CN105810941B - A kind of nanometer of stub self assembly four vulcanizes the preparation method and application of three vanadium micron balls - Google Patents

A kind of nanometer of stub self assembly four vulcanizes the preparation method and application of three vanadium micron balls Download PDF

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CN105810941B
CN105810941B CN201610284540.6A CN201610284540A CN105810941B CN 105810941 B CN105810941 B CN 105810941B CN 201610284540 A CN201610284540 A CN 201610284540A CN 105810941 B CN105810941 B CN 105810941B
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CN105810941A (en
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黄剑锋
李文斌
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

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Abstract

The present invention provides the preparation method and applications that a kind of nanometer of stub self assembly four vulcanizes three vanadium micron balls, molar ratio is respectively placed in two porcelain boats for the vanadium source of 1:10~1:15 and sulphur source substance, two porcelain boats are placed in tube-type atmosphere furnace, after draining air, it is in tube-type atmosphere furnace under -1~0MPa state.Then 300~1000 DEG C are warming up to the heating rate of 5~10 DEG C/min, 0.5~5h of heat preservation is calcined, after calcined sample is carried out cooling under conditions of persistently leading to inert gas, washes clean, collection, drying can be obtained nanometer stub self assembly four and vulcanize a three vanadium micron balls.This method simple process is easily-controllable, and four three vanadium nano-powder chemical compositions of vulcanization of preparation are uniform, and purity is higher, and has specific nanometer stub self-assembled structures, shows excellent performance when as ferromagnetic material and lithium/sodium ion battery electrode material.In addition, this method raw material is cheap and easy to get, at low cost, yield is high, is not necessarily to post-processing, environmentally friendly, can be suitble to be mass produced.

Description

A kind of nanometer of stub self assembly four vulcanizes the preparation method and application of three vanadium micron balls
[technical field]
The present invention relates to a kind of preparation methods of transient metal sulfide, and in particular to a kind of nanometer of four sulphur of stub self assembly Change the preparation method and application of three vanadium micron balls.
[background technique]
Vanadic sulfide has been to be concerned by more and more people, and it is answered in recent years as a kind of important layered inorganic material With the electricity for having been directed to the responding ability of moisture, catalysis characteristics, hydrogen storage property, lubrication property and lithium ion battery electrode material The fields such as chemical characteristic [Zhang Y, Wu X.Vanadium sulfide nanoribbons:Electronic and magnetic properties[J].Physics Letters A,2013,377(43):3154-3157]。
More mainly vanadium disulfide [Yin X.A novel VS is studied at present2nanosheet-based biosensor for rapid fluorescence detection of cytochrome c[J].New Journal of Chemistry, 2015,39:1892-1898] and four vanadic sulfides [Lui G, Jiang G, Duan A, et al.Synthesis and Characterization of Template-Free VS4Nanostructured Materials with Potential Application in Photocatalysis[J].Industrial&Engineering Chemistry Research, 2015] etc., and their photocatalysis performance and chemical property are reported.
Mujica C et al. reports four vulcanizations, three vanadium crystal structure [Mujica C, Llanos J, Wittke in nineteen ninety-five O.Structure refinement of monoclinic V3S4[J].Journal of Alloys&Compounds,1995, 226(1):136-138]。
Kitaoka Y et al. was in [Kitaoka Y, Yasuoka H, Oka Y, et al.Observation of in 1979 the Antiferromagnetic Order in Metallic Compounds V3S4and V3Se4[J].Journal of The Physical Society of Japan, 1979,46 (4): 1381-1382] have studied the ferromagnetism of four vulcanizations, three vanadium Energy.
Tazuke Y et al. nineteen eighty-two have studied four vulcanizations, three vanadium magnetic susceptibility and specific heat [Tazuke Y, Sato T, Miyako Y.Susceptibility and Specific Heat Studies on V3S4[J].Journal of the Physical Society of Japan,1982,51(7):2131-2135]。
However, the report in recent years about four three vanadium of vulcanization is rarely found, four are prepared especially with respect to by one-step calcination method The report for vulcanizing three vanadium is even more rare.
[summary of the invention]
The purpose of the present invention is to provide the preparation method and application that one kind four vulcanizes three vanadium nano materials, this method passes through Calcine technology prepares nanometer stub self assembly four and vulcanizes three vanadium micron balls.
To achieve the goals above, the present invention adopts the following technical scheme:
A kind of nanometer of stub self assembly four vulcanizes the preparation method of three vanadium micron balls, the vanadium for being 1:10~1:15 by molar ratio Source and sulphur source substance are placed in tube-type atmosphere furnace at 300 DEG C~1000 DEG C and are calcined, then that calcined sample is cooling, Washes clean, collection, drying.
Further, it before calcining, checks the air-tightness of tube-type atmosphere furnace and excludes the air in pipe, control the gas in pipe Pressure is -1~0MPa, the method that the air-tightness for checking tube-type atmosphere furnace uses up inner air tube side by side are as follows: inertia is passed through into pipe Gas then carries out 3~8 pumping-tonifying Qi, no longer tonifying Qi after last time is evacuated.
Further, the calcination process are as follows: be warming up to 300~1000 DEG C with the heating rate of 5~10 DEG C/min, heat preservation 1-6 hours.
Further, holding stage, control intraductal atmospheric pressure are 0.01~0.05MPa.
Further, after the holding stage, inert gas is led to constantly with 800~1500sccm air-flow at once, The sulphur steam generated during heat preservation is discharged and carries out cooling procedure under conditions of persistently leading to inert gas.
Further, the inert gas is one or both of nitrogen, argon gas.
Further, the mode of washing is filtering and washing or centrifuge washing, and collection mode is that collected by suction or centrifugation are received Collection；The washing is successively to be washed with deionized water and dehydrated alcohol.
Further, the temperature of the drying be 60~80 DEG C, the time be 6~for 24 hours.
Further, the vanadium source is vanadic anhydride；The sulphur source is CH3CSNH2、CN2H4S, sublimed sulfur, ammonium sulfide And one or more of copper reagent.
A kind of nanometer stub self assembly four prepared by the above method vulcanizes the application of three vanadium micron balls, this nanometer of stub Self assembly four vulcanizes three vanadium micron balls and is applied to electronics, magnetics, sensor, catalysis and lithium/sodium-ion battery field.
Compared with the existing technology, the present invention at least has the advantages that
The present invention is prepared for four three vanadium micron balls of vulcanization of nanometer stub self assembly, this method technique by one-step calcination method Simple and easy to control, raw material is cheap and easy to get, at low cost, and yield is high, is not necessarily to post-processing, environmentally friendly, can be suitble to extensive life It produces.Meanwhile the three vanadium micron ball chemical compositions of vulcanization of nanometer stub self assembly four of this method preparation are uniform, purity is higher, and has There are higher crystallinity and special nanometer stub self assembly micron spherical structure, is used as ferromagnetic material and lithium/sodium-ion battery Excellent performance is shown when electrode material.
[Detailed description of the invention]
Fig. 1 is the X-ray diffraction that nanometer stub self assembly four prepared by the embodiment of the present invention 1 vulcanizes three vanadium micron balls (XRD) map；
Fig. 2 is the scanning electron microscope (SEM) that nanometer stub self assembly four prepared by the embodiment of the present invention 1 vulcanizes three vanadium micron balls Photo.
[specific embodiment]
Invention is further described in detail with reference to the accompanying drawings and embodiments.
A kind of nanometer of stub self assembly four vulcanizes the preparation method of three vanadium micron balls, comprising the following steps:
Step 1: will be strict controlled in 1:10~1:15 for the molar ratio of vanadium source and sulphur source, to guarantee to have enough sulphur to fill Work as reducing agent；Then vanadium source and sulphur source are laid in porcelain boat respectively, and porcelain boat is placed in tube-type atmosphere furnace, and at pipe both ends Respectively put two pipe plugs.The vanadium source is vanadic anhydride；Sulphur source is CH3CSNH2、CN2H4S, sublimed sulfur, ammonium sulfide and copper examination One or more of agent.
Step 2: nitrogen or argon gas are passed through into pipe to check the air-tightness of tube furnace, then carry out 3~8 pumping-benefits Gas, to drain inner air tube, no longer tonifying Qi after last time is evacuated, and controlling intraductal atmospheric pressure is -1~0MPa；Then, with 5~ The heating rate of 10 DEG C/min is warming up to 300~1000 DEG C, and control intraductal atmospheric pressure is 0.01~0.05MPa, keeps the temperature as 1~6h. After heat preservation, nitrogen or argon gas are led to constantly with 800~1500sccm air-flow at once, steamed so that the sulphur generated during heat preservation is discharged Vapour simultaneously carries out cooling procedure under conditions of persistently leading to inert gas.
Step 3: by calcined sample it is cooling after, deionized water filtering and washing or centrifuge washing 2~5 times, dehydrated alcohol Filtering and washing or centrifuge washing 2~5 times, the then temperature by the sample collected by suction after washing or after being collected by centrifugation at 60~80 DEG C Degree lower dry 6~for 24 hours, nanometer stub self assembly four can be obtained and vulcanize three vanadium micron balls.
Vulcanize three vanadium micron balls by nanometer stub self assembly four prepared by the above method and is applied to electronics, magnetics, sensing Device, catalysis and lithium/sodium-ion battery field.
Embodiment 1
Step 1: the molar ratio for weighing vanadium and sulphur is the V of 1:102O5And CH3CSNH2, it is laid in porcelain boat both ends respectively, so Porcelain boat is placed in tube-type atmosphere furnace afterwards, and respectively puts two pipe plugs at pipe both ends.
Step 2: nitrogen or argon inert gas are passed through into pipe to check the air-tightness of tube furnace, then carry out 3 pumpings Gas-tonifying Qi, to drain inner air tube.No longer tonifying Qi after last time is evacuated, and controlling intraductal atmospheric pressure is -1~0MPa；Then, 600 DEG C are warming up to the heating rate of 10 DEG C/min, control intraductal atmospheric pressure is 0.01~0.05MPa, is kept the temperature as 2h.Heat preservation terminates Afterwards, nitrogen or argon gas are led to constantly with 800sccm air-flow at once, the sulphur steam generated during heat preservation is discharged and makes cooling procedure It is carried out under conditions of persistently leading to inert gas.
Step 3: after the cooling of calcined sample, deionized water is washed 3 times, and dehydrated alcohol washs 3 times, then will be washed In 60 DEG C of at a temperature of dry 12h after sample collection after washing, nanometer stub self assembly four can be obtained and vulcanize a three vanadium micron balls.
From figure 1 it appears that all X-ray powder diffraction peaks can refer to be designated as nanometer vulcanization of stub self assembly four three Vanadium micron ball, and almost without other impurity peaks appearance, therefore embodiment 1 is the high-purity nano stub self assembly four of synthesis Vulcanize three vanadium micron balls.
It can understand to see the microscopic appearance with nanometer stub self assembly micron ball from Fig. 2.
Embodiment 2
Step 1: the molar ratio for weighing vanadium and sulphur is the V of 1:112O5And CH3CSNH2, it is laid in porcelain boat both ends respectively, so Porcelain boat is placed in tube-type atmosphere furnace afterwards, and respectively puts two pipe plugs at pipe both ends.
Step 2: being passed through inert gas into pipe to check the air-tightness of tube furnace, then carry out 4 pumping-tonifying Qi, with Drain inner air tube.No longer tonifying Qi after last time is evacuated, and controlling intraductal atmospheric pressure is -1~0MPa；Then, with 6 DEG C/min's Heating rate is warming up to 300 DEG C, and control intraductal atmospheric pressure is 0.01~0.05MPa, keeps the temperature as 1h.After heat preservation, at once with 900sccm air-flow constantly leads to nitrogen or argon gas, the sulphur steam generated during heat preservation is discharged and is leading to cooling procedure persistently It is carried out under conditions of inert gas.
Step 3: after the cooling of calcined sample, deionized water is washed 2 times, and dehydrated alcohol washs 2 times, then will be washed In 70 DEG C of at a temperature of dry 6h after sample collection after washing, nanometer stub self assembly four can be obtained and vulcanize a three vanadium micron balls.
Embodiment 3
Step 1: the molar ratio for weighing vanadium and sulphur is the V of 1:122O5And CH3CSNH2, it is laid in porcelain boat both ends respectively, so Porcelain boat is placed in tube-type atmosphere furnace afterwards, and respectively puts two pipe plugs at pipe both ends.
Step 2: being passed through inert gas into pipe to check the air-tightness of tube furnace, then carry out 6 pumping-tonifying Qi, with Drain inner air tube.No longer tonifying Qi after last time is evacuated, and controlling intraductal atmospheric pressure is -1~0MPa；Then, with 5 DEG C/min's Heating rate is warming up to 800 DEG C, and control intraductal atmospheric pressure is 0.01~0.05MPa, keeps the temperature as 4h.After heat preservation, at once with 1200sccm air-flow constantly leads to nitrogen or argon gas, the sulphur steam generated during heat preservation is discharged and is leading to cooling procedure persistently It is carried out under conditions of inert gas.
Step 3: after the cooling of calcined sample, deionized water is washed 4 times, and dehydrated alcohol washs 4 times, then will be washed In 75 DEG C of at a temperature of dry 18h after sample collection after washing, nanometer stub self assembly four can be obtained and vulcanize a three vanadium micron balls.
Embodiment 4
Step 1: the molar ratio for weighing vanadium and sulphur is the V of 1:152O5And CH3CSNH2, it is laid in porcelain boat both ends respectively, so Porcelain boat is placed in tube-type atmosphere furnace afterwards, and respectively puts two pipe plugs at pipe both ends.
Step 2: being passed through inert gas into pipe to check the air-tightness of tube furnace, then carry out 8 pumping-tonifying Qi, with Drain inner air tube.No longer tonifying Qi after last time is evacuated, and controlling intraductal atmospheric pressure is -1~0MPa；Then, with 8 DEG C/min's Heating rate is warming up to 1000 DEG C, and control intraductal atmospheric pressure is 0.01~0.05MPa, keeps the temperature as 6h.After heat preservation, at once with 1500sccm air-flow constantly leads to nitrogen or argon gas, the sulphur steam generated during heat preservation is discharged and is leading to cooling procedure persistently It is carried out under conditions of inert gas.
Step 3: after the cooling of calcined sample, deionized water is washed 5 times, and dehydrated alcohol washs 5 times, then will be washed After sample collection after washing 80 DEG C at a temperature of it is dry for 24 hours, nanometer stub self assembly four can be obtained and vulcanize a three vanadium micron balls.
Compared with the existing technology, 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 this method is simply easy Control, raw material is cheap and easy to get, at low cost, and yield is high, is not necessarily to post-processing, environmentally friendly, can be suitble to be mass produced.Together When, the three vanadium micron ball chemical compositions of vulcanization of nanometer stub self assembly four of this method preparation are uniform, and purity is higher, and has higher Crystallinity and special nanometer stub self assembly micron spherical structure, be used as ferromagnetic material and lithium/sodium-ion battery electrode material Excellent performance is shown when material.

Claims (7)

1. the preparation method that a kind of nanometer of stub self assembly four vulcanizes three vanadium micron balls, which is characterized in that by molar ratio be 1:10 The vanadium source of~1:15 and sulphur source substance are laid in porcelain boat both ends respectively, are subsequently placed in tube-type atmosphere furnace at 300 DEG C~1000 DEG C Under calcined and control intraductal atmospheric pressure be 0.01~0.05MPa, calcination process are as follows: with the heating rate liter of 5~10 DEG C/min Temperature keeps the temperature 1-6 hours to 300~1000 DEG C, then constantly leads to one of nitrogen, argon gas with 800~1500sccm air-flow Or two kinds, the sulphur steam generated during heat preservation is discharged and makes cooling procedure in one or both of maintaining nitrogen purge, argon gas Under conditions of carry out；After finally calcined sample is cooled down, washes clean, collection, drying；The vanadium source is five oxidations Two vanadium；Before calcining, check the air-tightness of tube-type atmosphere furnace and exclude the air in pipe, control pipe in air pressure be -1~ 0MPa。
2. a kind of nanometer of stub self assembly four according to claim 1 vulcanizes the preparation method of three vanadium micron balls, feature It is, the method that the air-tightness for checking tube-type atmosphere furnace uses up inner air tube side by side are as follows: nitrogen is passed through into pipe, in argon gas One or two then carry out 3~8 pumping-tonifying Qi, no longer tonifying Qi after last time is evacuated.
3. a kind of nanometer of stub self assembly four according to claim 1 vulcanizes the preparation method of three vanadium micron balls, feature It is, holding stage, control intraductal atmospheric pressure is 0.01~0.05MPa.
4. a kind of nanometer of stub self assembly four according to claim 1 vulcanizes the preparation method of three vanadium micron balls, feature It is, the mode of washing is filtering and washing or centrifuge washing, and collection mode is collected by suction or is collected by centrifugation；The washing is Successively washed with deionized water and dehydrated alcohol.
5. a kind of nanometer of stub self assembly four according to claim 1 vulcanizes the preparation method of three vanadium micron balls, feature It is, the temperature of the drying is 60~80 DEG C, the time is 6~for 24 hours.
6. a kind of nanometer of stub self assembly four described in any one of -5 vulcanizes the preparation of three vanadium micron balls according to claim 1 Method, which is characterized in that the sulphur source is CH3CSNH2、CN2H4S, one of sublimed sulfur, ammonium sulfide and copper reagent or several Kind.
7. a kind of nanometer stub self assembly four of method according to claim 11 preparation vulcanizes the application of three vanadium micron balls, It is characterized in that, this nanometer of stub self assembly four, which vulcanizes three vanadium micron balls, is applied to ferromagnetic material and sodium-ion battery electrode material 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
CN109706479B (en) * 2018-12-25 2021-06-01 陕西科技大学 Sheet V3S4Preparation of (A) and application of electrocatalytic properties thereof
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
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
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
CN113413906B (en) * 2021-07-30 2022-09-09 陕西科技大学 Vanadium trisulfide/graphite phase carbon nitride photocatalyst and preparation method thereof

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