CN109745929A - A kind of preparation method of molybdenum oxide/molybdenum disulfide core-shell particles - Google Patents
A kind of preparation method of molybdenum oxide/molybdenum disulfide core-shell particles Download PDFInfo
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Abstract
The present invention relates to a kind of molybdenum oxide/molybdenum disulfide core-shell particles preparation methods, belong to nanocomposite technical field.Preparation method of the invention is the following steps are included: molybdenum source is placed in tube furnace by (1), and progress high-temperature oxydation calcining, obtains molybdenum oxide particle in air atmosphere；(2) urea and sulphur source are added in ethyl alcohol, are stirred to clarify, added molybdenum oxide particle, be transferred in hydrothermal reaction kettle after ultrasonic agitation is uniform；(3) product for obtaining reaction is centrifuged, and is dried in vacuo after washing to get molybdenum oxide/molybdenum disulfide core-shell particles are arrived.Preparation method synthetic route of the present invention is simple, easy to operate, without using additional sacrifice template and catalyst, meanwhile, the microballoon regular appearance and size uniformity of preparation, individually dispersion can be widely applied to the fields such as catalysis, battery, capacitor, lubrication without reuniting.
Description
Technical field
The invention belongs to composite function nano Material Fields, and in particular to a kind of molybdenum oxide/molybdenum disulfide core-shell particles
Preparation method.
Background technique
As a kind of significant two-dimension nano materials, molybdenum disulfide (MoS2) be widely used in battery, photoelectricity, urged
The fields such as change.Theoretical research and the experimental results showed that single layer or a small number of layer MoS2Than common MoS2Block shows higher anti-
Activity is answered, this is because most active sites are located at MoS2Edge, basal plane performance be inert.And the MoS of two-dimensional layer2
Tend to be formed the structure of closure, tend to stack between synusia, is reduced so as to cause exposed edge active site, so that MoS2
Reactivity seriously reduce.MoS2Reactivity be strongly depend on its structure, morphology and size, controllable appearance, structure and
The MoS of size2Nano material becomes the hot spot studied recently, such as MoS2Nanotube, multi-layer nano piece, nano wire etc..
Zhang et al. is by the method for easy chemical vapor deposition (CVD) by MoS2It is deposited on three-dimensional grapheme surface,
To effectively prevent MoS2The stacking of layer, the complex three-dimensional material of preparation show excellent chemical property, preparation
Lithium ion cell electrode possess very high capacitance and outstanding cyclical stability (small 2013,9, No. 20,
3433-3438), but this method is to CVD technology higher requirement, complex process and have difficulty.Later, Chang project
Group proposes a hollow MoS2The preparation method of nanocages, four thio ammonium molybdate are gone back under the strong reducing property of its hydrazine
Original, so that ammonia is generated, under its auxiliary, hollow MoS2Nanocages be able to be formed (J. Mater. Chem. A, 2016,
4,51-58), however this method needs the strong reducing property by means of hydrazine, and a large amount of ammonia of the generation in preparation process is to work
Making personnel and environment has harmfulness.Therefore, it is necessary to develop one kind synthetic method simple to operation and safe to prepare
MoS2Nano material.
Summary of the invention
Technical problem to be solved by the present invention lies in view of the above shortcomings of the prior art, provide a kind of molybdenum oxide/
The preparation method of molybdenum disulfide core-shell particles.Preparation method of the invention is easy to operate, controllable, does not need by means of any sacrifice
Template does not also need to add any catalyst, and molybdenum oxide/mos2 microsphere of preparation has apparent core-shell structure, ruler
Very little uniform, the state individually dispersed, the MoS of shell is presented in microballoon2Nanometer sheet founds Xiang Shengchang to three-dimensional space, and unique structure makes
It possesses outstanding electrocatalysis characteristic, has very big application potential in terms of catalysis, photoelectricity.
In order to solve the above technical problems, the technical solution adopted by the present invention is that: a kind of molybdenum oxide/molybdenum disulfide core-shell particles
Preparation method, which is characterized in that the molybdenum oxide/molybdenum disulfide core-shell particles preparation method have following characteristics
A kind of preparation method of molybdenum oxide/molybdenum disulfide core-shell particles, comprising the following steps:
(1) molybdenum source is placed in tube furnace, high-temperature oxydation calcining is carried out in air atmosphere, obtains molybdenum oxide particle；
(2) by urea and sulphur source with mass ratio 1:(0.2 ~ 0.5) it is added in ethyl alcohol, 15 ~ 30mins of stirring to clarification, then
Molybdenum oxide particle obtained in step (1) is added, is transferred in hydrothermal reaction kettle after ultrasonic agitation is uniform, reacts 12 ~ 72h；
(3) product for obtaining reaction is centrifuged, and is washed for several times with ethyl alcohol and deionized water, is dried in vacuo 12h under 60oC, obtains
To molybdenum oxide/molybdenum disulfide core-shell particles.
After molybdenum source described in step (1) is fully ground, then carry out high-temperature oxydation calcining.
The process conditions of the calcining of high-temperature oxydation described in step (1) are as follows: heating rate is 2 ~ 15oC/min, calcination temperature
It is 300 ~ 400 DEG C, the processing time is 2h.
Molybdenum source described in step (1) is one of four thio ammonium molybdate or sodium molybdate.
The temperature of the hydrothermal reaction kettle is 160 ~ 220 oC when step (2) hydro-thermal reaction.
Sulphur source described in step (2) is one of tetrathio acetamide, thiocarbamide or L-cysteine.
Molybdenum oxide of the present invention/molybdenum disulfide core-shell particles preparation method has the advantage that compared with prior art
1, the method that the present invention is combined using high-temperature calcination and hydro-thermal, by controlling high-temperature burning process and hydrothermal temperature,
It realizes and is is prepared by controllableization of micro-sphere structure, it is easy to operate controllable, it does not need also not needing to add by means of any sacrifice template
Any catalyst is conducive to further controllable metaplasia and produces.
2, molybdenum oxide/mos2 microsphere prepared by the present invention has apparent core-shell structure, and individually dispersion is presented in microballoon
State, Microsphere Size is uniform, can effectively avoid the reunion of microballoon.
3, the MoS of the obtained molybdenum oxide/molybdenum disulfide core-shell particles shell of the present invention2Nanometer sheet founds Xiang Sheng to three-dimensional space
It is long, its stacked in multi-layers is effectively hindered, so that more edge active sites are exposed, it is outstanding that unique texture possesses it
Electrocatalysis characteristic has very big application potential in terms of catalysis, photoelectricity.
Detailed description of the invention
Fig. 1 is the transmission electron microscope photo of 1 thus obtained microsphere of the embodiment of the present invention.
Fig. 2 is the transmission electron microscope photo of 2 thus obtained microsphere of the embodiment of the present invention.
Fig. 3 is the transmission electron microscope photo of 3 thus obtained microsphere of the embodiment of the present invention.
Fig. 4 is the transmission electron microscope photo of 4 thus obtained microsphere of the embodiment of the present invention.
Fig. 5 is the electron scanning micrograph of 3 thus obtained microsphere of the embodiment of the present invention.
With reference to the accompanying drawing and specific embodiment is described further technical solution of the present invention.
Specific embodiment
Embodiment 1
A kind of preparation method of molybdenum oxide/molybdenum disulfide core-shell particles, comprising the following steps:
(1) sodium molybdate powder is placed in tube furnace, high-temperature oxydation is carried out in air atmosphere and calcines 2h, obtains molybdenum oxide
Grain, the heating rate of high-temperature burning process are 10 DEG C/min, and calcination temperature is 400 DEG C；
(2) urea and tetrathio acetamide are added in ethyl alcohol with mass ratio 1:0.3,20 mins of stirring add step to clarifying
Suddenly molybdenum oxide particle obtained in (1) is transferred in hydrothermal reaction kettle after ultrasonic agitation is uniform, hydro-thermal conjunction is carried out at 180 DEG C
At for 24 hours；
(3) product for obtaining reaction is centrifuged, and is respectively washed 3 times with ethyl alcohol and deionized water, is dried in vacuo 12h at 60 DEG C, obtains
Molybdenum oxide/molybdenum disulfide core-shell particles.
Fig. 1 is molybdenum oxide/molybdenum disulfide core-shell particles transmission electron microscope photo made from the present embodiment.As schemed
Show, resulting microballoon is more uniform, and about 300 nanometers of average diameter, microsphere surface has visible MoS2Nanoscale twins generate.
Embodiment 2
A kind of preparation method of molybdenum oxide/molybdenum disulfide core-shell particles, comprising the following steps:
(1) four thio ammonium molybdate powder is placed in tube furnace, high-temperature oxydation is carried out in air atmosphere and calcines 2h, is aoxidized
Molybdenum particle, the heating rate of high-temperature burning process are 2 DEG C/min, and calcination temperature is 300 DEG C；
(2) urea and tetrathio acetamide are added in ethyl alcohol with mass ratio 1:0.4,30 mins of stirring are added to clarifying
Molybdenum oxide particle obtained in step (1) is transferred in hydrothermal reaction kettle after ultrasonic agitation is uniform, hydro-thermal is carried out at 180 DEG C
Synthesis is for 24 hours；
(3) product for obtaining reaction is centrifuged, and is respectively washed 3 times with ethyl alcohol and deionized water, is dried in vacuo 12h at 60 DEG C, obtains
Molybdenum oxide/molybdenum disulfide core-shell particles.
Fig. 2 is molybdenum oxide/molybdenum disulfide core-shell particles transmission electron microscope photo made from the present embodiment.As schemed
Showing, microsphere diameter obtained is smaller, and respectively less than 200 nanometers, and serious reunion adhesion phenomenon has occurred in microballoon.
Embodiment 3
A kind of preparation method of molybdenum oxide/molybdenum disulfide core-shell particles, comprising the following steps:
(1) four thio ammonium molybdate powder is placed in tube furnace, high-temperature oxydation is carried out in air atmosphere and calcines 2h, is aoxidized
Molybdenum particle, the heating rate of high-temperature burning process are 10 DEG C/min, and calcination temperature is 400 DEG C；
(2) urea and tetrathio acetamide are added in ethyl alcohol with mass ratio 1:0.3,30 mins of stirring are added to clarifying
Molybdenum oxide particle obtained in step (1) is transferred in hydrothermal reaction kettle after ultrasonic agitation is uniform, hydro-thermal is carried out at 180 DEG C
Synthesize 36h；
(3) product for obtaining reaction is centrifuged, and is respectively washed 3 times with ethyl alcohol and deionized water, is dried in vacuo 12h at 60 DEG C, obtains
Molybdenum oxide/molybdenum disulfide core-shell particles.
Fig. 3 is molybdenum oxide/molybdenum disulfide core-shell particles transmission electron microscope photo made from the present embodiment.As schemed
Show, microballoon forms apparent core-shell structure, and microsphere surface forms MoS abundant2Nanoscale twins.
Fig. 5 is molybdenum oxide/molybdenum disulfide core-shell particles electron scanning micrograph made from the present embodiment.By scanning
Electron micrograph can be seen that the sphere that microballoon shape manufactured in the present embodiment is rule, and the size uniformity of sphere is concentrated
It is distributed between 400 ~ 500 nanometers, and the state that individually dispersion is not adhered mutually is presented in ball.
Embodiment 4
A kind of preparation method of molybdenum oxide/molybdenum disulfide core-shell particles, comprising the following steps:
(1) four thio ammonium molybdate powder is placed in tube furnace, high-temperature oxydation is carried out in air atmosphere and calcines 2h, is aoxidized
Molybdenum particle, the heating rate of high-temperature burning process are 5 DEG C/min, and calcination temperature is 300 DEG C；
(2) urea and tetrathio acetamide are added in ethyl alcohol with mass ratio 1:0.3,30 mins of stirring are added to clarifying
Molybdenum oxide particle obtained in step (1) is transferred in hydrothermal reaction kettle after ultrasonic agitation is uniform, hydro-thermal is carried out at 180 DEG C
Synthesis is for 24 hours；
(3) product for obtaining reaction is centrifuged, and is respectively washed 3 times with ethyl alcohol and deionized water, is dried in vacuo 12h at 60 DEG C, obtains
Molybdenum oxide/molybdenum disulfide core-shell particles.
Fig. 4 is molybdenum oxide/molybdenum disulfide core-shell particles transmission electron microscope photo made from the present embodiment.It can by figure
To know, the microballoon core-shell structure of example preparation is it is obvious that still microballoon is adhered mutually seriously, while other than microballoon, nanometer rods
Also it generates simultaneously.
Embodiment 1-4 can be seen by the optimization to various experiment conditions in conjunction with transmission and electron scanning micrograph
Molybdenum oxide made from embodiment 3/molybdenum disulfide core-shell particles have apparent core-shell structure out, and the shape individually dispersed is presented in microballoon
State, and Microsphere Size is uniform, the MoS of shell2Nanometer sheet founds Xiang Shengchang to three-dimensional space, effectively hinders its stacked in multi-layers, makes
More edge active sites are obtained to be exposed.
The above is only presently preferred embodiments of the present invention, is not intended to limit the invention in any way.It is all according to the present invention
Essence any simple modification, change and equivalence change to the above embodiments, still fall within technical solution of the present invention
In protection scope.
Claims (6)
1. a kind of molybdenum oxide/molybdenum disulfide core-shell particles preparation method, which comprises the following steps:
(1) molybdenum source is placed in tube furnace, high-temperature oxydation calcining is carried out in air atmosphere, obtains molybdenum oxide particle；
(2) by urea and sulphur source with mass ratio 1:(0.2 ~ 0.5) it is added in ethyl alcohol, 15 ~ 30mins of stirring to clarification, then
Molybdenum oxide particle obtained in step (1) is added, is transferred in hydrothermal reaction kettle after ultrasonic agitation is uniform, reacts 12 ~ 72h；
(3) product for obtaining reaction is centrifuged, and is washed for several times with ethyl alcohol and deionized water, is dried in vacuo 12h under 60oC, obtains
To molybdenum oxide/molybdenum disulfide core-shell particles.
2. a kind of preparation method of molybdenum oxide/molybdenum disulfide core-shell particles according to claim 1, which is characterized in that step
Suddenly after molybdenum source described in (1) is fully ground, then high-temperature oxydation calcining is carried out.
3. a kind of preparation method of molybdenum oxide/molybdenum disulfide core-shell particles according to claim 1, which is characterized in that step
Suddenly the process conditions of the calcining of high-temperature oxydation described in (1) are as follows: heating rate is 2 ~ 15oC/min, and calcination temperature is 300 ~ 400
DEG C, the processing time is 2h.
4. a kind of preparation method of molybdenum oxide/molybdenum disulfide core-shell particles according to claim 1, which is characterized in that step
Suddenly molybdenum source described in (1) is one of four thio ammonium molybdate or sodium molybdate.
5. a kind of preparation method of molybdenum oxide/molybdenum disulfide core-shell particles according to claim 1, which is characterized in that step
Suddenly the temperature of the hydrothermal reaction kettle is 160 ~ 220 oC when hydro-thermal reaction in (2).
6. a kind of preparation method of molybdenum oxide/molybdenum disulfide core-shell particles according to claim 1, which is characterized in that step
Suddenly sulphur source described in (2) is one of tetrathio acetamide, thiocarbamide or L-cysteine.
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| WO2021125915A1 (en) * | 2019-12-20 | 2021-06-24 | 한양대학교에리카산학협력단 | Electrochemical catalyst and preparation method therefor |
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| CN112121824A (en) * | 2020-10-25 | 2020-12-25 | 泉州师范学院 | Preparation method and application of CoO @ CoS composite photocatalyst with core-shell structure |
| CN113617371A (en) * | 2021-08-23 | 2021-11-09 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of sandwich structure hollow nano reactor photocatalytic material, product and application |
| CN114609197A (en) * | 2022-03-25 | 2022-06-10 | 电子科技大学 | Gas sensitive material, preparation method and application thereof in NH3Application in gas sensor |
| CN114609197B (en) * | 2022-03-25 | 2023-11-21 | 电子科技大学 | Gas-sensitive material, preparation method and NH (NH) thereof 3 Application in gas sensor |
| CN114613969A (en) * | 2022-03-30 | 2022-06-10 | 西安热工研究院有限公司 | Molybdenum-based core-shell structure material and preparation method and application thereof |
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