CN106430306B - A kind of preparation method of vanadium disulfide micro-nano structure material - Google Patents
A kind of preparation method of vanadium disulfide micro-nano structure material Download PDFInfo
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- CN106430306B CN106430306B CN201610776884.9A CN201610776884A CN106430306B CN 106430306 B CN106430306 B CN 106430306B CN 201610776884 A CN201610776884 A CN 201610776884A CN 106430306 B CN106430306 B CN 106430306B
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Abstract
A kind of preparation method of vanadium disulfide micro-nano structure material, surfactant is used as by using polyvinylpyrrolidone (PVP), hydro-thermal prepares the vanadium disulfide micro-nano structure of pure phase.It is an advantage of the invention that：VS prepared by this method2Lamella size rule, ulking thickness are homogeneous, are successfully realized the controllable preparation of vanadium disulfide；The preparation method is simple to operate, controllability is strong, raw material is cheap and easy to get, is advantageous to produce in enormous quantities；Vanadium disulfide energy enhancing structure stability prepared by this method, the more avtive spots of exposure, be advantageous to it in electrochemistry, hydrogen reduction, the application for the numerous areas such as hydrogen separates out.
Description
Technical field
The present invention relates to nano material and novel energy resource material technology, more particularly to a kind of vanadium disulfide micro-nano structure material
Preparation method.
Background technology
Environmental pollution and energy shortage problem turn into most one of Tough questions of facing mankind, find regenerative resource and peace
Entirely, reliable energy storage technologies have been changed to very important problem.Lithium ion battery has that voltage is high, capacity is big, without note
The advantages that recalling effect and long lifespan is widely used in the electronic products such as mobile phone, digital camera and notebook, turns into battery
The emphasis of industry development.It is to find suitable electrode material to develop one of key of lithium ion battery, has battery sufficiently high
Lithium-inserting amount and good lithium deintercalation ability, to ensure the big specific capacity of battery, high circulation life-span and good security performance, because
This is, it is necessary to prepare the electrode material with high-efficiency energy-storage characteristic, to meet above-mentioned requirements.
In recent years, transient metal chalcogenide compound (TMDs) is because with unique electrical properties and catalytic property etc., as
A kind of very important material can be widely applied to energy field, be used for example as electrode of lithium cell, catalyst etc..Wherein two sulphur
Change vanadium (VS2) possess the layer structure of class graphene, there is larger interlamellar spacing, weak Van der Waals force between layers makes material easy
It is layered in peeling off, electrode can be significantly improved as electrode material with metal ions such as the lithiums of reversible embedded different proportion
Property.In addition, vanadium disulfide is in metallic state, there is good electric conductivity, charge density wave (Charge nearby can occur at 30 DEG C
Density Wave, CDW) phase transformation, therefore it has in numerous areas such as electrochemistry, hydrogen precipitation, optics, magnetic material, phase-change materials
Standby good application prospect.As what people were understood vanadium disulfide property further gos deep into, its application field and application
It will significantly be widened, produce significant social and economic benefit.
Because vanadium has multivalent state (II, III, IV, V etc.), vanadium disulfide is difficult to by the direct chemical combination of element, more organic
Synthesized in solvent, preparation method complex operation and be difficult control vanadium valence state, it is difficult to obtain VS2Pure phase and controllable preparation, are caused
Structure and performance it is unstable.For example, in electrochemical field, VS2As lithium ion battery electrode material due to material granule
Larger to cause stability of material poor, structure is easy to cave in, and causes capacity attenuation serious；In the research that relevant hydrogen separates out, pattern
Irregular vanadium disulfide particle can not expose more avtive spots, cause catalytic performance not good enough.Therefore, VS is obtained2Pure phase, reality
The controllable preparation of existing vanadium disulfide, turns into the key for studying its performance.
The content of the invention
The purpose of the present invention is to be directed to above-mentioned the deficiencies in the prior art, there is provided a kind of system of vanadium disulfide micro-nano structure material
Preparation Method, this method are used as surfactant by using polyvinylpyrrolidone (PVP), and hydro-thermal prepares the curing of pure phase
Vanadium micro-nano structure, the VS of preparation2Lamella size rule, ulking thickness are homogeneous, are successfully realized the controllable preparation of vanadium disulfide.
Technical scheme：
A kind of preparation method of vanadium disulfide micro-nano structure material, comprises the following steps：
1) polyvinylpyrrolidone (PVP) is added into ultra-pure water to being completely dissolved, obtains polyvinylpyrrolidonesolution solution；
2) vanadium source, sulphur source are added into above-mentioned polyvinylpyrrolidonesolution solution, then stirring is with concentration to dissolving
12mol/L ammoniacal liquor regulation pH value is 8-10；
3) gained mixed solution is placed in hydrothermal device and reacts 10h-20h at 120-200 DEG C；
4) after reaction completely, room temperature is naturally cooled to, products therefrom is scrubbed, centrifuges, vacuum drying, and collection is had
The homogeneous vanadium disulfide micro-nano structure of lamella size rule, ulking thickness.
The weight average molecular weight range of the polyvinylpyrrolidone (PVP) is 6000-150000, polyvinylpyrrolidone with
The amount ratio of ultra-pure water is 0.1-2g：15mL.
The vanadium source is ammonium metavanadate, sodium orthovanadate, vanadic anhydride, vanadium oxytrichloride, vanadium tetrachloride, vanadic sulfate or three
Vanadium chloride；Sulphur source is thioacetamide, thiocarbamide or sulphur simple substance；The amount ratio of polyvinylpyrrolidone, vanadium source and sulphur source is 0.1g-
2g：1mol：2-5mol.
It is an advantage of the invention that：This method is used as surfactant using polyvinylpyrrolidone (PVP), successfully plays control
The effect of products therefrom pattern processed and size, the vanadium disulfide micro-nano structure of pure phase, VS are prepared under hydrothermal conditions2Lamella is big
Small rule, ulking thickness are homogeneous, are successfully realized the controllable preparation of vanadium disulfide.Vanadium disulfide prepared by this method can strengthen knot
Structure stability, the more avtive spots of exposure, be advantageous to it in electrochemistry, hydrogen reduction, the application for the numerous areas such as hydrogen separates out；The system
Preparation Method is simple to operate, controllability is strong, raw material is cheap and easy to get, is advantageous to produce in enormous quantities.
Brief description of the drawings
Fig. 1 is the XRD of vanadium disulfide product prepared by embodiment 1.
Fig. 2 is the SEM figures of vanadium disulfide product prepared by embodiment 1.
Fig. 3 is the SEM figures of vanadium disulfide product prepared by embodiment 2.
Fig. 4 is the vanadium disulfide particle SEM figures that embodiment 3 is not added with PVP preparations.
Embodiment
The invention will be further described by way of example and in conjunction with the accompanying drawings, and these embodiments are only intended to explanation originally
Invention, is not intended to limit the present invention.
Embodiment 1：
A kind of preparation method of vanadium disulfide micro-nano structure material, comprises the following steps：
1) at room temperature, with 15mL ultra-pure waters are measured in 50mL beakers, by 0.5g PVP K30s (PVP-K30)
It is placed in beaker, 30 minutes is stirred to being completely dissolved in 800r/min through magnetic stirrer；
2) 0.2mmol ammonium metavanadates are added into above-mentioned solution and 0.1mmol thioacetamides continue to stir to completely molten
Solution, waits to be completely dissolved and dissolves color to dark-brown, it is 9 that the ammoniacal liquor that concentration is 12mol/L, which is added dropwise, and adjusts to pH value；
3) mixed solution is placed in 25ml polytetrafluoroethylliner liners, and inner bag is placed in high pressure water heating kettle.At 160 DEG C
Room temperature is naturally cooled to after reaction 15h；
4) take out black suspension be placed in 50ml centrifuge tubes, using centrifuge under 9800r/min rotating speed through ultrapure
The lower washing of water and absolute ethyl alcohol 6 times, taking precipitate matter, is dried using vacuum drying oven under conditions of 110 DEG C, 0.1MPa pressure
8h, collect product.
X-ray powder diffraction analysis is carried out to product manufactured in the present embodiment, as shown in figure 1, all peak positions and two sulphur
The diffraction peak match of change vanadium is good and peak shape is sharp, illustrates the pure phase vanadium disulfide that high-crystallinity has been made.Fig. 2 is vanadium disulfide
SEM (SEM) figure of product, therefrom visible vanadium disulfide pattern is homogeneous, for the nanoscale twins knot of height accumulation
Structure, and size uniform is distributed.
Embodiment 2：
A kind of preparation method of vanadium disulfide micro-nano structure material, comprises the following steps：
1) at room temperature, with 15mL ultra-pure waters are measured in 50mL beakers, by 0.5g polyvinylpyrrolidones K60 (PVP-K60)
It is placed in beaker, 30 minutes is stirred to being completely dissolved in 800r/min through magnetic stirrer；
2) 0.2mmol ammonium metavanadates are added into above-mentioned solution and 0.1mmol thioacetamides continue to stir to completely molten
Solution, waits to be completely dissolved and dissolves color to dark-brown, it is 9 that the ammoniacal liquor that concentration is 12mol/L, which is added dropwise, and adjusts to pH value；
3) mixed solution is placed in 25mL polytetrafluoroethylliner liners, and inner bag is placed in high pressure water heating kettle.At 160 DEG C
Room temperature is naturally cooled to after reaction 20h；
4) black suspension is taken out to be placed in 50m centrifuge tubes, using under centrifuge 9800r/min rotating speed through ultra-pure water and
The lower washing of absolute ethyl alcohol 6 times, taking precipitate matter, 8h is dried under conditions of 110 DEG C, 0.1MPa pressure using vacuum drying oven,
Collect product.
Fig. 3 is SEM (SEM) figure of the vanadium disulfide product prepared according to this example, it can be seen that two sulphur
It is homogeneous to change vanadium pattern, the nano-lamellar structure of high dispersive is presented, and size uniform is distributed.The extension in reaction time promotes product
Dispersiveness, vanadium disulfide nanoparticle size is further reduced, individual particle piece number of layers reduce.
Embodiment 3：
This example is not added with polyvinylpyrrolidone, and example has synthesized flower ball-shaped vanadium disulfide particle, step as a comparison
It is as follows：
1) at room temperature, with 15mL ultra-pure waters are measured in 50mL beakers, 0.2mmol ammonium metavanadates is added and 0.1mmol is thio
Acetamide, stir to being completely dissolved, wait to be completely dissolved and dissolve color to dark-brown, the ammonia that concentration is 12mol/L is added dropwise
It is 9 that water, which is adjusted to pH value,；
2) mixed solution is placed in 25mL polytetrafluoroethylliner liners, and inner bag is placed in high pressure water heating kettle.At 160 DEG C
Room temperature is naturally cooled to after reaction 20h；
3) take out black suspension be placed in 50mL centrifuge tubes, using under centrifuge 9800r/min rotating speed through ultra-pure water
And the lower washing of absolute ethyl alcohol 6 times, taking precipitate matter, dried using vacuum drying oven under conditions of 110 DEG C, 0.1MPa pressure
8h, collect product.
Fig. 4 is SEM (SEM) figure of the vanadium disulfide product prepared according to this example, it is seen that is not added with gathering
The reaction product of vinylpyrrolidone is in flower ball-shaped, and between particle diameter is about 30-40 μm, local shape is irregular.
Embodiment described above is only that embodiments of the present invention are described, and is not departing from design concept of the present invention
On the premise of, all variations and modifications that the R＆D personnel in this area is made to technical scheme all should fall
Enter protection scope of the present invention.
Claims (3)
1. a kind of preparation method of vanadium disulfide micro-nano structure material, it is characterised in that comprise the following steps：
1) polyvinylpyrrolidone is added into ultra-pure water to being completely dissolved, obtains polyvinylpyrrolidonesolution solution；
2) vanadium source, sulphur source are added into above-mentioned polyvinylpyrrolidonesolution solution, stirring is then 12mol/L with concentration to dissolving
Ammoniacal liquor regulation pH value be 8-10；
3) gained mixed solution is placed in hydrothermal device and reacts 10h-20h at 120-200 DEG C；
4) after reaction completely, room temperature is naturally cooled to, products therefrom is scrubbed, centrifuges, vacuum drying, and collection is obtained with lamella
The homogeneous vanadium disulfide micro-nano structure of size rule, ulking thickness.
2. the preparation method of vanadium disulfide micro-nano structure material according to claim 1, it is characterised in that：The polyethylene pyrrole
The weight average molecular weight range of pyrrolidone is 6000-150000, and the amount ratio of polyvinylpyrrolidone and ultra-pure water is 0.1-2g：
15mL。
3. the preparation method of vanadium disulfide micro-nano structure material according to claim 1, it is characterised in that：The vanadium source is inclined
Ammonium vanadate, sodium orthovanadate, vanadic anhydride, vanadium oxytrichloride, vanadium tetrachloride, vanadic sulfate or vanadium trichloride；Sulphur source is thio second
Acid amides, thiocarbamide or sulphur simple substance；The amount ratio of polyvinylpyrrolidone, vanadium source and sulphur source is 0.1g-2g：1mol：2-5mol.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107452631A (en) * | 2017-05-08 | 2017-12-08 | 北京大学 | A kind of method that electronic device electrode is prepared using metallic transition metals chalcogen compound |
| CN108862381B (en) * | 2018-06-26 | 2021-01-22 | 中国科学院宁波材料技术与工程研究所 | Vanadium tetrasulfide electrode material and preparation method and application thereof |
| CN109280938B (en) * | 2018-09-30 | 2021-02-05 | 陕西科技大学 | V-doped Ni in flower ball shape3S2NF self-supporting electrode material and preparation method thereof |
| CN112158883A (en) * | 2020-10-16 | 2021-01-01 | 成都先进金属材料产业技术研究院有限公司 | Process for preparing vanadium dioxide nano powder |
| CN113247951A (en) * | 2021-05-13 | 2021-08-13 | 陕西科技大学 | Self-assembly sheet VS2Preparation method of/S nanosheet |
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| CN102010004A (en) * | 2010-12-27 | 2011-04-13 | 中国科学技术大学 | Method for preparing vanadium disulphide nano powder |
| CN105819507A (en) * | 2016-04-29 | 2016-08-03 | 陕西科技大学 | Preparation method and application of nanosheet self-assembled microflower-shaped VS2 |
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| KR101471748B1 (en) * | 2013-03-26 | 2014-12-10 | 국립대학법인 울산과학기술대학교 산학협력단 | Synthesis method of hybrid consisting of vanadium sulfide and reduced graphite oxide and lithium ion battery comprising the hybrid |
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| CN102010004A (en) * | 2010-12-27 | 2011-04-13 | 中国科学技术大学 | Method for preparing vanadium disulphide nano powder |
| CN105819507A (en) * | 2016-04-29 | 2016-08-03 | 陕西科技大学 | Preparation method and application of nanosheet self-assembled microflower-shaped VS2 |
Non-Patent Citations (2)
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| Catalytic Hydrogenation of Alkali Lignin to Bio-oil Using Fullerenelike Vanadium Sulfide;Qingwen Tian et al.;《Energy Fuels》;20141205;第29卷;第255-261页 * |
| PVP-assisted synthesis of MoS2 nanosheets with improved lithium storage properties;Shuquan Liang et al.;《CrystEngComm》;20130403;第15卷;Supporting Information第1-12以及第4998-5002页 * |
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