CN108793251A - A kind of rodlike VS of thin slice self assembly micron2Nano-powder and preparation method thereof - Google Patents

A kind of rodlike VS of thin slice self assembly micron2Nano-powder and preparation method thereof Download PDF

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Publication number
CN108793251A
CN108793251A CN201810710062.XA CN201810710062A CN108793251A CN 108793251 A CN108793251 A CN 108793251A CN 201810710062 A CN201810710062 A CN 201810710062A CN 108793251 A CN108793251 A CN 108793251A
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rodlike
powder
self assembly
nano
thin slice
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黄剑锋
***
冯亮亮
曹丽云
何枢薇
王娜
范海鑫
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
    • B01J27/04—Sulfides
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    • B82—NANOTECHNOLOGY
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    • B82Y40/00—Manufacture or treatment of nanostructures
    • H—ELECTRICITY
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    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • 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
    • H01M4/581—Chalcogenides or intercalation compounds thereof
    • H01M4/5815—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
    • C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
    • C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
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    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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    • Y02E60/10—Energy storage using batteries

Abstract

A kind of rodlike VS of thin slice self assembly micron2Nano-powder and preparation method thereof prepares the rodlike VS of thin slice self assembly micron using simple step solvent-thermal method2Nano-powder, using water as solvent, it is respectively vanadium source and sulphur source with sodium metavanadate and thioacetamide, pass through the parameters such as their concentration of Collaborative Control and proportioning, reaction temperature, reaction time, reaction-filling ratio, solvent hot mode and drying mode, two parameters of quality for especially strictly controlling sodium metavanadate and thioacetamide, realize a step solvent-thermal method and prepare the rodlike VS of thin slice self assembly micron2Nano-powder.This method reaction process is simple, temperature is low, reaction condition that is easily-controllable and not needing large scale equipment and harshness, can realize ultra-thin VS2Nanometer sheet controllable self assembly.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 rodlike VS of thin slice self assembly micron2Nano-powder and preparation method thereof
Technical field
The present invention relates to a kind of VS2Nano-powder and preparation method thereof, and in particular to a kind of thin slice self assembly micron is rodlike VS2Nano-powder and preparation method thereof.
Background technology
Transition metal dichalcogenide such as MoS2、WS2And VS2Deng the larger interlayer space of layer structure, so that them is become A kind of very promising lithium/anode material of lithium-ion battery.Although recent research have shown that MoS2And WS2It can show Go out excellent storage lithium/sodium performance, but electron-transport poor caused by semiconductive limits their further development.Make For a prototypical member in transition metal dichalcogenide family, possess the metallic state VS of superior electrical conductivity2In cyclic process Excellent electronic transmission performance will be shown.Meanwhile VS2Space length between layers isCan be lithium/sodium from The embedded of son provides sufficient space, and Van der Waals force connection weak between layers contributes to lithium/sodium ion/electronics in layer Between quickly transmit without causing serious structure to be destroyed.In addition, correlative study also indicates that stratiform VS2With high theoretical capacity, Big surface-active, low ion diffusional resistance and low open-circuit voltage.These characteristics make VS2Become one kind having application very much Promising lithium/sodium ion negative material.However, low-dimensional V S2Big volume expansion/contraction to occur in cyclic process, into And cause dusting, finally substantially reduce its chemical property.Currently, alleviating volume expansion then improves VS2Chemical property Main method is and the Material claddings such as graphene, carbon nanotube and organic polymer.However, these materials are to VS2Volume expansion Inhibition only occur on the direction of contact point, result in and inapparent chemical property improve.VS at present2Preparation side Method is mainly hydro-thermal method and calcination method, and vanadium source is mainly sodium orthovanadate and ammonium metavanadate etc., and pattern is mainly that (Wu is long for nano flower-like Sign, a kind of method preparing vanadium disulphide nano powder of Sun Xu, Xie Yi:CN, CN102010004A [P] .2011.), and mostly Occur in the form of composite material (Zhong Mianzeng, Tang Xinping, Japanese plum are deep, wait a kind of vanadium disulfide/graphene composite materials of and its Preparation method:,CN105355865A[P].2016.).In addition, these are prepared separately or are bought by compound material needs, can make Entire building-up process becomes complicated, inefficient and high cost.In recent years, three-dimensional self-assembling electrode material is due to its unique physics limit Domain effect can greatly inhibit its dusting, so as to show excellent chemical property, and be concerned.Therefore, it visits Suo Gaoxiao, simple and inexpensive method, to prepare three-dimensional self assembly VS2Nano-powder is limited using the physics between construct Domain acts on significantly improving VS2Chemical property be to be highly desirable, and significantly.
Invention content
The purpose of the present invention is to provide a kind of rodlike VS of thin slice self assembly micron2Nano-powder and preparation method thereof.
In order to achieve the above objectives, the technical solution adopted by the present invention is：
Step 1：It takes 0.9~1.1g sodium metavanadates and 1.4~1.6g thioacetamides while to be added to 56~60ml anhydrous In ethyl alcohol, magnetic agitation uniformly obtains half clear 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, collect product after dry 12~18h, you can obtain thin slice from group Fill the rodlike VS of micron2Nano-powder.
The rotating speed of the step 1) magnetic agitation is 400~600r/min, and is carried out at normal temperatures.
The packing ratio that the step 2) solution A pours into reaction liner is 56~60%.
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 rodlike VS of thin slice self assembly micron made of preparation method by the present invention2Nano-powder, the powder are by uniform Diameter be about 5~10 μm the rodlike structure composition of micron, micron bar be about 20nm by thickness wide nanometer sheet with radial Intercalation mode self assembly forms, VS2Nanometer sheet has shown single crystal characteristics and the interlamellar spacing of 0.68nm, has preferable structure steady Qualitative and charge-transporting can store more lithium/sodium ions.
The rodlike VS of thin slice self assembly micron made of preparation method by the present invention2Application of nanopowder is in lithium/sodium ion Field of batteries and optical electrical catalytic field.
The present invention prepares the rodlike VS of thin slice self assembly micron using simple step solvent-thermal method2Nano-powder is made with water It is respectively vanadium source and sulphur source with sodium metavanadate and thioacetamide for solvent, by their concentration of Collaborative Control and proportioning, anti- The parameters such as temperature, reaction time, reaction-filling ratio, solvent hot mode and drying mode are answered, sodium metavanadate is especially strictly controlled With two parameters of quality of thioacetamide, realizes a step solvent-thermal method and prepare the rodlike VS of thin slice self assembly micron2Nano powder Body.This method reaction process is simple, temperature is low, reaction condition that is easily-controllable and not needing large scale equipment and harshness, can realize super Thin VS2Nanometer sheet controllable self assembly.It is catalyzed for sodium/lithium ion battery negative material and optical electrical when applying above-mentioned product When agent, 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) present invention passes through Collaborative Control vanadium source, the concentration of sulphur source and proportioning, reaction temperature, reaction time, reaction-filling Than parameters such as, solvent hot mode and drying modes, the rodlike VS of ultra thin single crystalline nanometer sheet self assembly micron is realized2Controllable conjunction At with higher control accuracy.
(5) it is arrived when by the controlling of quality of sodium metavanadate and thioacetamide, when except range described in claim 1, and It cannot obtain the rodlike VS of ultra thin single crystalline nanometer sheet self assembly micron2Nano-powder, therefore this unique quality control and range For VS involved by this patent2Synthesis play a key role.
(6) present invention does not introduce any template or surfactant during synthesis three-dimensional self-assembled structures, Entire self assembling process is the self-template effect control by reaction raw materials, thus entirely react it is simple, easily-controllable, efficient and it is low at This；
(7) product prepared by the present invention has unique self-assembled structures, wherein self assembly construct VS2Between nanometer sheet Unique physics confinement effect, can effectively inhibit charge and discharge process VS2Volume expansion/contraction, so as to promote material Cycle performance.
(8)VS2The well-developed mono-crystalline structures of nanometer sheet have excellent structural stability, for it in charge and discharge and electricity The stability of catalytic process plays important facilitation.
(9)VS2The ultra-thin thickness of nanometer sheet can not only generate larger specific surface area, but also can provide more Surface-active site, and then chemical property and catalytic performance can be promoted.In addition, this extra small thickness can not only shorten electricity Lotus transmission path, but also more active sites can be provided for the storage of charge, so as to promote the specific volume of material Amount and high rate performance.
(10)VS2The big interlamellar spacing structure of nanometer sheet, can not only store more Li+/Na+, additionally it is possible to it is Li+/Na+? The disengaging of interlayer provides more smoothly channel, can finally cooperate with and improve VS2Capacity and high rate 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 of product prepared by the embodiment of the present invention 1.
Fig. 5 is that the embodiment of the present invention 1 prepares VS2High-resolution-ration transmission electric-lens figure in nanometer sheet thickness.
Fig. 6 is that the embodiment of the present invention 1 prepares VS2The selective electron diffraction figure of nanometer sheet.
It is 3.6g (other conditions and embodiment 1 that Fig. 7, which is by the Mass adjust- ment of the thioacetamide in the embodiment of the present invention 1, It is identical) after, the scanning electron microscope (SEM) photograph of products therefrom.
Specific implementation mode
Invention is further described in detail with reference to the accompanying drawings and embodiments.
Embodiment 1：
Step 1：It takes 1.0g sodium metavanadates and 1.5g thioacetamides while being added in 58ml absolute ethyl alcohols, in room temperature Under half clear solution A uniformly obtained with 400r/min magnetic agitations；
Step 2：Sealing after pouring into solution A in reaction liner by 58% packing ratio, then by liner loaded in outer kettle Fixation is placed in homogeneous reaction instrument, then under the speed conditions of 8r/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 -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 15Pa, collects product after dry 16h, you can it is rodlike to obtain thin slice self assembly micron VS2Nano-powder.
It is observed that three apparent diffraction peaks are in 35.86 °, 45.1 ° and 57.26 ° from Fig. 1, correspond respectively to (011), (012) and (110) crystal face, with hexagonal phase VS2Standard card (PDF#89-1640) fit like a glove, illustrate synthesis Product is hexagonal phase VS2.It is worth noting that, (001) peak at 15.38 ° is very faint, illustrate VS2Nanometer sheet has extra small Thickness.
From figure 2 it can be seen that the rodlike structure composition of micron that it is about 5~10 μm by uniform diameter that products therefrom, which is, Micron bar is that self assembly forms in a manner of radial intercalation by wide nanometer sheet.
From figure 3, it can be seen that VS in products therefrom2The thickness of nanometer sheet is about 20nm, and the width of piece is larger.
It can further confirm that products therefrom is the rodlike VS of thin slice self assembly micron from Fig. 42Nano-powder.
It is able to observe that the irregular lattice fringe of bending from Fig. 5, further demonstrates that VS2Crystal grain has extra small thickness Degree and larger interlayer space (0.68nm).
Dot pattern can be clearly observed from Fig. 6, show that nanometer sheet has single crystal characteristics.
It can be seen from figure 7 that the self assembly mode of nanometer sheet is uneven, nanometer sheet has larger thickness and smaller Width, gained VS2Self-assembled structures and the desired protection of the present invention self-assembled structures it is entirely different.Therefore, reaction raw materials Quality for the present invention realization have the function of key.
Embodiment 2：
Step 1：It takes 0.9g sodium metavanadates and 1.4g thioacetamides while being added in 56ml absolute ethyl alcohols, in room temperature Under half clear solution A uniformly obtained with 500r/min magnetic agitations；
Step 2：Sealing after pouring into solution A in reaction liner by 56% 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 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 -50 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 10Pa, collects product after dry 18h, you can it is rodlike to obtain thin slice self assembly micron VS2Nano-powder.
Embodiment 3：
Step 1：It takes 1.05g sodium metavanadates and 1.45g thioacetamides while being added in 57ml absolute ethyl alcohols, normal Half clear solution A is uniformly obtained with 450r/min magnetic agitations under temperature；
Step 2：Sealing after pouring into solution A in reaction liner by 60% 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 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 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 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 20Pa, collects product after dry 12h, you can it is rodlike to obtain thin slice self assembly micron VS2Nano-powder.
Embodiment 4：
Step 1：It takes 0.95g sodium metavanadates and 1.55g thioacetamides while being added in 60ml absolute ethyl alcohols, normal Half clear solution A is uniformly obtained with 550r/min magnetic agitations under temperature；
Step 2：Sealing after pouring into solution A in reaction liner by 57% 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 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 a manner of filtering 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 18Pa, collects product after dry 14h, you can it is rodlike to obtain thin slice self assembly micron VS2Nano-powder.
Embodiment 5：
Step 1：It takes 1.1g sodium metavanadates and 1.6g thioacetamides while being added in 59ml absolute ethyl alcohols, in room temperature Under half clear solution A uniformly obtained with 600r/min magnetic agitations；
Step 2：Sealing after pouring into solution A in reaction liner by 59% packing ratio, then by liner loaded in outer kettle Fixation is placed in homogeneous reaction instrument, then under the speed conditions of 10r/min, reacts 23h at 182 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 -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 13Pa, collects product after dry 18h, you can it is rodlike to obtain thin slice self assembly micron VS2Nano-powder.

Claims (8)

1. a kind of rodlike VS of thin slice self assembly micron2The preparation method of nano-powder, it is characterised in that：
Step 1：It takes 0.9~1.1g sodium metavanadates and 1.4~1.6g thioacetamides while being added to 56~60ml absolute ethyl alcohols In, magnetic agitation uniformly obtains half clear 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, 10~20Pa is evacuated down to, collects product after dry 12~18h, you can it is micro- to obtain thin slice self assembly The rodlike VS of rice2Nano-powder.
2. the rodlike VS of thin slice self assembly micron according to claim 12The preparation method of nano-powder, it is characterised in that：Institute The rotating speed for stating step 1) magnetic agitation is 400~600r/min, and is carried out at normal temperatures.
3. the rodlike VS of thin slice self assembly micron according to claim 12The preparation method of nano-powder, it is characterised in that：Institute It is 56~60% to state step 2) solution A and pour into the packing ratio of reaction liner.
4. the rodlike VS of thin slice self assembly micron according to claim 12The preparation method of nano-powder, it is characterised in that：Institute It states step 3) washing and alcohol is washed using suction filtration or eccentric cleaning.
5. the rodlike VS of thin slice self assembly micron according to claim 12The preparation method of nano-powder, it is characterised in that：Institute The freezing conditions for stating step 4) are：It -60~-40 DEG C, freezes 2~5 hours.
6. the rodlike VS of thin slice self assembly micron according to claim 12The preparation method of nano-powder, it is characterised in that：Institute Step 4) product is stated before being put into pallet and being dried, is sealed with preservative film, and to preservative film prick hole processing ensure to its Abundant drying under lower pressure.
7. the rodlike VS of thin slice self assembly micron made of a kind of preparation method as described in claim 12Nano-powder, feature It is：The powder be about 5~10 μm by uniform diameter the rodlike structure composition of micron, it is about 20nm that micron bar, which is by thickness, Wide nanometer sheet in a manner of radial intercalation self assembly form, VS2Nanometer sheet has shown single crystal characteristics and the interlayer of 0.68nm Away from, have preferable structural stability and charge-transporting, more lithium/sodium ions can be stored.
8. the rodlike VS of thin slice self assembly micron made of a kind of preparation method as described in claim 12Nano-powder, feature It is：The rodlike VS of thin slice self assembly micron2Nano-powder is applied to lithium/sodium-ion battery field and optical electrical catalytic field.
CN201810710062.XA 2018-07-02 2018-07-02 A kind of rodlike VS of thin slice self assembly micron2Nano-powder and preparation method thereof Pending CN108793251A (en)

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CN110227493A (en) * 2019-07-05 2019-09-13 陕西科技大学 The preparation method of one type round pie vanadium disulfide elctro-catalyst
CN113604835A (en) * 2021-07-21 2021-11-05 北京化工大学 Preparation method of electrocatalytic material B-VS2 for ENRR
CN114220961A (en) * 2022-02-21 2022-03-22 浙江大学 Composite nano material for sodium ion battery and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN110227493A (en) * 2019-07-05 2019-09-13 陕西科技大学 The preparation method of one type round pie vanadium disulfide elctro-catalyst
CN113604835A (en) * 2021-07-21 2021-11-05 北京化工大学 Preparation method of electrocatalytic material B-VS2 for ENRR
CN114220961A (en) * 2022-02-21 2022-03-22 浙江大学 Composite nano material for sodium ion battery and preparation method thereof
CN114220961B (en) * 2022-02-21 2022-07-19 浙江大学 Composite nano material for sodium ion battery and preparation method thereof

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