CN106955695B - 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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- 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 42
- 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 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 9
- 239000008367 deionised water Substances 0.000 claims abstract description 5
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 5
- 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
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 239000010936 titanium Substances 0.000 claims description 11
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 8
- 238000001816 cooling Methods 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
- 239000012153 distilled water Substances 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 5
- 229910003705 H2Ti3O7 Inorganic materials 0.000 claims description 4
- 229910020293 Na2Ti3O7 Inorganic materials 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000000137 annealing Methods 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 229960000935 dehydrated alcohol Drugs 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
- 238000002242 deionisation method Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 11
- 239000002131 composite material Substances 0.000 description 4
- 238000005516 engineering process Methods 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
- 206010013786 Dry skin Diseases 0.000 description 2
- 238000004140 cleaning 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
- 238000011160 research Methods 0.000 description 2
- 239000011734 sodium Substances 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
- QBUKAFSEUHGMMX-MTJSOVHGSA-N (5z)-5-[[3-(1-hydroxyethyl)thiophen-2-yl]methylidene]-10-methoxy-2,2,4-trimethyl-1h-chromeno[3,4-f]quinolin-9-ol Chemical class C1=CC=2NC(C)(C)C=C(C)C=2C2=C1C=1C(OC)=C(O)C=CC=1O\C2=C/C=1SC=CC=1C(C)O QBUKAFSEUHGMMX-MTJSOVHGSA-N 0.000 description 1
- 206010034960 Photophobia Diseases 0.000 description 1
- 229910002367 SrTiO Inorganic materials 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
- 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
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 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
- 239000000203 mixture Substances 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
- 239000000126 substance Substances 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
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000005406 washing 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
- B01J23/10—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of rare earths
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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
- 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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- 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, is obtained after generation 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 being 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 semiconductor material of doping more particularly to a kind of Sr-TiO2/SrTiO3Nanometer is different
Matter knot and preparation method thereof.
Background technique
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 be concerned.But at present to the TiO with different-shape and size2The research of material
The requirement being growing has not been able to satisfy in many fields with application.In order to expand TiO2Performance, doping or and other
It is to improve TiO that material, which forms hetero-junctions,2A kind of effective way, the especially doping with transition metal and oxide.In recent years
To have synthesized many TiO2Material, TiO2Composite material can show chemistry and object new not available for single material
Rationality matter, this may generate novel performance in many technical applications.In the composite, to doped metallic oxide
TiO2Research and applying have a wide range of applications in catalyst field.
The nano material of various dimensions is compared with undoped with material, since 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 have unique performance, such as: good
Biocompatibility and light sensitivity, be expected to be used for photochemical catalyzing etc..
Summary of the invention
In order to solve the problems in the existing technology, the present invention provides a kind of Sr-TiO2/SrTiO3Nano heterojunction and
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, is obtained after generation hydro-thermal reaction in deionized water；The condition of the hydro-thermal reaction is 180 DEG C,
60 minutes.
Preferably, the TiO2Nanometer sheet the preparation method comprises the following steps:
(1) titanium sheet cleaned up is put into polytetrafluoroethyllining lining reaction kettle, NaOH aqueous solution is added, carry out hydro-thermal
Reaction, reaction temperature are 180 DEG C, and the reaction time is 120 minutes, after cleaning-drying, obtain the Na of black2Ti3O7Nanometer sheet；It will
Na2Ti3O7Nanometer sheet is immersed in a period of time in HCl, obtains H2Ti3O7Nanometer sheet；
(2) H for obtaining step (1)2Ti3O7Nanometer sheet is warming up to 500 DEG C, and heating and thermal insulation 120 minutes, heating rate was
10 DEG C/min, the TiO after annealing, after being annealed2Nanometer sheet.
Preferably, the NaOH and Sr (NO3)2·8H2The molar ratio of O are as follows: 1:0.007.
Sodium hydroxide serves not only as basic reaction conditions, and participates in reacting as reactive material, carries out corrosion titanium sheet, makes
It must react to obtain Na2Ti3O7Nanometer sheet, this substance are to prepare TiO2The presoma of nanometer sheet.NaOH and Sr (NO3)2·8H2O is protected
Hold aforementioned proportion be conducive to reaction obtain Sr-TiO of uniform morphology2/SrTiO3Nanometer sheet hetero-junctions.
Preferably, TiO2Nanometer sheet and Sr (NO3)2·8H2It is 30 points cooling after O carries out hydro-thermal reaction in deionized water
Clock, after then successively being washed for several times with secondary distilled water and dehydrated alcohol, 60 DEG C -70 DEG C of dryings 6 hours.
The present invention also provides the Sr-TiO being 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
Changing in terms of decomposing water has good application.
Detailed description of the invention
Attached drawing is used to provide further understanding of the present invention, and constitutes part of specification, with reality of the invention
It applies example to be used to explain the present invention together, not be 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；
TiO Fig. 4 of the invention2Nanometer sheet and Sr-TiO2/SrTiO3The i-t curve of nanometer sheet hetero-junctions schemes；
TiO Fig. 5 of the invention2Nanometer sheet and Sr-TiO2/SrTiO3The impedance spectra of nanometer sheet hetero-junctions.
Specific embodiment
Embodiment below facilitates a better understanding of the present invention, but does not limit the present invention.Experiment in following embodiments
Method is unless otherwise specified conventional method.Test material as used in the following examples is unless otherwise specified city
It sells.
Embodiment 1
Sr-TiO of the invention2/SrTiO3Nano heterojunction the preparation method comprises the following steps:
(1) titanium foil and cleaning titanium sheet are cut；
Titanium foil is cut into the square of the cm size of 2.5 cm × 1.5 first, obtains titanium sheet, is first washed three times with detergent, often
Secondary 20 min of ultrasound in ultrasonic wave remove surface and oil contaminant, are then successively cleaned by ultrasonic in acetone, ultrapure water, dehydrated alcohol,
20 min every time.The above cleaning process in triplicate, then uses ultrapure water surface, finally uses N2Drying is with spare.
(2) 4.0 g NaOH are weighed to be dissolved in 100 mL secondary distilled waters, forms uniform solution, it is anti-to generate alkalinity
Answer condition.A piece of titanium sheet is put into polytetrafluoroethyllining lining reaction kettle, the NaOH aqueous solution that 10mL is prepared is added, then stirs again
It mixes to solution and clarifies, autoclave is put into baking oven, control reaction temperature is 180 DEG C, after 120 min of hydro-thermal reaction, is taken
Reaction kettle out, it is 30 minutes cooling, natural cooling can be taken or force cooling.Secondary distilled water and nothing are successively used with gained sample
It is 6-10 hours dry 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+It swaps, obtains
To H2Ti3O7Nanometer sheet.Autoclave used in reaction can be any kind of autoclave, as long as it can satisfy this
The requirement of inventive method.
(3) by step (2) by obtained H2Ti3O7Nanometer sheet is put into tube furnace, is warming up to 500 DEG C, and heating rate is
10 DEG C/min, carry out 120 min of heating and thermal insulation, the TiO after annealing, after being annealed2Nanometer sheet.
Fig. 1 is TiO of the invention2The scanning electron microscope diagram of nanometer sheet；From the figure we can see that prepared
Material is laminated structure, and topographic profile does not occur reunion or other structures uniformly, illustrates that laminated structure is successfully to prepare
's.
(4) by 0.25 g Sr (NO3)2·8H2O is added in 40mL deionized water, and stirring to solution is clarified, and is added into
In the polytetrafluoroethyllining lining reaction kettle of titanium dioxide nanoplate containing a piece of step (3) preparation, at 180 DEG C, hydro-thermal is anti-
Reaction kettle should be taken out after sixty minutes, it is 30 minutes cooling.Gained sample is successively washed for several times with secondary distilled water and dehydrated alcohol
Afterwards, 60 DEG C -70 DEG C of dryings 6 hours, obtain the Sr-TiO of black2/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
Obviously occur one layer of white SrTiO to find out, 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 nanoparticle is 40-50 nm.
Under 1.5 G illumination of AM, using Pt piece as to electrode, saturated calomel electrode is as reference electrode, with preparation
Different sample thin film (the i.e. TiO of step (3) preparation2The Sr-TiO of nanometer sheet and step (4) preparation2/SrTiO3Nanometer sheet is heterogeneous
Knot) it is used as working electrode, 1.0 M NaOH are electrolyte, the i- for selecting i-t curve technology to measure on CHI660 work station
T curve curve.
Fig. 4 is TiO of the invention2Nanometer sheet and Sr-TiO2/SrTiO3The i-t curve of nanometer sheet hetero-junctions schemes.From figure
Middle comparison, 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 material prepared by the present invention is expected to be applied to photochemical catalyzing.
Under 1.5 G illumination of AM, using Pt piece as to electrode, saturated calomel electrode is as reference electrode, with preparation
Different sample thin film (the i.e. TiO of step (3) preparation2The Sr-TiO of nanometer sheet and step (4) preparation2/SrTiO3Nanometer sheet is heterogeneous
Knot) it is used as working electrode, 1.0 M NaOH are electrolyte, A.C Impedance technology is selected on CHI660 work station,
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
It can be concluded that, Sr-TiO2/SrTiO3Than original TiO2The resistance value of nanometer sheet is small, illustrates Sr-TiO2/SrTiO3Nanometer sheet is different
Matter knot and Sr2+Doping further improves its separation of charge, to make which raises electric conductivity.
Finally, it should be noted that the foregoing is only a preferred embodiment of the present invention, it is not intended to restrict the invention,
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features.
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in of the invention
Within protection scope.
Claims (5)
1. a kind of strontium-titanium dioxide/strontium titanate nano heterojunction preparation method, it is characterised in that: be with TiO2Nanometer sheet and Sr
(NO3)2·8H2O is raw material, is obtained after generation hydro-thermal reaction in deionized water；The condition of the hydro-thermal reaction is 180 DEG C,
60 minutes；
The TiO2Nanometer sheet the preparation method comprises the following steps:
(1) titanium sheet cleaned up is put into polytetrafluoroethyllining lining reaction kettle, NaOH aqueous solution is added, it is anti-to carry out hydro-thermal
It answers, reaction temperature is 180 DEG C, and the reaction time is 120 minutes, after cleaning-drying, obtains the Na of black2Ti3O7Nanometer sheet；It will
Na2Ti3O7Nanometer sheet is immersed in a period of time in HCl solution, obtains H2Ti3O7Nanometer sheet；
(2) H for obtaining step (1)2Ti3O7Nanometer sheet is warming up to 500 DEG C, and heating and thermal insulation 120 minutes, heating rate is 10 DEG C/
Min, the TiO after annealing, after being annealed2Nanometer sheet.
2. the method according to claim 1, it is characterised in that: the NaOH and Sr (NO3)2·8H2The molar ratio of O
Are as follows: 1:0.007.
3. method according to claim 1 or 2, it is characterised in that: TiO2Nanometer sheet and Sr (NO3)2·8H2O is in deionization
It is 30 minutes cooling after carrying out hydro-thermal reaction in water, after then successively being washed for several times with secondary distilled water and dehydrated alcohol, 60
DEG C -70 DEG C drying 6 hours.
4. the Sr-TiO being prepared using method of any of claims 1 or 22/SrTiO3Nano heterojunction.
5. Sr-TiO as claimed in claim 42/SrTiO3Application of the nano heterojunction in photochemical catalyzing.
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| 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 |
| 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 |
| 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 |
| 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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