CN105810941A - Preparation method and application of short nano-rod self-assembled vanadium tetrasulfide micro-sphere - Google Patents

Preparation method and application of short nano-rod self-assembled vanadium tetrasulfide micro-sphere Download PDF

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CN105810941A
CN105810941A CN201610284540.6A CN201610284540A CN105810941A CN 105810941 A CN105810941 A CN 105810941A CN 201610284540 A CN201610284540 A CN 201610284540A CN 105810941 A CN105810941 A CN 105810941A
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vanadium
preparation
self assembly
vulcanizes
nanometer stub
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CN105810941B (en
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黄剑锋
***
王海静
李瑞梓
费杰
曹丽云
任杰
任一杰
闻稼宝
程呈
罗晓敏
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Shaanxi University of Science and Technology
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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
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The invention provides a preparation method and application of a short nano-rod self-assembled vanadium tetrasulfide micro-sphere. The preparation method comprises the following steps: respectively placing vanadium source substance and sulfur source substance in mol ratio of 1: 10-1: 15 in two porcelain boats, placing two porcelain boats in a tubular atmosphere furnace, exhausting air so that the tubular atmosphere furnace is in a state of -1 to 0 MPa; warming the atmosphere furnace to 300-1000 DEG C in a warming speed of 5-10 DEG C/min, keeping temperature for 0.5-5, and then performing calcination; cooling a calcined sample under the condition of continuously piping the inert gas, cleanly washing, collecting and drying to obtain the short nano-rod self-assembled vanadium tetrasulfide micro-sphere. The method is simple and easily controlled in process, the prepared vanadium tetrasulfide nanometer powder is uniform in chemical constitutions, high in purity, and provided with a specific short nano-rod self-assembled structure, and has excellent performance while being used as ferromagnetic material and lithium/sodium ion battery electrode material. Furthermore, the raw material is cheap and easy to obtain, the method is low in cost, high in yield, free from after-treatment, friendly to environment, and suitable for large-scale production.

Description

A kind of nanometer stub self assembly four vulcanizes the preparation method and application of three vanadium micron balls
[technical field]
The present invention relates to the preparation method of a kind of transient metal sulfide, being specifically related to a kind of nanometer stub self assembly four, to vulcanize three vanadium micro- The preparation method and application of rice ball.
[background technology]
Vanadic sulfide, as a kind of important layered inorganic material, is the most increasingly paid close attention to by people, and its application has related to And the electrochemical properties etc. of the responding ability of moisture, catalysis characteristics, hydrogen storage property, lubrication property and lithium ion battery electrode material Field [Zhang Y, Wu X.Vanadium sulfide nanoribbons:Electronic and magnetic properties [J] .Physics Letters A,2013,377(43):3154-3157]。
Mainly vanadium disulfide [the Yin X.A novel VS that research at present is more2nanosheet-based biosensor for rapid Fluorescence detection of cytochrome c [J] .New Journal of Chemistry, 2015,39:1892-1898] and four sulfur Change vanadium [Lui G, Jiang G, Duan A, et al.Synthesis and Characterization of Template-Free VS4 Nanostructured Materials with Potential Application in Photocatalysis[J].Industrial&Engineering Chemistry Research, 2015] etc., and report their photocatalysis performance and chemical property.
Mujica C et al. reports four sulfuration three vanadium crystal structures [Mujica C, Llanos J, Wittke O.Structure in nineteen ninety-five refinement of monoclinic V3S4[J].Journal of Alloys&Compounds,1995,226(1):136-138]。
Kitaoka Y et al. was at [Kitaoka Y, Yasuoka H, Oka Y, et al.Observation of the in 1979 Antiferromagnetic Order in Metallic Compounds V3S4and V3Se4[J].Journal of the Physical Society Of Japan, 1979,46 (4): 1381-1382] have studied the ferromagnetic property of four sulfuration three vanadium.
Tazuke Y et al. have studied susceptibility and specific heat [Tazuke Y, Sato T, the Miyako Y. of four sulfuration three vanadium in nineteen eighty-two Susceptibility and Specific Heat Studies on V3S4[J].Journal of the Physical Society of Japan,1982, 51(7):2131-2135]。
But, the report about four sulfuration three vanadium is rarely found in recent years, prepares four sulfuration three vanadium especially with respect to by one-step calcination method Report the most rare.
[summary of the invention]
It is an object of the invention to provide the preparation method and application of a kind of four sulfuration three vanadium nano materials, the method passes through calcine technology Preparation nanometer stub self assembly four vulcanizes three vanadium micron balls.
To achieve these goals, the present invention adopts the following technical scheme that
A kind of nanometer stub self assembly four vulcanizes the preparation method of three vanadium micron balls, by vanadium source that mol ratio is 1:10～1:15 and sulfur source Material is placed in tube-type atmosphere furnace to be calcined at 300 DEG C～1000 DEG C, then will calcining after sample cooling, washes clean, Collect, be dried.
Further, before calcining, checking the air-tightness of tube-type atmosphere furnace and exclude the air in pipe, the air pressure controlled in pipe is -1～0MPa, the air-tightness of described inspection tube-type atmosphere furnace is use up the method for inner air tube side by side and is: is passed through noble gas in pipe, continues And-the QI invigorating that carries out 3～8 times bleeding, no longer QI invigorating after bleeding for the last time.
Further, described calcination process is: be warming up to 300～1000 DEG C with the heating rate of 5～10 DEG C/min, and 1-6 is little in insulation Time.
Further, holding stage, controlling intraductal atmospheric pressure is 0.01～0.05MPa.
Further, after described holding stage terminates, constantly lead to noble gas with 800～1500sccm air-flows at once, to discharge During insulation produce sulfur steam and make cooling procedure carry out under conditions of persistently leading to noble gas.
Further, one or both during described noble gas is nitrogen, argon.
Further, described mode of washing is filtering and washing or centrifuge washing, and collection mode is collected by suction or centrifugal collection；Described Washing is to wash with deionized water and dehydrated alcohol successively.
Further, described dry temperature is 60～80 DEG C, and the time is 6～24h.
Further, described vanadium source is vanadic anhydride；Described sulfur source is CH3CSNH2、CN2H4S, Sublimed Sulfur, ammonium sulfide And one or more in cupferron.
A kind of nanometer stub self assembly four prepared by said method vulcanizes the application of three vanadium micron balls, this nanometer stub self assembly four Vulcanize three vanadium micron balls and be applied to electronics, magnetics, sensor, catalysis and lithium/sodium-ion battery field.
Relative to prior art, the present invention at least has the advantages that
The present invention is prepared for four sulfuration three vanadium micron balls of nanometer stub self assembly by one-step calcination method, and the method technique is the easiest Control, cheaper starting materials is easy to get, low cost, and productivity is high, it is not necessary to the later stage processes, environmentally friendly, can be suitable for large-scale production.With Time, it is homogeneous that nanometer stub self assembly four prepared by the method vulcanizes three vanadium micron ball chemical compositions, and purity is higher, and has higher Degree of crystallinity and special nanometer stub self assembly micron ball structure, it is as table when ferromagnetic material and lithium/sodium ion battery electrode material Reveal the performance of excellence.
[accompanying drawing explanation]
Fig. 1 is X-ray diffraction (XRD) figure that nanometer stub self assembly four prepared by the embodiment of the present invention 1 vulcanizes three vanadium micron balls Spectrum；
Fig. 2 is scanning electron microscope (SEM) photo that nanometer stub self assembly four prepared by the embodiment of the present invention 1 vulcanizes three vanadium micron balls.
[detailed description of the invention]
Below in conjunction with the accompanying drawings and the present invention is described in further detail by embodiment.
A kind of nanometer stub self assembly four vulcanizes the preparation method of three vanadium micron balls, comprises the following steps:
Step one: by mol ratio 1:10～1:15 to be strict controlled in vanadium source and sulfur source, to ensure to have enough sulfur to serve as reducing agent； Then vanadium source and sulfur source are laid in porcelain boat respectively, and porcelain boat is placed in tube-type atmosphere furnace, and respectively put two pipe plugs at pipe two ends. Described vanadium source is vanadic anhydride；Sulfur source is CH3CSNH2、CN2H4One in S, Sublimed Sulfur, ammonium sulfide and cupferron Or it is several.
Step 2: being passed through nitrogen or the argon air-tightness with inspection tube furnace in pipe, carry out 3～8 times bleeding-QI invigorating then, with Drain inner air tube, no longer QI invigorating after bleeding for the last time, and to control intraductal atmospheric pressure be-1～0MPa；Then, with 5～10 DEG C/min Heating rate be warming up to 300～1000 DEG C, control intraductal atmospheric pressure be 0.01～0.05MPa, insulation is 1～6h.After insulation terminates, Constantly lead to nitrogen or argon with 800～1500sccm air-flows at once, with discharge insulation during produce sulfur steam and make cooling procedure Carry out under conditions of persistently leading to noble gas.
Step 3: after the sample cooling after calcining, deionized water filtering and washing or centrifuge washing 2～5 times, dehydrated alcohol sucking filtration is washed Wash or centrifuge washing 2～5 times, then by the sample collected by suction after washing or centrifugal collect after be dried at a temperature of 60～80 DEG C 6～24h, i.e. can get nanometer stub self assembly four and vulcanize three vanadium micron balls.
The nanometer stub self assembly four prepared by said method is vulcanized three vanadium micron balls and is applied to electronics, magnetics, sensor, catalysis And lithium/sodium-ion battery field.
Embodiment 1
Step one: weigh the V that mol ratio is 1:10 of vanadium and sulfur2O5And CH3CSNH2, it is laid in porcelain boat two ends respectively, then Porcelain boat is placed in tube-type atmosphere furnace, and respectively puts two pipe plugs at pipe two ends.
Step 2: be passed through nitrogen or the argon inert gas air-tightness with inspection tube furnace in pipe, then carry out 3 times bleeding-mending Gas, to drain inner air tube.No longer QI invigorating after bleeding for the last time, and to control intraductal atmospheric pressure be-1～0MPa；Then, with 10 DEG C The heating rate of/min is warming up to 600 DEG C, and controlling intraductal atmospheric pressure is 0.01～0.05MPa, is incubated as 2h.After insulation terminates, vertical Carve constantly lead to nitrogen or argon with 800sccm air-flow, with discharge insulation during produce sulfur steam and make cooling procedure persistently lead to Carry out under conditions of noble gas.
Step 3: after the sample cooling after calcining, deionized water wash 3 times, absolute ethanol washing 3 times, after then washing Sample collection after at a temperature of 60 DEG C be dried 12h, i.e. can get nanometer stub self assembly four and vulcanize three vanadium micron balls.
From figure 1 it appears that all of X-ray powder diffraction peak can index be all that nanometer stub self assembly four vulcanizes three vanadium microns Ball, and occur almost without other impurity peaks, therefore embodiment 1 is that the high-purity nano stub self assembly four synthesized vulcanizes three vanadium Micron ball.
Can understand to see the microscopic appearance with nanometer stub self assembly micron ball from Fig. 2.
Embodiment 2
Step one: weigh the V that mol ratio is 1:11 of vanadium and sulfur2O5And CH3CSNH2, it is laid in porcelain boat two ends respectively, then Porcelain boat is placed in tube-type atmosphere furnace, and respectively puts two pipe plugs at pipe two ends.
Step 2: being passed through the noble gas air-tightness with inspection tube furnace in pipe, carry out 4 times bleeding-QI invigorating then, to drain Inner air tube.No longer QI invigorating after bleeding for the last time, and to control intraductal atmospheric pressure be-1～0MPa；Then, with the intensification of 6 DEG C/min Ramp is to 300 DEG C, and controlling intraductal atmospheric pressure is 0.01～0.05MPa, is incubated as 1h.After insulation terminates, at once with 900sccm Air-flow constantly leads to nitrogen or argon, with discharge insulation during produce sulfur steam and make cooling procedure at the bar persistently leading to noble gas Carry out under part.
Step 3: after the sample cooling after calcining, deionized water wash 2 times, absolute ethanol washing 2 times, after then washing Sample collection after at a temperature of 70 DEG C be dried 6h, i.e. can get nanometer stub self assembly four and vulcanize three vanadium micron balls.
Embodiment 3
Step one: weigh the V that mol ratio is 1:12 of vanadium and sulfur2O5And CH3CSNH2, it is laid in porcelain boat two ends respectively, then Porcelain boat is placed in tube-type atmosphere furnace, and respectively puts two pipe plugs at pipe two ends.
Step 2: being passed through the noble gas air-tightness with inspection tube furnace in pipe, carry out 6 times bleeding-QI invigorating then, to drain Inner air tube.No longer QI invigorating after bleeding for the last time, and to control intraductal atmospheric pressure be-1～0MPa；Then, with the intensification of 5 DEG C/min Ramp is to 800 DEG C, and controlling intraductal atmospheric pressure is 0.01～0.05MPa, is incubated as 4h.After insulation terminates, at once with 1200sccm Air-flow constantly leads to nitrogen or argon, with discharge insulation during produce sulfur steam and make cooling procedure at the bar persistently leading to noble gas Carry out under part.
Step 3: after the sample cooling after calcining, deionized water wash 4 times, absolute ethanol washing 4 times, after then washing Sample collection after at a temperature of 75 DEG C be dried 18h, i.e. can get nanometer stub self assembly four and vulcanize three vanadium micron balls.
Embodiment 4
Step one: weigh the V that mol ratio is 1:15 of vanadium and sulfur2O5And CH3CSNH2, it is laid in porcelain boat two ends respectively, then Porcelain boat is placed in tube-type atmosphere furnace, and respectively puts two pipe plugs at pipe two ends.
Step 2: being passed through the noble gas air-tightness with inspection tube furnace in pipe, carry out 8 times bleeding-QI invigorating then, to drain Inner air tube.No longer QI invigorating after bleeding for the last time, and to control intraductal atmospheric pressure be-1～0MPa；Then, with the intensification of 8 DEG C/min Ramp is to 1000 DEG C, and controlling intraductal atmospheric pressure is 0.01～0.05MPa, is incubated as 6h.After insulation terminates, at once with 1500sccm Air-flow constantly leads to nitrogen or argon, with discharge insulation during produce sulfur steam and make cooling procedure at the bar persistently leading to noble gas Carry out under part.
Step 3: after the sample cooling after calcining, deionized water wash 5 times, absolute ethanol washing 5 times, after then washing Sample collection after at a temperature of 80 DEG C be dried 24h, i.e. can get nanometer stub self assembly four and vulcanize three vanadium micron balls.
Relative to prior art, the present invention at least has the advantages that
The present invention is prepared for nanometer stub self assembly four by one-step calcination method and vulcanizes three vanadium micron balls, and the method is simple and easy to control, raw material Cheap and easy to get, low cost, productivity is high, it is not necessary to the later stage processes, environmentally friendly, can be suitable for large-scale production.Meanwhile, the party Nanometer stub self assembly four prepared by method vulcanizes that three vanadium micron ball chemical compositions are homogeneous, and purity is higher, and have higher degree of crystallinity and Special nanometer stub self assembly micron ball structure, shows excellent when it is as ferromagnetic material and lithium/sodium ion battery electrode material Different performance.

Claims (10)

1. a nanometer stub self assembly four vulcanizes the preparation method of three vanadium micron balls, it is characterised in that be 1:10～1:15 by mol ratio Vanadium source and sulfur source material be placed in tube-type atmosphere furnace and calcine at 300 DEG C～1000 DEG C, then will calcining after sample cooling, Washes clean, collect, be dried.
A kind of nanometer stub self assembly four the most according to claim 1 vulcanizes the preparation method of three vanadium micron balls, and its feature exists In, before calcining, check the air-tightness of tube-type atmosphere furnace and exclude the air in pipe, the air pressure controlled in pipe is-1～0MPa, institute State and check that the method that the air-tightness of tube-type atmosphere furnace uses up inner air tube side by side is: in pipe, be passed through noble gas, then carry out 3～8 Secondary-QI invigorating of bleeding, no longer QI invigorating after bleeding for the last time.
A kind of nanometer stub self assembly four the most according to claim 1 vulcanizes the preparation method of three vanadium micron balls, and its feature exists In, described calcination process is: be warming up to 300～1000 DEG C with the heating rate of 5～10 DEG C/min, is incubated 1-6 hour.
A kind of nanometer stub self assembly four the most according to claim 3 vulcanizes the preparation method of three vanadium micron balls, and its feature exists In, holding stage, controlling intraductal atmospheric pressure is 0.01～0.05MPa.
A kind of nanometer stub self assembly four the most according to claim 4 vulcanizes the preparation method of three vanadium micron balls, and its feature exists In, after described holding stage terminates, constantly lead to noble gas with 800～1500sccm air-flows at once, produce during discharging insulation Raw sulfur steam also makes cooling procedure carry out under conditions of persistently leading to noble gas.
A kind of nanometer stub self assembly four the most according to claim 5 vulcanizes the preparation method of three vanadium micron balls, and its feature exists In, described noble gas is one or both in nitrogen, argon.
A kind of nanometer stub self assembly four the most according to claim 1 vulcanizes the preparation method of three vanadium micron balls, and its feature exists In, described mode of washing is filtering and washing or centrifuge washing, and collection mode is collected by suction or centrifugal collection；Described washing is successively Wash with deionized water and dehydrated alcohol.
A kind of nanometer stub self assembly four the most according to claim 1 vulcanizes the preparation method of three vanadium micron balls, and its feature exists In, described dry temperature is 60～80 DEG C, and the time is 6～24h.
9. the preparation method of three vanadium micron balls is vulcanized according to any one nanometer stub self assembly four described in claim 1-8, its Being characterised by, described vanadium source is vanadic anhydride；Described sulfur source is CH3CSNH2、CN2H4S, Sublimed Sulfur, ammonium sulfide and One or more in cupferron.
10. the nanometer stub self assembly four that prepared by method according to claim 1 vulcanizes an application for three vanadium micron balls, its Being characterised by, this nanometer stub self assembly four vulcanizes three vanadium micron balls and is applied to ferromagnetic material and lithium/sodium ion battery electrode material.
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CN109599560A (en) * 2018-12-11 2019-04-09 广东工业大学 Four vanadic sulfide anode material of lithium-ion batteries of one kind and preparation method thereof
CN109603857A (en) * 2018-12-25 2019-04-12 陕西科技大学 A kind of preparation and application of the vanadic sulfide elctro-catalyst of cobalt doped
CN109621982A (en) * 2018-12-25 2019-04-16 陕西科技大学 A kind of preparation and application of the vanadic sulfide elctro-catalyst of Fe2O3 doping
CN109706479A (en) * 2018-12-25 2019-05-03 陕西科技大学 A kind of sheet V3S4Preparation and its electrocatalysis characteristic application
CN109980208A (en) * 2019-04-10 2019-07-05 中南大学 A kind of flexible four vulcanize three vanadium-carbon composite anode material and its preparation method and application
CN113036103A (en) * 2021-03-04 2021-06-25 哈尔滨工程大学 Electrode material of vanadium sulfide composite carbonized common sow thistle for potassium ion battery
CN113413906A (en) * 2021-07-30 2021-09-21 陕西科技大学 Vanadium trisulfide/graphite phase carbon nitride photocatalyst and preparation method thereof

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109599560A (en) * 2018-12-11 2019-04-09 广东工业大学 Four vanadic sulfide anode material of lithium-ion batteries of one kind and preparation method thereof
CN109603857A (en) * 2018-12-25 2019-04-12 陕西科技大学 A kind of preparation and application of the vanadic sulfide elctro-catalyst of cobalt doped
CN109621982A (en) * 2018-12-25 2019-04-16 陕西科技大学 A kind of preparation and application of the vanadic sulfide elctro-catalyst of Fe2O3 doping
CN109706479A (en) * 2018-12-25 2019-05-03 陕西科技大学 A kind of sheet V3S4Preparation and its electrocatalysis characteristic application
CN109706479B (en) * 2018-12-25 2021-06-01 陕西科技大学 Sheet V3S4Preparation of (A) and application of electrocatalytic properties thereof
CN109980208A (en) * 2019-04-10 2019-07-05 中南大学 A kind of flexible four vulcanize three vanadium-carbon composite anode material and its preparation method and application
CN109980208B (en) * 2019-04-10 2022-01-25 中南大学 Flexible vanadium-carbon tetrasulfide composite cathode material and preparation method and application thereof
CN113036103A (en) * 2021-03-04 2021-06-25 哈尔滨工程大学 Electrode material of vanadium sulfide composite carbonized common sow thistle for potassium ion battery
CN113036103B (en) * 2021-03-04 2022-07-15 哈尔滨工程大学 Electrode material of vanadium sulfide composite carbonized common sow thistle for potassium ion battery
CN113413906A (en) * 2021-07-30 2021-09-21 陕西科技大学 Vanadium trisulfide/graphite phase carbon nitride photocatalyst and preparation method thereof

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