CN108636398B - Preparation method of vanadium-doped strontium titanate nano photocatalytic material - Google Patents
Preparation method of vanadium-doped strontium titanate nano photocatalytic material Download PDFInfo
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- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 23
- 239000000463 material Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims description 14
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 9
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 8
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 4
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- 239000003814 drug Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- 239000000725 suspension Substances 0.000 claims description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 6
- 229910002367 SrTiO Inorganic materials 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 238000011156 evaluation Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 10
- 229910052720 vanadium Inorganic materials 0.000 abstract description 10
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 abstract description 9
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract description 6
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 abstract description 6
- 150000001875 compounds Chemical class 0.000 abstract description 4
- 230000007246 mechanism Effects 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 239000010936 titanium Substances 0.000 abstract 1
- 230000007547 defect Effects 0.000 description 8
- 229910002370 SrTiO3 Inorganic materials 0.000 description 7
- 238000011160 research Methods 0.000 description 6
- 239000011941 photocatalyst Substances 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 150000001768 cations Chemical class 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 230000000704 physical effect Effects 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000001362 electron spin resonance spectrum Methods 0.000 description 2
- 230000004298 light response Effects 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 2
- 229910002902 BiFeO3 Inorganic materials 0.000 description 1
- 229910002971 CaTiO3 Inorganic materials 0.000 description 1
- 229910020470 K2Ti4O9 Inorganic materials 0.000 description 1
- 229910003781 PbTiO3 Inorganic materials 0.000 description 1
- 229910020698 PbZrO3 Inorganic materials 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 125000002572 propoxy group Chemical group [*]OC([H])([H])C(C([H])([H])[H])([H])[H] 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 229910000018 strontium carbonate Inorganic materials 0.000 description 1
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Inorganic materials [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical class [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 description 1
- 229910001456 vanadium ion Inorganic materials 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/20—Vanadium, niobium or tantalum
- B01J23/22—Vanadium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
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- Chemical & Material Sciences (AREA)
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention provides a method for preparing vanadium-doped strontium titanate nano photocatalytic material, which is based on the principle of hydro-thermal synthesis of compounds and comprises the steps of mixing a titanium source and a strontium source required by strontium titanate synthesis and a vanadium source required by doping, reacting for several hours under the condition of high temperature, and finally growing into vanadium-doped strontium titanate. The method has the characteristics of few raw material types, simple and convenient operation method, simple process, low cost, environmental protection and the like, and the prepared vanadium-doped strontium titanate photocatalytic material has important significance for researching the photoresponse photocatalytic mechanism and preparing other perovskite photocatalytic materials.
Description
Technical Field
The invention belongs to the technical field of photocatalytic nano material preparation and environmental pollutant treatment, and particularly relates to a preparation method and application of metal vanadium ion doped strontium titanate.
Background
In 1972, Japanese scientists Fujishima and Honda utilized TiO2The experiment of electrode photocatalytic water splitting opens the search for semiconductor oxides as photocatalysts. Then TiO2Then, it was found to have d0Titanates, niobates, tantalates in electronic configuration and having d in the p-region10The photocatalyst with electronic configuration has certain advantages in the aspect of visible light response, wherein titanate with perovskite structure is used as a semiconductor oxide light functional material, and becomes one of the key points of research in the field of photocatalysis for nearly more than ten years.
The perovskite has proper forbidden band width, stable crystal structure and high thermal stability, and has certain physical property and solid chemical propertyThe advantages of the base and the like are concerned in the field of photocatalysis. Perovskite-type metal oxides can be used of the general formula ABO3Or AA 'BB' O3-xThe latter indicates that impurity ions A 'and B' are substituted and doped at the A-position or the B-position, and x indicates the oxygen defect rate caused by doping elements with different valence states to maintain overall electrical neutrality. As shown in fig. 1, the perovskite-type composite is ideally of a cubic symmetry structure, and the a site of the perovskite is generally a metal cation with a large radius, such as an alkali metal, an alkaline earth metal, a rare earth metal, and the like, for example, Ba, Ca, Sr, and the like. The A-site ions do not directly participate in chemical reaction, and structurally have certain influence on the valence state of the B ions except for the functions of regulating B-O bonds and stabilizing the whole perovskite structure; the B position is generally metal cation with smaller radius such as transition metal element, such as W, Mo, Sb, etc., and is positioned in the center of octahedron composed of 6O atoms to form a structure with TiO2Similar BO6The structure is the photocatalytic activity center of the perovskite compound. The elements commonly used for B-site doping are Co, Fe, Ni, Cr, etc. Due to the interaction among atoms, slight buckling can cause lattice distortion, so that the symmetry of the structure is reduced, and the abundant electrical property, magnetism, dielectric property and the like of the perovskite also depend on the lattice distortion to a great extent, so that the substitution doping of cations can be used for fine adjustment of the physical properties of the perovskite.
SrTiO3And CaTiO3The perovskite photocatalyst is the first concerned, and in addition, some layered perovskite structure titanates, such as: na (Na)2Ti3O7、K2Ti2O5、K2Ti4O9、Cs2Ti5O11、Cs2Ti6O13And the like also have better photocatalytic activity under ultraviolet light.
At present, the most studied and applied field of perovskite-type compounds is solar cells, and great progress has been made in recent years. For example, the photoelectric conversion efficiency of the metal-halide perovskite photovoltaic cell is improved from 3% to more than 20%; perovskite type composites such as PbZrO3、BaTiO3、PbTiO3Etc. are widely used for piezoelectric composite materialsFeeding; BiFeO3Exhibit good multiferroic properties. In addition, metal oxides having a perovskite structure, such as titanates, tantalates, vanadates, niobates, and the like, have been widely used in the field of photocatalysts because they have been found to have a suitable energy gap and good light-responsive properties.
The perovskite-type oxide has the following advantages as a photocatalyst. The perovskite has various composition elements but similar basic structure, and past research on the perovskite provides a research basis for physical properties and solid chemical properties of the perovskite and provides a guiding function for the application of the perovskite; the good crystal form of the perovskite is beneficial to the characterization of a bulk phase structure and the surface performance of the perovskite is also beneficial to the deduction of the bulk phase structure, and because catalytic reaction mostly occurs on the surface of the catalyst, the mastering of the surface performance of the catalyst is very key to the analysis of a reaction mechanism; in addition, due to the diversity of elements and doping elements which form the perovskite, the valence, the stoichiometric ratio and the defect density of different perovskite composition elements have a plurality of differences, and the microstructure of the material has great adjustability.
Whether SrTiO3And simple perovskites with similar structures and more complex layered perovskites, an important problem to be solved in the research process is the controllable preparation of perovskite nano materials. If the perovskite can be properly subjected to band shearing and controlled synthesis, the method is an extremely important breakthrough for performing functional modification on the perovskite. Furthermore, the research on the photocatalytic mechanism of perovskite, such as electron transfer path, surface active group, etc., is far less advanced than that of TiO2Therefore, more intensive research is needed in aspects of morphology regulation, energy band tailoring and photocatalytic mechanism, and more theoretical support is provided for the photocatalytic behavior of perovskite.
Disclosure of Invention
Aiming at the problems in the prior art, the technical scheme adopted by the invention for solving the problems in the prior art is as follows:
a preparation method of a vanadium-doped strontium titanate nano photocatalytic material is characterized by comprising the following steps:
step 2, dropwise adding (C) into the solution obtained in the step 13H7O)4Ti is added and stirred to obtain a white suspension system which is dispersed as much as possible;
step 3, weighing a certain amount of V according to the preset doping amount2O5Adding the mixed system obtained in the step 2, fully stirring, and then adding a certain amount of NaOH;
step 4, sufficiently dissolving the traditional Chinese medicine in the step 3 by using an ultrasonic dispersion instrument, transferring the solution into a hydrothermal reaction kettle, and carrying out heat preservation reaction at 200 ℃ for 24 hours;
step 5, the SrTiO obtained in the step 33Washing off small amounts of SrCO with a 1% dilute nitric acid solution3Then washing with deionized water, and drying at 80 ℃ for later use to obtain yellow solid powder, namely the vanadium-doped strontium titanate.
The molar ratio of the elements Sr and Ti in the steps 1 and 2 is more than 1:1 so as to avoid TiO2The formation of the phases results in an impact on the evaluation of the material properties.
In said step 2 (C)3H7O)4The density of the Ti solution was ρ 0.9600 g/mL.
V in said step 32O5The weighed mass is determined by calculating the proportion of the doped V in the V-SrTiO 3.
The molar mass of NaOH in the step 3 is Sr (NO) in the step 13)2Twice the amount of material.
The concentration of NaOH in the step 3 is 0.5mol/L, and NaOH in Sr (NO) in the step 33)2、(C3H7O)4Ti and V2O5Then adding the alkali liquor to reduce CO in the air as much as possible2To reduce SrCO3And (4) generating.
The invention has the following advantages:
1. the method is simple, the preparation cost is low, the reaction temperature is low compared with a high-temperature molten salt method, and the obtained strontium titanate particles are smaller compared with a common hydrothermal synthesis method;
2. the prepared vanadium-doped strontium titanate has stronger visible light response capability and lower defect density, so that the strontium titanate material has wider application in the fields of solar cells and photocatalysis;
3. in the aspect of morphology regulation: spherical particles with the granularity of about 45nm and the stacking size of 50-250nm can be prepared more stably; the defect density is reduced;
4. in terms of band regulation: and impurity energy level is introduced to enhance the corresponding performance of visible light.
Drawings
FIG. 1 is ABO3Structural diagram of perovskite type;
FIG. 2 is an XRD pattern of pure phase and strontium vanadium-doped titanate obtained from examples 1, 2 and 3;
FIG. 3 is a scanning electron micrograph of the pure phase (a-b) and the vanadium-doped strontium titanate of 0.5% (c-d) and 1.0% (e-f) obtained in examples 1, 2 and 3, respectively;
FIG. 4 shows EPR spectra of pure phase and strontium vanadium-doped titanate obtained in examples 1, 2 and 3;
FIG. 5 is a UV-VIS absorption spectrum of pure phase and strontium vanadium-doped titanate obtained in examples 1, 2 and 3;
FIG. 6 is a calculated graph of the forbidden band widths of pure phase and strontium titanate doped with vanadium obtained in examples 1, 2 and 3;
s-0, S-0.5 and S-1.0 respectively represent strontium vanadium-doped titanate with V doping amounts of 0, 0.5 mol% and 1.0 mol%.
Detailed Description
The technical scheme of the invention is further concretely explained by the embodiment and the attached drawings,
example 1
1. 2.11g (0.01mol) Sr (NO) are weighed3)2Dissolving in 20ml deionized water, and stirring until completely dissolving;
2. to the solution obtained in a, 2.8ml (C) was added dropwise3H7O)4Ti (ρ 0.9600g/mL) was added thereto and stirred to obtain a white suspension system dispersed as much as possible;
3. immediately adding 0.8g of NaOH into the mixed system obtained in the step b, and fixing the volume to 40ml (the concentration of the NaOH is 0.5 mol/L);
4. fully dissolving the traditional Chinese medicine c by using an ultrasonic dispersion instrument, transferring the solution into a 50ml hydrothermal reaction kettle, and carrying out heat preservation reaction at 200 ℃ for 24 hours;
5. the obtained SrTiO3Washing off small amounts of SrCO with a 1% dilute nitric acid solution3Then washing with deionized water, drying at 80 ℃ for later use, and obtaining white solid powder which is undoped pure-phase strontium titanate.
Example 2
1. 2.11g (0.01mol) Sr (NO) are weighed3)2Dissolving in 20ml deionized water, and stirring until completely dissolving;
2. to the solution obtained in a, 2.8ml (C) was added dropwise3H7O)4Ti (ρ 0.9600g/mL) was added thereto and stirred to obtain a white suspension system dispersed as much as possible;
3. 0.0045g of V2O5Adding the mixed system obtained in the step b, fully stirring, then adding 0.8g of NaOH, and fixing the volume to 40ml (the concentration of the NaOH is 0.5 mol/L);
4. fully dissolving the traditional Chinese medicine c by using an ultrasonic dispersion instrument, transferring the solution into a 50ml hydrothermal reaction kettle, and carrying out heat preservation reaction at 200 ℃ for 24 hours;
5. the obtained SrTiO3Washing off small amounts of SrCO with a 1% dilute nitric acid solution3Then washing with deionized water, and drying at 80 ℃ for later use to obtain yellow solid powder, namely the vanadium-doped strontium titanate with the doping amount of 0.5 mol%.
Example 3
1. 2.11g (0.01mol) Sr (NO) are weighed3)2Dissolving in 20ml deionized water, and stirring until completely dissolving;
2. to the solution obtained in a, 2.8ml (C) was added dropwise3H7O)4Ti (ρ 0.9600g/mL) was added thereto and stirred to obtain a white suspension system dispersed as much as possible;
3. 0.0091g of V was added2O5Adding the mixed system obtained in the step b while fully stirring, then adding 0.8g of NaOH, and fixing the volume to 40ml (the concentration of the NaOH is 0.5 mo)l/L)；
4. Fully dissolving the traditional Chinese medicine c by using an ultrasonic dispersion instrument, transferring the solution into a 50ml hydrothermal reaction kettle, and carrying out heat preservation reaction at 200 ℃ for 24 hours;
5. the obtained SrTiO3Washing off small amounts of SrCO with a 1% dilute nitric acid solution3Then washing with deionized water, and drying at 80 ℃ for later use to obtain yellow solid powder, namely the vanadium-doped strontium titanate with the doping amount of 1.0 mol%.
A series of tests were performed on examples 1-3, and the results are shown in FIGS. 2-6:
FIG. 2 is an XRD pattern of pure phase and vanadium-doped strontium titanate obtained in examples 1, 2 and 3 of the present invention, the data is collected by a German Bruker D8X-ray diffractometer, and it can be seen from the figure that the vanadium-doped strontium titanate prepared by the method of the present invention is a single compound with good crystallinity and uniform chemical composition and structure;
FIG. 3 is a scanning electron micrograph of the pure phase (a-b) and the vanadium-doped strontium titanate of 0.5% (c-d) and 1.0% (e-f) obtained in examples 1, 2 and 3 of the present invention, respectively, and it can be seen that the strontium titanate of 1.0% (e-f) doped with vanadium has a uniform size and good dispersibility;
FIG. 4 is EPR spectra of pure phase and strontium vanadium-doped titanates obtained in examples 1, 2 and 3 of the present invention, the peak at g-2.003 is caused by one-electron oxygen vacancy, and the peak at g-1.976 is Ti3+Signal peak of (1), oxygen vacancy after V doping and Ti3+The EPR signal is weakened, which shows that the defect density is reduced by doping vanadium;
FIGS. 5 and 6 are the UV-VIS absorption spectra and forbidden band width calculations of pure phase and vanadium-doped strontium titanate obtained in examples 1, 2 and 3 of the present invention, and it can be seen from the figures that vanadium doping makes SrTiO3The absorption edge of the material has obvious red shift, which shows that the vanadium doping can enhance the absorption performance of the sample on visible light, but the forbidden bandwidth of the material is not obviously changed by the vanadium doping from the view of FIG. 6; oxygen defect and Ti after doping with vanadium3+The defect density is reduced, which shows that the improvement of visible light absorption by doping vanadium is not caused by defects, but rather by introducing impurity energy level into vanadium.
The preparation method of the invention is also suitable for doping other elements in the same subgroup as the V element, such as example 4:
1. 2.11g (0.01mol) Sr (NO) are weighed3)2Dissolving in 20ml deionized water, and stirring until completely dissolving;
2. to the solution obtained in a, 2.8ml (C) was added dropwise3H7O)4Ti (ρ 0.9600g/mL) was added thereto and stirred to obtain a white suspension system dispersed as much as possible;
3. nb of 0.0133 is added2O5Adding the mixed system obtained in the step b, fully stirring, then adding 0.8g of NaOH, and fixing the volume to 40ml (the concentration of the NaOH is 0.5 mol/L);
4. fully dissolving the traditional Chinese medicine c by using an ultrasonic dispersion instrument, transferring the solution into a 50ml hydrothermal reaction kettle, and carrying out heat preservation reaction at 200 ℃ for 24 hours;
5. the obtained SrTiO3Washing off small amounts of SrCO with a 1% dilute nitric acid solution3Then washing with deionized water, and drying at 80 ℃ for later use to obtain white solid powder, namely the niobium-doped strontium titanate with the doping amount of 1.0 mol%.
The protective scope of the present invention is not limited to the above-described embodiments, and it is apparent that various modifications and variations can be made to the present invention by those skilled in the art without departing from the scope and spirit of the present invention. It is intended that the present invention cover the modifications and variations of this invention provided they come within the scope of the appended claims and their equivalents.
Claims (6)
1. A preparation method of a vanadium-doped strontium titanate nano photocatalytic material is characterized by comprising the following steps:
step 1, weighing a certain amount of Sr (NO)3)2Dissolving in deionized water, and stirring to dissolve completely;
step 2, dropwise adding (C) into the solution obtained in the step 13H7O)4Ti is added and stirred to obtain a white suspension system which is dispersed as much as possible;
step 3, weighing a certain amount of V according to the preset doping amount2O5Adding the mixed system obtained in the step 2 while sufficiently stirring, and thenThen adding a certain amount of NaOH solution;
step 4, sufficiently dissolving the traditional Chinese medicine in the step 3 by using an ultrasonic dispersion instrument, transferring the solution into a hydrothermal reaction kettle, and carrying out heat preservation reaction at 200 ℃ for 24 hours;
step 5, the SrTiO obtained in the step 33Washing off small amounts of SrCO with a 1% dilute nitric acid solution3Then washing with deionized water, and drying at 80 ℃ for later use to obtain yellow solid powder, namely the vanadium-doped strontium titanate.
2. The preparation method of the vanadium-doped strontium titanate nano photocatalytic material according to claim 1, characterized by comprising the following steps: the molar ratio of the elements Sr and Ti in the steps 1 and 2 is more than 1:1 so as to avoid TiO2The formation of the phases results in an impact on the evaluation of the material properties.
3. The preparation method of the vanadium-doped strontium titanate nano photocatalytic material according to claim 1, characterized by comprising the following steps: (C) added dropwise in the step 23H7O)4The density of the Ti solution was ρ 0.9600 g/mL.
4. The preparation method of the vanadium-doped strontium titanate nano photocatalytic material according to claim 1, characterized by comprising the following steps: v in said step 32O5The weight is measured according to the V is in V-SrTiO after doping3The proportion of (B) is determined after calculation.
5. The preparation method of the vanadium-doped strontium titanate nano photocatalytic material according to claim 1, characterized by comprising the following steps: the amount of NaOH substance in the step 3 is Sr (NO) in the step 13)2Twice the amount of material.
6. The preparation method of the vanadium-doped strontium titanate nano photocatalytic material according to claim 1, characterized by comprising the following steps: after a certain amount of NaOH solution is added in the step 3, the concentration of NaOH in the mixed system is 0.5 mol/L.
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