectrode, construction and application thereof |
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