CN104310485B - A kind of Wolfram disulfide nano powdered material with aluminium sulfide shell and preparation method thereof - Google Patents

A kind of Wolfram disulfide nano powdered material with aluminium sulfide shell and preparation method thereof Download PDF

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CN104310485B
CN104310485B CN201410557604.6A CN201410557604A CN104310485B CN 104310485 B CN104310485 B CN 104310485B CN 201410557604 A CN201410557604 A CN 201410557604A CN 104310485 B CN104310485 B CN 104310485B
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shell
nano
aluminium
anode
sulfide
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CN104310485A (en
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孙玉萍
刘先国
赵越
李成涛
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Anhui University of Technology AHUT
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G41/00—Compounds of tungsten
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00—Compounds of aluminium
    • C01F7/68—Aluminium compounds containing sulfur
    • C01F7/70—Sulfides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer

Abstract

The invention discloses a kind of with aluminium sulfide (Al 2s 3) tungsten disulfide (WS of shell 2) nano-powder material and preparation method thereof, belong to technical field of nanometer material preparation.This nano-powder material is nucleocapsid structure, and kernel is WS 2nano particle, shell is Al 2s 3layer; Described WS 2the particle diameter of kernel is 10 ~ 100nm, described Al 2s 3outer shell is amorphous Al 2s 3layer, its thickness is 1 ~ 10nm.The present invention adopts plasma arc electric discharge, tungsten powder and aluminium powder are pressed into block as anode material by certain atomic percent, adopt graphite as cathode material, quote argon gas and stink damp as working gas, certain distance is kept between negative electrode and positive electrode, play arc-over between anode and cathode, obtain with Al 2s 3the WS of shell 2nano-powder material.Preparation process of the present invention is simple, without postprocessing working procedures and cost low, be easy to realize suitability for industrialized production.

Description

A kind of Wolfram disulfide nano powdered material with aluminium sulfide shell and preparation method thereof
Technical field
The invention belongs to technical field of nanometer material preparation, be specifically related to a kind of with aluminium sulfide (Al 2s 3) tungsten disulfide (WS of shell 2) nano-powder material and preparation method thereof.
Background technology
Metallic sulfide is the very important semiconductor material of a class.The research interest that the broad prospect of application of nano metal sulfide material in photocatalyst material, luminescent material, nonlinear optical material and photosensor material etc. causes people strong.Sulfide semiconductor we production with life in serve more and more important effect.As a kind of WS having peculiar property 2, also cause people's special concern, because when temperature exceedes its critical temperature, WS 2magnetic and electroconductibility conversion of energy can be produced.In solar cell, hydrodesulfurization catalytic reaction, and the aspect such as photoconductive material and lithium-sulfur cell cathode material all has a wide range of applications.At present, the WS of different morphologies 2nano material is synthesized in succession, as nanocrystalline, nanometer rod, triangular shape nanoprisms, three-dimensional flower-shaped etc.Then due to WS 2nano material badly influences WS because volumetric shrinkage changes the splintering problem brought in the application 2the practical application of nano material.In order to better address this problem, researchist have employed this special microtexture of nucleocapsid structure, to WS 2nano material superscribes crust, to reach provide protection.The sheating material be widely used now is carbon material, but carbon material cannot provide enough level and smooth passage for the transmission of S ion.Therefore, a kind of WS of sulfide shell is developed 2nano material, has become present study hotspot.Show, with Al through retrieval 2s 3the WS of shell 2nano-powder material is not reported.
Summary of the invention
The object of this invention is to provide a kind of with aluminium sulfide (Al 2s 3) tungsten disulfide (WS of shell 2) nano-powder material and preparation method thereof.
The invention provides a kind of with aluminium sulfide (Al 2s 3) tungsten disulfide (WS of shell 2) nano-powder material, this nano material is nucleocapsid structure, and kernel is tungsten disulfide (WS 2) nano particle, shell is aluminium sulfide (Al 2s 3) layer; Described WS 2the particle diameter of nano particle kernel is 10 ~ 100nm, described Al 2s 3outer shell is amorphous Al 2s 3layer, its thickness is 1 ~ 10nm.
Present invention also offers above-mentioned with aluminium sulfide (Al 2s 3) tungsten disulfide (WS of shell 2) preparation method of nano-powder material, this material utilizes plasma electrically arc discharge technology, and under working gas, original position prepares; Wherein:
Employing Graphite Electrodes is negative electrode, and tungsten aluminium powder form block is anode target material, keeps the distance of 2 ~ 30mm between negative electrode Graphite Electrodes and anode tungsten aluminium powder form block; The voltage of arc-over is 10 ~ 40V; Working gas is argon gas and hydrogen sulfide.
Described anode is tungsten aluminium powder form block, and tungsten powder and aluminium powder are pressed into the anode material of block as plasma arc furnace under pressure 1Mpa ~ 1Gpa, and the atomic percent in described anode material shared by tungsten is 95 ~ 99%.
The dividing potential drop of described argon working gas is 0.01 ~ 0.5Mpa, and the dividing potential drop of hydrogen sulfide is 0.01 ~ 0.3MPa.
Relative to prior art, outstanding advantages of the present invention is:
1) the present invention has prepared first with aluminium sulfide (Al 2s 3) tungsten disulfide (WS of shell 2) nano-powder material;
2) preparation process condition of the present invention is simple, is easy to control, for Al 2s 3the WS of shell 2the practical application of nano-powder material provides condition;
3) nano-powder material prepared by the present invention, due to Al 2s 3the existence of shell can effective control WS 2the splintering problem of nano particle among charge and discharge process, makes with Al 2s 3the WS of shell 2nano-powder material becomes the strong candidate material of lithium-sulfur cell negative pole.
Accompanying drawing explanation
Fig. 1 is for preparation the present invention is with aluminium sulfide (Al 2s 3) tungsten disulfide (WS of shell 2) the device schematic diagram of nano-powder material;
Wherein: 1, upper cover; 2, negative electrode; 3, valve; 4, target; 5, viewing window; 6, baffle plate; 7, copper anode; 8, chuck; 9, plumbago crucible; 10, DC pulse power supply; A, water coolant; B, argon gas; C, stink damp.
Fig. 2 be the present invention prepare with aluminium sulfide (Al 2s 3) tungsten disulfide (WS of shell 2) X-ray diffraction (XRD) collection of illustrative plates of nano-powder material;
According to JCPDSPDF card (JCPDS card, No.84-1399), gained can be retrieved with aluminium sulfide (Al 2s 3) tungsten disulfide (WS of shell 2) nano-powder material principal phase is WS 2crystalline phase is formed; Due to Al 2s 3xRD is non-crystalline state, and is in shell, so cannot detect Al 2s 3phase.
Fig. 3 be the present invention prepare with aluminium sulfide (Al 2s 3) tungsten disulfide (WS of shell 2) transmission electron microscope (TEM) image of nano-powder material;
As can be seen from the figure products therefrom has nucleocapsid structure, WS 2the particle diameter of nano particle kernel is 10 ~ 100nm, Al 2s 3the thickness of layer is 1 ~ 10nm.
Fig. 4 prepared by the present invention with aluminium sulfide (Al 2s 3) tungsten disulfide (WS of shell 2) the high resolution transmission electron microscopy image of nano-powder material;
As can be seen from the figure gained is with aluminium sulfide (Al 2s 3) tungsten disulfide (WS of shell 2) nano-powder material kernel is WS 2, shell is the Al of amorphous 2s 3shell.
Embodiment
Below in conjunction with embodiment, the invention will be further described, but the present invention is not limited to following embodiment.
Embodiment 1
Device upper cover 1 shown in Fig. 1 is opened, making negative electrode 2 with graphite is fixed on chuck 8, the composition of institute's consumable anode target 4 is the block that pure tungsten powder and pure aluminium powder (atomic ratio 99:1) are pressed into, be placed on the copper anode 7 of logical water coolant, be plumbago crucible 9 between the copper anode and target of logical water coolant.The distance of 30mm is kept between negative electrode Graphite Electrodes and anode tungsten aluminium powder form block.Lid mounted device upper cover 1, logical water coolant a, after whole working spaces being vacuumized by valve 3, pass into argon gas b and stink damp c, the dividing potential drop of argon gas is 0.5Mpa, and the dividing potential drop of stink damp is 0.3Mpa, and connect DC pulse power supply 10, voltage is 40V.Working current and voltage is regulated to keep relative stability in arc discharge process.Obtained with aluminium sulfide (Al 2s 3) tungsten disulfide (WS of shell 2) nano-powder material, there is nucleocapsid structure, crystalline state WS 2the particle diameter of nano particle kernel is 10 ~ 100nm, amorphous Al 2s 3the thickness of layer is 1 ~ 10nm.
Embodiment 2
Device upper cover 1 shown in Fig. 1 is opened, making negative electrode 2 with graphite is fixed on chuck 8, the composition of institute's consumable anode target 4 is the block that pure tungsten powder and pure aluminium powder (atomic ratio 95:5) are pressed into, be placed on the copper anode 7 of logical water coolant, be plumbago crucible 9 between the copper anode and target of logical water coolant.The distance of 2mm is kept between negative electrode Graphite Electrodes and anode tungsten aluminium powder form block.Lid mounted device upper cover 1, logical water coolant a, after whole working spaces being vacuumized by valve 3, pass into argon gas b and stink damp c, the dividing potential drop of argon gas is 0.01Mpa, and the dividing potential drop of stink damp is 0.01Mpa, and connect DC pulse power supply 10, voltage is 10V.Working current and voltage is regulated to keep relative stability in arc discharge process.Obtained with aluminium sulfide (Al 2s 3) tungsten disulfide (WS of shell 2) nano-powder material, there is nucleocapsid structure, crystalline state WS 2the particle diameter of nano particle kernel is 10 ~ 100nm, amorphous Al 2s 3the thickness of layer is 1 ~ 10nm.
Embodiment 3
Device upper cover 1 shown in Fig. 1 is opened, making negative electrode 2 with graphite is fixed on chuck 8, the composition of institute's consumable anode target 4 is the block that pure tungsten powder and pure aluminium powder (atomic ratio 98:2) are pressed into, be placed on the copper anode 7 of logical water coolant, be plumbago crucible 9 between the copper anode and target of logical water coolant.The distance of 10mm is kept between negative electrode Graphite Electrodes and anode tungsten aluminium powder form block.Lid mounted device upper cover 1, logical water coolant a, after whole working spaces being vacuumized by valve 3, pass into argon gas b and stink damp c, the dividing potential drop of argon gas is 0.1Mpa, and the dividing potential drop of stink damp is 0.1Mpa, and connect DC pulse power supply 10, voltage is 20V.Working current and voltage is regulated to keep relative stability in arc discharge process.Obtained with aluminium sulfide (Al 2s 3) tungsten disulfide (WS of shell 2) nano-powder material, there is nucleocapsid structure, crystalline state WS 2the particle diameter of nano particle kernel is 10 ~ 100nm, amorphous Al 2s 3the thickness of layer is 1 ~ 10nm.
Embodiment 4
Device upper cover 1 shown in Fig. 1 is opened, making negative electrode 2 with graphite is fixed on chuck 8, the composition of institute's consumable anode target 4 is the block that pure tungsten powder and pure aluminium powder (atomic ratio 97:3) are pressed into, be placed on the copper anode 7 of logical water coolant, be plumbago crucible 9 between the copper anode and target of logical water coolant.The distance of 10mm is kept between negative electrode Graphite Electrodes and anode tungsten aluminium powder form block.Lid mounted device upper cover 1, logical water coolant a, after whole working spaces being vacuumized by valve 3, pass into argon gas b and stink damp c, the dividing potential drop of argon gas is 0.1Mpa, and the dividing potential drop of stink damp is 0.1Mpa, and connect DC pulse power supply 10, voltage is 20V.Working current and voltage is regulated to keep relative stability in arc discharge process.Obtained with aluminium sulfide (Al 2s 3) tungsten disulfide (WS of shell 2) nano-powder material, there is nucleocapsid structure, crystalline state WS 2the particle diameter of nano particle kernel is 10 ~ 100nm, amorphous Al 2s 3the thickness of layer is 1 ~ 10nm.
Embodiment 5
Device upper cover 1 shown in Fig. 1 is opened, making negative electrode 2 with graphite is fixed on chuck 8, the composition of institute's consumable anode target 4 is the block that pure tungsten powder and pure aluminium powder (atomic ratio 98:2) are pressed into, be placed on the copper anode 7 of logical water coolant, be plumbago crucible 9 between the copper anode and target of logical water coolant.The distance of 10mm is kept between negative electrode Graphite Electrodes and anode tungsten aluminium powder form block.Lid mounted device upper cover 1, logical water coolant a, after whole working spaces being vacuumized by valve 3, pass into argon gas b and stink damp c, the dividing potential drop of argon gas is 0.2Mpa, and the dividing potential drop of stink damp is 0.2Mpa, and connect DC pulse power supply 10, voltage is 30V.Working current and voltage is regulated to keep relative stability in arc discharge process.Obtained with aluminium sulfide (Al 2s 3) tungsten disulfide (WS of shell 2) nano-powder material, there is nucleocapsid structure, crystalline state WS 2the particle diameter of nano particle kernel is 10 ~ 100nm, amorphous Al 2s 3the thickness of layer is 1 ~ 10nm.
Embodiment 6
Device upper cover 1 shown in Fig. 1 is opened, making negative electrode 2 with graphite is fixed on chuck 8, the composition of institute's consumable anode target 4 is the block that pure tungsten powder and pure aluminium powder (atomic ratio 98:2) are pressed into, be placed on the copper anode 7 of logical water coolant, be plumbago crucible 9 between the copper anode and target of logical water coolant.The distance of 20mm is kept between negative electrode Graphite Electrodes and anode tungsten aluminium powder form block.Lid mounted device upper cover 1, logical water coolant a, after whole working spaces being vacuumized by valve 3, pass into argon gas b and stink damp c, the dividing potential drop of argon gas is 0.4Mpa, and the dividing potential drop of stink damp is 0.1Mpa, and connect DC pulse power supply 10, voltage is 30V.Working current and voltage is regulated to keep relative stability in arc discharge process.Obtained with aluminium sulfide (Al 2s 3) tungsten disulfide (WS of shell 2) nano-powder material, there is nucleocapsid structure, crystalline state WS 2the particle diameter of nano particle kernel is 10 ~ 100nm, amorphous Al 2s 3the thickness of layer is 1 ~ 10nm.
Embodiment 7
Device upper cover 1 shown in Fig. 1 is opened, making negative electrode 2 with graphite is fixed on chuck 8, the composition of institute's consumable anode target 4 is the block that pure tungsten powder and pure aluminium powder (atomic ratio 98:2) are pressed into, be placed on the copper anode 7 of logical water coolant, be plumbago crucible 9 between the copper anode and target of logical water coolant.The distance of 20mm is kept between negative electrode Graphite Electrodes and anode tungsten aluminium powder form block.Lid mounted device upper cover 1, logical water coolant a, after whole working spaces being vacuumized by valve 3, pass into argon gas b and stink damp c, the dividing potential drop of argon gas is 0.1Mpa, and the dividing potential drop of stink damp is 0.1Mpa, and connect DC pulse power supply 10, voltage is 40V.Working current and voltage is regulated to keep relative stability in arc discharge process.Obtained with aluminium sulfide (Al 2s 3) tungsten disulfide (WS of shell 2) nano-powder material, there is nucleocapsid structure, crystalline state WS 2the particle diameter of nano particle kernel is 10 ~ 100nm, amorphous Al 2s 3the thickness of layer is 1 ~ 10nm.

Claims (2)

1. with a Wolfram disulfide nano powdered material for aluminium sulfide shell, it is characterized in that, this nano material is nucleocapsid structure, and kernel is Wolfram disulfide nano particle, and shell is aluminum sulfide layer;
The particle diameter of described Wolfram disulfide nano particle kernel is 10 ~ 100nm; Described aluminium sulfide outer shell is amorphous aluminum sulfide layer, and its thickness is 1 ~ 10nm.
2. as claimed in claim 1 with the preparation method of the Wolfram disulfide nano powdered material of aluminium sulfide shell, it is characterized in that: this material utilizes plasma electrically arc discharge technology, and under working gas, original position prepares; Wherein:
Employing Graphite Electrodes is negative electrode, and tungsten aluminium powder form block is anode, keeps the distance of 2 ~ 30mm between negative electrode Graphite Electrodes and anode tungsten aluminium powder form block; The voltage of arc-over is 10 ~ 40V; Working gas is argon gas and hydrogen sulfide; Atomic percent in described anode shared by tungsten is 95 ~ 99%; The dividing potential drop of described argon gas is 0.01 ~ 0.5MPa, and the dividing potential drop of hydrogen sulfide is 0.01 ~ 0.3MPa.
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