CN108715462A - The method of the molybdenum disulfide particles of water/solvent-thermal process different morphologies - Google Patents
The method of the molybdenum disulfide particles of water/solvent-thermal process different morphologies Download PDFInfo
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Abstract
The method that the present invention proposes the molybdenum disulfide particles of water/solvent-thermal process different morphologies, this method include：(1) reaction solution is prepared, wherein reaction solution includes molybdenum source, sulphur source and solvent；(2) thermal synthesis reaction and separating treatment are carried out to reaction solution, to obtain the molybdenum disulfide particles of different morphologies.Synthetic method proposed by the invention selects water/solvent-thermal method and is realized to MoS by controlling pre-reaction material and reaction dissolvent2Effective control of the pattern and grain size of particle, makes its size control in 20~2000nm, also, the preparation method yield is high, MoS2The pattern of particle is uniform, to have a good application prospect.
Description
Technical field
The present invention relates to technical field of nano material, specifically, the present invention relates to the two of water/solvent-thermal process different morphologies
The method of molybdenum sulfide particle.
Background technology
Currently, as typical transition-metal sulphides, molybdenum disulfide (MoS2) because its unique structure and performance by
It gradually attracts attention, has important application in fields such as energy storage, biology, catalysis, lubrications.In recent years, with the development of nanotechnology,
Researcher continuously attempts to MoS2Particle is introduced into lubricating oil, and points out MoS2Particle has preferable lubricant effect.MoS2?
The antifriction antiwear mechanism that grain is used as lubricating additive includes mainly three ball effect, interlayer slip and stripping transfer aspects.Together
When, MoS2Stripping metastasis of the particle in friction process is affected by its form.It can be seen that MoS2The shape of particle
Looks and structure have its tribological property important influence.Prepare the MoS of different shape2Particle is inorganic material synthesis always
The research hotspot in field.
At this stage, MoS is prepared2The method of material is broadly divided into two major classes, and the first kind is with micromechanical forces stripping, lithium ion
Intercalation, liquid phase stripping are " from bottom to top " stripping method of representative, and the second class is with presoma decomposition method, high temperature vulcanized method, water/molten
The hot method of agent, vapour deposition process etc. are " from bottom to top " synthetic method of representative.Wherein, synthetic method has raw material easy " from bottom to top "
, operability it is strong, the advantages that product purity is high, have a clear superiority in terms of extensive preparation.However, each " from lower and
On " synthetic method has respective advantage and disadvantage.Wherein, presoma decomposition method is easy to operate, but technology stability is poor, can not answer extensively
With；High temperature vulcanized method is at low cost, but preparation condition is stringent；MoS prepared by chemical vapour deposition technique2Material purity is higher, crystallization
Degree is preferable, but the method requires harshness to reaction kit, equipment etc..In contrast, water/solvent-thermal method carries out in the liquid phase,
Condition is comparatively mild, at low cost, and operability is strong, while MoS2The structure and pattern of material are easily controllable.
Invention content
The present invention is the following discovery based on inventor and completes：
The present inventor has found in the course of the research, the MoS prepared using water/solvent-thermal method2Particle, can be anti-by controlling
Predecessor and reaction dissolvent is answered to regulate and control MoS2The specific form of particle.Also, MoS prepared by the present invention2Particle yield is high, shape
Looks are uniform, to have a good application prospect.
In view of this, an object of the present invention is to provide it is a kind of by regulate and control water/solvent heat condition can synthesize it is more
The method of the molybdenum disulfide particles of kind pattern.
In the first aspect of the present invention, the present invention proposes a kind of molybdenum disulfide of water/solvent-thermal process different morphologies
The method of grain.
According to an embodiment of the invention, the method includes：(1) reaction solution is prepared, wherein the reaction solution includes molybdenum
Source, sulphur source and solvent；(2) thermal synthesis reaction and separating treatment are carried out to the reaction solution, to obtain the two of the different morphologies
Molybdenum sulfide particle.
Inventor has found that using the synthetic method of the embodiment of the present invention, selects water/solvent-thermal method and pass through control
Pre-reaction material (including molybdenum source and sulphur source) processed and reaction dissolvent are realized to MoS2Effective control of the pattern and grain size of particle, makes
Its size control is in 20~2000nm, also, the preparation method yield is high, MoS2The pattern of particle is uniform, to good
Application prospect.
In addition, synthetic method according to the above embodiment of the present invention, can also have following additional technical characteristic：
According to an embodiment of the invention, the different morphologies include petal-shaped, spherical, nano flower-like, crescent shape, sheet and
Ultra-thin stratiform.
According to an embodiment of the invention, the molybdenum source is sodium molybdate, and the sulphur source includes thiocarbamide, L-cysteine, thio
Acetamide, and the solvent includes the deionized water or organic amine optionally containing at least one of ethylene glycol and polyethylene glycol.
According to an embodiment of the invention, the reaction solution further includes at least one of reducing agent and surfactant, institute
It is azanol or hydrazine hydrate to state reducing agent, and the surfactant is cetyl ammonia bromide.
According to an embodiment of the invention, the pattern of the molybdenum disulfide particles is petal-shaped, and the sulphur source is thiocarbamide, institute
It is deionized water to state solvent.
According to an embodiment of the invention, the molar ratio of the molybdenum source, the sulphur source and the reducing agent is 1:(2~10):
(2~10), and based on the volume of the reaction solution, the total mass concentration of the molybdenum source, the sulphur source and the reducing agent is
The mass concentration of 0.015~0.5g/mL, the surfactant are 0.001~0.03g/mL.
According to an embodiment of the invention, the pattern of the molybdenum disulfide particles is spherical, and the sulphur source is thiocarbamide, described
Solvent is the mixed solvent of ethylene glycol, polyethylene glycol and organic amine, wherein a length of C16~C22 of carbochain chain of the organic amine.
According to an embodiment of the invention, the molar ratio of the molybdenum source, the sulphur source and the reducing agent is 1:(2~10):
(2~10), and based on the volume of the reaction solution, the total mass concentration of the molybdenum source, the sulphur source and the reducing agent is
0.015~0.5g/mL, also, the mass ratio of the in the mixed solvent ethylene glycol, polyethylene glycol and organic amine is (1~5):1:
(1~5).
According to an embodiment of the invention, the pattern of the molybdenum disulfide particles is nano flower-like, and the sulphur source is L- half
Cystine, the solvent are deionized water.
According to an embodiment of the invention, the molar ratio of the molybdenum source and the sulphur source is 1:(1~5), and based on described anti-
Answer the volume of liquid, the total mass concentration of the molybdenum source and the sulphur source is 0.015~0.5g/mL.
According to an embodiment of the invention, the pattern of the molybdenum disulfide particles is crescent shape, and the sulphur source is thio second
Amide, the solvent are deionized water.
According to an embodiment of the invention, the molar ratio of the molybdenum source and the sulphur source is 1:(1~5), and based on described anti-
Answer the volume of liquid, the total mass concentration of the molybdenum source and the sulphur source is 0.015~0.5g/mL.
According to an embodiment of the invention, the pattern of the molybdenum disulfide particles is sheet, and the sulphur source is thioacetyl
Amine, the solvent are the mixed solvent of polyethylene glycol and deionized water.
According to an embodiment of the invention, the molar ratio of the molybdenum source and the sulphur source is 1:(5~30), and based on described anti-
Answer the volume of liquid, the total mass concentration of the molybdenum source and the sulphur source is 0.015~0.5g/mL, also, the in the mixed solvent
Polyethylene glycol and the mass ratio of deionized water are 1:(0.2~5).
According to an embodiment of the invention, the pattern of the molybdenum disulfide particles is ultra-thin stratiform, and the sulphur source is thiocarbamide,
The solvent is organic amine, wherein a length of C16~C22 of carbochain chain of the organic amine.
According to an embodiment of the invention, the molar ratio of the molybdenum source and the sulphur source is 1:(5~30), and based on described anti-
Answer the volume of liquid, the total mass concentration of the molybdenum source and the sulphur source is 0.015~0.5g/mL.
The additional aspect and advantage of the present invention will be set forth in part in the description, and will partly become from the following description
Obviously, or practice through the invention is recognized.
Description of the drawings
The above-mentioned aspect combination following accompanying drawings of the present invention explains the description of embodiment, wherein：
Fig. 1 is the method flow of the molybdenum disulfide particles of water/solvent-thermal process different morphologies of one embodiment of the invention
Schematic diagram；
Fig. 2 is the MoS of two embodiments of the invention2The XRD spectra and 2H-MoS of particle2Standard spectrogram；
Fig. 3 is the MoS of the other three embodiment of the present invention2The XRD spectra and 2H-MoS of particle2Standard spectrogram；
Fig. 4 is the MoS of another embodiment of the present invention2The XRD spectra and 2H-MoS of particle2Standard spectrogram；
Fig. 5 is the petal-like MoS of one embodiment of the invention2The TEM photos of particle；
Fig. 6 is the spherical MoS of one embodiment of the invention2The TEM photos of particle；
Fig. 7 is the MoS of the nano flower-like of one embodiment of the invention2The TEM photos of particle；
Fig. 8 is the MoS of the crescent shape of one embodiment of the invention2The TEM photos of particle；
Fig. 9 is the MoS of the sheet of one embodiment of the invention2The TEM photos of particle；
Figure 10 is the MoS of the ultra-thin stratiform of one embodiment of the invention2The TEM photos of particle.
Specific implementation mode
The embodiment of the present invention is described below in detail, those skilled in the art is it will be appreciated that following example is intended for solving
The present invention is released, and is not construed as limitation of the present invention.Unless stated otherwise, it is not expressly recited in embodiment below specific
Technology or condition, those skilled in the art can be according to common technology in the art or condition or according to product description
It carries out.
In one aspect of the invention, the present invention proposes a kind of molybdenum disulfide of water/solvent-thermal process different morphologies
The method of grain.It should be noted that " a variety of " herein specifically refer to two or more.Implementation according to the present invention
Example, the different morphologies of molybdenum disulfide particles may particularly include petal-shaped, spherical, nano flower-like, crescent shape, sheet and superthin layer
Shape.It should also be noted that, " ultra-thin stratiform " specifically refers to the size of particle in the range of 10~50nm.
According to an embodiment of the invention, with reference to figure 1, which includes：
S100：Prepare reaction solution.
In this step, preparation includes the reaction solution of molybdenum source, sulphur source and solvent, in this way, after prepared reaction solution is used as
The pre-reaction material of continuous thermal synthesis reaction.
The present inventor has found in the course of the research, the MoS prepared using water/solvent-thermal method2Particle, can be anti-by controlling
Predecessor (molybdenum source and the specific type of sulphur source and proportioning) and reaction dissolvent (specific type) is answered to regulate and control MoS2Particle it is specific
Form, for example, can be formed petal-shaped, spherical, nano flower-like, crescent shape, sheet or ultra-thin stratiform MoS2Particle can also make it
Size control is in 20~2000nm.Also, MoS prepared by the present invention2Particle yield is high, and pattern is uniform, to good
Application prospect.
According to an embodiment of the invention, molybdenum source can be sodium molybdate, in this way, using sodium molybdate as the curing of molybdenum source thermal synthesis
The better crystallinity degree of molybdenum particle, yield are high, and sodium molybdate is cheap and easy to get, derives from a wealth of sources.According to an embodiment of the invention, sulphur source is selected from
Thiocarbamide, L-cysteine or thioacetamide can effectively regulate and control the two of formation in this way, using above-mentioned different types of sulphur source
The specific pattern of molybdenum oxide particle.According to an embodiment of the invention, solvent may include optionally containing in ethylene glycol and polyethylene glycol
At least one deionized water or organic amine, specifically such as deionized water, octadecylamine, ethylene glycol, polyethylene glycol and octadecylamine
The mixed solvent, etc. of mixed solvent, polyethylene glycol and deionized water, two sulphur that those skilled in the art can be formed as needed
The specific pattern for changing molybdenum particle is correspondingly selected.
In some embodiments of the invention, reaction solution can also include at least one in reducing agent and surfactant
Kind, in this way, reducing agent can help to the synthesis of molybdenum disulfide particles, and surfactant can further regulate and control the curing of formation
The specific pattern of molybdenum particle.According to an embodiment of the invention, reducing agent can be azanol or hydrazine hydrate, in this way, using above-mentioned difference
The reducing agent of type, the molybdenum disulfide of synthesis can be made yield higher, and azanol or hydrazine hydrate are cheap and easy to get, derive from a wealth of sources.Root
According to the embodiment of the present invention, surfactant can be cetyl ammonia bromide, in this way, the surfactant using mentioned kind can
Contribute to that the surface topography of molybdenum disulfide particles is more complicated, specific surface area bigger, there is better lubricant effect, also, the table
Face activating agent is cheap and easy to get, derives from a wealth of sources.
In some specific examples, molybdenum source can be sodium molybdate, and sulphur source can be thiocarbamide, and deionized water may be selected in solvent, restores
Agent can be azanol or hydrazine hydrate, and surfactant can be cetyl ammonia bromide, and the molar ratio of molybdenum source, sulphur source and reducing agent is
1:(2~10):The total mass concentration of (2~10), also, the volume based on reaction solution, molybdenum source, sulphur source and reducing agent is 0.015
The mass concentration of~0.5g/mL, surfactant are 0.001~0.03g/mL.In this way, using the reaction of above-mentioned composition and ratio
Liquid can synthesize the pattern of petal-like molybdenum disulfide particles by subsequent hydro-thermal reaction.
In other specific examples, molybdenum source can be sodium molybdate, and sulphur source can be thiocarbamide, and reducing agent can be azanol or hydration
The mixed solvent of ethylene glycol, polyethylene glycol and organic amine may be selected in hydrazine, solvent, wherein and a length of C16 of carbochain chain of organic amine~
C22, molecular weight polyethylene glycol are 200~1000, and the molar ratio of molybdenum source, sulphur source and reducing agent is 1:(2~10):(2~10),
Also, the total mass concentration of the volume based on reaction solution, molybdenum source, sulphur source and reducing agent is 0.015~0.5g/mL, moreover, mixing
The mass ratio of ethylene glycol, polyethylene glycol and organic amine is (1~5) in solvent:1:(1~5).In this way, using above-mentioned composition and ratio
The reaction solution of example can synthesize spherical molybdenum disulfide particles by subsequent thermal synthesis reaction.
In other specific examples, molybdenum source can be sodium molybdate, and sulphur source can be L-cysteine, and solvent can be deionization
Water, and the molar ratio of molybdenum source and sulphur source is 1:The total mass concentration of (1~5), and the volume based on reaction solution, molybdenum source and sulphur source is
0.015~0.5g/mL.In this way, using the reaction solution of above-mentioned composition and ratio, nanometer can be synthesized by subsequent hydro-thermal reaction
Flower-shaped molybdenum disulfide particles.
In other specific examples, molybdenum source can be sodium molybdate, and sulphur source can be thioacetamide, and solvent can be deionization
Water, and the molar ratio of molybdenum source and sulphur source is 1:The total mass concentration of (1~5), and the volume based on reaction solution, molybdenum source and sulphur source is
0.015~0.5g/mL.In this way, using the reaction solution of above-mentioned composition and ratio, crescent moon can be synthesized by subsequent hydro-thermal reaction
The molybdenum disulfide particles of shape.
In other specific examples, molybdenum source can be sodium molybdate, and sulphur source can be thioacetamide, and solvent can be polyethylene glycol
With the mixed solvent of deionized water, wherein molecular weight polyethylene glycol is 200~1000, and the molar ratio of molybdenum source and sulphur source is 1:
The total mass concentration of (5~30), also, the volume based on reaction solution, molybdenum source and sulphur source is 0.015~0.5g/mL, moreover, mixed
Polyethylene glycol and the mass ratio of deionized water are 1 in bonding solvent:(0.2~5).In this way, using the reaction of above-mentioned composition and ratio
Liquid, by subsequent thermal synthesis reaction can synthesizing flaky molybdenum disulfide particles.
In other specific examples, molybdenum source can be sodium molybdate, and sulphur source can be thiocarbamide, and solvent can be organic amine, wherein have
A length of C16~the C22 of carbochain chain of machine amine, and the molar ratio of molybdenum source and sulphur source is 1:(5~30), also, the body based on reaction solution
The total mass concentration of product, molybdenum source and sulphur source is 0.015~0.5g/mL.In this way, using the reaction solution of above-mentioned composition and ratio, lead to
The molybdenum disulfide particles of ultra-thin stratiform can be synthesized by crossing subsequent thermal synthesis reaction.
S200：Hydro-thermal reaction and separating treatment are carried out to reaction solution, to obtain the molybdenum disulfide particles of different morphologies.
In this step, thermal synthesis reaction and separating treatment are carried out to the reaction solution that step S100 is prepared, it is a variety of to obtain
The molybdenum disulfide particles of pattern.
According to an embodiment of the invention, thermal synthesis reaction temperature can be 180~220 degrees Celsius, the time be 12~24 small
When, in this way, using above-mentioned condition thermal synthesis react, can make the pattern type of the molybdenum disulfide particles synthesized it is more uniform,
Grain grain size is more concentrated and yield higher.
It in some embodiments of the invention, can also be after separating treatment, to precipitating the rear place washed and dried
Reason specifically, being washed respectively 3 times with deionized water or hexamethylene, ethyl alcohol respectively, then dries 6~12 under 40~60 degrees Celsius
Hour, in this way, the molybdenum disulfide particles that can be dried, be shaped.
In conclusion according to an embodiment of the invention, the present invention proposes a kind of synthetic method, water/solvent-thermal method is selected
And it is realized to MoS by controlling pre-reaction material (including molybdenum source and sulphur source) and reaction dissolvent2The pattern of particle and having for grain size
Effect control, makes its size control in 20~2000nm, also, the preparation method yield is high, MoS2The pattern of particle is uniform, to
It has a good application prospect.
Below with reference to specific embodiment, present invention is described, it should be noted that these embodiments are only descriptive
, without limiting the invention in any way.
Embodiment 1
In this embodiment, petal-like molybdenum dioxide particle is prepared.Specific steps are as follows：
(a) the cetyl bromination of the sodium molybdate of 2.5mmol, the thiocarbamide of 10mmol, the azanol of 10mmol and 0.1g are weighed
Amine is dissolved in the deionized water of 30mL, forms reaction solution；
(b) reaction solution stirred evenly is transferred in the reaction kettle of 50mL, thermal synthesis reaction 18h at a temperature of 200 DEG C,
Room temperature is naturally cooled to after reaction；
(c) black precipitate is obtained by filtration in thermal synthesis reaction product, then is respectively washed 3 times with deionized water and ethyl alcohol, and
It is placed in 40 DEG C of vacuum drying chamber and dries 6h.
The MoS of the embodiment prepared2Particle, X-ray diffraction (XRD) spectrogram is as shown in the curve 1 in Fig. 2.By
Fig. 2 can be seen that, the MoS2Particle is hexagonal crystal system (2H-MoS2)。
The MoS of the embodiment prepared2Particle, transmission electron microscope (TEM) photo are as shown in Figure 5.It can by Fig. 5
Find out, the MoS2Particle is in petal-shaped pattern, and petal-shaped MoS also can be observed at 1.5 μm or so in average grain diameter2It is
By number, the aggregation of equal nanometer sheet does not assemble.
Embodiment 2
In this embodiment, spherical molybdenum dioxide particle is prepared according to the method and condition of embodiment 1.But, area
It is not：(a) azanol for weighing the sodium molybdate of 2.5mmol, the thiocarbamide of 10mmol and 10mmol, is dissolved in the ethylene glycol of 15mL
((CH2OH)2), the in the mixed solvent of the polyethylene glycol (PEG-400) of the octadecylamine of 15mL and 5mL, form reaction solution.
The MoS of the embodiment prepared2Particle, X-ray diffraction (XRD) spectrogram is as shown in the curve 2 in Fig. 2.By
Fig. 2 can be seen that, the MoS2Particle is hexagonal crystal system (2H-MoS2), while the intensity at the X-ray diffraction peak of the particle is also observed
Weaker and appearance widthization, illustrates obtained MoS2Grain crystalline is poor.
The MoS of the embodiment prepared2Particle, transmission electron microscope (TEM) photo are as shown in Figure 6.It can by Fig. 6
Find out, the MoS2Particle is in spherical morphology, while observing MoS2Spherical particle be by the layer structure that is bent uniformly and disorderly
It stacks.
Embodiment 3
In this embodiment, the molybdenum dioxide particle of nano flower-like is prepared according to the method and condition of embodiment 1.No
It crosses, difference lies in：(a) sodium molybdate of 2mmol and the L-cysteine of 2mmol are weighed, is dissolved in the deionized water of 30mL, shape
At reaction solution.
The MoS of the embodiment prepared2Particle, X-ray diffraction (XRD) spectrogram is as shown in the curve 1 in Fig. 3.By
Fig. 3 can be seen that, the MoS2Particle is hexagonal crystal system (2H-MoS2)。
The MoS of the embodiment prepared2Particle, transmission electron microscope (TEM) photo are as shown in Figure 7.It can by Fig. 7
Find out, the MoS2Particle diametrically be about 100-200nm nano flower-like structure, while observe the nano flower-like structure be by
Nanometer sheet assembles.
Embodiment 4
In this embodiment, the molybdenum dioxide particle of crescent shape is prepared according to the method and condition of embodiment 1.But,
Difference lies in：(a) sodium molybdate of 2mmol and the thioacetamide of 3.5mmol are weighed, is dissolved in the deionized water of 30mL, shape
At reaction solution.
The MoS of the embodiment prepared2Particle, X-ray diffraction (XRD) spectrogram is as shown in the curve 2 in Fig. 3.By
Fig. 3 can be seen that, the MoS2Particle is hexagonal crystal system (2H-MoS2)。
The MoS of the embodiment prepared2Particle, transmission electron microscope (TEM) photo are as shown in Figure 8.It can by Fig. 8
Find out, the MoS2Particle is made of the nanometer sheet of the similar crescent shape crimped, while being observed that these nanometer sheets squeeze mutually and being in
Bending distribution.
Embodiment 5
In this embodiment, the molybdenum dioxide particle of sheet is prepared according to the method and condition of embodiment 1.But, area
It is not：(a) sodium molybdate of 1mmol and the thioacetamide of 10mmol are weighed, the deionized water and 22.5mL of 7.5mL are dissolved in
Polyethylene glycol (PEG-200) in, formed reaction solution.
The MoS of the embodiment prepared2Particle, X-ray diffraction (XRD) spectrogram is as shown in the curve 3 in Fig. 3.By
Fig. 3 can be seen that the angle of diffraction is that 8.6 ° and 17.6 ° of position two diffraction maximums occurs, is belonging respectively to MoS2(002) and
(004) diffraction maximum that crystal face is shifted to low angle, and the MoS2Particle is still hexagonal crystal system (2H-MoS2)。
The MoS of the embodiment prepared2Particle, transmission electron microscope (TEM) photo are as shown in Figure 9.It can by Fig. 9
Find out, the MoS2Fluffy and height fold nano-sheet pattern is presented in particle, and the lateral dimension of nanometer sheet is about 300nm.
Embodiment 6
In this embodiment, the molybdenum dioxide particle of sheet is prepared according to the method and condition of embodiment 1.But, area
It is not：(a) sodium molybdate of 1mmol and the thiocarbamide of 5mmol are weighed, is dissolved in the octadecylamine of 30mL, reaction solution is formed.
The MoS of the embodiment prepared2Particle, X-ray diffraction (XRD) spectrogram is as shown in the graph in fig. 4.By scheming
4 can be seen that, the angle of diffraction and 2H-MoS of particle obtained2The position at main diffractive features peak is corresponding, does not find other miscellaneous
The presence of mass peak illustrates that obtained particle is hexagonal crystal system (2H-MoS2)。
The MoS of the embodiment prepared2Particle, transmission electron microscope (TEM) photo are as shown in Figure 10.By Figure 10
It can be seen that, the MoS2Nano-sheet pattern is presented in particle, and lateral dimension is in 20-30nm, favorable dispersibility.Observe system simultaneously
Standby MoS2Particle has ultra-thin layer structure, each nano-sheet MoS2It is made of 1-4 layers of atomic layer.
In the description of the present invention, it is to be understood that, term "center", " longitudinal direction ", " transverse direction ", " length ", " width ",
" thickness ", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outside", " up time
The orientation or positional relationship of the instructions such as needle ", " counterclockwise ", " axial direction ", " radial direction ", " circumferential direction " be orientation based on ... shown in the drawings or
Position relationship is merely for convenience of description of the present invention and simplification of the description, and does not indicate or imply the indicated device or element must
There must be specific orientation, with specific azimuth configuration and operation, therefore be not considered as limiting the invention.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show
The description of example " or " some examples " etc. means specific features, structure, material or spy described in conjunction with this embodiment or example
Point is included at least one embodiment or example of the invention.In the present specification, schematic expression of the above terms are not
It must be directed to identical embodiment or example.Moreover, particular features, structures, materials, or characteristics described can be in office
It can be combined in any suitable manner in one or more embodiments or example.In addition, without conflicting with each other, the skill of this field
Art personnel can tie the feature of different embodiments or examples described in this specification and different embodiments or examples
It closes and combines.
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example
Property, it is not considered as limiting the invention, those skilled in the art within the scope of the invention can be to above-mentioned
Embodiment is changed, changes, replacing and modification.
Claims (10)
1. a kind of method of the molybdenum disulfide particles of water/solvent-thermal process different morphologies, which is characterized in that including：
(1) reaction solution is prepared, wherein the reaction solution includes molybdenum source, sulphur source and solvent；
(2) thermal synthesis reaction and separating treatment are carried out to the reaction solution, to obtain the molybdenum disulfide particles of the different morphologies.
2. according to the method described in claim 1, it is characterized in that, the different morphologies include petal-shaped, spherical, nano flower
Shape, crescent shape, sheet and ultra-thin stratiform.
3. according to the method described in claim 2, it is characterized in that, the molybdenum source is sodium molybdate, the sulphur source includes thiocarbamide, L-
Cysteine, thioacetamide, and the solvent includes the deionization optionally containing at least one of ethylene glycol and polyethylene glycol
Water or organic amine.
4. according to the method described in claim 3, it is characterized in that, the reaction solution further includes in reducing agent and surfactant
At least one, the reducing agent be azanol or hydrazine hydrate, the surfactant be cetyl ammonia bromide.
5. according to the method described in claim 4, it is characterized in that, the pattern of the molybdenum disulfide particles is petal-shaped, and institute
It is thiocarbamide to state sulphur source, and the solvent is deionized water；
Optionally, the molar ratio of the molybdenum source, the sulphur source and the reducing agent is 1:(2~10):(2~10), and it is based on institute
The volume of reaction solution is stated, the total mass concentration of the molybdenum source, the sulphur source and the reducing agent is 0.015~0.5g/mL, described
The mass concentration of surfactant is 0.001~0.03g/mL.
6. according to the method described in claim 4, it is characterized in that wherein, the pattern of the molybdenum disulfide particles is spherical, and
The sulphur source is thiocarbamide, and the solvent is the mixed solvent of ethylene glycol, polyethylene glycol and organic amine, wherein the organic amine
A length of C16~the C22 of carbochain chain；
Optionally, the molar ratio of the molybdenum source, the sulphur source and the reducing agent is 1:(2~10):(2~10), and it is based on institute
The volume of reaction solution is stated, the total mass concentration of the molybdenum source, the sulphur source and the reducing agent is 0.015~0.5g/mL, and
And the mass ratio of the in the mixed solvent ethylene glycol, polyethylene glycol and organic amine is (1~5):1:(1~5).
7. according to the method described in claim 3, it is characterized in that wherein, the pattern of the molybdenum disulfide particles is nano flower
Shape, and the sulphur source is L-cysteine, the solvent is deionized water；
Optionally, the molar ratio of the molybdenum source and the sulphur source is 1:(1~5), and based on the volume of the reaction solution, the molybdenum
The total mass concentration of source and the sulphur source is 0.015~0.5g/mL.
8. according to the method described in claim 3, it is characterized in that wherein, the pattern of the molybdenum disulfide particles is crescent shape,
And the sulphur source is thioacetamide, the solvent is deionized water；
Optionally, the molar ratio of the molybdenum source and the sulphur source is 1:(1~5), and based on the volume of the reaction solution, the molybdenum
The total mass concentration of source and the sulphur source is 0.015~0.5g/mL.
9. according to the method described in claim 3, it is characterized in that wherein, the pattern of the molybdenum disulfide particles is sheet, and
The sulphur source is thioacetamide, and the solvent is the mixed solvent of polyethylene glycol and deionized water；
Optionally, the molar ratio of the molybdenum source and the sulphur source is 1:(5~30), and based on the volume of the reaction solution, it is described
The total mass concentration of molybdenum source and the sulphur source be 0.015~0.5g/mL, also, the in the mixed solvent polyethylene glycol and go from
The mass ratio of sub- water is 1:(0.2~5).
10. according to the method described in claim 3, it is characterized in that wherein, the pattern of the molybdenum disulfide particles is superthin layer
Shape, and the sulphur source is thiocarbamide, the solvent is organic amine, wherein a length of C16~C22 of carbochain chain of the organic amine；
Optionally, the molar ratio of the molybdenum source and the sulphur source is 1:(5~30), and based on the volume of the reaction solution, it is described
The total mass concentration of molybdenum source and the also sulphur source is 0.015~0.5g/mL.
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| CN114249315A (en) * | 2021-12-30 | 2022-03-29 | 齐鲁工业大学 | Preparation method of organic amine derived carbon and molybdenum disulfide composite material |
| CN114249315B (en) * | 2021-12-30 | 2023-08-29 | 齐鲁工业大学 | Preparation method of organic amine derived carbon and molybdenum disulfide composite material |
| CN114768530A (en) * | 2022-04-29 | 2022-07-22 | 中国工程物理研究院材料研究所 | Application of molybdenum disulfide in hydrogen isotope electrolytic separation |
| CN115888766A (en) * | 2022-11-09 | 2023-04-04 | 福州大学 | Preparation and application of molybdenum disulfide/carbon composite catalyst with flower-shaped structure |
| CN115888766B (en) * | 2022-11-09 | 2024-05-14 | 福州大学 | Preparation and application of flower-like structure molybdenum disulfide/carbon composite catalyst |
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