CN106955695A - A kind of strontium titanium dioxide/strontium titanate nano heterojunction and its preparation method and application - Google Patents
A kind of strontium titanium dioxide/strontium titanate nano heterojunction and its preparation method and application Download PDFInfo
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- CN106955695A CN106955695A CN201710111797.6A CN201710111797A CN106955695A CN 106955695 A CN106955695 A CN 106955695A CN 201710111797 A CN201710111797 A CN 201710111797A CN 106955695 A CN106955695 A CN 106955695A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- DQKZBBLOXVFMJQ-UHFFFAOYSA-N [O--].[O--].[Ti+4].[Sr++] Chemical compound [O--].[O--].[Ti+4].[Sr++] DQKZBBLOXVFMJQ-UHFFFAOYSA-N 0.000 title claims abstract description 4
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 title claims abstract description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 44
- 229910002370 SrTiO3 Inorganic materials 0.000 claims abstract description 32
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 9
- 239000008367 deionised water Substances 0.000 claims abstract description 4
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- 239000010936 titanium Substances 0.000 claims description 9
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 229910003705 H2Ti3O7 Inorganic materials 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 229910052719 titanium Inorganic materials 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910020293 Na2Ti3O7 Inorganic materials 0.000 claims description 4
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 206010013786 Dry skin Diseases 0.000 claims description 3
- 238000000137 annealing Methods 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 11
- 238000005516 engineering process Methods 0.000 description 5
- 239000002131 composite material Substances 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 238000005352 clarification Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 238000001453 impedance spectrum Methods 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 229910021642 ultra pure water Inorganic materials 0.000 description 2
- 239000012498 ultrapure water Substances 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- 206010034960 Photophobia Diseases 0.000 description 1
- 229910002367 SrTiO Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003814 drug Substances 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
- 208000013469 light sensitivity Diseases 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002055 nanoplate Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Classifications
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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
- B01J23/10—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of rare earths
-
- 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)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention provides a kind of preparation method of strontium titanium dioxide/strontium titanate nano heterojunction, is with TiO2Nanometer sheet and Sr (NO3)2·8H2O is raw material, occurs what is obtained after hydro-thermal reaction in deionized water；The condition of the hydro-thermal reaction is 180 DEG C, 120 minutes.The present invention also provides the Sr TiO prepared using this method2/SrTiO3Nano heterojunction and its application.The present invention is successfully by Sr2+Mix TiO2/SrTiO3In, improve TiO2Photo-generated carrier separative efficiency, Sr2+Doping improve TiO2/SrTiO3Photoelectrochemical behaviour, Sr TiO2/SrTiO3Nanometer sheet heterojunction material has good application in terms of photochemical catalyzing.
Description
Technical field
The present invention relates to a kind of preparation of the semi-conducting material of doping, more particularly to a kind of Sr-TiO2/SrTiO3Nanometer is different
Matter knot and preparation method thereof.
Background technology
One-dimensional nano structure, is all that scholars further investigate all the time due to its interesting characteristic and unique application
Theme.TiO2As a kind of important transition metal oxide, due to its environmental protection, biological medicine, photoelectric sensor,
The extensive use in the fields such as photocatalysis and receive much concern.But at present to the TiO with different-shape and size2The research of material
With require that for expanding day by day using can not be met in many fields.In order to expand TiO2Performance, doping or and other
Material formation hetero-junctions is to improve TiO2A kind of effective way, the especially doping with transition metal and oxide.In recent years
To have synthesized many TiO2Material, TiO2Composite can show the new chemistry and thing not available for single material
Rationality matter, this may produce the performance of novelty in the application of many technologies.In the composite, to doped metallic oxide
TiO2Research and applying had a wide range of applications in catalyst field.
The nano material of various dimensions is compared with undoped with material, because it is in electricity, optics, calorifics and mechanical property
Significant, and attracted extensive concern.With the further development of nanometer science and technology, composite nano materials are also extensive
Using preparing electrochemical sensing and bio-sensing.In metal oxide, TiO2Nanometer sheet there is unique performance, such as：It is good
Biocompatibility and light sensitivity, be expected to be used for photochemical catalyzing etc..
The content of the invention
In order to solve problems of the prior art, the present invention provides a kind of Sr-TiO2/SrTiO3Nano heterojunction and
Its preparation method and application.
The present invention provides a kind of Sr-TiO2/SrTiO3The preparation method of nano heterojunction, is with TiO2Nanometer sheet and Sr
(NO3)2·8H2O is raw material, occurs what is obtained after hydro-thermal reaction in deionized water；The condition of the hydro-thermal reaction is 180 DEG C,
60 minutes.
Preferably, the TiO2The preparation method of nanometer sheet is：
（1）The titanium sheet cleaned up is put into polytetrafluoroethyllining lining reactor, the NaOH aqueous solution is added, hydro-thermal is carried out anti-
Should, reaction temperature is 180 DEG C, and the reaction time is 120 minutes, after cleaning-drying, obtains the Na of black2Ti3O7Nanometer sheet；Will
Na2Ti3O7Nanometer sheet is immersed in a period of time in HCl, obtains H2Ti3O7Nanometer sheet；
（2）By step（1）Obtained H2Ti3O7Nanometer sheet is warming up to 500 DEG C, heating and thermal insulation 120 minutes, and heating rate is 10 DEG C/
Min, after annealing, the TiO after being annealed2Nanometer sheet.
Preferably, the NaOH and Sr (NO3)2·8H2O mol ratio is：1：0.007.
NaOH serves not only as basic reaction conditions, and participates in reaction as reactive material, carries out corrosion titanium sheet, makes
It must react and obtain Na2Ti3O7Nanometer sheet, this material is to prepare TiO2The presoma of nanometer sheet.NaOH and Sr (NO3)2·8H2O is protected
Holding aforementioned proportion is conducive to reaction to obtain the uniform Sr-TiO of pattern2/SrTiO3Nanometer sheet hetero-junctions.
Preferably, TiO2Nanometer sheet and Sr (NO3)2·8H2O is carried out after hydro-thermal reaction in deionized water, cools down 30 points
Clock, then successively with redistilled water and absolute ethanol washing for several times after, in 60 DEG C of -70 DEG C of dryings 6 hours.
The present invention also provides the Sr-TiO prepared using the above method2/SrTiO3Nano heterojunction.
The present invention also provides Sr-TiO2/SrTiO3Application of the nano heterojunction in photochemical catalyzing.
The present invention is successfully by Sr2+Mix TiO2/SrTiO3In, improve TiO2Photo-generated carrier separative efficiency,
Sr2+Doping improve TiO2/SrTiO3Photoelectrochemical behaviour, Sr-TiO2/SrTiO3Nanometer sheet heterojunction material is urged in light
There is good application in terms of changing decomposition water.
Brief description of the drawings
Accompanying drawing is used for providing a further understanding of the present invention, and constitutes a part for specification, the reality with the present invention
Applying example is used to explain the present invention together, is not construed as limiting the invention.In the accompanying drawings：
Fig. 1 is TiO of the invention2The scanning electron microscope diagram of nanometer sheet；
Fig. 2 is Sr-TiO of the invention2/SrTiO3The low power electron microscope picture of nanometer sheet hetero-junctions；
Fig. 3 is Sr-TiO of the invention2/SrTiO3The high power electron microscope picture of nanometer sheet hetero-junctions；
The TiO of Fig. 4 present invention2Nanometer sheet and Sr-TiO2/SrTiO3The i-t curve figures of nanometer sheet hetero-junctions；
The TiO of Fig. 5 present invention2Nanometer sheet and Sr-TiO2/SrTiO3The impedance spectra of nanometer sheet hetero-junctions.
Embodiment
Following embodiment facilitates a better understanding of the present invention, but does not limit the present invention.Experiment in following embodiments
Method, unless otherwise specified, is conventional method.Test material used, unless otherwise specified, is city in following embodiments
Sell.
Embodiment 1
The Sr-TiO of the present invention2/SrTiO3The preparation method of nano heterojunction is：
（1）Cut titanium foil and cleaning titanium sheet；
Titanium foil is cut into the square of the cm sizes of 2.5 cm × 1.5 first, titanium sheet is obtained, is first washed three times, existed every time with detergent
Ultrasonic 20 min in ultrasonic wave, removes surface and oil contaminant, is then cleaned by ultrasonic successively in acetone, ultra-pure water, absolute ethyl alcohol, every time
20 min.Above cleaning process uses ultrapure water surface in triplicate, then, finally uses N2Drying is with standby.
（2）Weigh 4.0 g NaOH to be dissolved in 100 mL redistilled waters, form uniform solution, it is alkaline anti-to produce
Answer condition.A piece of titanium sheet is put into polytetrafluoroethyllining lining reactor, the NaOH aqueous solution that 10mL is prepared is added, then stirs again
Mix to solution clarification, autoclave is put into baking oven, controlling reaction temperature is 180 DEG C, after the min of hydro-thermal reaction 120, is taken
Go out reactor, cool down 30 minutes, natural cooling can be taken or cooling is forced.Redistilled water and nothing are used successively with gained sample
It is dry 6-10 hours at 60 DEG C -70 DEG C after water-ethanol washing for several times, obtain the Na of black2Ti3O7Nanometer sheet.By this Na2Ti3O7
Nanometer sheet is immersed in 120 min in the HCl that 100 mL concentration are 0.6 mol/L, it is therefore an objective to so that Na+And H+Swap, obtain
To H2Ti3O7Nanometer sheet.Autoclave used can be any kind of autoclave in reaction, as long as it disclosure satisfy that this
The requirement of inventive method.
（3）By step（2）By resulting H2Ti3O7Nanometer sheet is put into tube furnace, is warming up to 500 DEG C, and heating rate is
10 DEG C/min, carry out the min of heating and thermal insulation 120, after annealing, the TiO after being annealed2Nanometer sheet.
Fig. 1 is TiO of the invention2The scanning electron microscope diagram of nanometer sheet；We can see that prepared from figure
Material is laminated structure, and topographic profile does not occur reunion or other structures uniformly, and it is successfully to prepare to illustrate laminated structure
's.
（4）By 0.25 g Sr (NO3)2·8H2O is added in 40mL deionized waters, and stirring is added into solution clarification
Contain a piece of step（3）In the polytetrafluoroethyllining lining reactor of the titanium dioxide nanoplate of preparation, at 180 DEG C, hydro-thermal is anti-
Answer after 60 minutes, take out reactor, cool down 30 minutes.Gained sample uses redistilled water and absolute ethanol washing for several times successively
Afterwards, in 60 DEG C of -70 DEG C of dryings 6 hours, the Sr-TiO of black is obtained2/SrTiO3Nanometer sheet hetero-junctions.
Fig. 2 is Sr-TiO of the invention2/SrTiO3The low power electron microscope picture of nanometer sheet hetero-junctions；We can from figure
To find out, substantially occur one layer of white SrTiO in laminated structure3Particle, these are evengranular to be distributed in nanometer sheet, explanation
Sr-TiO2/SrTiO3Nanometer sheet hetero-junctions is successfully prepared.
Fig. 3 is Sr-TiO of the invention2/SrTiO3The high power electron microscope picture of nanometer sheet hetero-junctions.From its high power figure
In we can see that prepared SrTiO3The size of nano-particle is 40-50 nm.
Under the G illumination of AM 1.5, using Pt pieces as to electrode, saturated calomel electrode is as reference electrode, with preparation
Different sample thin films（That is step（3）The TiO of preparation2Nanometer sheet and step（4）The Sr-TiO of preparation2/SrTiO3Nanometer sheet is heterogeneous
Knot）As working electrode, 1.0 M NaOH are electrolyte, the i- measured on CHI660 work stations from i-t curve technologies
T curve curves.
Fig. 4 is TiO of the invention2Nanometer sheet and Sr-TiO2/SrTiO3The i-t curve figures of nanometer sheet hetero-junctions.From figure
Middle contrast, it has been found that Sr-TiO2/SrTiO3The electric current of nanometer sheet hetero-junctions is than original TiO2The current density of nanometer sheet is big,
Further demonstrate that this composite prepared by the present invention is expected to be applied to photochemical catalyzing.
Under the G illumination of AM 1.5, using Pt pieces as to electrode, saturated calomel electrode is as reference electrode, with preparation
Different sample thin films（That is step（3）The TiO of preparation2Nanometer sheet and step（4）The Sr-TiO of preparation2/SrTiO3Nanometer sheet is heterogeneous
Knot）As working electrode, 1.0 M NaOH are electrolyte, and A.C Impedance technologies are selected on CHI660 work stations,
0.5V vs Hg/HgCl2The electrochemical impedance spectrogram measured.
Fig. 5 is TiO of the invention2Nanometer sheet and Sr-TiO2/SrTiO3The impedance spectra of nanometer sheet hetero-junctions.From figure I
Can draw, Sr-TiO2/SrTiO3Than original TiO2The resistance of nanometer sheet is small, illustrates Sr-TiO2/SrTiO3Nanometer sheet is different
Matter knot and Sr2+Doping further increases its separation of charge, so which raises electric conductivity.
Finally it should be noted that：The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention,
Although the present invention is described in detail with reference to the foregoing embodiments, for a person skilled in the art, it still may be used
To be modified to the technical scheme described in foregoing embodiments, or to which part technical characteristic progress equivalent.
Within the spirit and principles of the invention, any modifications, equivalent substitutions and improvements made etc., should be included in the present invention's
Within protection domain.
Claims (6)
1. a kind of preparation method of strontium-titanium dioxide/strontium titanate nano heterojunction, it is characterised in that：It is with TiO2Nanometer sheet and Sr
(NO3)2·8H2O is raw material, occurs what is obtained after hydro-thermal reaction in deionized water；The condition of the hydro-thermal reaction is 180 DEG C,
60 minutes.
2. according to the method described in claim 1, it is characterised in that：The TiO2The preparation method of nanometer sheet is：
（1）The titanium sheet cleaned up is put into polytetrafluoroethyllining lining reactor, the NaOH aqueous solution is added, hydro-thermal is carried out anti-
Should, reaction temperature is 180 DEG C, and the reaction time is 120 minutes, after cleaning-drying, obtains the Na of black2Ti3O7Nanometer sheet；Will
Na2Ti3O7Nanometer sheet is immersed in a period of time in HCl solution, obtains H2Ti3O7Nanometer sheet；
（2）By step（1）Obtained H2Ti3O7Nanometer sheet is warming up to 500 DEG C, heating and thermal insulation 120 minutes, and heating rate is 10 DEG C/
Min, after annealing, the TiO after being annealed2Nanometer sheet.
3. method according to claim 2, it is characterised in that：The NaOH and Sr (NO3)2·8H2O mol ratio is：1：
0.007。
4. according to any described methods of claim 1-3, it is characterised in that：TiO2Nanometer sheet and Sr (NO3)2·8H2O go from
Carry out after hydro-thermal reaction, cool down 30 minutes in sub- water, after redistilled water and absolute ethanol washing are then used successively for several times, 60
DEG C of -70 DEG C dryings 6 hours.
5. the Sr-TiO that any described methods of application claim 1-4 are prepared2/SrTiO3Nano heterojunction.
6. the Sr-TiO described in claim 52/SrTiO3Application of the nano heterojunction in photochemical catalyzing.
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| CN107670692A (en) * | 2017-11-06 | 2018-02-09 | 常州大学 | A kind of Z-type SrTiO3@TiO2/ ATP hetero-junctions composite denitration catalyst and its preparation method and application |
| CN113713814A (en) * | 2021-09-06 | 2021-11-30 | 齐鲁工业大学 | Au/SrTiO3/TiO2Hollow nano-sphere photocatalytic material, and preparation method and application thereof |
| CN115007128A (en) * | 2022-06-28 | 2022-09-06 | 山东大学 | SrTiO 3 /TiO 2 Hetero-epitaxial photocatalyst and preparation method and application thereof |
| CN115532249A (en) * | 2022-08-26 | 2022-12-30 | 南昌航空大学 | Method for preparing heterojunction by utilizing in-situ load |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107617435A (en) * | 2017-10-31 | 2018-01-23 | 上海师范大学 | A kind of SrTiO3Titanium oxide nanotubes heterojunction photocatalyst of load and its preparation method and application |
| CN107670692A (en) * | 2017-11-06 | 2018-02-09 | 常州大学 | A kind of Z-type SrTiO3@TiO2/ ATP hetero-junctions composite denitration catalyst and its preparation method and application |
| CN107670692B (en) * | 2017-11-06 | 2020-02-14 | 常州大学 | Z-type SrTiO3@TiO2ATP heterojunction composite denitration catalyst and preparation method and application thereof |
| CN113713814A (en) * | 2021-09-06 | 2021-11-30 | 齐鲁工业大学 | Au/SrTiO3/TiO2Hollow nano-sphere photocatalytic material, and preparation method and application thereof |
| CN115007128A (en) * | 2022-06-28 | 2022-09-06 | 山东大学 | SrTiO 3 /TiO 2 Hetero-epitaxial photocatalyst and preparation method and application thereof |
| CN115007128B (en) * | 2022-06-28 | 2023-11-10 | 山东大学 | SrTiO 3 /TiO 2 Heteroepitaxial photocatalyst and preparation method and application thereof |
| CN115532249A (en) * | 2022-08-26 | 2022-12-30 | 南昌航空大学 | Method for preparing heterojunction by utilizing in-situ load |
| CN117504892A (en) * | 2023-12-14 | 2024-02-06 | 中国水产科学研究院渔业机械仪器研究所 | La-Fe co-doped SrTiO 3 /TiO 2 Composite material, preparation method and application thereof |
| CN117504892B (en) * | 2023-12-14 | 2024-04-30 | 中国水产科学研究院渔业机械仪器研究所 | La-Fe co-doped SrTiO3/TiO2Composite material, preparation method and application thereof |
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