CN108557888A - A kind of metal phase molybdenum disulfide nano structure and preparation method thereof - Google Patents
A kind of metal phase molybdenum disulfide nano structure and preparation method thereof Download PDFInfo
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Abstract
A kind of metal phase molybdenum disulfide nano structure of present invention offer and preparation method thereof, method includes；1. in deionized water according to the molar ratio ratio dissolving more than sulphur in molybdenum disulfide and molybdenum by molybdate and sulfur-bearing small molecule, stirring forms homogeneous phase solution；2. keeping the temperature 6~30 hours at a temperature of homogeneous phase solution is heated to 180~200 DEG C, reaction naturally cools to room temperature after stopping；3. the precipitation and centrifugal separation that will be obtained after reaction removes supernatant after washing repeatedly, obtains metal phase molybdenum disulfide nano structure.The present invention realizes the hydrothermal synthesis of the proof gold symbolic animal of the birth year molybdenum disulfide nano structure of reduced size, and there is the active site that more marginality, defect etc. can be more on the metal phase molybdenum disulfide surface synthesized.
Description
Technical field
The invention belongs to the preparing technical field of molybdenum disulfide, it is related to preparing metal phase molybdenum disulfide nano based on hydro-thermal method
The method of structure, specially a kind of metal phase molybdenum disulfide nano structure and preparation method thereof.
Background technology
The molybdenum disulfide of stratiform two-dimensional structure is due to possessing preferable chemical stability, with unique optical electro-chemistry
The advantages that matter.It is considered as one to have an opportunity instead of noble metal sill in electro-catalysis field due to its advantage cheap and easy to get
Kind catalyst material.Its unique layer structure makes it can be applied in lithium ion battery and ultracapacitor.Thus curing
Molybdenum is by the extensive concern being catalyzed with energy storage field.
Up to the present, molybdenum disulfide has found that there are three kinds of phase structures, 1T phases, 2H phases, 3R phases.Two existing for nature
Molybdenum sulfide is 2H phases, as semiconductor phase.The application of the molybdenum disulfide of semiconductor phase is because of poor electric conductivity and less work
Property site and be restricted.1T phase molybdenum disulfide is metal phase molybdenum disulfide, can only be synthesized in laboratory, and is possessed preferable
Electric conductivity and more active site and possess huge application prospect.Either semiconductor phase or metal phase possess more preferable
Catalysis and the molybdenum disulfide of performance of energy storage should be：Expose more marginalities, the molybdenum disulfide in defect isoreactivity site is received
Rice structure.
Due to the huge application prospect of metal phase molybdenum disulfide, there are a large amount of methods for preparing metal phase molybdenum disulfide at present
It is reported.Mainly there are CVD growth method, lithium ion stripping method to also have hydro-thermal method.Such as CVD method, the preferable metal phase of quality can be obtained
Molybdenum disulfide, which obtains, disposably has to a small amount of semiconductor phase or metal phase molybdenum disulfide, this makes the extensive of metal phase molybdenum disulfide
Using being restricted.And lithium ion stripping method (J.Am.Chem.Soc.2013,135,10274), using to just in preparation process
Butyl lithium, it is dangerous higher, it is unfriendly to environment.And the hydro-thermal method reported at present synthesizes to obtain metal phase molybdenum disulfide, needs
Add the plurality of raw materials such as reducing agent.The method of wherein obtainable proof gold symbolic animal of the birth year molybdenum disulfide, nanostructure size obtained compared with
Greatly, exposed marginality is less, causes its activity relatively low (Nat.Commun.2016,7,10672).
The step of acquisition metal phase molybdenum disulfide that laboratory is often used at present is that first hydro-thermal or stripping obtain molybdenum sulfide and receive
Rice piece, then the after-treatments such as lithium ion are carried out, finally obtain metal phase molybdenum disulfide.Or by during synthesis of carbon/molybdenum disulfide, add
Enter sulphur source, molybdenum source precursor, while the other materials such as graphene are added, under hydrothermal condition, obtains the gold compound with other materials
Symbolic animal of the birth year molybdenum disulfide.The former step is more, and has certain risk, and the latter's synthesis cost is higher and can not obtain pure metal phase
Molybdenum disulfide.
As can be seen that either CVD growth method, the method for lithium ion stripping method etc., synthesis metal phase molybdenum disulfide are all deposited
In certain defect, prevent it from disposably simply, safely, largely obtaining rich defect, the metal phase of reduced size two of pure phase
Molybdenum sulfide.
Invention content
For problems of the prior art, a kind of metal phase molybdenum disulfide nano structure of present invention offer and its preparation
Method obtains product by a step hydro-thermal, and method is simple, safe, environmental-friendly, and large-scale production is suitble to prepare, easy to operate
Quickly, the metal phase molybdenum disulfide nano structure size obtained is smaller, and rich defect.
The present invention is to be achieved through the following technical solutions：
A kind of preparation method of metal phase molybdenum disulfide nano structure, includes the following steps：
Step 1, molybdate and sulfur-bearing small molecule are dissolved according to the molar ratio ratio more than sulphur in molybdenum disulfide and molybdenum
In deionized water, stirring forms homogeneous phase solution；
Step 2,6~30 hours are kept the temperature at a temperature of homogeneous phase solution being heated to 180~200 DEG C, reaction is natural after stopping
It is cooled to room temperature；
Step 3, the precipitation and centrifugal separation that will be obtained after reaction removes supernatant after washing repeatedly, obtains metal phase curing
Molybdenum nanostructure.
Preferably：Molybdate uses at least one of ammonium molybdate and sodium molybdate in step 1.
Further：The molar concentration of ammonium molybdate is 0.09~1.79mmol/L, the molar concentration of sodium molybdate is 0.625~
12.5mmol/L。
Preferably：When step 1 molybdate is sodium molybdate, the molar concentration rate of sulfur-bearing small molecule and sodium molybdate is 3~9.6,
The molar concentration of sulfur-bearing small molecule is 1.88~120mmol/L；
When molybdate is ammonium molybdate, the molar concentration rate of sulfur-bearing small molecule and ammonium molybdate is 21~67.2, sulfur-bearing small molecule
Molar concentration be 1.88~120mmol/L.
Preferably：Sulfur-bearing small molecule in step 1 uses at least one of thioacetamide and L-cysteine.
Preferably：In step 1, it stirs 10~40 minutes and forms homogeneous phase solution.
Preferably：In step 3, centrifuge speeds are 6500~9500rpm.
A kind of metal phase molybdenum disulfide nano structure is obtained by any one of above-mentioned preparation method.
Preferably, when the metal phase molybdenum disulfide nano structure is nanometer sheet, average-size is 75 nanometers；Described
When metal phase molybdenum disulfide nano structure is nanosphere, 151 nanometers of average-size.Compared with prior art, the present invention have with
Beneficial technique effect down：
The present invention uses molybdate and sulfur-bearing small molecule as molybdenum source and sulphur source, is obtained using one step hydro thermal method.Pass through throwing
Enter to be more than the sulphur source amount of molybdenum disulfide stoichiometric ratio, realizes the hydro-thermal of the proof gold symbolic animal of the birth year molybdenum disulfide nano structure of reduced size
Synthesis, and there is the active site that more marginality, defect etc. can be more on the metal phase molybdenum disulfide surface synthesized.To metal
It is highly beneficial that phase molybdenum disulfide is applied to the fields such as catalysis, energy storage.In water-heat process, sulphur source will as the reducing agent of reaction system
Mo in molybdenum source6+It is restored to Mo4+.Meanwhile excessive sulphur source is adsorbed on the surface of molybdenum disulfide structure, limits molybdenum disulfide
Growth in all directions, to prevent the size of molybdenum disulfide nano structure from continuing to increase, further such that two sulphur of synthesis
Changing molybdenum surface, there are a large amount of defect and marginalities.In addition, being incorporated in the sulphur source on surface, has and prevent metal phase molybdenum disulfide nano
Structure is undergone phase transition in water-heat process, is further transformed to the effect of semiconductor phase molybdenum disulfide.It follows that excessive sulphur
Source not only acts as the effect of reducing agent in hydrothermal reaction process.Meanwhile having regulation and control pattern and increasing active site, it prevents to close
At molybdenum disulfide Metal Phase Transition be semiconductor phase.
Therefore, hydrothermal synthesis richness defect, reduced size metal phase molybdenum disulfide during, excessive sulphur source be to close weight
It wants.
The metal phase molybdenum disulfide nano sheet average-size of synthesis is 50-75nm, and the nanosphere size of synthesis is 100-
151nm, smaller size make molybdenum disulfide nano structure possess high specific surface area, to possess more active sites.When
When putting into stoichiometric ratio of the sulphur source amount slightly larger than molybdenum disulfide, the metal phase molybdenum disulfide of small size can be obtained.
The input amount for further increasing sulphur source, when sulphur source amount be much larger than molybdenum disulfide stoichiometric ratio when, can with arrive ruler
Very little metal phase molybdenum disulfide smaller, surface defect is more, a large amount of defect make the activity of metal phase molybdenum disulfide increase.
Description of the drawings
Fig. 1 a are the transmission electron microscopy of metal phase molybdenum disulfide nano sheet prepared by the method described in present example 1
Mirror figure (TEM).
Fig. 1 b are the transmission electron microscope for the metal phase molybdenum disulfide nano sheet that described in present example 3 prepared by method
Scheme (TEM).
Fig. 2 a are the transmission electron microscopy of metal phase molybdenum disulfide nano ball prepared by the method described in present example
Mirror figure (TEM).Nanosphere average-size is 150nm.
Fig. 2 b are the transmission of the nano flower for the metal phase curing molybdenum sheet assembling that described in present example 36 prepared by method
Electron microscope picture (TEM).The size of nanostructure is 120nm.
Fig. 3 a are the atomic force microscopy diagram for the metal phase molybdenum disulfide nano sheet that described in present example 1 prepared by method
(AFM)。
Fig. 3 b are the thickness distribution curve in the white line region in Fig. 3 a.
Fig. 4 is the Raman figure for the metal phase molybdenum disulfide nano structure that described in present example 1 prepared by method
(Raman)。
Fig. 5 is drawing of the metal phase molybdenum disulfide nano structure of method preparation described in present example 1 after 70 days
Graceful figure (Raman).
Specific implementation mode
With reference to specific embodiment, the present invention is described in further detail, it is described be explanation of the invention and
It is not to limit.
Method of the present invention is a kind of non-lithium ion stripping, but hydro-thermal one-step synthesis metal phase molybdenum disulfide nano
The method of structure.Sulphur source, molybdenum source are dissolved in deionized water by this method by a certain percentage, are put into reaction kettle, in a constant temperature
Degree is lower to keep the temperature certain time length, obtains metal phase molybdenum disulfide nano structure.Synthetic method is simple, safer, environmentally friendly,
The metal phase molybdenum disulfide of more rich defect can disposably be obtained.The metal phase molybdenum disulfide nano sheet of synthesis and synthesis
Metal phase molybdenum disulfide nano ball, possessing smaller size makes molybdenum disulfide nano sheet possess high specific surface area, to possess
More active sites.The molybdenum disulfide of synthesis possesses high conductive metal phase, and reactivity site can be distributed in two sulphur
Change in molybdenum sheet.Meanwhile there is more defect in the metal phase molybdenum disulfide nano structure of synthesis.The spy of metal phase and rich defect
The active site that sign makes molybdenum disulfide participate in catalysis reaction increases, and activity is greatly improved.Meanwhile preferable electric conductivity and higher
It can be applied in lithium ion battery and ultracapacitor when theoretical capacitance.Thus metal phase molybdenum disulfide is in catalysis and energy storage neck
Domain has wide practical use.
Specifically as described in following instance.
Example 1
A kind of preparation method of metal phase molybdenum disulfide nano structure, includes the following steps,
1. 0.06g sodium molybdates and 0.12g thioacetamides are dissolved in 40mL deionized waters, it is vigorously stirred 40 minutes shapes
At homogeneous phase solution, the wherein molar concentration of sodium molybdate is 6.25mmol/L, and the addition of thioacetamide is sodium molybdate substance
6.4 times of concentration is measured, is 40mmol/L.
2. solution is transferred to stainless steel cauldron, for 24 hours, reaction naturally cools to after stopping for 200 DEG C of reactions in an oven
Room temperature.
3. by being centrifuged under the black precipitate 6500rpm rotating speeds in reaction kettle, then being washed with deionized three times, finally
It is dispersed in deionized water.Obtain the dispersion liquid of metal phase molybdenum disulfide nano structure.
It is smaller to obtain size, the more marginalities of exposure, average-size is the metal phase molybdenum disulfide nano sheet of 75nm, is such as schemed
Shown in 1a.Its atomic force microscopy diagram AFM is as shown in Figure 3a, and the thickness distribution curve in white line region is as shown in Figure 3b in Fig. 3 a.
As shown in figure 4, have the Raman peaks of typical gold symbolic animal of the birth year molybdenum disulfide in its Raman figure, and there is no the molybdenum disulfide of semiconductor phase
Raman peaks, that is, the metal phase molybdenum disulfide prepared be pure phase.Raman figure after 70 days is as shown in figure 5, with freshly prepd metal
The Raman signal of phase molybdenum disulfide is similar, almost without there is the characteristic peak of the Raman of molybdenum trioxide, it can thus be appreciated that the gold prepared
Symbolic animal of the birth year molybdenum disulfide has preferable stability.
Embodiment 2-3：The influence of the Concentration on Metal phase molybdenum disulfide growth size of thioacetamide is added in step 2.
Example 2
Except being added in step 2 in the present embodiment, the thioacetamide of addition is 3 times of the substance withdrawl syndrome of sodium molybdate,
Outside for 18.75mmol/L, remaining step is same as Example 1, and the average-size of obtained metal phase molybdenum disulfide nano sheet is
90nm。
Example 3
Except being added in step 2 in the present embodiment, the thioacetamide of addition is that 9.6 times of the substance withdrawl syndrome of sodium molybdate is
Outside 60mmol/L, remaining step is same as Example 1, and the average-size of obtained metal phase molybdenum disulfide nano sheet is 50nm,
As shown in Figure 1 b.
Embodiment 4-5：Change reaction temperature in step 2 and obtains metal phase molybdenum disulfide nano sheet.
Example 4
It removes and is added in step 2 in the present embodiment, at a temperature of homogeneous phase solution is heated to 180 DEG C, remaining step and implementation
Example 1 is identical, obtains metal phase molybdenum disulfide nano sheet.
Example 5
It removes and is added in step 2 in the present embodiment, at a temperature of homogeneous phase solution is heated to 190 DEG C, remaining step and implementation
Example 1 is identical, obtains metal phase molybdenum disulfide nano sheet.
Embodiment 6-7：Change soaking time in step 2 and metal phase molybdenum disulfide nano structure can be obtained.
Example 6
It is 6 hours by the homogeneous phase solution heating and thermal insulation time except being added in step 2 in the present embodiment, remaining step and implementation
Example 1 is identical, obtains metal phase molybdenum disulfide nano structure, and pattern is sheet, and the yield of metal phase molybdenum disulfide is less than example 1.
Example 7
It is 30 hours by the homogeneous phase solution heating and thermal insulation time except being added in step 2 in the present embodiment, remaining step and implementation
Example 1 is identical, obtains metal phase molybdenum disulfide nano structure, and pattern is sheet, and the yield of metal phase molybdenum disulfide is slightly more than example 1.
Example 8
1. 0.006g sodium molybdates and 0.012g thioacetamides are dissolved in 40mL deionized waters, it is vigorously stirred 40 minutes
Homogeneous phase solution is formed, the wherein molar concentration of sodium molybdate is 0.625mmol/L, and the addition of thioacetamide is sodium molybdate substance
6.4 times of amount concentration, be 4mmol/L.
2. solution is transferred to stainless steel cauldron, for 24 hours, reaction naturally cools to after stopping for 200 DEG C of reactions in an oven
Room temperature.
3. by being centrifuged under the black precipitate 6500rpm rotating speeds in reaction kettle, then being washed with deionized three times, finally
It is dispersed in deionized water.Obtain the dispersion liquid of metal phase molybdenum disulfide nano structure.
It is smaller to obtain size, the more marginalities of exposure, average-size is the metal phase molybdenum disulfide nano sheet of 80nm.
Embodiment 9-10：The influence of the Concentration on Metal phase molybdenum disulfide growth size of thioacetamide is added in step 2.
Example 9
Except being added in step 2 in the present embodiment, the thioacetamide of addition is 3 times of the substance withdrawl syndrome of sodium molybdate,
Outside for 1.88mmol/L, remaining step is same as Example 8, and the average-size of obtained metal phase molybdenum disulfide nano sheet is
100nm。
Example 10
Except being added in step 2 in the present embodiment, the thioacetamide of addition is that 9.6 times of the substance withdrawl syndrome of sodium molybdate is
Outside 6mmol/L, remaining step is same as Example 8, and the average-size of obtained metal phase molybdenum disulfide nano sheet is 70nm.
Embodiment 11-12：Change reaction temperature in step 2 and obtains metal phase molybdenum disulfide nano sheet.
Example 11
It removes and is added in step 2 in the present embodiment, at a temperature of homogeneous phase solution is heated to 180 DEG C, remaining step and implementation
Example 8 is identical, obtains metal phase molybdenum disulfide nano sheet.
Example 12
It removes and is added in step 2 in the present embodiment, at a temperature of homogeneous phase solution is heated to 190 DEG C, remaining step and implementation
Example 8 is identical, obtains metal phase molybdenum disulfide nano sheet.
Embodiment 13-14：Change soaking time in step 2 and metal phase molybdenum disulfide nano structure can be changed.
Example 13
It is 6 hours by the homogeneous phase solution heating and thermal insulation time except being added in step 2 in the present embodiment, remaining step and implementation
Example 8 is identical, obtains metal phase molybdenum disulfide nano structure, and pattern is sheet, and the yield of metal phase molybdenum disulfide is less than example 8.
Example 14
It is 30 hours by the homogeneous phase solution heating and thermal insulation time except being added in step 2 in the present embodiment, remaining step and implementation
Example 8 is identical, obtains metal phase molybdenum disulfide nano structure, and pattern is sheet, and the yield of metal phase molybdenum disulfide is slightly more than example 8.
Example 15
1. 0.12g sodium molybdates and 0.24g thioacetamides are dissolved in 40mL deionized waters, it is vigorously stirred 40 minutes shapes
At homogeneous phase solution, the wherein molar concentration of sodium molybdate is 12.5mmol/L, and the addition of thioacetamide is sodium molybdate substance
Measure concentration 6.4 times are 80mmol/L.
2. solution is transferred to stainless steel cauldron, for 24 hours, reaction naturally cools to after stopping for 200 DEG C of reactions in an oven
Room temperature.
3. by being centrifuged under the black precipitate 6500rpm rotating speeds in reaction kettle, then being washed with deionized three times, finally
It is dispersed in deionized water.Obtain metal phase molybdenum disulfide nano structure.
It is smaller to obtain size, the more marginalities of exposure, average-size is the metal phase molybdenum disulfide nano sheet of 65nm.
Embodiment 16-17：The shadow of the Concentration on Metal phase molybdenum disulfide growth size of thioacetamide is added in step 2
It rings.
Example 16
Except being added in step 2 in the present embodiment, the thioacetamide of addition is 3 times of the substance withdrawl syndrome of sodium molybdate,
Outside for 37.5mmol/L, remaining step is identical as embodiment 15, and the average-size of obtained metal phase molybdenum disulfide nano sheet is
80nm。
Example 17
Except being added in step 2 in the present embodiment, the thioacetamide of addition is that 9.6 times of the substance withdrawl syndrome of sodium molybdate is
Outside 120mmol/L, remaining step is same as Example 8, and the average-size of obtained metal phase molybdenum disulfide nano sheet is 55nm.
Embodiment 18-19：Change reaction temperature in step 2 and obtains metal phase molybdenum disulfide nano sheet.
Example 18
It removes and is added in step 2 in the present embodiment, at a temperature of homogeneous phase solution is heated to 180 DEG C, remaining step and implementation
Example 15 is identical, obtains metal phase molybdenum disulfide nano sheet.
Example 19
It removes and is added in step 2 in the present embodiment, at a temperature of homogeneous phase solution is heated to 190 DEG C, remaining step and implementation
Example 15 is identical, obtains metal phase molybdenum disulfide nano sheet.
Embodiment 20-21：Change soaking time in step 2 and metal phase molybdenum disulfide nano structure yield can be changed.
Example 20
It is 6 hours by the homogeneous phase solution heating and thermal insulation time except being added in step 2 in the present embodiment, remaining step and implementation
Example 15 is identical, obtains metal phase molybdenum disulfide nano structure, and pattern is sheet, and the yield of metal phase molybdenum disulfide is less than example 15.
Example 21
It is 30 hours by the homogeneous phase solution heating and thermal insulation time except being added in step 2 in the present embodiment, remaining step and implementation
Example 15 is identical, obtains metal phase molybdenum disulfide nano structure, and pattern is sheet, and the yield of metal phase molybdenum disulfide is slightly more than example
15。
Example 22
A kind of preparation method of metal phase molybdenum disulfide nano structure, includes the following steps,
1. 0.06g sodium molybdates and 0.19g L-cysteines are dissolved in 40mL deionized waters, it is vigorously stirred 10 minutes
Homogeneous phase solution is formed, the wherein molar concentration of sodium molybdate is 6.25mmol/L, and the addition of L-cysteine is sodium molybdate substance
6.4 times of amount concentration, be 40mmol/L.
2. solution is transferred to stainless steel cauldron, for 24 hours, reaction naturally cools to after stopping for 200 DEG C of reactions in an oven
Room temperature.
3. by being centrifuged under the black precipitate 6500rpm rotating speeds in reaction kettle, then being washed with deionized three times, finally
It is dispersed in deionized water.Metal phase molybdenum disulfide nano ball is obtained, such as Fig. 2 a.
It is smaller to obtain size, the more marginalities of exposure, average-size is the metal phase molybdenum disulfide nano ball of 150nm.
Embodiment 23-24：The shadow of the Concentration on Metal phase molybdenum disulfide growth size of L-cysteine is added in step 2
It rings.
Example 23
Except being added in step 2 in the present embodiment, the L-cysteine of addition is 3 times of the substance withdrawl syndrome of sodium molybdate,
Outside for 18.75mmol/L, remaining step is identical as embodiment 22, and the average-size of obtained metal phase molybdenum disulfide nano ball is
180nm。
Example 24
Except being added in step 2 in the present embodiment, the L-cysteine of addition is that 9.6 times of the substance withdrawl syndrome of sodium molybdate is
Outside 60mmol/L, remaining step is identical as embodiment 22, and the average-size of obtained metal phase molybdenum disulfide nano ball is
140nm。
Embodiment 25-26：Change reaction temperature in step 2 and obtains metal phase molybdenum disulfide nano ball.
Example 25
It removes and is added in step 2 in the present embodiment, at a temperature of homogeneous phase solution is heated to 180 DEG C, remaining step and implementation
Example 22 is identical, obtains metal phase molybdenum disulfide nano ball.
Example 26
It removes and is added in step 2 in the present embodiment, at a temperature of homogeneous phase solution is heated to 190 DEG C, remaining step and implementation
Example 22 is identical, obtains metal phase molybdenum disulfide nano ball.
Embodiment 27-28：Change soaking time in step 2 and metal phase molybdenum disulfide nano ball can be obtained.
Example 27
It is 6 hours by the homogeneous phase solution heating and thermal insulation time except being added in step 2 in the present embodiment, remaining step and implementation
Example 1 is identical, obtains metal phase molybdenum disulfide nano structure, and pattern is spherical, and the yield of metal phase molybdenum disulfide is less than example 22.
Example 28
It is 30 hours by the homogeneous phase solution heating and thermal insulation time except being added in step 2 in the present embodiment, remaining step and implementation
Example 22 is identical, obtains metal phase molybdenum disulfide nano structure, and pattern is spherical, and the yield of metal phase molybdenum disulfide is slightly more than example
22。
Example 29
1. 0.006g sodium molybdates and 0.019g L-cysteines are dissolved in 40mL deionized waters, it is vigorously stirred 40 points
It is bell at homogeneous phase solution, wherein the molar concentration of sodium molybdate is 0.625mmol/L, and the addition of L-cysteine is sodium molybdate object
6.4 times of the amount concentration of matter are 4mmol/L.
2. solution is transferred to stainless steel cauldron, for 24 hours, reaction naturally cools to after stopping for 200 DEG C of reactions in an oven
Room temperature.
3. by being centrifuged under the black precipitate 6500rpm rotating speeds in reaction kettle, then being washed with deionized three times, finally
It is dispersed in deionized water.Obtain metal phase molybdenum disulfide nano ball.
It is smaller to obtain size, the more marginalities of exposure, average-size is the metal phase molybdenum disulfide nano ball of 160nm.
Embodiment 30-31：The Concentration on Metal phase molybdenum disulfide nano ball growth size of L-cysteine is added in step 2
Influence.
Example 30
Except being added in step 2 in the present embodiment, the L-cysteine of addition is 3 times of the substance withdrawl syndrome of sodium molybdate,
Outside for 1.88mmol/L, remaining step is identical as embodiment 29, and the average-size of obtained metal phase molybdenum disulfide nano ball is
180nm。
Example 31
Except being added in step 2 in the present embodiment, the thioacetamide of addition is that 9.6 times of the substance withdrawl syndrome of sodium molybdate is
Outside 6mmol/L, remaining step is same as Example 2, and the average-size of obtained metal phase molybdenum disulfide nano ball is 155nm.
Embodiment 32-33：Change reaction temperature in step 2 and obtains metal phase molybdenum disulfide nano ball.
Example 32
It removes and is added in step 2 in the present embodiment, at a temperature of homogeneous phase solution is heated to 180 DEG C, remaining step and implementation
Example 29 is identical, obtains metal phase molybdenum disulfide nano ball.
Example 33
It removes and is added in step 2 in the present embodiment, at a temperature of homogeneous phase solution is heated to 190 DEG C, remaining step and implementation
Example 8 is identical, obtains metal phase molybdenum disulfide nano ball.
Embodiment 34-35：Change the yield that metal phase molybdenum disulfide nano structure can be changed in soaking time in step 2.
Example 34
It is 6 hours by the homogeneous phase solution heating and thermal insulation time except being added in step 2 in the present embodiment, remaining step and implementation
Example 29 is identical, obtains metal phase molybdenum disulfide nano structure, and pattern is spherical, and the yield of metal phase molybdenum disulfide is less than example 29.
Example 35
It is 30 hours by the homogeneous phase solution heating and thermal insulation time except being added in step 2 in the present embodiment, remaining step and implementation
Example 29 is identical, obtains metal phase molybdenum disulfide nano structure, and pattern is sheet, and the yield of metal phase molybdenum disulfide is slightly more than example
29。
Example 36
1. 0.12g sodium molybdates and 0.38g thioacetamides are dissolved in 40mL deionized waters, it is vigorously stirred 40 minutes shapes
At homogeneous phase solution, the wherein molar concentration of sodium molybdate is 12.5mmol/L, and the addition of thioacetamide is sodium molybdate substance
Measure concentration 6.4 times are 80mmol/L.
2. solution is transferred to stainless steel cauldron, for 24 hours, reaction naturally cools to after stopping for 200 DEG C of reactions in an oven
Room temperature.
3. by being centrifuged under the black precipitate 6500rpm rotating speeds in reaction kettle, then being washed with deionized three times, finally
It is dispersed in deionized water.Obtain metal phase molybdenum disulfide nano structure.
It is smaller to obtain size, the more marginalities of exposure, average-size is the metal phase molybdenum disulfide nano structure of 120nm,
Pattern is flower-shaped, such as Fig. 2 b.
Embodiment 37-38：The Concentration on Metal phase molybdenum disulfide nano flower growth size of L-cysteine is added in step 2
Influence.
Example 37
Except being added in step 2 in the present embodiment, the L-cysteine of addition is 3 times of the substance withdrawl syndrome of sodium molybdate,
Outside for 37.5mmol/L, remaining step is identical as embodiment 36, and the average-size of obtained metal phase molybdenum disulfide nano flower is
135nm。
Example 38
Except being added in step 2 in the present embodiment, the thioacetamide of addition is that 9.6 times of the substance withdrawl syndrome of sodium molybdate is
Outside 120mmol/L, remaining step is identical as embodiment 36, and the average-size of obtained metal phase molybdenum disulfide nano flower is
116nm。
Embodiment 39-40：Change reaction temperature in step 2 and obtains metal phase molybdenum disulfide nano flower.
Example 39
It removes and is added in step 2 in the present embodiment, at a temperature of homogeneous phase solution is heated to 180 DEG C, remaining step and implementation
Example 36 is identical, obtains metal phase molybdenum disulfide nano flower.
Example 40
It removes and is added in step 2 in the present embodiment, at a temperature of homogeneous phase solution is heated to 190 DEG C, remaining step and implementation
Example 36 is identical, obtains metal phase molybdenum disulfide nano flower.
Embodiment 41-42：Change the yield that metal phase molybdenum disulfide nano flower can be changed in soaking time in step 2.
Example 41
It is 6 hours by the homogeneous phase solution heating and thermal insulation time except being added in step 2 in the present embodiment, remaining step and implementation
Example 36 is identical, obtains metal phase molybdenum disulfide nano structure, and pattern is flower-shaped, and the yield of metal phase molybdenum disulfide is less than example 36.
Example 42
It is 30 hours by the homogeneous phase solution heating and thermal insulation time except being added in step 2 in the present embodiment, remaining step and implementation
Example 36 is identical, obtains metal phase molybdenum disulfide nano structure, and pattern is flower-shaped, and the yield of metal phase molybdenum disulfide is slightly more than example
36。
Example 43
A kind of preparation method of metal phase molybdenum disulfide nano structure, includes the following steps,
1. 0.044g ammonium molybdates and 0.12g thioacetamides are dissolved in 40mL deionized waters, it is vigorously stirred 40 minutes
Homogeneous phase solution is formed, the wherein molar concentration of ammonium molybdate is 0.9mmol/L, and the addition of thioacetamide is mole of ammonium molybdate
45 times of concentration is 40mmol/L.
2. solution is transferred to stainless steel cauldron, for 24 hours, reaction naturally cools to after stopping for 200 DEG C of reactions in an oven
Room temperature.
3. by being centrifuged under the black precipitate 6500rpm rotating speeds in reaction kettle, then being washed with deionized three times, finally
It is dispersed in deionized water.Obtain the dispersion liquid of metal phase molybdenum disulfide nano structure.
It is smaller to obtain size, the more marginalities of exposure, average-size is the metal phase molybdenum disulfide nano sheet of 80nm.
Embodiment 44-45：The shadow of the Concentration on Metal phase molybdenum disulfide growth size of thioacetamide is added in step 2
It rings.
Example 44
Except being added in step 2 in the present embodiment, the thioacetamide of addition is 3 times of the substance withdrawl syndrome of ammonium molybdate,
Outside for 18.75mmol/L, remaining step is same as Example 1, and the average-size of obtained metal phase molybdenum disulfide nano sheet is
94nm。
Example 45
Except being added in step 2 in the present embodiment, the thioacetamide of addition is that 9.6 times of the substance withdrawl syndrome of sodium molybdate is
Outside 60mmol/L, remaining step is same as Example 1, and the average-size of obtained metal phase molybdenum disulfide nano sheet is 81nm.
Embodiment 46-47：Change reaction temperature in step 2 and obtains metal phase molybdenum disulfide nano sheet.
Example 46
It removes and is added in step 2 in the present embodiment, at a temperature of homogeneous phase solution is heated to 180 DEG C, remaining step and implementation
Example 43 is identical, obtains metal phase molybdenum disulfide nano sheet.
Example 47
It removes and is added in step 2 in the present embodiment, at a temperature of homogeneous phase solution is heated to 190 DEG C, remaining step and implementation
Example 43 is identical, obtains metal phase molybdenum disulfide nano sheet.
Embodiment 48-49：Change the yield that metal phase molybdenum disulfide nano structure can be changed in soaking time in step 2.
Example 48
It is 6 hours by the homogeneous phase solution heating and thermal insulation time except being added in step 2 in the present embodiment, remaining step and implementation
Example 43 is identical, obtains metal phase molybdenum disulfide nano structure, and pattern is sheet, and the yield of metal phase molybdenum disulfide is less than example 43.
Example 49
It is 30 hours by the homogeneous phase solution heating and thermal insulation time except being added in step 2 in the present embodiment, remaining step and implementation
Example 43 is identical, obtains metal phase molybdenum disulfide nano structure, and pattern is sheet, and the yield of metal phase molybdenum disulfide is slightly more than example
43。
Example 50
1. 0.0044g ammonium molybdates and 0.012g thioacetamides are dissolved in 40mL deionized waters, it is vigorously stirred 40 points
It is bell at homogeneous phase solution, wherein the molar concentration of ammonium molybdate is 0.09mmol/L, and the addition of thioacetamide is ammonium molybdate object
45 times of the amount concentration of matter are 4mmol/L.
2. solution is transferred to stainless steel cauldron, for 24 hours, reaction naturally cools to after stopping for 200 DEG C of reactions in an oven
Room temperature.
3. by being centrifuged under the black precipitate 6500rpm rotating speeds in reaction kettle, then being washed with deionized three times, finally
It is dispersed in deionized water.Obtain the dispersion liquid of metal phase molybdenum disulfide nano structure.
It is smaller to obtain size, the more marginalities of exposure, average-size is the metal phase molybdenum disulfide nano sheet of 100nm.
The influence of the Concentration on Metal phase molybdenum disulfide growth size of thioacetamide is added in embodiment 51-52.
Example 51
Except being added in step 2 in the present embodiment, the thioacetamide of addition is 3 times of the substance withdrawl syndrome of ammonium molybdate,
Outside for 1.88mmol/L, remaining step and embodiment 50, the average-size of obtained metal phase molybdenum disulfide nano sheet are
105nm。
Example 52
Except being added in step 2 in the present embodiment, the thioacetamide of addition is 67.2 times of the substance withdrawl syndrome of ammonium molybdate
Outside for 6mmol/L, remaining step is identical as embodiment 50, and the average-size of obtained metal phase molybdenum disulfide nano sheet is
90nm。
Embodiment 53-54：Change reaction temperature in step 2 and obtains metal phase molybdenum disulfide nano sheet.
Example 53
It removes and is added in step 2 in the present embodiment, at a temperature of homogeneous phase solution is heated to 180 DEG C, remaining step and implementation
Example 50 is identical, obtains metal phase molybdenum disulfide nano sheet.
Example 54
It removes and is added in step 2 in the present embodiment, at a temperature of homogeneous phase solution is heated to 190 DEG C, remaining step and implementation
Example 50 is identical, obtains metal phase molybdenum disulfide nano sheet.
Embodiment 55-56：Change the yield that metal phase molybdenum disulfide nano structure can be changed in soaking time in step 2.
Example 55
It is 6 hours by the homogeneous phase solution heating and thermal insulation time except being added in step 2 in the present embodiment, remaining step and implementation
Example 50 is identical, obtains metal phase molybdenum disulfide nano structure, and pattern is sheet, and the yield of metal phase molybdenum disulfide is less than example 50.
Example 56
It is 30 hours by the homogeneous phase solution heating and thermal insulation time except being added in step 2 in the present embodiment, remaining step and implementation
Example 50 is identical, obtains metal phase molybdenum disulfide nano structure, and pattern is sheet, and the yield of metal phase molybdenum disulfide is slightly more than example
50。
Example 57
1. 0.098g ammonium molybdates and 0.24g thioacetamides are dissolved in 40mL deionized waters, it is vigorously stirred 40 minutes
Homogeneous phase solution is formed, the wherein molar concentration of ammonium molybdate is 1.79mmol/L, and the addition of thioacetamide is ammonium molybdate substance
45 times of amount concentration, be 80mmol/L.
2. solution is transferred to stainless steel cauldron, for 24 hours, reaction naturally cools to after stopping for 200 DEG C of reactions in an oven
Room temperature.
3. by being centrifuged under the black precipitate 6500rpm rotating speeds in reaction kettle, then being washed with deionized three times, finally
It is dispersed in deionized water.Obtain metal phase molybdenum disulfide nano structure.
It is smaller to obtain size, the more marginalities of exposure, average-size is the metal phase molybdenum disulfide nano sheet of 95nm.
Embodiment 58-59：The shadow of the Concentration on Metal phase molybdenum disulfide growth size of thioacetamide is added in step 2
It rings.
Example 58
Except being added in step 2 in the present embodiment, the thioacetamide of addition is 21 times of the substance withdrawl syndrome of ammonium molybdate,
Outside for 37.5mmol/L, remaining step is identical as embodiment 57, and the average-size of obtained metal phase molybdenum disulfide nano sheet is
103nm。
Example 59
Except being added in step 2 in the present embodiment, the thioacetamide of addition is 67.2 times of the substance withdrawl syndrome of ammonium molybdate
Outside for 120mmol/L, remaining step is identical as embodiment 57, and the average-size of obtained metal phase molybdenum disulfide nano sheet is
95nm。
Embodiment 60-61：Change reaction temperature in step 2 and obtains metal phase molybdenum disulfide nano sheet.
Example 60
It removes and is added in step 2 in the present embodiment, at a temperature of homogeneous phase solution is heated to 180 DEG C, remaining step and implementation
Example 57 is identical, obtains metal phase molybdenum disulfide nano sheet.
Example 61
It removes and is added in step 2 in the present embodiment, at a temperature of homogeneous phase solution is heated to 190 DEG C, remaining step and implementation
Example 57 is identical, obtains metal phase molybdenum disulfide nano sheet.
Embodiment 62-63：Change soaking time in step 2 and metal phase molybdenum disulfide nano structure yield can be changed.
Example 62
It is 6 hours by the homogeneous phase solution heating and thermal insulation time except being added in step 2 in the present embodiment, remaining step and implementation
Example 57 is identical, obtains metal phase molybdenum disulfide nano structure, and pattern is sheet, and the yield of metal phase molybdenum disulfide is less than example 57.
Example 63
It is 30 hours by the homogeneous phase solution heating and thermal insulation time except being added in step 2 in the present embodiment, remaining step and implementation
Example 57 is identical, obtains metal phase molybdenum disulfide nano structure, and pattern is sheet, and the yield of metal phase molybdenum disulfide is slightly more than example
57。
Example 64
A kind of preparation method of metal phase molybdenum disulfide nano structure, includes the following steps,
1. 0.044g ammonium molybdates and 0.19g L-cysteines are dissolved in 40mL deionized waters, it is vigorously stirred 40 minutes
Homogeneous phase solution is formed, the wherein molar concentration of ammonium molybdate is 0.9mmol/L, and the addition of L-cysteine is ammonium molybdate substance
Measure concentration 45 times are 40mmol/L.
2. solution is transferred to stainless steel cauldron, for 24 hours, reaction naturally cools to after stopping for 200 DEG C of reactions in an oven
Room temperature.
3. by being centrifuged under the black precipitate 9500rpm rotating speeds in reaction kettle, then being washed with deionized three times, finally
It is dispersed in deionized water.Obtain metal phase molybdenum disulfide nano ball.
It is smaller to obtain size, the more marginalities of exposure, average-size is the metal phase molybdenum disulfide nano ball of 160nm.
Embodiment 65-66：The shadow of the Concentration on Metal phase molybdenum disulfide growth size of L-cysteine is added in step 2
It rings.
Example 65
Except being added in step 2 in the present embodiment, the L-cysteine of addition is 21 times of the substance withdrawl syndrome of ammonium molybdate,
Outside for 18.75mmol/L, remaining step is identical as embodiment 64, and the average-size of obtained metal phase molybdenum disulfide nano ball is
180nm。
Example 66
Except being added in step 2 in the present embodiment, the L-cysteine of addition is that 45 times of the substance withdrawl syndrome of ammonium molybdate is
Outside 60mmol/L, remaining step is identical as embodiment 64, and the average-size of obtained metal phase molybdenum disulfide nano ball is
170nm。
Embodiment 67-68：Change reaction temperature in step 2 and obtains metal phase molybdenum disulfide nano ball.
Example 67
It removes and is added in step 2 in the present embodiment, at a temperature of homogeneous phase solution is heated to 180 DEG C, remaining step and implementation
Example 64 is identical, obtains metal phase molybdenum disulfide nano ball.
Example 68
It removes and is added in step 2 in the present embodiment, at a temperature of homogeneous phase solution is heated to 190 DEG C, remaining step and implementation
Example 64 is identical, obtains metal phase molybdenum disulfide nano ball.
Embodiment 69-70：Change soaking time in step 2 and metal phase molybdenum disulfide nano ball can be obtained.
Example 69
It is 6 hours by the homogeneous phase solution heating and thermal insulation time except being added in step 2 in the present embodiment, remaining step and implementation
Example 64 is identical, obtains metal phase molybdenum disulfide nano structure, and pattern is spherical, and the yield of metal phase molybdenum disulfide is less than example 64.
Example 70
It is 30 hours by the homogeneous phase solution heating and thermal insulation time except being added in step 2 in the present embodiment, remaining step and implementation
Example 64 is identical, obtains metal phase molybdenum disulfide nano structure, and pattern is spherical, and the yield of metal phase molybdenum disulfide is slightly more than example
64。
Example 71
1. 0.004g ammonium molybdates and 0.019g L-cysteines are dissolved in 40mL deionized waters, it is vigorously stirred 40 points
It is bell at homogeneous phase solution, wherein the molar concentration of ammonium molybdate is 0.09mmol/L, and the addition of L-cysteine is ammonium molybdate object
45 times of the amount concentration of matter are 4mmol/L.
2. solution is transferred to stainless steel cauldron, for 24 hours, reaction naturally cools to after stopping for 200 DEG C of reactions in an oven
Room temperature.
3. by being centrifuged under the black precipitate 6500rpm rotating speeds in reaction kettle, then being washed with deionized three times, finally
It is dispersed in deionized water.Obtain metal phase molybdenum disulfide nano ball.
It is smaller to obtain size, the more marginalities of exposure, average-size is the metal phase molybdenum disulfide nano ball of 160nm.
Embodiment 72-73：The Concentration on Metal phase molybdenum disulfide nano ball growth size of L-cysteine is added in step 2
Influence.
Example 72
Except being added in step 2 in the present embodiment, the L-cysteine of addition is 21 times of the substance withdrawl syndrome of ammonium molybdate,
Outside for 1.88mmol/L, remaining step is identical as embodiment 71, and the average-size of obtained metal phase molybdenum disulfide nano flower is
171nm。
Example 73
Except being added in step 2 in the present embodiment, the L-cysteine of addition is 67.2 times of the substance withdrawl syndrome of ammonium molybdate
Outside for 6mmol/L, remaining step is identical as embodiment 71, and the average-size of obtained metal phase molybdenum disulfide nano flower is
154nm。
Embodiment 74-75：Change reaction temperature in step 2 and obtains metal phase molybdenum disulfide nano flower.
Example 74
It removes and is added in step 2 in the present embodiment, at a temperature of homogeneous phase solution is heated to 180 DEG C, remaining step and implementation
Example 71 is identical, obtains metal phase molybdenum disulfide nano flower.
Example 75
It removes and is added in step 2 in the present embodiment, at a temperature of homogeneous phase solution is heated to 190 DEG C, remaining step and implementation
Example 71 is identical, obtains metal phase molybdenum disulfide nano flower.
Embodiment 76-77：Change the yield that metal phase molybdenum disulfide nano structure can be changed in soaking time in step 2.
Example 76
It is 6 hours by the homogeneous phase solution heating and thermal insulation time except being added in step 2 in the present embodiment, remaining step and implementation
Example 71 is identical, obtains metal phase molybdenum disulfide nano structure, and pattern is flower-shaped, and the yield of metal phase molybdenum disulfide is less than example 71.
Example 77
It is 30 hours by the homogeneous phase solution heating and thermal insulation time except being added in step 2 in the present embodiment, remaining step and implementation
Example 71 is identical, obtains metal phase molybdenum disulfide nano structure, and pattern is flower-shaped, and the yield of metal phase molybdenum disulfide is slightly more than example
71。
Example 78
1. 0.098g ammonium molybdates and 0.38g L-cysteines are dissolved in 40mL deionized waters, it is vigorously stirred 40 minutes
Homogeneous phase solution is formed, the wherein molar concentration of ammonium molybdate is 1.78mmol/L, and the addition of thioacetamide is ammonium molybdate substance
6.4 times of amount concentration, be 120mmol/L.
2. solution is transferred to stainless steel cauldron, for 24 hours, reaction naturally cools to after stopping for 200 DEG C of reactions in an oven
Room temperature.
3. by being centrifuged under the black precipitate 6500rpm rotating speeds in reaction kettle, then being washed with deionized three times, finally
It is dispersed in deionized water.Obtain metal phase molybdenum disulfide nano structure.
It is smaller to obtain size, the more marginalities of exposure, average-size is the metal phase molybdenum disulfide nano structure of 130nm,
Pattern is flower-shaped.
Embodiment 79-80：The Concentration on Metal phase molybdenum disulfide nano flower growth size of L-cysteine is added in step 2
Influence.
Example 79
Except being added in step 2 in the present embodiment, the L-cysteine of addition is 21 times of the substance withdrawl syndrome of ammonium molybdate,
Outside for 37.5mmol/L, remaining step is identical as embodiment 78, and the average-size of obtained metal phase molybdenum disulfide nano flower is
135nm。
Example 80
Except being added in step 2 in the present embodiment, the thioacetamide of addition is 67.2 times of the substance withdrawl syndrome of ammonium molybdate
Outside for 120mmol/L, remaining step is identical as embodiment 78, and the average-size of obtained metal phase molybdenum disulfide nano flower is
110nm。
Embodiment 81-88：Change reaction temperature in step 2 and obtains metal phase molybdenum disulfide nano flower.
Example 81
It removes and is added in step 2 in the present embodiment, at a temperature of homogeneous phase solution is heated to 180 DEG C, remaining step and implementation
Example 78 is identical, obtains metal phase molybdenum disulfide nano flower.
Example 82
It removes and is added in step 2 in the present embodiment, at a temperature of homogeneous phase solution is heated to 190 DEG C, remaining step and implementation
Example 78 is identical, obtains metal phase molybdenum disulfide nano flower.
Embodiment 83-84：Change the yield that metal phase molybdenum disulfide nano flower can be changed in soaking time in step 2.
Example 83
It is 6 hours by the homogeneous phase solution heating and thermal insulation time except being added in step 2 in the present embodiment, remaining step and implementation
Example 78 is identical, obtains metal phase molybdenum disulfide nano structure, and pattern is flower-shaped, and the yield of metal phase molybdenum disulfide is less than example 78.
Example 84
It is 30 hours by the homogeneous phase solution heating and thermal insulation time except being added in step 2 in the present embodiment, remaining step and implementation
Example 78 is identical, obtains metal phase molybdenum disulfide nano structure, and pattern is flower-shaped, and the yield of metal phase molybdenum disulfide is slightly more than example
78。
Claims (9)
1. a kind of preparation method of metal phase molybdenum disulfide nano structure, which is characterized in that include the following steps：
Step 1, by molybdate and sulfur-bearing small molecule according to the molar ratio ratio more than sulphur in molybdenum disulfide and molybdenum be dissolved in from
In sub- water, stirring forms homogeneous phase solution；
Step 2,6~30 hours are kept the temperature at a temperature of homogeneous phase solution being heated to 180~200 DEG C, natural cooling after reaction stops
To room temperature；
Step 3, the precipitation and centrifugal separation that will be obtained after reaction removes supernatant after washing repeatedly, obtains metal phase molybdenum disulfide and receive
Rice structure.
2. a kind of preparation method of metal phase molybdenum disulfide nano structure according to claim 1, it is characterised in that：Step
Molybdate uses at least one of ammonium molybdate and sodium molybdate in 1.
3. a kind of preparation method of metal phase molybdenum disulfide nano structure according to claim 2, it is characterised in that：Molybdic acid
The molar concentration of ammonium is 0.09~1.79mmol/L, and the molar concentration of sodium molybdate is 0.625~12.5mmol/L.
4. a kind of preparation method of metal phase molybdenum disulfide nano structure according to claim 1, it is characterised in that：Step
When 1 molybdate is sodium molybdate, the molar concentration rate of sulfur-bearing small molecule and sodium molybdate is 3~9.6, the molar concentration of sulfur-bearing small molecule
For 1.88~120mmol/L；
When molybdate is ammonium molybdate, the molar concentration rate of sulfur-bearing small molecule and ammonium molybdate is 21~67.2, and sulfur-bearing small molecule is rubbed
You are a concentration of 1.88~120mmol/L.
5. a kind of preparation method of metal phase molybdenum disulfide nano structure according to claim 1, it is characterised in that：Step
Sulfur-bearing small molecule in 1 uses at least one of thioacetamide and L-cysteine.
6. a kind of preparation method of metal phase molybdenum disulfide nano structure according to claim 1, it is characterised in that：In step
In rapid 1, stirs 10~40 minutes and form homogeneous phase solution.
7. a kind of preparation method of metal phase molybdenum disulfide nano structure according to claim 1, it is characterised in that：In step
In rapid 3, centrifuge speeds are 6500~9500rpm.
8. a kind of metal phase molybdenum disulfide nano structure, which is characterized in that by any one of the claim 1-7 preparation methods
It obtains.
9. a kind of metal phase molybdenum disulfide nano structure according to claim 8, which is characterized in that the metal phase two
When molybdenum sulfide nanostructure is nanometer sheet, average-size is 75 nanometers；The metal phase molybdenum disulfide nano structure is nanometer
When ball, 151 nanometers of average-size.
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| CN113247955A (en) * | 2021-05-14 | 2021-08-13 | 同济大学 | Composite material and preparation method and application thereof |
| CN114314667A (en) * | 2022-01-18 | 2022-04-12 | 中国石油大学(北京) | Molybdenum disulfide quantum dot, modified molybdenum disulfide quantum dot, and preparation methods and applications of molybdenum disulfide quantum dot and modified molybdenum disulfide quantum dot |
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| CN110258104A (en) * | 2019-07-22 | 2019-09-20 | 信阳学院 | A method of synthesis 1T phase molybdenum disulfide/carbon cloth nanocomposite |
| CN111847514A (en) * | 2020-07-27 | 2020-10-30 | 吉林大学 | Metal phase molybdenum disulfide, self-supporting electrode, preparation method and application |
| CN111847514B (en) * | 2020-07-27 | 2021-12-31 | 吉林大学 | Metal phase molybdenum disulfide, self-supporting electrode, preparation method and application |
| CN112290003A (en) * | 2020-11-04 | 2021-01-29 | 齐鲁工业大学 | Molybdenum disulfide titanium dioxide cathode material of lithium ion battery and preparation method and application thereof |
| CN112290003B (en) * | 2020-11-04 | 2021-07-23 | 齐鲁工业大学 | Molybdenum disulfide titanium dioxide cathode material of lithium ion battery and preparation method and application thereof |
| CN113247955A (en) * | 2021-05-14 | 2021-08-13 | 同济大学 | Composite material and preparation method and application thereof |
| CN114314667A (en) * | 2022-01-18 | 2022-04-12 | 中国石油大学(北京) | Molybdenum disulfide quantum dot, modified molybdenum disulfide quantum dot, and preparation methods and applications of molybdenum disulfide quantum dot and modified molybdenum disulfide quantum dot |
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