CN107601557A - One kind prepares 1T@2H MoS2/ black TiO2Method - Google Patents
One kind prepares 1T@2H MoS2/ black TiO2Method Download PDFInfo
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- CN107601557A CN107601557A CN201710938537.6A CN201710938537A CN107601557A CN 107601557 A CN107601557 A CN 107601557A CN 201710938537 A CN201710938537 A CN 201710938537A CN 107601557 A CN107601557 A CN 107601557A
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Abstract
The present invention discloses one kind and prepares 1T@2H MoS2/ black TiO2The method of core shell structure, the preparation method include, and first, using alcohol as solvent, white vitriol, butyl titanate are stirred into 2h, 200 DEG C of reaction 24h of regulation temperature, that is, obtain TiO2Micron ball；Secondly, using deionized water as solvent, the TiO that will be prepared2Micron ball, ammonium heptamolybdate and thiocarbamide stirring 1h, 200 DEG C of reaction 20h of regulation temperature, that is, obtain 1T 2H MoS2/TiO2Core shell structure；Finally, by equivalent 1T@2H MoS2/TiO2Core shell structure and NaBH4After powder mull, 350 DEG C of calcining 3h, that is, obtain 1T 2H MoS in argon gas2/ black TiO2Core shell structure.The inventive method is simple to operate, reproducible, and cost is low, and gained sample topography is uniform.
Description
Technical field
The invention belongs to Nano semiconductor field of compounding, and in particular to prepare 1T@2H-MoS2/ black TiO2Core shell structure
Method.
Background technology
At present, black TiO2As a kind of semi-conducting material with multiple functions characteristic be widely used to photocatalysis,
Optical electro-chemistry sensor, Li+The fields such as rechargeable battery, super resistor- capacitor, Flied emission, energy battery and microwave absorption.It is black
Color TiO2Energy gap is narrower, it is seen that light absorpting ability is stronger.Change black TiO2Pattern have to its photocatalysis property it is important
Influence, including nano wire, nanometer rods, nano particle, micron ball etc. reported by different researchers.In photocatalytic applications
In, black TiO2The advantage of micron ball is mainly reflected in following three aspects：First, specific surface area is big, there is provided more reactions is lived
Property site, absorb more visible ray in sunshine；Second, density is low, the possibility of particle agglomeration is reduced, promotes material surface
Carrier is combined with corresponding electron acceptor and electron donor, and then redox reaction occurs；Third, Lacking oxygen is more, have
Effect improves the separation in light induced electron and hole, lifts photocatalysis effect.Therefore, black TiO is prepared2Micron ball is in photocatalysis
It will be with a wide range of applications.
It is numerous at present to prepare black TiO2Method, common preparation method has：1 HTHP or normal pressure hydrogenation
Method；2 chemical reduction methods；3 chemical oxidization methods.
Now preparation method is summarized as follows：
1. HTHP or normal pressure hydrogenation method：Chen et al. [1] is under 200 DEG C of bar pressure conditions of hydrogen environment 20 to white
TiO2Hydrogenation treatment obtains black TiO in 5 days2；He et al. is using 6 % hydrogen and 94 % nitrogen as gaseous mixture, under the conditions of 350 DEG C
The h of calcinated titanium dioxide nano wire 2 obtains black TiO2Nano wire.
2. chemical reduction method：Zhu et al. [3] is by TiO2Nano particle and aluminium powder are respectively at 800 DEG C and 300 ~ 600
It is placed under the conditions of DEG C in binary channels tube furnace and calcines 4 h and obtain black TiO2Nano particle.
3. chemical oxidization method：Grabstanowicz et al. [4] is added to titanium hydride powders with hydrogen peroxide as strong oxidizer
In at 100 DEG C react 12 ~ 20 h, obtain black TiO in 630 DEG C of ar gas environment calcining, 3 h afterwards2Powder.
4. other method：Li et al. [5] is by TiO2450 DEG C of 4 h of calcining of nanotube, are including 0.27 wt% afterwards
NH4The s of 40 V voltage responses 200 obtains black TiO in F ethylene glycol solution2Nanotube.
MoS2Because its unique layer structure is widely used to include luminescence generated by light, lithium ion battery, Flied emission, biography
The fields such as sensor, catalysis.MoS2Crystal structure mainly has two kinds of 1T phases and 2H phases.1T@2H-MoS2Have in photocatalysis field huge
Application potential.First, 2H phase have narrow gap semiconductor property, can directly absorb the visible ray in sunshine；Second, 1T phase
With metalline, the transfer that can accelerate light induced electron as co-catalyst promotes redox reaction；3rd, 1T phase and 2H phases
Cooperative effect is combined to form, effectively suppresses compound, the raising photocatalytic pollutant degradation in electronics and hole pair.Therefore, prepare
The MoS of two-phase coexistent2（1T@2H-MoS2）Good application prospect in photocatalysis field be present.
Existing numerous preparation 1T phases, 2H phases and 1T@2H-MoS at present2Method, common preparation method has：1 chemistry stripping
From method；2 critical CO2Revulsion；3 ball-milling methods.
Now preparation method is summarized as follows：
1. chemical stripping method:Wu et al. [6] is by adding Li super hydride in body phase MoS2In, through processing such as ultrasound, strippings
Obtain the MoS containing different phase structures2.Lukowski et al. [7] is chemical from 2H phase molybdenum disulfide block by lithium ion intercalation
1T phases are peeled off, it is grown directly upon in graphene nano structure.
2. critical CO2Revulsion:Qi et al. [8] is preferably outside using CO 2 supercritical carbon dioxide as one
Stimulation expands 2H phase molybdenum disulfide interlamellar spacing, forms 1T phases, has obtained the molybdenum disulfide of two-phase coexistent.
3. ball-milling method:1T@2H-MoS are prepared by ball milling molybdenum disulfide powder in Cheng et al. [9]2。
From above-mentioned report, existing black TiO2With 1T@2H-MoS2Compound document is less, is mostly to prepare black TiO2Or
1T@2H-MoS2Pure item.It is existing to prepare black TiO2Or 1T@2H-MoS2Method：Complex operation, Part Methods need hydrogen,
Condition is whard to control and potential safety hazard be present.For other method, hydro-thermal method and chemical reduction method it is simple to operate, without hydrogen
Gas, it is inexpensive, pollution-free, it is a kind of method beneficial to industrialized production.
The content of the invention
It is an object of the invention to provide be that a kind of hydro-thermal method prepares 1T@2H-MoS2/ black TiO2Method.
Hydro-thermal method advantage：
（1）Good dispersion, the high nano material of crystallinity can be directly obtained；
（2）Reaction is carried out in enclosed system, so as to avoid component volatilization；
（3）The stoichiometric(al) and structural form of product are controlled well；
（4）Powder sample caused by avoiding high temperature sintering is reunited；
（5）Reaction temperature is relatively low.
The present invention is realized by following technical process：
In hydrothermal reaction kettle, first, using alcohol as solvent, white vitriol, butyl titanate are stirred into 2 h, adjust temperature 200
DEG C 24 h of reaction, after naturally cooling to room temperature, centrifugation is repeatedly washed with deionized water, then dry in 70 DEG C of vacuum drying chambers
Dry 8 h, that is, obtain TiO2Micron ball；Secondly, using deionized water as solvent, the TiO that will be prepared2Micron ball, ammonium heptamolybdate and
Thiocarbamide stirs 1 h, and 200 DEG C of 20 h of reaction of regulation temperature, after naturally cooling to room temperature, with deionized water, absolute ethyl alcohol is repeatedly washed
Centrifugation is washed, 8 h are dried in 60 DEG C of vacuum drying chambers, that is, obtain 1T 2H-MoS2/TiO2Core shell structure；Finally, by equivalent 1T@
2H-MoS2/TiO2Core shell structure and NaBH4After powder mull, calcined in argon gas, that is, obtain 1T 2H-MoS2/ black TiO2Core
Shell structure.
It is easy to spread meanwhile the inventive method is simple to operate, it is suitable for large-scale industrial production.
Brief description of the drawings
Fig. 1 is embodiment 1, the XRD of embodiment 2.
Fig. 2 is that the SEM of embodiment 1 schemes.
Fig. 3 is that the HRTEM of embodiment 1 schemes.
Fig. 4 is that the SEM of embodiment 2 schemes.
Fig. 5 is that the HRTEM of embodiment 2 schemes.
Fig. 6 is the XRD spectra of embodiment 3.
Fig. 7 is that the SEM of embodiment 3 schemes.
Fig. 8 is EDS (Mapping) figure of embodiment 3.
Embodiment
The present invention is described in further details below in conjunction with drawings and examples.
Embodiment 1
1 g white vitriol is dissolved in 60 ml absolute ethyl alcohol, be placed in 50 ml polytetrafluoroethyllining lining,
Continuing magnetic force stirs 1 h or so at room temperature；Above-mentioned solution is added dropwise in 4 ml butyl titanate, forms colloidal solution, is protected
The h of magnetic agitation 1 is held, stirring finishes, and liner is transferred in supporting autoclave and sealed, and is placed in 200 DEG C of drying box
It is incubated 24 h；After naturally cooling to room temperature, centrifugation is repeatedly washed with deionized water, 8 are then dried in 70 DEG C of vacuum drying chambers
H, and collect and obtain TiO2Sample.As shown in figure 1, the XRD for gained sample.As a result it is Anatase to show products therefrom
TiO2, its diffraction maximum is consistent with PDF# 21-1272 cards；As shown in Fig. 2 scheme for the SEM of gained sample；As shown in figure 3, it is
The HRTEM figures of gained sample, as a result show that sample lattice fringe is clear, sample interplanar distance is 0.35nm, illustrates sample crystallization
It is functional.
Embodiment 2
The thiocarbamide of 1 mmol ammonium heptamolybdate and 15 mmol is dissolved in 35 ml deionized water, is placed in the poly- of 50 ml
In tetrafluoroethene liner, continuing magnetic force stirs 20 min or so at room temperature, forms uniform settled solution.Stirring finishes, will
Liner is transferred in supporting autoclave and sealed, and is placed in being incubated 20 h in 200 DEG C of drying box, after naturally cooling to room temperature,
With deionized water, absolute ethyl alcohol repeatedly washs centrifugation.Then 8 h are dried in 60 DEG C of vacuum drying chambers, and collects and obtains 1T@
2H-MoS2Sample.As shown in figure 1, being the XRD of gained sample, as a result show what products therefrom coexisted for 1T phases with 2H phases
MoS2, its diffraction maximum is consistent with PDF#37-1492 cards.As shown in figure 4, scheming for the SEM of gained sample, show prepared by this technique
Product be nano flower.As shown in figure 5, scheming for HRTEM, 1T-MoS is as a result shown2Interplanar distance be 0.27 nm, 2H-MoS2
Interplanar distance be 0.30 nm, illustrate that sample crystallization is functional.
Embodiment 3
The thiocarbamide of 1 mmol ammonium heptamolybdate and 15 mmol is dissolved in 35 ml deionized water, is placed in the poly- of 50 ml
In tetrafluoroethene liner, continuing magnetic force stirs 20 min or so at room temperature, forms uniform settled solution, prepared by 1 mmol
Obtained TiO2Sample is added in above-mentioned settled solution, and continuing magnetic force stirs 30 min or so stirrings and finished at room temperature, will
Liner is transferred in supporting autoclave and sealed, and is placed in being incubated 20 h in 200 DEG C of drying box；After naturally cooling to room temperature,
With deionized water, absolute ethyl alcohol repeatedly washs centrifugation, 8 h is then dried in 60 DEG C of vacuum drying chambers, and collect and obtain 1T
2H-MoS2/TiO2Sample.0.5 g black powder sample and 0.5 g sodium borohydrides are put into agate mortar and are fully ground 30
Min or so, sample is contained in ceramic boat and is placed in CVD tube furnaces, is passed through argon gas, in 350 DEG C of h of temperature lower calcination 3,
Naturally room temperature is down to, collection obtains black powder sample.The sample deionized water that will be collected into, absolute ethyl alcohol repeatedly wash from
The heart, 8 h are then dried in 60 DEG C of vacuum drying chambers, and collect and obtain 1T@2H-MoS2/ black TiO2Sample.
Embodiment 4
The thiocarbamide of 1 mmol ammonium heptamolybdate and 15 mmol is dissolved in 35 ml deionized water, is placed in the poly- of 50 ml
In tetrafluoroethene liner, continuing magnetic force stirs 20 min or so at room temperature, forms uniform settled solution, prepared by 3 mmol
Obtained TiO2Sample is added in above-mentioned settled solution, and continuing magnetic force stirs 30 min or so stirrings and finished at room temperature, will
Liner is transferred in supporting autoclave and sealed, and is placed in being incubated 20 h in 200 DEG C of drying box；After naturally cooling to room temperature,
With deionized water, absolute ethyl alcohol repeatedly washs centrifugation, 8 h is then dried in 60 DEG C of vacuum drying chambers, and collect and obtain 1T
2H-MoS2/TiO2Sample.0.5 g black powder sample and 0.5 g sodium borohydrides are put into agate mortar and are fully ground 30
Min or so, sample is contained in ceramic boat and is placed in CVD tube furnaces, is passed through argon gas, 3 h are calcined at 350 DEG C, it is natural
Room temperature is down to, is collected into black powder sample.The sample deionized water that will be collected into, absolute ethyl alcohol repeatedly wash centrifugation, so
8 h are dried in 60 DEG C of vacuum drying chambers afterwards, and collects and obtains 1T@2H-MoS2/ black TiO2Sample.
Embodiment 5
The thiocarbamide of 1 mmol ammonium heptamolybdate and 15 mmol is dissolved in 35 ml deionized water, is placed in the poly- of 50 ml
In tetrafluoroethene liner, continuing magnetic force stirs 20 min or so at room temperature, forms uniform settled solution, prepared by 5 mmol
Obtained TiO2Sample is added in above-mentioned settled solution, and continuing magnetic force stirs 30 min or so stirrings and finished at room temperature, will
Liner is transferred in supporting autoclave and sealed, and is placed in being incubated 20 h in 200 DEG C of drying box；After naturally cooling to room temperature,
With deionized water, absolute ethyl alcohol repeatedly washs centrifugation, 8 h is then dried in 60 DEG C of vacuum drying chambers, and be collected into 1T 2H-
MoS2/TiO2Sample.By 0.5 g 1T@2H-MoS2/TiO2Sample and 0.5 g sodium borohydride are put into agate mortar fully
30 min or so are ground, sample is contained in ceramic boat and is placed in CVD tube furnaces, is passed through argon gas, at a temperature of 350 DEG C
3 h are calcined, are down to room temperature naturally, are collected into black powder sample.The sample deionized water that will be collected into, absolute ethyl alcohol are multiple
Washing centrifugation, then dries 8 h, and be collected into 1T@2H-MoS in 60 DEG C of vacuum drying chambers2/ black TiO2Sample.Such as Fig. 6
It is shown, it is the XRD of sample described in embodiment 3-5, XRD diffraction maximums and PDF# 21-1272 cards and the PDF#37- of each sample
1492 cards are consistent, as Anatase TiO2The MoS coexisted with 1T phases with 2H phases2, show black TiO2It is common with 2H phases with 1T phases
The MoS deposited2Compound success, as shown in fig. 7, scheming for the SEM of the gained sample of embodiment 3.Understand in black TiO2Micron ball surface bag
The MoS that 1T phases coexist with 2H phases is covered2Nanometer sheet.As shown in figure 8, EDS (Mapping) figure for the gained of embodiment 3.Understand
Mo, S, O, Ti element are equally distributed.
Bibliography
[1]X. Chen, L. Liu, P. Y. Yu, S. S. Mao, Increasing solar absorption for
photocatalysis with black hydrogenated titanium dioxide nanocrystals. Science
2011; 331:746.
[2]H. He, K. Yang, N. Wang, F. Luo, H. Chen, Hydrogenated TiO2 film for
enhancing photovoltaic properties of solar cells and self-sensitized effect.
J. Appl. Phys 2013; 114:213505.
[3]G. Zhu, T. Lin, X. Lu, W. Zhao, C. Yang, Z. Wang, H. Yin, Z. Liu, F.
Huang, J. Lin, Black brookite titania with high solar absorption and
excellent photocatalytic performance.J. Mater.Chem. A 2013; 1:9650.
[4]L. R. Grabstanowicz, S. Gao, T. Li, R. M. Rickard, T. Rajh, D.J. Liu,
T. Xu, Facile oxidative conversion of TiH2 to high-concentration Ti3+-self-
doped rutile TiO2 with visible-light photoactivity. Inorg. Chem2013; 52:
3884.
[5]H. Li, Z. Chen, C. K. Tsang, Z. Li, X. Ran, C. Lee, B. Nie, L. Zheng,
T. Hung, J. Lu, B. Pan, Y. Y. Li, Electrochemical doping of anatase TiO2 in
organic electrolytes for high-performance supercapacitors and photocatalysts.J. Mater. Chem.A 2014; 2:229.
[6]PengR, Liang L, Hood Z D, Boulesbaa A, Puretzky A , Ievlev A, Come J,
Ovchinnikova O, Wang HMa C, In-plane heterojunctions enable multiphasic 2D
MoS2 nanosheets as efficient photocatalysts for hydrogen evolution from water
reduction. J.Acs Catalysis 2016; 6(10).
[7]Lukowski. M. A, Daniel. A. S, Meng. F, Forticaux. A, Li. L, Jin. S,
Enhanced hydrogen evolution catalysis from chemically exfoliated metallic
MoS2 Nanosheets. J. Am. Chem. Soc 2013; 135(28):10274-10277.
[8]Yuhang Qi, Qun Xu, Yun Wang, Bo Yan, Yumei Ren, Zhimin Chen. CO2-
induced phase engineering: protocol for enhanced photoelectrocatalytic
performance of 2D MoS2 nanosheets. ACS Nano 2016; 10:2903−2909.
[9]Cheng P, Sun K, Hu Y H, Mechanically-induced reverse phase
transformation of MoS2 from stable 2H to metal stable 1T and its memristive
behavior. J. Rsc Advances 2016; 6(70).
Claims (3)
1. one kind prepares 1T@2H-MoS2/ black TiO2The method of core shell structure, the preparation method include, first, using alcohol to be molten
Agent, white vitriol, butyl titanate are stirred into 2 h, 200 DEG C of 24 h of reaction of regulation temperature, that is, obtain TiO2Micron ball；Secondly,
Using deionized water as solvent, the TiO that will be prepared2Micron ball, ammonium heptamolybdate and thiocarbamide stir 1 h, adjust 200 DEG C of temperature
20 h are reacted, that is, obtain 1T 2H-MoS2/TiO2Core shell structure；Finally, by equivalent 1T@2H-MoS2/TiO2Core shell structure and
NaBH4After powder mull, 350 DEG C of 3 h of calcining, that is, obtain 1T 2H-MoS in argon gas2/ black TiO2Core shell structure.
2. according to claim 1, it is characterised in that the mol ratio 1 of the ammonium heptamolybdate, thiocarbamide and titanium dioxide:(10~
15):(1~5)。
3. according to claim 2, it is characterised in that the mol ratio 1 of the ammonium heptamolybdate, thiocarbamide and titanium dioxide:15:(1
~5)。
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109553181A (en) * | 2018-12-11 | 2019-04-02 | 中国科学院生态环境研究中心 | A kind of method generated free radicals using trivalent molybdenum and its method for handling organic wastewater |
| CN109742362A (en) * | 2019-01-08 | 2019-05-10 | 福建师范大学 | A kind of tin dope induction synthesis mixed phase molybdenum disulfide-derivative carbon composite preparation of chlorella and application |
| CN112121826A (en) * | 2020-10-16 | 2020-12-25 | 安徽理工大学 | 1T @2H-MoS2/SnS2Preparation method, product and application of visible light response photocatalyst |
| CN112121819A (en) * | 2019-06-24 | 2020-12-25 | 中国石油化工股份有限公司 | Preparation method of cadmium sulfide self-doped titanium dioxide composite catalyst |
| US11795329B2 (en) | 2019-11-12 | 2023-10-24 | Toyota Motor Engineering & Manufacturing North America, Inc. | Black titanium dioxide LiDAR reflecting particles and vehicles comprising the same |
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2017
- 2017-10-11 CN CN201710938537.6A patent/CN107601557A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109553181A (en) * | 2018-12-11 | 2019-04-02 | 中国科学院生态环境研究中心 | A kind of method generated free radicals using trivalent molybdenum and its method for handling organic wastewater |
| CN109742362A (en) * | 2019-01-08 | 2019-05-10 | 福建师范大学 | A kind of tin dope induction synthesis mixed phase molybdenum disulfide-derivative carbon composite preparation of chlorella and application |
| CN109742362B (en) * | 2019-01-08 | 2021-09-28 | 福建师范大学 | Preparation and application of tin-doped induced synthesized 1T-2H mixed phase few-layer molybdenum disulfide-chlorella derived carbon composite material |
| CN112121819A (en) * | 2019-06-24 | 2020-12-25 | 中国石油化工股份有限公司 | Preparation method of cadmium sulfide self-doped titanium dioxide composite catalyst |
| CN112121819B (en) * | 2019-06-24 | 2023-08-04 | 中国石油化工股份有限公司 | Preparation method of cadmium sulfide self-doped titanium dioxide composite catalyst |
| US11795329B2 (en) | 2019-11-12 | 2023-10-24 | Toyota Motor Engineering & Manufacturing North America, Inc. | Black titanium dioxide LiDAR reflecting particles and vehicles comprising the same |
| CN112121826A (en) * | 2020-10-16 | 2020-12-25 | 安徽理工大学 | 1T @2H-MoS2/SnS2Preparation method, product and application of visible light response photocatalyst |
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