CN107362792A - A kind of preparation method of strontium titanates/niobic acid tin composite nano materials - Google Patents
A kind of preparation method of strontium titanates/niobic acid tin composite nano materials Download PDFInfo
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- CN107362792A CN107362792A CN201710477853.8A CN201710477853A CN107362792A CN 107362792 A CN107362792 A CN 107362792A CN 201710477853 A CN201710477853 A CN 201710477853A CN 107362792 A CN107362792 A CN 107362792A
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- 239000002131 composite material Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 239000002253 acid Substances 0.000 title claims abstract description 14
- 229910052712 strontium Inorganic materials 0.000 title claims abstract description 14
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 12
- 229910002370 SrTiO3 Inorganic materials 0.000 claims abstract description 38
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 24
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 24
- 235000019441 ethanol Nutrition 0.000 claims abstract description 20
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 19
- 238000013019 agitation Methods 0.000 claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 14
- 239000001257 hydrogen Substances 0.000 claims abstract description 14
- 238000005406 washing Methods 0.000 claims abstract description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000004519 manufacturing process Methods 0.000 claims abstract description 13
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 12
- 239000002245 particle Substances 0.000 claims abstract description 11
- 230000001699 photocatalysis Effects 0.000 claims abstract description 10
- 230000000694 effects Effects 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000005516 engineering process Methods 0.000 claims abstract description 5
- 229910002367 SrTiO Inorganic materials 0.000 claims description 20
- 230000035484 reaction time Effects 0.000 claims description 5
- 239000002105 nanoparticle Substances 0.000 abstract description 6
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 abstract description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 125000005909 ethyl alcohol group Chemical group 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 238000007704 wet chemistry method Methods 0.000 description 8
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 6
- 238000005119 centrifugation Methods 0.000 description 6
- 238000000034 method Methods 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
- 150000001875 compounds Chemical group 0.000 description 5
- 238000007146 photocatalysis Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000033228 biological regulation Effects 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
- 239000011941 photocatalyst Substances 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 235000011150 stannous chloride Nutrition 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002023 wood Substances 0.000 description 2
- 206010013786 Dry skin Diseases 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006243 chemical reaction 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
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000013507 mapping Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000003643 water by type Substances 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
- B01J23/002—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
-
- 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
-
- 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 present invention is directed to the problem of single strontium titanate nanoparticles visible light catalytic efficiency is low, provides a kind of preparation method of strontium titanates/niobic acid tin composite nano materials.SnNb is weighed respectively2O6、SrTiO3Powder is dissolved in absolute ethyl alcohol, ultrasonic disperse, then by SrTiO3SnNb is added dropwise in solution2O6In solution, magnetic agitation, solution is transferred in the reactor that liner is polytetrafluoroethylene (PTFE), be put into baking oven, hydro-thermal reaction, after room temperature, be centrifuged out pale yellow coloured particles, washing and alcohol centrifuge after washing, and drying obtains the SrTiO3/SnNb2O6Composite；Granular SrTiO3It is dispersed in SNO nanometer sheets.Preparation technology is simple, and strontium titanates/niobic acid tin composite nano materials of preparation have good photocatalytic hydrogen production activity.
Description
Technical field
The present invention is directed to the problem of single strontium titanate nanoparticles visible light catalytic efficiency is low, provides a kind of simple titanium
The preparation method of sour strontium/niobic acid tin composite nano materials, is mainly used in the technology of photocatalysis Decomposition aquatic products hydrogen, belongs to composite wood
Expect technical field and clean energy resource field.
Background technology
Solar energy is as a kind of clean energy resource of cheap reproducible, using Driven by Solar Energy semiconductor light-catalyst hydrogen manufacturing,
People have been subjected to widely to pay close attention to；In the development of the past few decades, a large amount of photochemical catalysts are studied and applied, in crowd
In more catalysis materials, strontium titanates (SrTiO3) due to its excellent photocatalytic activity, corrosion resistance, heat resistance, chemical stability, super
The property led is by widely studied.But SrTiO3Energy gap wider (3.2eV), it is necessary to ultraviolet light competence exertion to go out its excellent
Different performance, to the utilization ratio of solar energy than relatively low；In order to improve SrTiO3Visible absorption scope and suppress photoproduction
Charge recombination, researchers attempt a variety of methods and it are modified, including metal or it is nonmetallic ion-doped (H.Yu,
S.Ouyang, S.Yan, Z.Li, T.Yu, Z.Zou, J.Mater.Chem.21 (2011) 11347-11351.), noble metal loading
(X.Yan, S.F.Sun, B.Hu, X.Y.Wang, W.Lu, W.D.Shi, Micro Nano Lett.0452 (2013) 1-4.), with
The compound structure hetero-junctions of other semiconductor light-catalysts (X.J.Guan, L.J.Guo, ACS Catal.4 (2014) 3020-3026.)；
In the above-mentioned methods, it is the most frequently used and effective means to build hetero-junctions, can be effectively promoted the separation in light induced electron and hole,
Suppress light induced electron and compound, the raising SrTiO in hole3Photocatalysis hydrogen production efficiency.
Niobic acid tin (SnNb2O6) typical layer niobate semi-conducting material is used as, due to its unique crystal structure and conjunction
Extensive concern of the suitable band structure in visible light catalytic hydrogen production by water decomposition field by researcher.SnNb2O6With narrower
Band gap (~2.3eV) and suitable position of energy band, be advantageous to visible ray capture and photocatalysis hydrogen production, in addition, SnNb2O6With
SrTiO3With the conduction band valence band location to match, II types hetero-junctions can be formed in theory and improves photo-generate electron-hole pair
Separative efficiency, so as to improve photocatalytic hydrogen production activity.
So far, not yet someone's report prepares SrTiO using two step wet chemistry methods3/SnNb2O6Composite, it is used
SNO chemical and physical features are stable, and raw material are cheap and easy to get, nontoxic, and prepare SrTiO using it as carrier3/SnNb2O6Composite wood
The reaction process of material is simple, and products obtained therefrom photocatalytic hydrogen production activity is good, and stability is high, and production process is green.
The content of the invention
It is an object of the present invention to provide it is a kind of it is new at ambient temperature, synthesized with two simple and easy step wet chemistry methods
SrTiO3/SnNb2O6The method of composite.
The present invention is realized by following steps：
(1) niobic acid tin (SnNb is prepared2O6) nanometer sheet：Niobium pentaoxide is weighed, potassium hydroxide is polytetrafluoroethylene (PTFE) in liner
Reactor in, add deionized water thereto, then reactor be put into baking oven, first time hydro-thermal reaction；Treat that nature is cold
But to after room temperature, obtaining clarifying precursor solution, solution ph is adjusted with watery hydrochloric acid, adds two hydrated stannous chlorides, again
PH value is adjusted with watery hydrochloric acid, solution is transferred in the reactor that liner is polytetrafluoroethylene (PTFE), reactor is put into baking oven, the
Secondary hydro-thermal reaction, after room temperature, yellow particle is centrifuged out, washing and alcohol are washed for several times, centrifuged, 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 time hydro-thermal reaction is 160~200 DEG C, and the reaction time is 45~50h.
The concentration of the dilute hydrochloric acid solution is 2molL-1。
The first time watery hydrochloric acid regulation solution ph is 7~9.
Second of the watery hydrochloric acid regulation solution ph is 1~3.
The temperature of second of hydro-thermal reaction is 180~220 DEG C, and the reaction time is 45~50h.
(2) strontium titanates (SrTiO is prepared3) nano particle：Measure butyl titanate (TBT) to be dissolved in ethylene glycol, for the first time
Magnetic agitation, strontium nitrate, sodium hydroxide solution are added, again magnetic agitation, solution is transferred to liner as polytetrafluoroethylene (PTFE)
In reactor, reactor is put into baking oven, hydro-thermal reaction, after room temperature, is centrifuged out white particle, washing and
Alcohol centrifuges after being washed till neutrality, drying；Specifically refer to X.J.Guan, L.J.Guo, ACS Cata, 4 (2014) 3020-3026.
The time of the first time magnetic agitation is 5~20min.
The concentration of the strontium nitrate solution is 0.5molL-1。
The concentration of the sodium hydroxide solution is 5molL-1。
The time of second of magnetic agitation is 20~40min.
The temperature of the hydro-thermal reaction is 180~220 DEG C, and the reaction time is 22~26h.
(3) SrTiO is prepared3/SnNb2O6Composite：SnNb is weighed respectively2O6、SrTiO3Powder is dissolved in absolute ethyl alcohol,
Ultrasonic disperse, then by SrTiO3SnNb is added dropwise in solution2O6In solution, magnetic agitation, it is polytetrafluoro that solution is transferred into liner
In the reactor of ethene, be put into baking oven, hydro-thermal reaction, after room temperature, be centrifuged out pale yellow coloured particles, washing and
Alcohol centrifuges after washing, and drying obtains the SrTiO3/SnNb2O6Composite；Granular SrTiO3It is dispersed in SNO nanometer sheets.
The ultrasonic disperse refers to use power as 250W ultrasonic machine in ultrasonic 20-40min.
The time of the magnetic agitation is 2~6h.
The temperature of the hydro-thermal reaction is 140~180 DEG C, and the reaction time is 10~14h.
The SrTiO3/SnNb2O6SrTiO in composite3With SnNb2O6Mass ratio be 0.1-0.4:1；It is preferred that 0.2:
1。
Compared with prior art, the advantage of the invention is that：
1st, the present invention employs a kind of simple two steps wet chemistry method and successfully prepares visible light-responded SrTiO first3/SnNb2O6
Heterojunction material, its preparation technology is simple, easily-controllable, and cost is low, and power consumption is few, and the heterojunction material has good ambient stable
Property, there is good application prospect in terms of solving environmental pollution and energy crisis.
2、SnNb2O6Laminated structure has higher specific surface area, can realize SrTiO3The high degree of dispersion of nano particle,
Suppress SrTiO3Reunion of the nano particle in preparation and application process, while SnNb2O6Two-dimension plane structure is beneficial to SrTiO3Light
The abundant exposure of catalyst, beneficial to the utilization ratio and the further photocatalysis hydrogen production effect for improving material improved to visible ray.
3、SrTiO3/SnNb2O6Heterojunction material can be as the visible-light photocatalyst of function admirable.SrTiO3With
SnNb2O6The heterojunction structure formed after compound is not only advantageous to improve the life-span in light induced electron and hole, promotes photogenerated charge
Transmission, and effectively improve the stability of compound rear catalyst.Therefore, SrTiO3/SnNb2O6Heterojunction material is notable
Ground improves visible ray hydrogen production activity, is had broad prospects in photocatalysis practical application area.
In summary, the present invention is successfully prepared SrTiO using two step wet chemistry methods3/SnNb2O6Composite photocatalyst material.
By having carried out a series of signs such as XRD, TEM, DRS to the sample of preparation, as a result show prepared composite at interface
Hetero-junctions is formd, improves migration rate of the light induced electron on interface, is decomposed so as to improve strontium titanate visible light catalyst
Water H2-producing capacity.By investigating the H2-producing capacity of compound under visible light illumination, it is found that it is preferable this composite has
The ability of photodissociation aquatic products hydrogen.
Brief description of the drawings
Fig. 1 is prepared simple SrTiO3、SnNb2O6、SrTiO3/SnNb2O6The XRD diffraction spectrograms of composite；From figure
In it can be seen that different quality than SrTiO3/SnNb2O6XRD spectrum mainly by SrTiO3And SnNb2O6Diffraction maximum form,
And with SrTiO3The increase of mass fraction, SrTiO3Diffraction maximum it is more and more obvious.
Fig. 2 is prepared simple SnNb2O6、SrTiO3/SnNb2O6The transmission electron microscope photo of composite sample；Fig. 2 a are
Simple SnNb2O6Transmission electron microscope picture；Fig. 2 b-2e are respectively 10%~40%-SrTiO3/SnNb2O6Transmission electron microscope picture；Fig. 2 f are
20%-SrTiO3/SnNb2O6High-resolution-ration transmission electric-lens figure；As can be seen from the figure SrTiO3It is dispersed in SnNb2O6Sheet surface,
Form hetero-junctions.
Fig. 3 is the SrTiO prepared3/SnNb2O6The UV-vis DRS abosrption spectrogram of composite, can be with from figure
Find out SrTiO3Absorb in ultra-violet (UV) band, SnNb2O6There is very strong absorption at 440nm, work as SrTiO3It is supported on SnNb2O6On, inhale
Receive intensity decreases.
Fig. 4 is simple SrTiO3、SnNb2O6And different quality than SrTiO3/SnNb2O6Composite is in visible ray
Lower photocatalytic hydrogen production by water decomposition Yield mapping, as can be seen from the figure 20%-SrTiO3/SnNb2O6Composite has highest light
Catalyzing manufacturing of hydrogen activity.
Embodiment
The SnNb of embodiment 12O6The preparation of nanometer sheet
SnNb2O6Preparation using hydro-thermal reaction method：Weigh 0.5g niobium pentaoxides, 2.2443g potassium hydroxide
In 50mL liners in the reactor of polytetrafluoroethylene (PTFE), to add 35mL deionized waters thereto, reactor is put into baking oven, 180
DEG C hydro-thermal reaction 48h, after room temperature, obtain clarifying precursor solution, solution is transferred in 50mL beakers, use
Concentration is that 2mol/L watery hydrochloric acid adjusts pH value of solution to 8, adds the hydrated stannous chlorides of 0.4245g bis-, magnetic agitation 10min, then
Secondary with concentration is that 2mol/L watery hydrochloric acid adjusts pH value of solution to 2, and solution is transferred into the reactor that 100mL liners are polytetrafluoroethylene (PTFE)
In, be put into baking oven, 200 DEG C of hydro-thermal reaction 48h are cooled to room temperature, and centrifugation obtains yellow particle, washing and alcohol wash it is each three times, from
The heart, 60 DEG C of dry 12h in baking oven.
The SrTiO of embodiment 23The preparation of nano particle
SrTiO3Preparation using hydro-thermal reaction method：Measure 10mmol butyl titanates and be dissolved in 20ml second two
Alcohol, magnetic agitation 10min, settled solution is formed, adds 20ml 0.5M strontium nitrate solutions and 10ml5M sodium hydroxide solutions,
Magnetic agitation 30min, solution is transferred in the reactor that 100mL liners are polytetrafluoroethylene (PTFE), is put into baking oven, 200 DEG C of hydro-thermals
24h is reacted, is cooled to room temperature, centrifugation obtains white particle, and washing and alcohol are washed till neutrality, centrifuge, 60 DEG C of dryings in baking oven
12h。
The 10%-SrTiO of embodiment 33/SnNb2O6The preparation of composite
SrTiO3/SnNb2O6The preparation of composite is using two step wet chemistry methods：50mg SnNb are weighed respectively2O6It is molten
In 60ml absolute ethyl alcohols, 5.6mg SrTiO3Powder is dissolved in 20ml absolute ethyl alcohols, then in the ultrasonic machine that power is 250W
Middle ultrasonic 30min, then by SrTiO3SnNb is added dropwise in solution2O6In solution, magnetic agitation 4h, solution is transferred in 100mL
Serve as a contrast in the reactor for polytetrafluoroethylene (PTFE), be put into baking oven, 160 DEG C of hydro-thermal reaction 12h, after room temperature, centrifugation
Go out yellow particle, washing and alcohol are washed respectively to be centrifuged afterwards three times, and 60 DEG C of dry 12h obtain the 10%-SrTiO in baking oven3/
SnNb2O6Composite.
The 20%-SrTiO of embodiment 43/SnNb2O6The preparation of composite
SrTiO3/SnNb2O6The preparation of composite is using two step wet chemistry methods：50mg SnNb are weighed respectively2O6It is molten
In 60ml absolute ethyl alcohols, 12.5mg SrTiO3Powder is dissolved in 20ml absolute ethyl alcohols, then in the ultrasonic machine that power is 250W
Middle ultrasonic 30min, then by SrTiO3SnNb is added dropwise in solution2O6In solution, magnetic agitation 4h, solution is transferred in 100mL
Serve as a contrast in the reactor for polytetrafluoroethylene (PTFE), be put into baking oven, 160 DEG C of hydro-thermal reaction 12h, after room temperature, centrifugation
Go out yellow particle, washing and alcohol are washed respectively to be centrifuged afterwards three times, and 60 DEG C of dry 12h obtain the 20%-SrTiO in baking oven3/
SnNb2O6Composite.
The 30%-SrTiO of embodiment 53/SnNb2O6The preparation of composite
SrTiO3/SnNb2O6The preparation of composite is using two step wet chemistry methods：50mg SnNb are weighed respectively2O6It is molten
In 60ml absolute ethyl alcohols, 21.4mg SrTiO3Powder is dissolved in 20ml absolute ethyl alcohols, then in the ultrasonic machine that power is 250W
Middle ultrasonic 30min, then by SrTiO3SnNb is added dropwise in solution2O6In solution, magnetic agitation 4h, solution is transferred in 100mL
Serve as a contrast in the reactor for polytetrafluoroethylene (PTFE), be put into baking oven, 160 DEG C of hydro-thermal reaction 12h, after room temperature, centrifugation
Go out pale yellow coloured particles, washing and alcohol are washed respectively to be centrifuged afterwards three times, and 60 DEG C of dry 12h obtain the 30%-SrTiO in baking oven3/
SnNb2O6Composite.
The 40%-SrTiO of embodiment 63/SnNb2O6The preparation of composite
SrTiO3/SnNb2O6The preparation of composite is using two step wet chemistry methods：50mg SnNb are weighed respectively2O6It is molten
In 60ml absolute ethyl alcohols, 33.3mg SrTiO3Powder is dissolved in 20ml absolute ethyl alcohols, then in the ultrasonic machine that power is 250W
Middle ultrasonic 30min, then by SrTiO3SnNb is added dropwise in solution2O6In solution, magnetic agitation 4h, solution is transferred in 100mL
Serve as a contrast in the reactor for polytetrafluoroethylene (PTFE), be put into baking oven, 160 DEG C of hydro-thermal reaction 12h, after room temperature, centrifugation
Go out pale yellow coloured particles, washing and alcohol are washed respectively to be centrifuged afterwards three times, and 60 DEG C of dry 12h obtain the 40%-SrTiO in baking oven3/
SnNb2O6Composite.
Claims (6)
1. a kind of preparation method of strontium titanates/niobic acid tin composite nano materials, preparation technology is simple, strontium titanates/niobic acid of preparation
Tin composite nano materials have good photocatalytic hydrogen production activity, it is characterised in that：SnNb is weighed respectively2O6、SrTiO3Powder is molten
In absolute ethyl alcohol, ultrasonic disperse, then by SrTiO3SnNb is added dropwise in solution2O6In solution, magnetic agitation, solution is shifted
To liner for polytetrafluoroethylene (PTFE) reactor in, be put into baking oven, hydro-thermal reaction, after room temperature, be centrifuged out shallow
Yellow particle, washing and alcohol centrifuge after washing, and drying obtains the SrTiO3/SnNb2O6Composite；Granular SrTiO3Point
It is dispersed in SNO nanometer sheets.
A kind of 2. preparation method of strontium titanates/niobic acid tin composite nano materials as claimed in claim 1, it is characterised in that：Institute
State ultrasonic disperse refer to use power as 250W ultrasonic machine in ultrasonic 20-40min.
A kind of 3. preparation method of strontium titanates/niobic acid tin composite nano materials as claimed in claim 1, it is characterised in that：Institute
The time for stating magnetic agitation is 2~6h.
A kind of 4. preparation method of strontium titanates/niobic acid tin composite nano materials as claimed in claim 1, it is characterised in that：Institute
The temperature for stating hydro-thermal reaction is 140~180 DEG C, and the reaction time is 10~14h.
A kind of 5. preparation method of strontium titanates/niobic acid tin composite nano materials as claimed in claim 1, it is characterised in that：Institute
State SrTiO3/SnNb2O6SrTiO in composite3With SnNb2O6Mass ratio be 0.1-0.4:1.
A kind of 6. preparation method of strontium titanates/niobic acid tin composite nano materials as claimed in claim 5, it is characterised in that：Institute
State SrTiO3/SnNb2O6SrTiO in composite3With SnNb2O6Mass ratio be 0.2:1.
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| CN110052260A (en) * | 2019-03-20 | 2019-07-26 | 常州大学 | There is strontium titanates/carbon composite of three-dimensional interworking architecture based on bacteria cellulose synthesis |
| CN110054215A (en) * | 2019-03-20 | 2019-07-26 | 常州大学 | Morphology controllable SrTiO3The preparation and its application of flower ball-shaped serial nano material |
| CN114672844A (en) * | 2022-04-02 | 2022-06-28 | 西安交通大学 | Preparation method and application of composite material |
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