CN108217730A - A kind of method of hydrothermal synthesis molybdenum disulfide nano sheet under cryogenic conditions - Google Patents
A kind of method of hydrothermal synthesis molybdenum disulfide nano sheet under cryogenic conditions Download PDFInfo
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- CN108217730A CN108217730A CN201810068334.0A CN201810068334A CN108217730A CN 108217730 A CN108217730 A CN 108217730A CN 201810068334 A CN201810068334 A CN 201810068334A CN 108217730 A CN108217730 A CN 108217730A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
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- C01G39/06—Sulfides
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C01P2004/00—Particle morphology
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
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Abstract
A kind of method of hydrothermal synthesis molybdenum disulfide nano sheet under cryogenic conditions belongs to the technical field of molybdenum disulfide layer material.The invention solves existing hydrothermal synthesis molybdenum disulfide nano sheet method, there are the technical problems such as a large amount of impurity, molybdenum disulfide interlamellar spacing be smaller.The method of the present invention：First, ammonium molybdate powder and thiocarbamide powder are dissolved in deionized water, magnetic agitation；It two and then ammonium hydroxide is added dropwise adjusts pH value to 9~10, be then transferred in the reactor of polytetrafluoroethyllining lining, seal；3rd, it is subsequently placed in stainless steel autoclave, 20h~28h is reacted under the conditions of 145 DEG C~185 DEG C, is cooled to room temperature, obtains black powder；4th, it is then dispersed in ammonium hydroxide, centrifuges；5th, the operation of repetition step 4 at least 3 times；Six then ultrasonic disperse in absolute ethyl alcohol, then centrifuge；7th, the operation of repetition step 6 at least 3 times；8th, it is dried in vacuo after pre-freeze.The present invention can be used as the high performance negative material of lithium ion battery.
Description
Technical field
The invention belongs to the technical fields of molybdenum disulfide layer material；More particularly to hydrothermal synthesis two under a kind of cryogenic conditions
The method of molybdenum sulfide nanometer sheet.
Background technology
With the extensive use of two-dimensional film material, more and more two-dimensional materials are found by people and use catalysis
In the fields such as degradation, lithium ion battery.Molybdenum disulfide compared with graphene, and can lead to as a kind of typical two-dimensional material
It crosses insertion functional group and adjusts its band gap width；In addition molybdenum disulfide interlamellar spacing is bigger than graphene, is conducive to insert in lithium ion battery
The progress of layer reaction.
The method of existing molybdenum disulfide hydrothermal synthesis, when preparing under cryogenic, molybdenum disulfide yield is relatively low, adjoint
The generation of a large amount of molybdenum trioxide impurity, the decline of active principle content in final material can be caused；Meanwhile existing high-temperature water
The interlamellar spacing of molybdenum disulfide prepared by hot method is smaller (0.62nm), is unfavorable for the progress of intercalation.
Invention content
The invention solves existing hydrothermal synthesis molybdenum disulfide nano sheet method, there are a large amount of impurity, molybdenum disulfide interlamellar spacings
The technical problems such as smaller, and the method for providing hydrothermal synthesis molybdenum disulfide nano sheet under a kind of cryogenic conditions.The side of the present invention
Method solves molybdenum disulfide under low-temperature hydrothermal synthesis condition, the problem of can not obtaining pure phase.
In order to solve the above technical problems, the present invention cryogenic conditions under hydrothermal synthesis molybdenum disulfide nano sheet method be by
What following step carried out：
Step 1: purity is not less than to the thiocarbamide of 99% (quality) not less than the ammonium molybdate powder and purity of 99% (quality)
Powder is dissolved in deionized water, and magnetic agitation is until form the dark solution of stable homogeneous；
Step 2: ammonium hydroxide, which is then added dropwise, adjusts pH value to 9~10, it is then transferred in the reactor of polytetrafluoroethyllining lining,
Sealing；
Step 3: being subsequently placed in stainless steel autoclave, 20h~28h is reacted under the conditions of 145 DEG C~185 DEG C, is cooled to
Room temperature obtains black powder；
Step 4: the black powder that step 3 is obtained is scattered in ammonium hydroxide, centrifuge；
Step 5: the repeatedly operation of step 4 at least 3 times；
Step 6: being then dispersed in absolute ethyl alcohol, centrifuge；
Step 7: the repeatedly operation of step 6 at least 3 times；
Step 8: then pre-freeze, is dried in vacuo later；Obtain molybdenum disulfide nano sheet.
It further limits, is dissolved in 0.5mmol ammonium molybdate powders and 12~14mmol thiocarbamide powder in step 1
In ionized water.
It further limits, the volume fraction of ammonium hydroxide described in step 2 is 20%~35%.
It further limits, liquor capacity is the 70%-80% of reactor capacity in step 2.
It further limits, the volume fraction of ammonium hydroxide described in step 4 is 20%~35%.
It further limits, is centrifuged in step 4 with the rotating speed of 1000~3000r/min.
It further limits, is centrifuged in step 6 with the rotating speed of 1000~3000r/min.
Further limit, in step 8 at a temperature of -90 DEG C~-80 DEG C pre-freeze 8h~12h.
It further limits, is done in the environment that vacuum degree is 6Pa~10Pa, temperature is -90 DEG C~-76 DEG C in step 8
Dry 20h~30h.
The present invention prepares molybdenum disulfide, and carry out catalysis dissolving using ammonium hydroxide by low-temperature hydro-thermal synthesis, goes to remove water
By-product molybdenum trioxide impurity during thermal synthesis, so as to obtain a kind of purity height, interlamellar spacing greatly two under relatively low synthesis temperature
Molybdenum sulfide nanometer sheet material can be used as the high performance negative material of lithium ion battery.The present invention simultaneously take into account larger interlamellar spacing and
The problem of material purity, the pure molybdenum disulfide nano sheet material finally obtained, lamellar spacing are less than 10nm, and interlamellar spacing is
0.69nm or so.
Description of the drawings
Fig. 1 is the molybdenum disulfide XRD diagram of hydrothermal synthesis under condition of different temperatures；
Fig. 2 is the SEM figures of the hydrothermal synthesis product under the conditions of 185 DEG C；
Fig. 3 is the SEM figures of the hydrothermal synthesis product under the conditions of 165 DEG C；
Fig. 4 is the SEM figures in 145 DEG C of condition hydrothermal synthesis products；
Fig. 5 is SEM figure of the hydrothermal synthesis product after ammonium hydroxide quenches purification processes under the conditions of 165 DEG C；
Fig. 6 is the molybdenum disulfide nano sheet that hydrothermal synthesis product obtains after ammonium hydroxide quenches purification processes under the conditions of 165 DEG C
Transmission electron microscope (TEM) figure.
Specific embodiment
Specific embodiment one：Under the cryogenic conditions of present embodiment the method for hydrothermal synthesis molybdenum disulfide nano sheet be by
What following step carried out：
Step 1: 0.5mmol ammonium molybdate powders (analysis is pure) and 12mmol thiocarbamides powder (analysis is pure) are dissolved in
In 50mL ionized waters, magnetic agitation is until form the dark solution (taking 5min~10min) of stable homogeneous；
Step 2: the ammonium hydroxide that volume fraction is 35%, which is then added dropwise, adjusts pH value to 9~10, it is then transferred to polytetrafluoroethylene (PTFE)
In the reactor of liner, liquor capacity is the 70% of reactor capacity, is sealed；
Step 3: being subsequently placed in stainless steel autoclave, reacted under the conditions of 145 DEG C, 165 DEG C or 185 DEG C for 24 hours, cooling
To room temperature, black powder is obtained；
Step 4: the black powder that step 3 is obtained is scattered in the ammonium hydroxide that 50ml volume fractions are 35%, with
The rotating speed centrifugation of 2000r/min；
Step 5: the repeatedly operation of step 43 times, to remove the soluble ion of dereaction generation and side reaction life
Into MoO3Impurity；
Step 6: being then dispersed in absolute ethyl alcohol, centrifuge；
Step 7: the repeatedly operation of step 63 times；
Step 8: the then pre-freeze 12h at a temperature of -80 DEG C, later in the environment that vacuum degree is 8Pa, temperature is -83 DEG C
Drying is for 24 hours；Obtain molybdenum disulfide nano sheet.
The big spacing molybdenum disulfide nano sheet material of high-purity prepared by present embodiment is under the conditions of different synthesis temperatures
X-ray diffraction (XRD) figure it is as shown in Figure 1.It can be found that with the reduction of synthesis temperature, molybdenum disulfide (002) crystal face spreads out
It penetrates peak to deviate to the left, by X-ray diffraction Bragg equations：(wherein d is interplanar distance to 2dsin (θ)=n λ, and θ is the angle of diffraction, and n is
Diffraction progression, λ are Alpha-ray wavelength=1.54 of CuK) it is found that diffraction angle reduces, the interplanar distance of molybdenum disulfide (002) crystal face
D increases.Meanwhile the intensity of the diffraction maximum of the molybdenum trioxide impurity near 29 ° is compared, it is found that molybdenum trioxide is miscellaneous in material
The content of matter increases with the reduction of temperature.
Fig. 2, Fig. 3 and Fig. 4 are without AMMONIA TREATMENT, hydrothermal synthesis product scanning electron microscope (SEM) figure, wherein petal-shaped
Structure is molybdenum disulfide nano sheet, and club shaped structure is molybdenum trioxide impurity.It can be found that (the figure under 185 DEG C of synthesis condition
2), impurity content is very low in synthetic product；And when synthesis temperature is reduced to 165 DEG C (Fig. 3), impurity content is apparent in synthetic product
Increase；Continue to reduce synthesis temperature to 145 DEG C (Fig. 4), impurity phase size further increases, quantity further increases.This explanation
Content with the reduction impurity phase of hydrothermal synthesis temperature increases.
Fig. 5 is pattern of the hydrothermal synthesis product after ammonia-catalyzed purification processes under the conditions of 165 DEG C, compares and sends out with Fig. 3
Existing, the impurity phase (i.e. club shaped structure) in material is removed, only the petal of remaining molybdenum disulfide nano sheet composition.
The molybdenum disulfide nano sheet that hydrothermal synthesis product obtains after ammonium hydroxide quenches purification processes under the conditions of Fig. 6 is 165 DEG C
Transmission electron microscope (TEM) figure, it can be found that its (002) interplanar distance be 0.69nm, higher than what is provided in standard PDF cards
0.62nm.Molybdenum disulfide thin layer is 7 layers herein, thickness 4.14nm.The tem analysis of multiple regions shows the layer of molybdenum disulfide
Number is less than 10 layers, all layers of thickness and less than 10nm.
Specific embodiment two：Under the cryogenic conditions of present embodiment the method for hydrothermal synthesis molybdenum disulfide nano sheet be by
What following step carried out：
Step 1: 0.5mmol ammonium molybdate powders (analysis is pure) and 14mmol thiocarbamides powder (analysis is pure) are dissolved in
In 35mL ionized waters, magnetic agitation is until form the dark solution (taking 5min~10min) of stable homogeneous；
Step 2: the ammonium hydroxide that volume fraction is 20%, which is then added dropwise, adjusts pH value to 9~10, it is then transferred to polytetrafluoroethylene (PTFE)
In the reactor of liner, liquor capacity is the 80% of reactor capacity, is sealed；
Step 3: being subsequently placed in stainless steel autoclave, 20h is reacted under the conditions of 165 DEG C, is cooled to room temperature, obtained black
Color powder；
Step 4: the black powder that step 3 is obtained is scattered in the ammonium hydroxide that 50ml volume fractions are 20%, with
The rotating speed centrifugation of 3000r/min；
Step 5: the repeatedly operation of step 43 times, to remove the soluble ion of dereaction generation and side reaction life
Into MoO3Impurity；
Step 6: being then dispersed in absolute ethyl alcohol, centrifuge；
Step 7: the repeatedly operation of step 6 at least 3 times；
Step 8: the then pre-freeze 8h at a temperature of -85 DEG C, later in the environment that vacuum degree is 6Pa, temperature is -80 DEG C
Dry 30h；Obtain molybdenum disulfide nano sheet.
Claims (10)
1. a kind of method of hydrothermal synthesis molybdenum disulfide nano sheet under cryogenic conditions, it is characterised in that the method is by following steps
Suddenly it carries out：
Step 1: purity is not less than to the thiocarbamide powder of 99% (quality) not less than the ammonium molybdate powder and purity of 99% (quality)
It is dissolved in deionized water, magnetic agitation is until form the dark solution of stable homogeneous；
Step 2: ammonium hydroxide, which is then added dropwise, adjusts pH value to 9~10, it is then transferred in the reactor of polytetrafluoroethyllining lining, seals；
Step 3: being subsequently placed in stainless steel autoclave, 20h~28h is reacted under the conditions of 145 DEG C~185 DEG C, is cooled to room
Temperature obtains black powder；
Step 4: the black powder that step 3 is obtained is scattered in ammonium hydroxide, centrifuge；
Step 5: the repeatedly operation of step 4 at least 3 times；
Step 6: being then dispersed in absolute ethyl alcohol, centrifuge；
Step 7: the repeatedly operation of step 6 at least 3 times；
Step 8: then pre-freeze, is dried in vacuo, obtains molybdenum disulfide nano sheet later.
2. the method for hydrothermal synthesis molybdenum disulfide nano sheet, feature exist under a kind of cryogenic conditions according to claim 1
0.5mmol ammonium molybdate powders and 12~14mmol thiocarbamide powder are dissolved in deionized water in step 1.
3. the method for hydrothermal synthesis molybdenum disulfide nano sheet, feature exist under a kind of cryogenic conditions according to claim 1
The volume fraction of the ammonium hydroxide described in step 2 is 20%~35%.
4. the method for hydrothermal synthesis molybdenum disulfide nano sheet, feature exist under a kind of cryogenic conditions according to claim 1
Liquor capacity is the 70%-80% of reactor capacity in step 2.
5. the method for hydrothermal synthesis molybdenum disulfide nano sheet, feature exist under a kind of cryogenic conditions according to claim 1
It is reacted for 24 hours under the conditions of 165 DEG C in step 3.
6. the method for hydrothermal synthesis molybdenum disulfide nano sheet, feature exist under a kind of cryogenic conditions according to claim 1
The volume fraction of the ammonium hydroxide described in step 4 is 20%~35%.
7. the method for hydrothermal synthesis molybdenum disulfide nano sheet, feature exist under a kind of cryogenic conditions according to claim 1
It is centrifuged in step 4 with the rotating speed of 1000~3000r/min.
8. the method for hydrothermal synthesis molybdenum disulfide nano sheet, feature exist under a kind of cryogenic conditions according to claim 1
It is centrifuged in step 6 with the rotating speed of 1000~3000r/min.
9. the method for hydrothermal synthesis molybdenum disulfide nano sheet, feature exist under a kind of cryogenic conditions according to claim 1
In step 8 at a temperature of -90 DEG C~-80 DEG C pre-freeze 8h~12h.
10. the method for hydrothermal synthesis molybdenum disulfide nano sheet, feature exist under a kind of cryogenic conditions according to claim 1
In step 8 vacuum degree 6Pa~10Pa, -90 DEG C~-76 DEG C of temperature environment in dry 20h~30h.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108987116A (en) * | 2018-07-04 | 2018-12-11 | 阜阳师范学院 | Molybdenum disulfide-carbon composite preparation method and its application in dye-sensitized solar cells |
| CN111111702A (en) * | 2019-12-04 | 2020-05-08 | 西安交通大学 | Molybdenum disulfide/carbon composite material with super large interlayer spacing and preparation method thereof |
| CN111533186A (en) * | 2020-05-12 | 2020-08-14 | 哈尔滨工业大学 | Preparation method and application of spherical expanded molybdenum disulfide |
| CN111704165A (en) * | 2020-08-04 | 2020-09-25 | 湘潭大学 | Hexagonal MoTe2Nanosheet and preparation method |
| CN112642291A (en) * | 2020-12-30 | 2021-04-13 | 陕西科技大学 | Amino acid bonded molybdenum disulfide reverse osmosis membrane and preparation method and application thereof |
| CN112960696A (en) * | 2020-12-04 | 2021-06-15 | 汕头大学 | Wide-layer-spacing molybdenum disulfide nanosheet and preparation method thereof |
| CN113140803A (en) * | 2021-04-29 | 2021-07-20 | 天能帅福得能源股份有限公司 | Based on lamella MoS2Preparation method of high-rate lithium ion battery as anode |
| CN113144910A (en) * | 2021-03-30 | 2021-07-23 | 哈尔滨工业大学（深圳） | Preparation method of composite ultrafiltration membrane with catalytic self-cleaning function |
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2018
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108987116A (en) * | 2018-07-04 | 2018-12-11 | 阜阳师范学院 | Molybdenum disulfide-carbon composite preparation method and its application in dye-sensitized solar cells |
| CN111111702A (en) * | 2019-12-04 | 2020-05-08 | 西安交通大学 | Molybdenum disulfide/carbon composite material with super large interlayer spacing and preparation method thereof |
| CN111533186A (en) * | 2020-05-12 | 2020-08-14 | 哈尔滨工业大学 | Preparation method and application of spherical expanded molybdenum disulfide |
| CN111533186B (en) * | 2020-05-12 | 2022-10-04 | 哈尔滨工业大学 | Preparation method and application of spherical expanded molybdenum disulfide |
| CN111704165A (en) * | 2020-08-04 | 2020-09-25 | 湘潭大学 | Hexagonal MoTe2Nanosheet and preparation method |
| CN111704165B (en) * | 2020-08-04 | 2022-04-08 | 湘潭大学 | Hexagonal MoTe2Nanosheet and preparation method |
| CN112960696A (en) * | 2020-12-04 | 2021-06-15 | 汕头大学 | Wide-layer-spacing molybdenum disulfide nanosheet and preparation method thereof |
| CN112642291A (en) * | 2020-12-30 | 2021-04-13 | 陕西科技大学 | Amino acid bonded molybdenum disulfide reverse osmosis membrane and preparation method and application thereof |
| CN113144910A (en) * | 2021-03-30 | 2021-07-23 | 哈尔滨工业大学（深圳） | Preparation method of composite ultrafiltration membrane with catalytic self-cleaning function |
| CN113144910B (en) * | 2021-03-30 | 2022-05-03 | 哈尔滨工业大学（深圳） | Preparation method of composite ultrafiltration membrane with catalytic self-cleaning function |
| CN113140803A (en) * | 2021-04-29 | 2021-07-20 | 天能帅福得能源股份有限公司 | Based on lamella MoS2Preparation method of high-rate lithium ion battery as anode |
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