CN108249481A - One step hydro thermal method prepares molybdenum disulfide and hollow micron piece - Google Patents
One step hydro thermal method prepares molybdenum disulfide and hollow micron piece Download PDFInfo
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- CN108249481A CN108249481A CN201810285762.9A CN201810285762A CN108249481A CN 108249481 A CN108249481 A CN 108249481A CN 201810285762 A CN201810285762 A CN 201810285762A CN 108249481 A CN108249481 A CN 108249481A
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- molybdenum disulfide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/06—Sulfides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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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- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
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Abstract
The invention discloses a kind of one step hydro thermal methods to prepare molybdenum disulfide, with molybdenum pentachloride (MoCl5) and sodium diethyldithiocarbamate ((C2H5)2NCSSNa·3H2O it is) raw material, with polyvinylpyrrolidone (PVP) for surfactant, the aqueous solution of configuration is reacted in water reaction kettle, and cleaning can obtain hollow MoS after natural cooling2Micron sheet material.The present invention is by the way that simple traditional hydro-thermal method is made with special appearance, specific surface area is larger, active site is more, the MoS of electrocatalytic hydrogen evolution better performances2Hollow micron sheet material, principle is simple, and reaction step is few, and process is succinct, easy to operate, and device requirement is few, and reaction condition is low, has the advantages that preparation is efficient, pollution-free, at low cost, has very strong practicability and wide applicability.
Description
Technical field
The present invention relates to the synthesis of molybdenum disulfide, and in particular to one step hydro thermal method prepares molybdenum disulfide and hollow micron sheet material
Material.
Background technology
Molybdenum disulfide (MoS2) it is a kind of typical transient metal sulfide, with class graphene layer structure, interlayer
It stacks to be formed by weaker Van der Waals force.2H-MoS2It is MoS2In it is most common be also most stable of one kind, since it is with electrostatic
Repulsive interaction and be easier to shear, therefore it is with excellent lubrication property.As a kind of semiconductor, (indirect band gap width is
1.3eV)MoS2Possessing than more typical layer structure, marginal texture is more complicated, has higher unsaturation, so that its
There is higher application in catalysis and electrochemical field.In addition, MoS2Unique properties, density of electronic states are high, specific surface area is larger,
It can be applied to superconductor and each sensor etc..
In recent years, MoS2It is the research hotspot in multifunctional semiconductor field, suffers from widely acting in all fields,
It is particularly wider in new energy catalytic field application, it is embodied in the application in terms of electrocatalytic decomposition aquatic products hydrogen.Due to it
It is resourceful, environment friendly and pollution-free and be concerned, in recent years experimental studies have found that, MoS2Catalytic hydrogen evolution active site master
If the electrocatalytic hydrogen evolution at both ends (100) and the edge of the sulphur atom on (010) crystal face or molybdenum atom, and in its layer structure
Ability is most strong.
Therefore, the MoS with more edge active sites is prepared2It is one of research emphasis for improving catalytic hydrogen evolution ability.
It, can be by preparing MoS from electric conductivity aspect2With the composite material of other materials to improve its liberation of hydrogen
Energy；From special appearance on, can prepare to provide the MoS of bigger specific surface area by different methods2, have more
Catalytic reaction activity site, so as to increase substantially the ability of its electrocatalytic decomposition aquatic products hydrogen.
Invention content
To solve the deficiencies in the prior art, it is prepared the purpose of the present invention is to provide a kind of by simple traditional hydro-thermal method
Obtain having that special appearance, specific surface area are larger, active site is more, the MoS of electrocatalytic hydrogen evolution better performances2It is hollow micro-
Rice sheet material.
In order to realize above-mentioned target, the present invention adopts the following technical scheme that：
One step hydro thermal method prepares molybdenum disulfide, includes the following steps：
S1, molybdenum pentachloride and sodium diethyldithiocarbamate by certain mol proportion, are dissolved in containing surfactant
In aqueous solution, precursor solution is made；
S2, above-mentioned precursor solution is placed in hydrothermal reaction kettle, after reacting a period of time, product is made in natural cooling.
Above-mentioned surfactant is including PVP, CTAB, CTACI etc..
The molar ratio of above-mentioned molybdenum pentachloride and sodium diethyldithiocarbamate is 1:2-2:1.
Reaction temperature in above-mentioned steps S2 is 200-300 DEG C, reaction time 12-48h.
The preparation of molybdenum disulfide hollow micron piece by product made from above-mentioned step S2, is made after cleaning, drying.
Above-mentioned cleaning includes deionized water and/or absolute ethyl alcohol centrifuge washing.
Above-mentioned drying temperature is 30-80 DEG C, time 12-36h.
The invention has the beneficial effects that：
The one step hydro thermal method of the present invention prepares molybdenum disulfide, with molybdenum pentachloride (MoCl5) and diethyl-dithio amino first
Sour sodium ((C2H5)2NCSSNa·3H2O it is) raw material, with polyvinylpyrrolidone (PVP) for surfactant, the aqueous solution of configuration
It is reacted in water reaction kettle, and cleaning can obtain hollow MoS after natural cooling2Micron sheet material.
The present invention is made by simple traditional hydro-thermal method with special appearance, specific surface area is larger, active site
More, electrocatalytic hydrogen evolution better performances MoS2Hollow micron sheet material, principle is simple, and reaction step is few, and process is succinct, behaviour
Facilitate, device requirement is few, and reaction condition is low, has the advantages that preparation is efficient, pollution-free, at low cost, has very strong practicality
Property and wide applicability.
Description of the drawings
Fig. 1 is the MoS of the embodiment of the present invention 42The XRD spectrum of hollow micron piece.
Fig. 2 is the MoS of the embodiment of the present invention 3 and 42The SEM spectrum of hollow micron piece, wherein a) be the hydro-thermal reaction time
12h, b) be the hydro-thermal reaction time 18h, c) be the hydro-thermal reaction time for 24 hours, d) be the hydro-thermal reaction time 36h.
Specific embodiment
Make specific introduce to the present invention below in conjunction with the drawings and specific embodiments.
Reagent in the present invention is all purchased in market.
Pertinent instruments are respectively：
Electronic balance (model：BSM-220.3, producer：Shanghai Zhuojing Electronic Technology Co., Ltd.)；
Constant temperature blender with magnetic force (model：RCT basic models, producer：German IKA)；
Electric heating constant-temperature blowing drying box (model：DHG-9036A, producer：The upper macro experimental facilities Co., Ltd of Nereid)；
Supercentrifuge (model：LG20-W, producer：System in Beijing Jing founds centrifuge Co., Ltd)；
Electric heating constant-temperature blowing drying box (model：DHG-9036A, producer：The upper macro experimental facilities Co., Ltd of Nereid)；
One step hydro thermal method prepares molybdenum disulfide, includes the following steps：
S1, the MoCl by certain mol proportion5(C2H5)2NCSSNa·3H2O is dissolved in containing a certain amount of surfactant
In 40mL deionized waters, precursor solution is made in magnetic agitation 30min；
S2, above-mentioned precursor solution is transferred in the high temperature and pressure hydro-thermal reaction kettle of 50mL, reacted at a certain temperature
For a period of time, after natural cooling, product is made.
The preparation of molybdenum disulfide hollow micron piece,
S3, by product made from step S2, respectively with deionized water and/or absolute ethyl alcohol centrifuge washing twice, be placed in dry
In dry case, dry a period of time, that is, obtain MoS under certain temperature2Hollow micron sheet material.
Molar ratio of the molar ratio for molybdenum pentachloride and sodium diethyldithiocarbamate in upper table.
Specifically, 4 preferred MoCl of embodiment 3 and embodiment5(C2H5)2NCSSNa·3H2The molar ratio of O is 1:2.
Fig. 1 is MoS prepared by embodiment 42The knot of the XRD spectrum of hollow micron sheet material, as can be seen from the figure sample
Brilliant degree is good, without dephasign.MoS2PDF standard cards be：37-1492.
" c) " figure in Fig. 2 is the MoS prepared by embodiment 32The SEM spectrum of micron sheet material, the hydro-thermal reaction time
For 24 hours, in figure there are apparent micron chip architecture, and MoS2Micron film is made of ultrathin nanometer piece, and size is larger, and diameter is 600
Ran.
" d) " figure is the MoS prepared by embodiment 4 in Fig. 22The SEM spectrum of hollow micron sheet material, the hydro-thermal reaction time
36h, there are apparent hollow micron chip architecture in figure, and MoS2Hollow micron piece is made of ultrathin nanometer piece, and size is larger.
From Figure 2 it can be seen that the reaction condition of " a), b), c), d) " is basically identical, the reaction time be respectively 12h, 18h, for 24 hours,
36h, hollow micron chip architecture is in increasingly visible trend.
The basic principles, main features and advantages of the invention have been shown and described above.The technical staff of the industry should
Understand, the invention is not limited in any way above-described embodiment, all to be obtained by the way of equivalent substitution or equivalent transformation
Technical solution is all fallen in protection scope of the present invention.
Claims (7)
1. one step hydro thermal method prepares molybdenum disulfide, which is characterized in that includes the following steps：
S1, molybdenum pentachloride and sodium diethyldithiocarbamate by certain mol proportion, are dissolved in containing the water-soluble of surfactant
In liquid, precursor solution is made；
S2, above-mentioned precursor solution is placed in hydrothermal reaction kettle, after reacting a period of time, product is made in natural cooling.
2. one step hydro thermal method according to claim 1 prepares molybdenum disulfide, which is characterized in that the surfactant includes
PVP, CTAB, CTACI etc..
3. one step hydro thermal method according to claim 1 prepares molybdenum disulfide, which is characterized in that the molybdenum pentachloride and diethyl
The molar ratio of base nabam is 1:2-2:1.
4. one step hydro thermal method according to claim 1 prepares molybdenum disulfide, which is characterized in that the reaction in the step S2
Temperature is 200-300 DEG C, reaction time 12-48h.
5. the preparation of molybdenum disulfide hollow micron piece, which is characterized in that by any one step hydro thermal method system of claim 14
Product made from the step S2 of standby molybdenum disulfide is made after cleaning, drying.
6. the preparation of molybdenum disulfide hollow micron piece according to claim 5, which is characterized in that it is described cleaning include go from
Sub- water and/or absolute ethyl alcohol centrifuge washing.
7. the preparation of molybdenum disulfide hollow micron piece according to claim 5, which is characterized in that the drying temperature is
30-80 DEG C, time 12-36h.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109112564A (en) * | 2018-09-11 | 2019-01-01 | 青岛科技大学 | A kind of carbon load pyrite FeS2Application of the nanoparticle in electrocatalytic decomposition water hydrogen manufacturing |
| CN111533186A (en) * | 2020-05-12 | 2020-08-14 | 哈尔滨工业大学 | Preparation method and application of spherical expanded molybdenum disulfide |
| CN114457369A (en) * | 2022-01-28 | 2022-05-10 | 南京邮电大学 | CP @ MoS2Preparation method and application of (E) -PtNi catalyst |
| CN114892142A (en) * | 2022-06-10 | 2022-08-12 | 烟台先进材料与绿色制造山东省实验室 | Molybdenum disulfide composite film with wear resistance and preparation method and application thereof |
| CN115448365A (en) * | 2022-09-19 | 2022-12-09 | 西北工业大学 | Preparation method of single-layer 1T' phase TMDS hollow structure electrocatalyst |
-
2018
- 2018-04-03 CN CN201810285762.9A patent/CN108249481A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| AISHI CHEN等: "Self-assembly of hollow MoS2 microflakes by one-pot hydrothermal synthesis for efficient electrocatalytic hydrogen evolution", 《APPLIED SURFACE SCIENCE》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109112564A (en) * | 2018-09-11 | 2019-01-01 | 青岛科技大学 | A kind of carbon load pyrite FeS2Application of the nanoparticle in electrocatalytic decomposition water hydrogen manufacturing |
| 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 |
| CN114457369A (en) * | 2022-01-28 | 2022-05-10 | 南京邮电大学 | CP @ MoS2Preparation method and application of (E) -PtNi catalyst |
| CN114457369B (en) * | 2022-01-28 | 2023-06-20 | 南京邮电大学 | CP@MoS 2 Preparation method and application of PtNi catalyst |
| CN114892142A (en) * | 2022-06-10 | 2022-08-12 | 烟台先进材料与绿色制造山东省实验室 | Molybdenum disulfide composite film with wear resistance and preparation method and application thereof |
| CN114892142B (en) * | 2022-06-10 | 2024-05-28 | 烟台先进材料与绿色制造山东省实验室 | Molybdenum disulfide composite film with wear resistance, and preparation method and application thereof |
| CN115448365A (en) * | 2022-09-19 | 2022-12-09 | 西北工业大学 | Preparation method of single-layer 1T' phase TMDS hollow structure electrocatalyst |
| CN115448365B (en) * | 2022-09-19 | 2024-01-16 | 西北工业大学 | Preparation method of single-layer 1T' phase TMDs hollow structure electrocatalyst |
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| CB03 | Change of inventor or designer information |
Inventor after: Li Xingao Inventor after: Chen Aishi Inventor after: Zhang Jian Inventor after: He Yanna Inventor after: Cui Renjie Inventor before: Li Xingao Inventor before: Zhang Jian Inventor before: Chen Aishi Inventor before: He Yanna Inventor before: Cui Renjie |
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Application publication date: 20180706 |
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| RJ01 | Rejection of invention patent application after publication |