CN108636398A - A kind of preparation method of vanadium doping strontium titanates nano-photocatalyst material - Google Patents
A kind of preparation method of vanadium doping strontium titanates nano-photocatalyst material Download PDFInfo
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- CN108636398A CN108636398A CN201810549430.7A CN201810549430A CN108636398A CN 108636398 A CN108636398 A CN 108636398A CN 201810549430 A CN201810549430 A CN 201810549430A CN 108636398 A CN108636398 A CN 108636398A
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- strontium titanates
- vanadium
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- photocatalyst material
- vanadium doping
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- 229910052712 strontium Inorganic materials 0.000 title claims abstract description 23
- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 23
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 23
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 239000000463 material Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 10
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 8
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 47
- 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
- 229910002367 SrTiO Inorganic materials 0.000 claims description 6
- 239000003814 drug Substances 0.000 claims description 6
- 229940079593 drug Drugs 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910002370 SrTiO3 Inorganic materials 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000012360 testing method Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 2
- 239000010936 titanium Substances 0.000 abstract description 14
- VIIJTIRNANJGHH-UHFFFAOYSA-N strontium vanadium Chemical compound [V].[Sr] VIIJTIRNANJGHH-UHFFFAOYSA-N 0.000 abstract description 13
- 238000002156 mixing Methods 0.000 abstract description 12
- 230000001699 photocatalysis Effects 0.000 abstract description 9
- 238000000034 method Methods 0.000 abstract description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract description 6
- 150000001875 compounds Chemical class 0.000 abstract description 6
- 238000006555 catalytic reaction Methods 0.000 abstract description 4
- 230000007246 mechanism Effects 0.000 abstract description 4
- 229910052788 barium Inorganic materials 0.000 abstract description 2
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 abstract 1
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000011017 operating method Methods 0.000 abstract 1
- 230000001681 protective effect Effects 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 230000007547 defect Effects 0.000 description 8
- 239000003054 catalyst Substances 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- 238000011160 research Methods 0.000 description 7
- 230000008901 benefit Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- 239000003643 water by type Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 150000001768 cations Chemical class 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- -1 PbZrO3 Chemical class 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 230000000877 morphologic effect Effects 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 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
- 229910020293 Na2Ti3O7 Inorganic materials 0.000 description 1
- 229910003781 PbTiO3 Inorganic materials 0.000 description 1
- 229910020698 PbZrO3 Inorganic materials 0.000 description 1
- 230000010748 Photoabsorption Effects 0.000 description 1
- JTCFNJXQEFODHE-UHFFFAOYSA-N [Ca].[Ti] Chemical compound [Ca].[Ti] JTCFNJXQEFODHE-UHFFFAOYSA-N 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 239000002253 acid 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
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 125000002572 propoxy group Chemical group [*]OC([H])([H])C(C([H])([H])[H])([H])[H] 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 229910000018 strontium carbonate Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer 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 compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 description 1
- 229910001456 vanadium ion Inorganic materials 0.000 description 1
- IBYSTTGVDIFUAY-UHFFFAOYSA-N vanadium monoxide Chemical compound [V]=O IBYSTTGVDIFUAY-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
-
- B01J35/39—
-
- B01J35/40—
Abstract
The invention discloses a kind of preparation methods of vanadium doping strontium titanates nano-photocatalyst material for present invention offer, principle of this method based on hydrothermal synthesis compound, it include the mixing as titanium source and barium source and the required vanadium source of doping needed for synthesis strontium titanates, it reacts under the high temperature conditions again a few hours, finally grows into and mix vanadium strontium titanates.This method has raw material type few, operating method is easy, and simple process and low cost is honest and clean, the features such as environmentally protective, prepared mixes vanadium strontium titanates catalysis material for studying its photoresponse photocatalytic mechanism and having great significance for the preparation of other perovskite catalysis materials.
Description
Technical field
The invention belongs to photocatalysis nano materials to prepare and environmental contaminants processing technology field, and in particular to a kind of metal
The preparation method and application of vanadium ion strontium titanate doping.
Background technology
Japanese Scientists Fujishima and Honda utilize TiO within 19722The experiment of electrode photochemical catalyzing opens
Research of the conductor oxidate as photochemical catalyst.After TiO2Later, it has been found that there is d0Titanate, the niobic acid of electron configuration
Salt, tantalates and be in the areas p have d10The photochemical catalyst of electron configuration has certain advantage at visible light-responded aspect,
In the titanate with perovskite structure as a kind of conductor oxidate optical function material, become photocatalysis over the past decade and lead
One of the emphasis of domain research.
For perovskite because stablizing with suitable energy gap, crystal structure, thermal stability is high and has certain physical
The advantages such as the Research foundation of matter and solid state chemistry property attract attention in photocatalysis field.Perovskite type metal oxide is available
General formula ABO3Or AA ' BB ' O3-xThe case where expression, the latter indicates foreign ion A ', B ' carry out A or B substitute dopings, x tables
Show oxygen defect rate caused by being the whole electroneutral of holding due to different valence state element doping.As shown in Figure 1, ideal calcium titanium
Mine type compound is cubic symmetry type structure, and the location A of perovskite is usually the radiuses such as alkali metal, alkaline-earth metal, rare earth metal
Larger metal cation, such as Ba, Ca, Sr.A ions do not participate in chemical reaction directly, in structure except adjust B-O keys,
Outside the effect for stablizing entire perovskite structure, have a certain impact to B ionic valence conditions；B location is usually transition metal element etc.
The smaller metal cation of radius, such as W, Mo, Sb, in the octahedron center of 6 O atom compositions, composition and TiO2It is similar
BO6Structure is the photocatalytic activity center of perovskite compound.The member for being generally used for B doping is known as Co, Fe, Ni, Cr
Deng.Due to interatomic interaction, slight buckling can cause distortion of lattice so that the symmetry of its structure reduces, and calcium
Abundant electrical, the magnetic and dielectric properties etc. of titanium ore also heavily depend on distortion of lattice, therefore the substitution of cation
Doping can be used for the fine tuning of perovskite physical property.
SrTiO3And CaTiO3It is the perovskite photochemical catalyst being concerned earliest, in addition also has some laminated perovskites
The titanate of structure, such as：Na2Ti3O7、K2Ti2O5、K2Ti4O9、Cs2Ti5O11、Cs2Ti6O13Also have Deng under ultraviolet light preferable
Photocatalytic activity.
Currently, perovskite-type compounds research and the most field of application are solar cells, and achieved in recent years
Larger progress.Such as the photronic electricity conversion of metal-halide perovskite is promoted from 3% to 20% or more；Calcium titanium
Mine type compound such as PbZrO3、BaTiO3、PbTiO3Deng by more applied to piezo-electricity composite material；BiFeO3It shows good
Multi-ferrum property.In addition, titanate, tantalates, vanadate, niobates etc. have the metal oxide of perovskite structure because being sent out
Now there is suitable energy gap and good photo absorption property and be widely used in photochemical catalyst field.
Perofskite type oxide has the advantage that as photochemical catalyst.The component of perovskite is various, but basic
Structure is similar, and the past provides its physical property and solid state chemistry property Research foundation about the research of perovskite, is perovskite
Application provide directive function；The good crystal form of perovskite is conducive to the characterization of bulk structure, is also beneficial to push away from bulk structure
Know its surface property, because catalysis reaction mostly occurs in catalyst surface, thus it is anti-for analyzing to grasp catalyst surface property
Answer mechanism extremely crucial；The diversity of element and doped chemical additionally, due to composition perovskite itself, different perovskite groups
At the valence state of element, stoichiometric ratio and defect concentration there is also many differences, the microfabricated tunable of material is big.
Either SrTiO3And simple perovskite with similar structure or increasingly complex laminated perovskite, it is grinding
A major issue to be solved is exactly the controllable preparation of perovskite nano material during studying carefully.If can realize suitable to perovskite
Local energy band tailoring simultaneously controllably synthesizes, this will be the extremely important breakthrough that functional modification is carried out to perovskite.Furthermore just
Be in terms of the photocatalytic mechanism for perovskite, such as electronics transfer path, the depth of investigation of surface active groups etc. much
Not as good as TiO2, thus Morphological control, energy band cut and photocatalytic mechanism in terms of need deeper into research, be perovskite light
Catalysis behavior provides more theory supports.
Invention content
In view of the problems of the existing technology, the present invention is the technical solution for solving problems of the prior art and using
It is as follows：
A kind of preparation method of vanadium doping strontium titanates nano-photocatalyst material, which is characterized in that include the following steps：
Step 1 weighs a certain amount of Sr (NO3)2It is dissolved in deionized water, stirring is to being completely dissolved；
(C is added dropwise in step 2, the solution obtained to step 13H7O)4Ti is stirred while adding, and is divided as far as possible
The scattered suspended liquid system of white；
Step 3 weighs a certain amount of V by scheduled doping2O5The mixed system obtained by step 2 is added, while fully stirring
It mixes, then adds a certain amount of NaOH；
Step 4 is transferred to after fully being dissolved drug in step 3 using ultrasonic disperse instrument in hydrothermal reaction kettle, at 200 DEG C
Insulation reaction is for 24 hours；
Step 5, the SrTiO that will be obtained in step 33A small amount of SrCO is washed away with 1% dilute nitric acid solution3, then spend from
Sub- water washing, 80 DEG C are dried for standby, and obtained yellow solid powder is vanadium doping strontium titanates.
Elements Sr and Ti molar ratios are more than 1 in the step 1 and 2:1, to avoid because of TiO2The generation of phase and cause to material
Expect the influence of performance measuring and evaluating.
(C in the step 23H7O)4The density of Ti solution is ρ=0.9600g/mL.
V in the step 32O5Weigh after quality is calculated according to shared ratios of the V after doping in V-SrTiO3 really
It is fixed.
The molal weight of NaOH is Sr (NO in step 1 in the step 33)2Twice of the amount of substance.
A concentration of 0.5mol/L of NaOH in the step 3, in step 3, NaOH is in Sr (NO3)2、(C3H7O)4Ti and V2O5
It is added later to reduce lye to the greatest extent to the CO in air2Absorption to reduce SrCO3Generation.
The invention has the advantages that：
1, this method is simple, and manufacturing cost is cheap, and compared with high-temperature molten salt method, reaction temperature is low, with common hydrothermal synthesis
Method is compared, the strontium titanates particle smaller of acquisition；
2, vanadium strontium titanates obtained of mixing has stronger visible light-responded ability, lower defect concentration so that strontium titanates
Material has widely application in solar cell, photocatalysis field；
3, in terms of Morphological control：Granularity can be prepared relatively stablely in 45nm or so, stack size is in 50-250nm
Between spheroidal particle；Reduce defect concentration；
4, in terms of band engineering：Impurity energy level is introduced, visible light respective performances are enhanced.
Description of the drawings
Fig. 1 is ABO3Type perovskite structure figure；
Fig. 2 is the pure phase and the XRD spectrum for mixing vanadium strontium titanates that embodiment 1,2,3 obtains；
Fig. 3 is the obtained pure phase (a-b) of embodiment 1,2,3 and to mix vanadium amount be respectively 0.5% (c-d) and 1.0% (e-
F) scanning electron microscope (SEM) photograph of strontium titanates；
Fig. 4 is the pure phase and the EPR collection of illustrative plates for mixing vanadium strontium titanates that embodiment 1,2,3 obtains；
Fig. 5 is the pure phase and the uv-visible absorption spectra for mixing vanadium strontium titanates that embodiment 1,2,3 obtains；
Fig. 6 is the pure phase and the energy gap calculating figure for mixing vanadium strontium titanates that embodiment 1,2,3 obtains；
S-0, S-0.5, S-1.0 respectively represent V dopings and mix vanadium strontium titanates for 0,0.5mol%, 1.0mol%.
Specific implementation mode
Below with reference to the embodiments and with reference to the accompanying drawing the technical solutions of the present invention will be further described,
Embodiment 1
1,2.11g (0.01mol) Sr (NO are weighed3)2It is dissolved in 20ml deionized waters, stirring is to being completely dissolved；
2,2.8ml (C are added dropwise in the solution obtained to a3H7O)4Ti (ρ=0.9600g/mL), stirs while adding,
The suspended liquid system of white disperseed as far as possible；
3,0.8g NaOH are added to the mixed system obtained by b at once, are settled to 40ml (a concentration of 0.5mol/ of NaOH
L)；
4, it is transferred to after fully being dissolved drug in c using ultrasonic disperse instrument in 50ml hydrothermal reaction kettles, is kept the temperature at 200 DEG C
Reaction is for 24 hours；
5, the SrTiO obtained3A small amount of SrCO is washed away with 1% dilute nitric acid solution3, then it is washed with deionized, 80 DEG C
It is dried for standby, obtained white solid powder is undoped pure phase strontium titanates.
Embodiment 2
1,2.11g (0.01mol) Sr (NO are weighed3)2It is dissolved in 20ml deionized waters, stirring is to being completely dissolved；
2,2.8ml (C are added dropwise in the solution obtained to a3H7O)4Ti (ρ=0.9600g/mL), stirs while adding,
The suspended liquid system of white disperseed as far as possible；
3, by the V of 0.0045g2O5The mixed system obtained by b is added, is sufficiently stirred simultaneously, then adds 0.8g NaOH,
It is settled to 40ml (a concentration of 0.5mol/L of NaOH)；
4, it is transferred to after fully being dissolved drug in c using ultrasonic disperse instrument in 50ml hydrothermal reaction kettles, is kept the temperature at 200 DEG C
Reaction is for 24 hours；
5, the SrTiO obtained3A small amount of SrCO is washed away with 1% dilute nitric acid solution3, then it is washed with deionized, 80 DEG C
It is dried for standby, obtained yellow solid powder is that doping mixes vanadium strontium titanates for 0.5mol%.
Embodiment 3
1,2.11g (0.01mol) Sr (NO are weighed3)2It is dissolved in 20ml deionized waters, stirring is to being completely dissolved；
2,2.8ml (C are added dropwise in the solution obtained to a3H7O)4Ti (ρ=0.9600g/mL), stirs while adding,
The suspended liquid system of white disperseed as far as possible；
3, the V of 0.0091g is added2O5The mixed system obtained by b is added, is sufficiently stirred simultaneously, then adds 0.8g
NaOH is settled to 40ml (a concentration of 0.5mol/L of NaOH)；
4, it is transferred to after fully being dissolved drug in c using ultrasonic disperse instrument in 50ml hydrothermal reaction kettles, is kept the temperature at 200 DEG C
Reaction is for 24 hours；
5, the SrTiO obtained3A small amount of SrCO is washed away with 1% dilute nitric acid solution3, then it is washed with deionized, 80 DEG C
It is dried for standby, obtained yellow solid powder is that doping mixes vanadium strontium titanates for 1.0mol%.
A series of tests are done for embodiment 1-3, test result is as shown in figures 2-6：
Fig. 2 is the pure phase and the XRD spectrum for mixing vanadium strontium titanates that the embodiment of the present invention 1,2,3 obtains, and data are by German cloth
Luke D8 type X-ray diffractometers acquire, it can be seen from the figure that the prepared according to the methods of the invention strontium titanates mixed after vanadium is knot
Crystalline substance is good, the uniform single compound of chemical composition and structure；
Fig. 3 be the pure phase (a-b) that the embodiment of the present invention 1,2,3 obtains and mix vanadium amount be respectively 0.5% (c-d) and
The scanning electron microscope (SEM) photograph of 1.0% (e-f) strontium titanates, it can be seen that mix vanadium amount be 1.0% (e-f) strontium titanates size it is more uniform,
Good dispersion；
Fig. 4 is the pure phase and the EPR collection of illustrative plates for mixing vanadium strontium titanates that the embodiment of the present invention 1,2,3 obtains, at g=2.003
Signal peak caused by single electron Lacking oxygen, at g=1.976 be Ti3+Signal peak, V doping after Lacking oxygen and Ti3+EPR letter
Number weaken, illustrate that mixing vanadium reduces above two defect concentration；
Fig. 5, Fig. 6 are the pure phase and the uv-visible absorption spectra for mixing vanadium strontium titanates that the embodiment of the present invention 1,2,3 obtains
And energy gap calculates, and as can be seen from the figure mixes vanadium and makes SrTiO3ABSORPTION EDGE there is apparent red shift, showing to mix vanadium can
Enhance sample to the absorbent properties of visible light, but mixes from the point of view of Fig. 6 the energy gap that vanadium does not substantially change material；After mixing vanadium
Oxygen defect and Ti3+Defect concentration reduces, and shows that mixing vanadium raising visible absorption is not due to defect, and should be that vanadium introducing is miscellaneous
Mass-energy grade.
Preparation method of the present invention is equally applicable to the doping with the other elements of subgroup with V element, such as embodiment 4：
1,2.11g (0.01mol) Sr (NO are weighed3)2It is dissolved in 20ml deionized waters, stirring is to being completely dissolved；
2,2.8ml (C are added dropwise in the solution obtained to a3H7O)4Ti (ρ=0.9600g/mL), stirs while adding,
The suspended liquid system of white disperseed as far as possible；
3,0.0133 Nb is added2O5The mixed system obtained by b is added, is sufficiently stirred simultaneously, then adds 0.8g
NaOH is settled to 40ml (a concentration of 0.5mol/L of NaOH)；
4, it is transferred to after fully being dissolved drug in c using ultrasonic disperse instrument in 50ml hydrothermal reaction kettles, is kept the temperature at 200 DEG C
Reaction is for 24 hours；
5, the SrTiO obtained3A small amount of SrCO is washed away with 1% dilute nitric acid solution3, then it is washed with deionized, 80 DEG C
It is dried for standby, obtained white solid powder is the niobium-doped strontium titanate that doping is 1.0mol%.
Protection scope of the present invention is not limited to the above embodiments, it is clear that those skilled in the art can be to this hair
It is bright to carry out various changes and deformation without departing from scope and spirit of the present invention.If these changes and deformation belong to power of the present invention
In the range of profit requirement and its equivalent technologies, then including the intent of the present invention also includes these changes and deforms.
Claims (6)
1. a kind of preparation method of vanadium doping strontium titanates nano-photocatalyst material, which is characterized in that include the following steps：
Step 1 weighs a certain amount of Sr (NO3)2It is dissolved in deionized water, stirring is to being completely dissolved；
(C is added dropwise in step 2, the solution obtained to step 13H7O)4Ti is stirred while adding, and is disperseed as far as possible
The suspended liquid system of white；
Step 3 weighs a certain amount of V by scheduled doping2O5The mixed system obtained by step 2 is added, is sufficiently stirred simultaneously,
Then add a certain amount of NaOH solution；
Step 4 is transferred to after fully being dissolved drug in step 3 using ultrasonic disperse instrument in hydrothermal reaction kettle, is kept the temperature at 200 DEG C
Reaction is for 24 hours；
Step 5, the SrTiO that will be obtained in step 33A small amount of SrCO is washed away with 1% dilute nitric acid solution3, then use deionized water
Washing, 80 DEG C are dried for standby, and obtained yellow solid powder is vanadium doping strontium titanates.
2. a kind of preparation method of vanadium doping strontium titanates nano-photocatalyst material as described in claim 1, it is characterised in that：Institute
It states elements Sr and Ti molar ratios in step 1 and 2 and is more than 1:1, to avoid because of TiO2The generation of phase and cause to material property test and assess
Influence.
3. a kind of preparation method of vanadium doping strontium titanates nano-photocatalyst material as described in claim 1, it is characterised in that：Institute
(C is stated in step 23H7O)4The density of Ti solution is ρ=0.9600g/mL.
4. a kind of preparation method of vanadium doping strontium titanates nano-photocatalyst material as described in claim 1, it is characterised in that：Institute
State V in step 32O5Weigh after quality is calculated according to shared ratios of the V after doping in V-SrTiO3 and determine.
5. a kind of preparation method of vanadium doping strontium titanates nano-photocatalyst material as described in claim 1, it is characterised in that：Institute
The molal weight for stating NaOH in step 3 is Sr (NO in step 13)2Twice of the amount of substance.
6. a kind of preparation method of vanadium doping strontium titanates nano-photocatalyst material as described in claim 1, it is characterised in that：Institute
State a concentration of 0.5mol/L of NaOH in step 3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201810549430.7A CN108636398B (en) | 2018-05-31 | 2018-05-31 | Preparation method of vanadium-doped strontium titanate nano photocatalytic material |
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| CN113797910A (en) * | 2020-06-16 | 2021-12-17 | 中国科学院化学研究所 | Defect-containing nano microspheric perovskite catalyst and preparation method and application thereof |
| CN114308034A (en) * | 2021-12-07 | 2022-04-12 | 南京航空航天大学 | Strontium titanate semiconductor catalyst co-doped with (III) and (V) valence double transition metal ions and preparation method thereof |
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| CN114308034A (en) * | 2021-12-07 | 2022-04-12 | 南京航空航天大学 | Strontium titanate semiconductor catalyst co-doped with (III) and (V) valence double transition metal ions and preparation method thereof |
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