CN107362792B - Preparation method of strontium titanate/tin niobate composite nano material - Google Patents
Preparation method of strontium titanate/tin niobate composite nano material Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 12
- AGNPPWAGEICIGZ-UHFFFAOYSA-N strontium tin Chemical compound [Sr].[Sn] AGNPPWAGEICIGZ-UHFFFAOYSA-N 0.000 title claims abstract description 12
- 229910002370 SrTiO3 Inorganic materials 0.000 claims abstract description 57
- 238000006243 chemical reaction Methods 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 16
- 239000001257 hydrogen Substances 0.000 claims abstract description 16
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000001816 cooling Methods 0.000 claims abstract description 13
- 238000004519 manufacturing process Methods 0.000 claims abstract description 13
- 230000001699 photocatalysis Effects 0.000 claims abstract description 13
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 13
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 13
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 11
- 239000002245 particle Substances 0.000 claims abstract description 11
- 238000005406 washing Methods 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 238000005303 weighing Methods 0.000 claims abstract description 9
- 230000000694 effects Effects 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 7
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 5
- 229910002367 SrTiO Inorganic materials 0.000 claims description 17
- 238000003760 magnetic stirring Methods 0.000 claims description 7
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 5
- 239000002135 nanosheet Substances 0.000 abstract description 4
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 235000019441 ethanol Nutrition 0.000 description 9
- 239000000126 substance Substances 0.000 description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Chemical compound [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 description 6
- 239000002105 nanoparticle Substances 0.000 description 5
- 239000011941 photocatalyst Substances 0.000 description 5
- 230000006798 recombination Effects 0.000 description 5
- 238000005215 recombination Methods 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 4
- FWPIDFUJEMBDLS-UHFFFAOYSA-L tin(II) chloride dihydrate Chemical compound O.O.Cl[Sn]Cl FWPIDFUJEMBDLS-UHFFFAOYSA-L 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 239000013590 bulk material Substances 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 230000005764 inhibitory process Effects 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 description 2
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000007704 wet chemistry method Methods 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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- 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
-
- B01J35/39—
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
-
- 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
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/10—Catalysts for performing the hydrogen forming reactions
- C01B2203/1041—Composition of the catalyst
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention aims at low visible light catalytic efficiency of single strontium titanate nano-particlesProvides a method for preparing the strontium titanate/tin niobate composite nano material. Separately weighing SnNb2O6、SrTiO3Dissolving the powder in anhydrous ethanol, performing ultrasonic dispersion, and then performing SrTiO3Adding SnNb into the solution drop by drop2O6Magnetically stirring the solution, transferring the solution into a reaction kettle with a polytetrafluoroethylene lining, putting the reaction kettle into an oven, carrying out hydrothermal reaction, centrifuging to obtain light yellow particles after naturally cooling to room temperature, washing with water and alcohol, centrifuging, and drying to obtain the SrTiO3/SnNb2O6A composite material; particulate SrTiO3Dispersed on the SNO nanosheets. The preparation process is simple, and the prepared strontium titanate/tin niobate composite nano material has good photocatalytic hydrogen production activity.
Description
Technical Field
The invention provides a simple preparation method of a strontium titanate/tin niobate composite nano material, which aims at the problem of low visible light catalytic efficiency of single strontium titanate nano particles, is mainly used in the technology of photocatalytic water decomposition to produce hydrogen, and belongs to the technical field of composite materials and the field of clean energy.
Background
Solar energy is used as a cheap and renewable clean energy source, and the solar energy is used for driving a semiconductor photocatalyst to produce hydrogen, so that the solar energy has been widely concerned by people; during the last decades a large number of photocatalysts have been studied and applied, among the numerous photocatalytic materials, strontium titanate (SrTiO)3) They have been widely studied for their excellent photocatalytic activity, corrosion resistance, heat resistance, chemical stability, and superconductivity. However, SrTiO3The forbidden band width of the solar cell is wide (3.2eV), the excellent performance of the solar cell can be exerted only by ultraviolet irradiation, and the utilization efficiency of solar energy is low; to increase SrTiO3The visible light absorption range and the inhibition of photo-generated charge recombination, researchers try various methods to modify the visible light absorption range and the inhibition of photo-generated charge recombination, including metal or nonmetal ion doping (h.yu, s.ouyang, s.yan, z.li, t.yu, z.zuo, j.mater.chem.21(2011) 11347-; in the method, the heterojunction is the most common and effective means, can effectively promote the separation of photogenerated electrons and holes, inhibit the recombination of the photogenerated electrons and the holes, and improve the SrTiO3Photocatalytic hydrogen production efficiency.
Tin niobate (SnNb)2O6) As a typical layered niobate semiconductorThe bulk material has attracted extensive attention of researchers in the field of hydrogen production by water decomposition under catalysis of visible light due to the unique crystal structure and the proper energy band structure of the bulk material. SnNb2O6Has narrower band gap (2.3 eV) and proper energy band position, is beneficial to visible light capture and photocatalytic hydrogen production, and in addition, SnNb2O6With SrTiO3The structure has matched conduction band and valence band positions, and theoretically can form a II-type heterojunction to improve the separation efficiency of photo-generated electron-hole pairs, thereby improving the activity of photocatalytic hydrogen production.
To date, the preparation of SrTiO by a two-step wet chemical process has not been reported3/SnNb2O6The SNO used in the composite material has stable chemical and physical properties, the raw material is cheap and easy to obtain, and the composite material is nontoxic, and the SrTiO prepared by using the SNO as a carrier3/SnNb2O6The reaction process of the composite material is simple, the obtained product has good photocatalytic hydrogen production activity and high stability, and the production process is green and environment-friendly.
Disclosure of Invention
The invention aims to provide a novel method for synthesizing SrTiO by a simple and feasible two-step wet chemical method at room temperature3/SnNb2O6A method of compounding a material.
The invention is realized by the following steps:
(1) preparation of tin niobate (SnNb)2O6) Nanosheet: weighing niobium pentoxide and potassium hydroxide in a reaction kettle with a polytetrafluoroethylene lining, adding deionized water into the reaction kettle, and then putting the reaction kettle into an oven for a first hydrothermal reaction; naturally cooling to room temperature to obtain a clear precursor solution, adjusting the pH value of the solution by using dilute hydrochloric acid, adding stannous chloride dihydrate, adjusting the pH value by using dilute hydrochloric acid again, transferring the solution to a reaction kettle with a polytetrafluoroethylene lining, putting the reaction kettle into an oven, carrying out a second hydrothermal reaction, naturally cooling to room temperature, centrifuging to obtain yellow particles, washing with water and alcohol for several times, centrifuging, and drying; specifically, refer to Z.Y.Zhang, D.L.Jiang, D.Li, M.He, M.Chen, appl.Catal.B: environ.183(2016) 113-123.
The temperature of the first hydrothermal reaction is 160-200 ℃, and the reaction time is 45-50 h.
The concentration of the dilute hydrochloric acid solution is 2 mol.L-1。
And adjusting the pH value of the solution to 7-9 by using the first dilute hydrochloric acid.
And adjusting the pH value of the solution to be 1-3 by using the second dilute hydrochloric acid.
The temperature of the second hydrothermal reaction is 180-220 ℃, and the reaction time is 45-50 h.
(2) Preparation of strontium titanate (SrTiO)3) Nano-particles: measuring tetrabutyl titanate (TBT), dissolving in ethylene glycol, performing magnetic stirring for the first time, adding strontium nitrate and sodium hydroxide solution, performing magnetic stirring again, transferring the solution to a reaction kettle with a polytetrafluoroethylene lining, putting the reaction kettle into an oven, performing hydrothermal reaction, naturally cooling to room temperature, centrifuging to obtain white particles, washing with water and alcohol to neutrality, centrifuging, and drying; specifically, X.J.Guan, L.J.Guo, ACS Cata,4(2014)3020-3026 can be referred to.
The time of the first magnetic stirring is 5-20 min.
The concentration of the strontium nitrate solution is 0.5 mol.L-1。
The concentration of the sodium hydroxide solution is 5 mol.L-1。
And the time of the second magnetic stirring is 20-40 min.
The temperature of the hydrothermal reaction is 180-220 ℃, and the reaction time is 22-26 h.
(3) Preparation of SrTiO3/SnNb2O6The composite material comprises the following components: separately weighing SnNb2O6、SrTiO3Dissolving the powder in anhydrous ethanol, performing ultrasonic dispersion, and then performing SrTiO3Adding SnNb into the solution drop by drop2O6Magnetically stirring the solution, transferring the solution into a reaction kettle with a polytetrafluoroethylene lining, putting the reaction kettle into an oven, carrying out hydrothermal reaction, centrifuging to obtain light yellow particles after naturally cooling to room temperature, washing with water and alcohol, centrifuging, and drying to obtain the SrTiO3/SnNb2O6A composite material; particulate SrTiO3Dispersed on the SNO nanosheets.
The ultrasonic dispersion refers to ultrasonic treatment in an ultrasonic machine with the power of 250W for 20-40 min.
The magnetic stirring time is 2-6 h.
The temperature of the hydrothermal reaction is 140-180 ℃, and the reaction time is 10-14 h.
The SrTiO3/SnNb2O6SrTiO in composite material3And SnNb2O6The mass ratio of (A) to (B) is 0.1-0.4: 1; preferably 0.2: 1.
Compared with the prior art, the invention has the advantages that:
1. the invention successfully prepares the visible light response SrTiO by adopting a simple two-step wet chemical method for the first time3/SnNb2O6The heterojunction material has the advantages of simple preparation process, easy control, low cost and low energy consumption, has good environmental stability, and has good application prospect in the aspects of solving the environmental pollution and energy crisis.
2、SnNb2O6The sheet structure has higher specific surface area and can realize SrTiO3High dispersion of nanoparticles, suppression of SrTiO3The agglomeration of nano particles in the preparation and application processes, and SnNb2O6The two-dimensional plane structure is beneficial to SrTiO3The full exposure of the photocatalyst is beneficial to improving the utilization efficiency of visible light and further improving the photocatalytic hydrogen production effect of the material.
3、SrTiO3/SnNb2O6The heterojunction material can be used as a visible light photocatalyst with excellent performance. SrTiO3And SnNb2O6The heterojunction structure formed after the recombination is beneficial to prolonging the service life of photo-generated electrons and holes, promoting the transmission of photo-generated charges and effectively improving the stability of the catalyst after the recombination. Thus, SrTiO3/SnNb2O6The heterojunction material remarkably improves the hydrogen production activity of visible light and has wide prospect in the field of photocatalytic practical application.
In conclusion, the SrTiO is successfully prepared by adopting a two-step wet chemical method3/SnNb2O6A composite photocatalytic material. By aligning the prepared samplesA series of characteristics such as XRD, TEM, DRS and the like are carried out on the product, and the result shows that the prepared composite material forms a heterojunction on the interface, and the migration rate of photo-generated electrons on the semiconductor interface is improved, so that the hydrogen production performance of the strontium titanate photocatalyst in water decomposition is improved. By investigating the hydrogen production performance of the composite under the irradiation of visible light, the composite material is found to have better capability of photolyzing water to produce hydrogen.
Drawings
FIG. 1 shows the preparation of pure SrTiO3、SnNb2O6、SrTiO3/SnNb2O6XRD diffraction pattern of the composite material; from the figure, SrTiO with different mass ratios can be seen3/SnNb2O6The XRD pattern of (A) is mainly composed of SrTiO3And SnNb2O6With SrTiO3Increase in mass fraction of SrTiO3The diffraction peaks of (a) become more and more pronounced.
FIG. 2 shows the preparation of pure SnNb2O6、SrTiO3/SnNb2O6A transmission electron microscope photograph of the composite material sample; FIG. 2a shows a pure SnNb2O6A transmission electron microscope image; FIGS. 2b-2e are 10% -40% SrTiO, respectively3/SnNb2O6A transmission electron microscope image; FIG. 2f is 20% -SrTiO3/SnNb2O6High resolution transmission electron microscopy images; from the figure, SrTiO can be seen3Dispersed in SnNb2O6And forming a heterojunction on the surface of the thin sheet.
FIG. 3 shows SrTiO prepared3/SnNb2O6The ultraviolet-visible diffuse reflection absorption spectrogram of the composite material can be seen from the figure, and SrTiO3Absorbed in the ultraviolet region, SnNb2O6Has strong absorption at 440nm when SrTiO3Loaded in SnNb2O6Above, the absorption strength decreases.
FIG. 4 shows pure SrTiO3、SnNb2O6And SrTiO with different mass ratios3/SnNb2O6The yield of hydrogen produced by photocatalytic decomposition of water of the composite material under visible light can be seen from the graph, and 20% -SrTiO3/SnNb2O6The composite material has the highest photocatalytic hydrogen production activity.
Detailed Description
Example 1 SnNb2O6Preparation of nanosheets
SnNb2O6The preparation adopts a hydrothermal reaction method: weighing 0.5g of niobium pentoxide and 2.2443g of potassium hydroxide in a 50mL reaction kettle with a polytetrafluoroethylene lining, adding 35mL of deionized water into the reaction kettle, putting the reaction kettle into an oven, carrying out hydrothermal reaction at 180 ℃ for 48h, naturally cooling to room temperature to obtain a clear precursor solution, transferring the solution into a 50mL beaker, adjusting the pH of the solution to 8 by using 2mol/L dilute hydrochloric acid, adding 0.4245g of stannous chloride dihydrate, carrying out magnetic stirring for 10min, adjusting the pH of the solution to 2 by using 2mol/L dilute hydrochloric acid again, transferring the solution into a 100mL reaction kettle with a polytetrafluoroethylene lining, putting the reaction kettle into the oven, carrying out hydrothermal reaction at 200 ℃ for 48h, cooling to room temperature, centrifuging to obtain yellow particles, washing with water and alcohol for three times respectively, centrifuging, and drying in the oven at 60 ℃ for 12 h.
Example 2 SrTiO3Preparation of nanoparticles
SrTiO3The preparation adopts a hydrothermal reaction method: measuring 10mmol of tetrabutyl titanate, dissolving in 20mL of ethylene glycol, magnetically stirring for 10min to form a clear solution, adding 20mL of 0.5M strontium nitrate solution and 10mL of 5M sodium hydroxide solution, magnetically stirring for 30min, transferring the solution to a 100mL reaction kettle with a polytetrafluoroethylene lining, putting the reaction kettle into an oven, carrying out hydrothermal reaction at 200 ℃ for 24h, cooling to room temperature, centrifuging to obtain white particles, washing with water and alcohol to neutrality, centrifuging, and drying in the oven at 60 ℃ for 12 h.
Example 310% -SrTiO3/SnNb2O6Preparation of composite materials
SrTiO3/SnNb2O6The preparation of the composite material adopts a two-step wet chemical method: respectively weighing 50mg of SnNb2O65.6mg SrTiO dissolved in 60ml absolute ethyl alcohol3Dissolving the powder in 20ml of absolute ethyl alcohol, then carrying out ultrasonic treatment for 30min in an ultrasonic machine with the power of 250W, and then carrying out SrTiO3Adding SnNb into the solution drop by drop2O6Magnetically stirring the solution for 4 hours, transferring the solution into a 100mL reaction kettle with a polytetrafluoroethylene lining, putting the reaction kettle into an oven, carrying out hydrothermal reaction for 12 hours at 160 ℃, centrifuging yellow particles after naturally cooling to room temperature, washing with water and alcohol for three times respectively, centrifuging, and drying in the oven for 12 hours at 60 ℃ to obtain the 10% -SrTiO3/SnNb2O6A composite material.
Example 420% -SrTiO3/SnNb2O6Preparation of composite materials
SrTiO3/SnNb2O6The preparation of the composite material adopts a two-step wet chemical method: respectively weighing 50mg of SnNb2O6Dissolved in 60ml of absolute ethanol and 12.5mg of SrTiO3Dissolving the powder in 20ml of absolute ethyl alcohol, then carrying out ultrasonic treatment for 30min in an ultrasonic machine with the power of 250W, and then carrying out SrTiO3Adding SnNb into the solution drop by drop2O6Magnetically stirring the solution for 4 hours, transferring the solution into a 100mL reaction kettle with a polytetrafluoroethylene lining, putting the reaction kettle into an oven, carrying out hydrothermal reaction for 12 hours at 160 ℃, centrifuging yellow particles after naturally cooling to room temperature, washing with water and alcohol for three times respectively, centrifuging, and drying in the oven for 12 hours at 60 ℃ to obtain the 20% -SrTiO3/SnNb2O6A composite material.
Example 530% -SrTiO3/SnNb2O6Preparation of composite materials
SrTiO3/SnNb2O6The preparation of the composite material adopts a two-step wet chemical method: respectively weighing 50mg of SnNb2O621.4mg SrTiO dissolved in 60ml absolute ethyl alcohol3Dissolving the powder in 20ml of absolute ethyl alcohol, then carrying out ultrasonic treatment for 30min in an ultrasonic machine with the power of 250W, and then carrying out SrTiO3Adding SnNb into the solution drop by drop2O6Magnetically stirring the solution for 4 hours, transferring the solution into a 100mL reaction kettle with a polytetrafluoroethylene lining, putting the reaction kettle into an oven, carrying out hydrothermal reaction for 12 hours at 160 ℃, centrifuging to obtain light yellow particles after naturally cooling to room temperature, washing with water and alcohol for three times respectively, centrifuging, and drying in the oven for 12 hours at 60 ℃ to obtain the 30% -SrTiO3/SnNb2O6A composite material.
Example 640% -SrTiO3/SnNb2O6Preparation of composite materials
SrTiO3/SnNb2O6The preparation of the composite material adopts a two-step wet chemical method: respectively weighing 50mg of SnNb2O6Dissolved in 60ml of absolute ethanol, 33.3mg of SrTiO3Dissolving the powder in 20ml of absolute ethyl alcohol, then carrying out ultrasonic treatment for 30min in an ultrasonic machine with the power of 250W, and then carrying out SrTiO3Adding SnNb into the solution drop by drop2O6Magnetically stirring the solution for 4 hours, transferring the solution into a 100mL reaction kettle with a polytetrafluoroethylene lining, putting the reaction kettle into an oven, carrying out hydrothermal reaction for 12 hours at 160 ℃, centrifuging to obtain light yellow particles after naturally cooling to room temperature, washing with water and alcohol for three times respectively, centrifuging, and drying in the oven for 12 hours at 60 ℃ to obtain the 40% -SrTiO3/SnNb2O6A composite material.
Claims (6)
1. A preparation method of strontium titanate/tin niobate composite nano-material has simple preparation process, and the prepared strontium titanate/tin niobate composite nano-material has good photocatalytic hydrogen production activity, and is characterized in that: separately weighing SnNb2O6、SrTiO3Dissolving the powder in anhydrous ethanol, performing ultrasonic dispersion, and then performing SrTiO3Adding SnNb into the solution drop by drop2O6Magnetically stirring the solution, transferring the solution into a reaction kettle with a polytetrafluoroethylene lining, putting the reaction kettle into an oven, carrying out hydrothermal reaction, centrifuging to obtain light yellow particles after naturally cooling to room temperature, washing with water and alcohol, centrifuging, and drying to obtain the SrTiO3/SnNb2O6A composite material; particulate SrTiO3Dispersed in SnNb2O6And (4) nano-chips.
2. The method for preparing the strontium titanate/tin niobate composite nanomaterial of claim 1, wherein the method comprises the following steps: the ultrasonic dispersion refers to ultrasonic treatment in an ultrasonic machine with the power of 250W for 20-40 min.
3. The method for preparing the strontium titanate/tin niobate composite nanomaterial of claim 1, wherein the method comprises the following steps: the magnetic stirring time is 2-6 h.
4. The method for preparing the strontium titanate/tin niobate composite nanomaterial of claim 1, wherein the method comprises the following steps: the temperature of the hydrothermal reaction is 140-180 ℃, and the reaction time is 10-14 h.
5. The method for preparing the strontium titanate/tin niobate composite nanomaterial of claim 1, wherein the method comprises the following steps: the SrTiO3/SnNb2O6SrTiO in composite material3And SnNb2O6The mass ratio of (A) to (B) is 0.1-0.4: 1.
6. The method for preparing strontium titanate/tin niobate composite nanomaterial of claim 5, wherein: the SrTiO3/SnNb2O6SrTiO in composite material3And SnNb2O6The mass ratio of (A) to (B) is 0.2: 1.
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