CN108585042A - A kind of extra small flower-shaped VS of nanometer sheet self assembly2Powder and preparation method thereof - Google Patents

A kind of extra small flower-shaped VS of nanometer sheet self assembly2Powder and preparation method thereof Download PDF

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CN108585042A
CN108585042A CN201810738037.2A CN201810738037A CN108585042A CN 108585042 A CN108585042 A CN 108585042A CN 201810738037 A CN201810738037 A CN 201810738037A CN 108585042 A CN108585042 A CN 108585042A
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nanometer sheet
extra small
shaped
self assembly
flower
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黄剑锋
***
冯亮亮
曹丽云
任杰
任一杰
范海鑫
王娜
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Shaanxi University of Science and Technology
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G31/00Compounds of vanadium
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-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
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/80Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/04Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/30Particle morphology extending in three dimensions

Abstract

A kind of extra small flower-shaped VS of nanometer sheet self assembly2Powder and preparation method thereof, using solvent-thermal method, using N-methyl pyrrolidones as solvent, it is respectively vanadium source and sulphur source with sodium metavanadate and thioacetamide, by their concentration of Collaborative Control and proportioning, reaction temperature, in the reaction time, realizes one-step method and prepare the extra small flower-shaped VS of nanometer sheet self assembly2Powder.This method reaction process is simple, temperature is low, reaction condition that is easily-controllable and not needing large scale equipment and harshness, can be acted on by the structure regulating of solvent, generate extra small, ultra-thin VS2Nanometer sheet, and nanometer sheet is allowed to be self-assembled into small scale flower-like structure in a particular manner.When by above-mentioned product using being sodium/lithium ion battery negative material and optical electrical catalyst, it can show excellent chemical property and catalytic performance.

Description

A kind of extra small flower-shaped VS of nanometer sheet self assembly2Powder and preparation method thereof
Technical field
The present invention relates to a kind of VS2A kind of powder and preparation method thereof, and in particular to extra small flower-shaped VS of nanometer sheet self assembly2 Powder and preparation method thereof.
Background technology
Transition metal dichalcogenide such as MoS2、WS2And VS2Etc. unique physicochemical properties and crystal structure, make they at For a kind of very promising lithium/sodium ion battery electrode material and photoelectrocatalysimaterial material [Yang E, Ji H, Jung Y.Two-Dimensional Transition Metal Dichalcogenide Monolayers as Promising Sodium Ion Battery Anodes.J Phys Chem C.2015;119:26374-80].Although recent research is Show MoS2And WS2It can show excellent electrochemistry and catalytic performance, but electron-transport poor caused by semiconductive Limit their further development.As a prototypical member in transition metal dichalcogenide family, possess excellent conduction The metallic state VS of property2Excellent electronic transmission performance will be shown in electrochemical reaction and catalytic process.Meanwhile VS2Big layer Spacing is connected with weak interlayer Van der Waals force not only facilitates the more lithium/sodium ions of storage, and contribute to lithium/sodium ion/ Electronics is quickly transmitted in interlayer without causing serious structure to be destroyed.In addition, correlative study also indicates that stratiform VS2With high reason By capacity, big surface-active, low ion diffusional resistance and low open-circuit voltage.These characteristics make VS2Become a kind of non- Often have using promising lithium/sodium ion negative material.However, the VS to have reported for work at present2The scale of nanometer sheet is all larger, by it A kind of scale bigger [methods preparing vanadium disulphide nano powder of Wu Changzheng, Sun Xu, Xie Yi of the construct of assembling:CN, CN102010004A [P] .2011.], this makes the specific surface area of entire powder smaller, is unfavorable for electrochemistry and is catalyzed reaction Occur.Therefore, efficient, simple and inexpensive method is explored, to prepare the small scale VS of extra small nanometer sheet self assembly2It constructs Body, improves electrochemistry using its unique crystal structure and microstructure and catalytic performance is is highly desirable, and very Significant.In addition, before about VS2The report of hydrothermal/solvent thermal synthesis, the solvent used are mainly water and ethyl alcohol, Few reports using N-methyl pyrrolidones as solvent.
Invention content
The purpose of the present invention is to provide a kind of extra small flower-shaped VS of nanometer sheet self assembly2Powder and preparation method thereof.
In order to achieve the above objectives, the preparation method that the present invention uses for:
Step 1:It takes the sodium metavanadate of 0.9~1.1g and the thioacetamide of 3.4~3.8g while being added to 48~52ml N-methyl pyrrolidones in, be uniformly mixing to obtain solution A;
Step 2:Solution A is poured into sealing after reacting in liner, is then placed on liner homogeneously loaded on fixed in outer kettle It reacts in instrument, then under the speed conditions of 5~10r/min, 23~25h is reacted at 175~185 DEG C;
Step 3:Reaction kettle is naturally cooled into room temperature after reaction, is then taken out the product for reacting postcooling, warp Cross washing, alcohol is washed after alternately cleaning and collects product;
Step 4:The product of collection is placed in the cold well of freeze drier and is freezed, then by the product after freezing It is placed in pallet, covers seal closure, be evacuated down to 10~20Pa, product is collected after dry 12~18h to get to extra small nanometer sheet The flower-shaped VS of self assembly2Powder.
The stirring of the step 1) uses magnetic agitation or ultrasound, and carry out at normal temperatures, the rotating speed of magnetic agitation For 400~600r/min.
The packing ratio that the step 2) solution A pours into reaction liner is 48~52%.
Step 3) the washing and alcohol are washed using suction filtration or eccentric cleaning.
The freezing conditions of the step 4) are:It -60~-40 DEG C, freezes 2~5 hours.
Step 4) the product is sealed before being put into pallet and being dried with preservative film, and pricks hole processing to preservative film Ensure to its abundant drying under lower pressure.
The extra small flower-shaped VS of nanometer sheet self assembly made of preparation method by the present invention2Powder, the powder are by uniform The ball-type flower-like structure of a diameter of 500~800nm forms, which is by extra small VS2Nanometer sheet self assembly forms, and receives The thickness of rice piece is that 8~10nm, a diameter of 100~200nm, interlayer space 0.66nm, and nanometer sheet have shown monocrystalline spy Property.
The extra small flower-shaped VS of nanometer sheet self assembly made of preparation method by the present invention2Powder application is in lithium/sodium ion electricity Pond field, optical electrical catalytic field.
The present invention uses solvent-thermal method, using N-methyl pyrrolidones as solvent, with sodium metavanadate and thioacetamide point Not Wei vanadium source and sulphur source, by their concentration of Collaborative Control and proportioning, reaction temperature, the reaction time, realize one-step method system The standby extra small flower-shaped VS of nanometer sheet self assembly2Powder.This method reaction process is simple, temperature is low, easily-controllable and do not need large scale equipment It with harsh reaction condition, can be acted on by the structure regulating of solvent, generate extra small, ultra-thin VS2Nanometer sheet, and allow nanometer Piece is self-assembled into small scale flower-like structure in a particular manner.It is sodium/lithium ion battery negative material when applying above-mentioned product When with optical electrical catalyst, it can show excellent chemical property and catalytic performance.
Specifically have the beneficial effect that:
(1) present invention using a step solvent thermal reaction due to directly synthesizing final product, thus has low synthesis Temperature, simple synthesis path do not need large scale equipment and harsh reaction condition;
(2) vanadium source used in the present invention is sodium metavanadate, sulphur source is thioacetamide, both raw materials are common materials, It is cheap and easy to get, at low cost, yield is high, reaction is easily-controllable, be not necessarily to post-processing, it is environmentally friendly, can be suitble to mass produce;
(3) the product chemistry composition of the invention prepared is uniform, purity is high, pattern is uniform, negative as lithium/sodium-ion battery Excellent performance can be shown when pole material and optical electrical catalyst;
(4) it is reaction dissolvent that the present invention, which selects N-methyl pyrrolidones, passes through the volume of stringent Collaborative Control solvent, vanadium The parameters such as source, the concentration of sulphur source and proportioning, reaction temperature, reaction time, reaction-filling ratio, realize reaction in vanadium sulphur there are shapes The control of state makes full use of the self-template and inducing action of N-methyl pyrrolidones, finally realizes extra small nanometer sheet self assembly Flower-shaped VS2The controlledly synthesis of powder;
(5) present invention in solvent N-methyl pyrrolidones for the extra small flower-shaped VS of nanometer sheet self assembly2Powder plays key Effect can not be synthesized with the structure when N-methyl pyrrolidones is changed the ethyl alcohol, ethylene glycol and acetone of making equivalent VS2Powder.
(6) VS prepared by the present invention2Powder product have unique micro- and crystal structure, i.e., thickness be 8~10nm, A diameter of 500~800nm of single crystal nanoplate (interlamellar spacing can reach 0.66nm) self assembly of a diameter of 100~200nm is spent Shape structure, the structure can greatly promote VS2Electrification when as lithium/anode material of lithium-ion battery and optical electrical catalyst Learn performance and catalytic performance.
Description of the drawings
Fig. 1 is the X-ray diffractogram that the embodiment of the present invention 1 prepares product.
Fig. 2 is the low power scanning electron microscope (SEM) photograph that the embodiment of the present invention 1 prepares product.
Fig. 3 is the high power scanning electron microscope (SEM) photograph that the embodiment of the present invention 1 prepares product.
Fig. 4 is the transmission electron microscope picture that the embodiment of the present invention 1 prepares product.
Fig. 5 is the high-resolution-ration transmission electric-lens figure that the embodiment of the present invention 1 prepares nanometer sheet thickness direction.
Fig. 6 is that the embodiment of the present invention 1 prepares the diametric high-resolution-ration transmission electric-lens figure of nanometer sheet.
Fig. 7 is the selective electron diffraction figure that the embodiment of the present invention 1 prepares nanometer sheet.
Fig. 8 is that products therefrom is swept after the ethyl alcohol that the N-methyl pyrrolidones in the embodiment of the present invention 1 is replaced with to equivalent Retouch electron microscope.
Fig. 9 is products therefrom after the ethylene glycol that the N-methyl pyrrolidones in the embodiment of the present invention 1 is replaced with to equivalent Scanning electron microscope (SEM) photograph.
Figure 10 is that products therefrom is swept after the acetone that the N-methyl pyrrolidones in the embodiment of the present invention 1 is replaced with to equivalent Retouch electron microscope.
Specific implementation mode
Invention is further described in detail with reference to the accompanying drawings and embodiments.
Embodiment 1:
Step 1:It takes the sodium metavanadate of 1.0g and the thioacetamide of 3.6g while being added to the N-methyl pyrrolidines of 50ml In ketone, solution A is uniformly obtained with the rotating speed magnetic agitation of 500r/min at normal temperatures;
Step 2:Sealing after pouring into solution A in reaction liner by 50% packing ratio, then by liner loaded in outer kettle Fixation is placed in homogeneous reaction instrument, then under the speed conditions of 10r/min, is reacted for 24 hours at 180 DEG C;
Step 3:Reaction kettle is naturally cooled into room temperature after reaction, then the product for reacting postcooling is taken out, is adopted Product is collected after alternately being cleaned 3 times in a manner of filtering with water and alcohol;
Step 4:The product of collection is placed in the cold well of freeze drier at -50 DEG C, is freezed 4 hours, it then will freezing Product afterwards is placed in pallet, is sealed with preservative film, and it is abundant under lower pressure to it to prick hole processing guarantee to preservative film It is dry, then seal closure is covered, it is evacuated down to 15Pa, product is collected after dry 15h to get flower-shaped to extra small nanometer sheet self assembly VS2Powder.
It can be clearly seen that all diffraction maximums can be well matched with VS from Fig. 12Standard card PDF#89- 1640, illustrate that the product of synthesis is VS2.It is worth noting that, (001) diffraction maximum is very weak, VS is implied2Nanometer sheet has There is smaller thickness.
From figure 2 it can be seen that products therefrom is made of the ball-type flower-like structure of uniform a diameter of 500~800nm, And the flower-like structure is by extra small VS2Nanometer sheet self assembly forms.
From figure 3, it can be seen that the thickness of nanometer sheet is 8~10nm, a diameter of 100~200nm.
Figure 4, it is seen that the flower-like structure is solid construction.Meanwhile it may further determine that the straight of flower-like structure Diameter is 500~800nm.
From figure 5 it can be seen that the thickness direction of nanometer sheet is formed by (001) crystal face is regularly arranged, interplanar distance 0.66nm can be reached, as the channel of lithium/sodium ion storage and diffusion, be conducive to the storage and diffusion of lithium/sodium ion.
From fig. 6 it can be seen that the diametric(al) of nanometer sheet is mainly formed by (011) crystal face is regularly arranged, meaning should Nanometer sheet has shown single crystal characteristics.
It can be clearly seen that part point diffraction from Fig. 7, the VS be more fully explained2Nanometer sheet is single crystal nanoplate.
It will be clear that products therefrom is the VS of nanometer sheet self assembly from Fig. 82Micron bar structure, nanometer sheet and Micron bar all shows larger scale.
It will be clear that products therefrom is smaller VS from Fig. 92Nanometer sheet and larger S simple substance mixtures, and It cannot obtain the VS of pure phase2Nanometer sheet.
It will be clear that products therefrom remains as the band-like NaVO of micron from Figure 103, there is no anti-for vanadium source and sulphur source It answers, more without VS2Synthesis.
Embodiment 2:
Step 1:It takes the sodium metavanadate of 0.9g and the thioacetamide of 3.4g while being added to the N-methyl pyrrolidines of 48ml In ketone, solution A is uniformly obtained with the rotating speed magnetic agitation of 400r/min at normal temperatures;
Step 2:Sealing after pouring into solution A in reaction liner by 49% packing ratio, then by liner loaded in outer kettle Fixation is placed in homogeneous reaction instrument, then under the speed conditions of 8r/min, reacts 25h at 175 DEG C;
Step 3:Reaction kettle is naturally cooled into room temperature after reaction, then the product for reacting postcooling is taken out, is adopted Product is collected after alternately being cleaned 4 times in a manner of filtering with water and alcohol;
Step 4:The product of collection is placed in the cold well of freeze drier at -40 DEG C, is freezed 5 hours, it then will freezing Product afterwards is placed in pallet, is sealed with preservative film, and it is abundant under lower pressure to it to prick hole processing guarantee to preservative film It is dry, then seal closure is covered, it is evacuated down to 12Pa, product is collected after dry 18h to get flower-shaped to extra small nanometer sheet self assembly VS2Powder.
Embodiment 3:
Step 1:It takes the sodium metavanadate of 1.1g and the thioacetamide of 3.8g while being added to the N-methyl pyrrolidines of 52ml In ketone, solution A is uniformly obtained with the rotating speed magnetic agitation of 600r/min at normal temperatures;
Step 2:Sealing after pouring into solution A in reaction liner by 52% packing ratio, then by liner loaded in outer kettle Fixation is placed in homogeneous reaction instrument, then under the speed conditions of 5r/min, reacts 23h at 185 DEG C;
Step 3:Reaction kettle is naturally cooled into room temperature after reaction, then the product for reacting postcooling is taken out, is adopted Product is collected after alternately being cleaned 5 times in a manner of filtering with water and alcohol;
Step 4:The product of collection is placed in the cold well of freeze drier at -60 DEG C, is freezed 2 hours, it then will freezing Product afterwards is placed in pallet, is sealed with preservative film, and it is abundant under lower pressure to it to prick hole processing guarantee to preservative film It is dry, then seal closure is covered, it is evacuated down to 20Pa, product is collected after dry 12h to get flower-shaped to extra small nanometer sheet self assembly VS2Powder.
Embodiment 4:
Step 1:It takes the sodium metavanadate of 0.95g and the thioacetamide of 3.7g while being added to the N-methyl pyrroles of 49ml In alkanone, solution A is uniformly obtained using ultrasonic disperse at normal temperatures;
Step 2:Sealing after pouring into solution A in reaction liner by 48% packing ratio, then by liner loaded in outer kettle Fixation is placed in homogeneous reaction instrument, then under the speed conditions of 9r/min, reacts 25h at 183 DEG C;
Step 3:Reaction kettle is naturally cooled into room temperature after reaction, then the product for reacting postcooling is taken out, is adopted Product is collected after alternately being cleaned 5 times in eccentric fashion with water and alcohol;
Step 4:The product of collection is placed in the cold well of freeze drier at -45 DEG C, is freezed 3 hours, it then will freezing Product afterwards is placed in pallet, is sealed with preservative film, and it is abundant under lower pressure to it to prick hole processing guarantee to preservative film It is dry, then seal closure is covered, it is evacuated down to 18Pa, product is collected after dry 14h to get flower-shaped to extra small nanometer sheet self assembly VS2Powder.
Embodiment 5:
Step 1:It takes the sodium metavanadate of 1.05g and the thioacetamide of 3.5g while being added to the N-methyl pyrroles of 51ml In alkanone, solution A is uniformly obtained using ultrasonic disperse at normal temperatures;
Step 2:Sealing after pouring into solution A in reaction liner by 51% packing ratio, then by liner loaded in outer kettle Fixation is placed in homogeneous reaction instrument, then under the speed conditions of 7r/min, reacts 23h at 178 DEG C;
Step 3:Reaction kettle is naturally cooled into room temperature after reaction, then the product for reacting postcooling is taken out, is adopted Product is collected after alternately being cleaned 4 times in eccentric fashion with water and alcohol;
Step 4:The product of collection is placed in the cold well of freeze drier at -55 DEG C, is freezed 4 hours, it then will freezing Product afterwards is placed in pallet, is sealed with preservative film, and it is abundant under lower pressure to it to prick hole processing guarantee to preservative film It is dry, then seal closure is covered, it is evacuated down to 16Pa, product is collected after dry 15h to get flower-shaped to extra small nanometer sheet self assembly VS2Powder.

Claims (8)

1. a kind of extra small flower-shaped VS of nanometer sheet self assembly2Raw powder's production technology, it is characterised in that:
Step 1:Take the sodium metavanadate of 0.9~1.1g and the thioacetamide of 3.4~3.8g while the nitrogen for being added to 48~52ml In methyl pyrrolidone, it is uniformly mixing to obtain solution A;
Step 2:Liner is then placed on homogeneous reaction by sealing after solution A is poured into reaction liner loaded on fixation in outer kettle In instrument, then under the speed conditions of 5~10r/min, 23~25h is reacted at 175~185 DEG C;
Step 3:Reaction kettle is naturally cooled into room temperature after reaction, is then taken out the product for reacting postcooling, by water It washes, alcohol is washed after alternately cleaning and collects product;
Step 4:The product of collection is placed in the cold well of freeze drier and is freezed, is then placed in the product after freezing In pallet, seal closure is covered, is evacuated down to 10~20Pa, product is collected after dry 12~18h to get to extra small nanometer sheet from group Fill flower-shaped VS2Powder.
2. the extra small flower-shaped VS of nanometer sheet self assembly according to claim 12Raw powder's production technology, it is characterised in that:It is described The stirring of step 1) uses magnetic agitation or ultrasound, and carry out at normal temperatures, the rotating speed of magnetic agitation is 400~600r/ min。
3. the extra small flower-shaped VS of nanometer sheet self assembly according to claim 12Raw powder's production technology, it is characterised in that:It is described The packing ratio that step 2) solution A pours into reaction liner is 48~52%.
4. the extra small flower-shaped VS of nanometer sheet self assembly according to claim 12Raw powder's production technology, it is characterised in that:It is described Step 3) is washed and alcohol is washed using suction filtration or eccentric cleaning.
5. the extra small flower-shaped VS of nanometer sheet self assembly according to claim 12Raw powder's production technology, it is characterised in that:It is described The freezing conditions of step 4) are:It -60~-40 DEG C, freezes 2~5 hours.
6. the extra small flower-shaped VS of nanometer sheet self assembly according to claim 12Raw powder's production technology, it is characterised in that:It is described Step 4) product is sealed before being put into pallet and being dried with preservative film, and is pricked hole processing to preservative film and ensured to it low Abundant drying under the conditions of pressure.
7. the extra small flower-shaped VS of nanometer sheet self assembly made of a kind of preparation method as described in claim 12Powder, feature exist In:The powder is made of the ball-type flower-like structure of uniform a diameter of 500~800nm, which is by extra small VS2 Nanometer sheet self assembly forms, and the thickness of nanometer sheet is 8~10nm, a diameter of 100~200nm, interlayer space 0.66nm, and is received Rice piece has shown single crystal characteristics.
8. the extra small flower-shaped VS of nanometer sheet self assembly made of a kind of preparation method as described in claim 12Powder, feature exist In:The extra small flower-shaped VS of nanometer sheet self assembly2Powder application is in lithium/sodium-ion battery field, optical electrical catalytic field.
CN201810738037.2A 2018-07-02 2018-07-02 A kind of extra small flower-shaped VS of nanometer sheet self assembly2Powder and preparation method thereof Pending CN108585042A (en)

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CN111960468A (en) * 2020-08-21 2020-11-20 中国科学院宁波材料技术与工程研究所 Two-dimensional transition metal chalcogenide wave-absorbing material, preparation method and application thereof
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109110812A (en) * 2018-10-29 2019-01-01 陕西科技大学 A kind of 3D multilevel structure VS2Electrocatalytic Activity for Hydrogen Evolution Reaction agent and preparation method thereof
CN109704405A (en) * 2019-02-28 2019-05-03 陕西师范大学 A kind of preparation method of hollow flower ball-shaped vanadium disulfide
CN109704405B (en) * 2019-02-28 2021-04-27 陕西师范大学 Preparation method of hollow flower-ball-shaped vanadium disulfide
CN110699702A (en) * 2019-11-05 2020-01-17 陕西科技大学 Hillock-shaped in-situ nickel-vanadium double metal hydroxide catalyst and preparation method and application thereof
CN111960468A (en) * 2020-08-21 2020-11-20 中国科学院宁波材料技术与工程研究所 Two-dimensional transition metal chalcogenide wave-absorbing material, preparation method and application thereof
CN113697856A (en) * 2021-08-30 2021-11-26 齐齐哈尔大学 NbS2Solvothermal preparation method of nanosheet self-assembled hollow microsphere
CN113991104A (en) * 2021-12-30 2022-01-28 成都大学 Vanadium-based material and preparation method and application thereof
CN113991104B (en) * 2021-12-30 2022-03-25 成都大学 Vanadium-based material and preparation method and application thereof
CN114725375A (en) * 2022-04-18 2022-07-08 齐鲁工业大学 One-step solvothermal method for preparing VS2Method for preparing negative electrode material of sodium ion battery

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Application publication date: 20180928