CN109516444B - Preparation method of tungsten ditelluride - Google Patents
Preparation method of tungsten ditelluride Download PDFInfo
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- CN109516444B CN109516444B CN201811520412.2A CN201811520412A CN109516444B CN 109516444 B CN109516444 B CN 109516444B CN 201811520412 A CN201811520412 A CN 201811520412A CN 109516444 B CN109516444 B CN 109516444B
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Abstract
The invention discloses a preparation method of tungsten ditelluride, which comprises the following steps: uniformly mixing a tungsten raw material solution consisting of a first solvent with a complexing effect and a tungsten raw material with a tellurium raw material solution consisting of a second solvent with a reducing effect and a tellurium raw material, reacting at a high temperature under the protection of inert gas, and cooling to obtain the compound preparation; the tungsten raw material is tungsten hexachloride and/or tungsten powder, the first solvent is ethylenediamine, the tellurium raw material is tellurium powder and/or tellurium dioxide, and the second solvent is ethylenediamine and/or hydrazine hydrate. The invention provides the preparation method of tungsten ditelluride, which adopts new raw materials and has a milder preparation process, effectively overcomes the defects of high energy consumption and long time of the preparation method in the prior art, and the preparation method has simple and common equipment and instruments and has important popularization value; the product of the invention has good crystallinity, large yield, high purity and great theoretical and practical significance.
Description
Technical Field
The invention belongs to the technical field of preparation of non-magnetic semi-metal materials, and relates to a preparation method of a transition metal chalcogenide compound, in particular to a preparation method of tungsten ditelluride.
Background
Transition-metal Dichalcogenides (TMDCs) are a typical graphene-like layered material, commonly denoted as MX2(M represents a transition metal, X represents a chalcogen), of which tungsten ditelluride is a member.
Tungsten ditelluride is of significant interest since professor r.j.cava 2014 professor princeton university found its large magnetoresistance effect (LMR) at atmospheric pressure and low temperature, and remained unsaturated under extremely high applied magnetic fields. In 2015, Lv H Y et al calculated the electronic structure of tungsten ditelluride by a first principle and confirmed that perfect electron-hole compensation existed in the tungsten ditelluride material; in the same year, researchers at the institute of physics of the academy of sciences of china have explored the superconductivity of tungsten ditelluride.
The exploration and research on the thermoelectric property, the giant magnetoresistance effect and the superconductivity of the tungsten ditelluride are continuously carried out, but the preparation process of the tungsten ditelluride mainly comprises the synthesis under laboratory conditions, including the purification by a chemical vapor deposition method, a high-temperature high-pressure method, a chemical vapor transport method and the like, but only thin film products can be prepared, or single crystal samples basically have the size of only 1.5mm x 0.7mm x 0.02mm, the reaction heat preservation time is one to two weeks, and the tungsten ditelluride can be grown even as long as three months.
To date, no reports have been made on a method for rapidly and mass-producing tungsten ditelluride.
Disclosure of Invention
The invention aims to provide a milder preparation method of tungsten ditelluride aiming at the problems of high energy consumption, long process, product doping and the like in the preparation process of tungsten ditelluride in the prior art, which is suitable for the rapid and mass production of the future application of tungsten ditelluride in the manufacture of electromagnetic components and provides some possible references.
The invention adopts the following technical scheme:
a method for preparing tungsten ditelluride, comprising: uniformly mixing a tungsten raw material solution consisting of a first solvent with complexing action and a tungsten raw material with a tellurium raw material solution consisting of a second solvent with reducing action and a tellurium raw material, reacting at high temperature under the protection of inert gas, and cooling to obtain the compound.
In the technical scheme, the tungsten raw material is tungsten hexachloride and/or tungsten powder, and the purity is more than or equal to 99.5%.
In the technical scheme, the tellurium raw material is tellurium powder and/or tellurium dioxide, and the purity is more than or equal to 99.95%.
In the technical scheme, the first solvent is ethylenediamine, and the purity is more than or equal to 99.5%.
In the technical scheme, the second solvent is ethylenediamine and/or hydrazine hydrate, and the purity is more than or equal to 99.5%.
Further, in the above technical solution, in the tungsten raw material solution, a solution-to-solution ratio of the tungsten raw material to the first solvent is 1 g: 12-18 ml.
Further, in the above technical solution, in the tellurium raw material liquid, a liquid-to-feed ratio of the tellurium raw material to the second solvent is 1 g: 6-15 ml.
In the above technical scheme, the inert gas is argon or nitrogen.
Preferably, in the above technical solution, the purity of the inert gas is greater than or equal to 99.99%, and the flow rate of the inert gas is 10-400 SCCM.
In the technical scheme, the reaction temperature and the reaction time of the high-temperature reaction are respectively 750-850 ℃ and 10-20 h.
Further, in the above technical scheme, the preparation method further comprises, before the high-temperature reaction, centrifugally separating the uniformly mixed tungsten raw material liquid and tellurium raw material liquid, and then placing in a vacuum drying oven for low-temperature drying.
Still further, in the above technical scheme, the centrifugation rotation speed of the centrifugation is 3000-4500rpm, and the centrifugation time is 3-5 min.
Furthermore, in the technical scheme, the drying temperature of the low-temperature drying is 29-55 ℃, and the drying time is 4.5-8.5 h.
Still further, in the above technical scheme, the high temperature reaction process further comprises an operation of closing the opening of the furnace tube to the atmosphere furnace, specifically, introducing inert gas at 120-205 ℃, opening the gas outlet by loosening the rubber tube, keeping for 5-20min, not introducing inert gas, recovering the closing operation, introducing inert gas at 320-410 ℃, opening the gas outlet by loosening the rubber tube, keeping for 5-20min, not introducing inert gas, and recovering the closing operation.
Still further, in the above technical solution, the preparation method comprises the steps of:
s1, dropwise adding a first solvent with a complexing effect into a tungsten raw material, uniformly mixing to obtain a tungsten raw material solution, simultaneously dropwise adding a second solvent with a reducing effect into a tellurium raw material, and uniformly mixing to obtain a tellurium raw material solution;
s2, uniformly mixing the tungsten raw material liquid and the tellurium raw material liquid in the step S1, performing centrifugal separation to obtain a reaction mixture, and then placing the reaction mixture in a vacuum drying oven for low-temperature drying;
s3, placing the dried reaction mixture in the step S2 in an atmosphere furnace, reacting at high temperature in an inert atmosphere, and cooling to obtain the catalyst.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention provides the preparation method of tungsten ditelluride, which adopts new raw materials and has a milder preparation process, effectively overcomes the defects of high energy consumption and long time of the preparation method in the prior art, and the preparation method has simple and common equipment and instruments and has important popularization value;
(2) the tungsten ditelluride product prepared by the preparation method provided by the invention has good crystallinity, large yield and high purity, is not doped with other elements, does not need a series of steps such as water washing, alcohol washing and the like, and provides theoretical reference for mass production of tungsten ditelluride materials with high-quality thermoelectric property, giant magnetoresistance effect and superconductivity.
Drawings
FIG. 1 is an X-ray diffraction pattern of self-doped non-stoichiometric tungsten ditelluride prepared according to examples 1-3 of the present invention;
FIG. 2 is a Raman spectrum of stoichiometric pure phase tungsten ditelluride prepared in example 2 of the present invention.
Detailed Description
In order to facilitate an understanding of the present invention, the method of preparing tungsten ditelluride of the present invention is further described in more detail below with reference to the accompanying drawings and examples.
The preferred embodiment of the present invention is shown in the drawings; this invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein; rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The raw materials and the related experimental equipment used in the examples and comparative examples of the present invention are all commercially available products.
Example 1
The embodiment of the invention provides a preparation method of tungsten ditelluride, which comprises the following steps:
s1, placing 1.19g of tungsten hexachloride in a 50ml beaker, dropwise adding 15ml of ethylenediamine into the beaker, stirring for 30min, and uniformly mixing to obtain a tungsten raw material solution; and (3) dropwise adding 15ml of ethylenediamine into a beaker filled with 1.952g of tellurium powder, stirring for 30min, and uniformly mixing to obtain a tellurium raw material solution.
S2, uniformly mixing the tungsten raw material liquid and the tellurium raw material liquid in the step S1 (the molar ratio of the tungsten raw material to the tellurium raw material is 1: 2.55), stirring for 30min, transferring into a 50ml centrifuge tube, centrifuging at the rotating speed of 4000rpm for 5min, and putting into a vacuum drying oven to dry for 7h at the temperature of 30 ℃.
S3, transferring the reaction mixture dried in the step S2 to a corundum crucible, covering, placing the corundum crucible in a tube furnace, introducing 400SCCM nitrogen to clean the furnace tube, vacuumizing to 0.10MPa, introducing 80SCCM nitrogen, sealing the furnace tube when the pressure is normal atmospheric pressure, stopping introducing the nitrogen, heating to 150 ℃, continuing introducing the nitrogen and opening an air outlet, then sealing the furnace tube, closing a gas valve, heating to 360 ℃, introducing the nitrogen, starting the furnace tube, continuing introducing the nitrogen and sealing the furnace tube, heating to 800 ℃, preserving the temperature for 12 hours, stopping heating, closing the nitrogen, and cooling the crucible to room temperature along with the furnace to obtain the tungsten ditelluride powder material with the giant magnetoresistance property.
Example 2
The embodiment of the invention provides a preparation method of tungsten ditelluride, which comprises the following steps:
s1, placing 1.19g of tungsten hexachloride in a 50ml beaker, dropwise adding 15ml of ethylenediamine into the beaker, stirring for 30min, and uniformly mixing to obtain a tungsten raw material solution; and (3) dropwise adding 15ml of ethylenediamine into a beaker filled with 2.297g of tellurium powder, stirring for 30min, and uniformly mixing to obtain a tellurium raw material solution.
S2, uniformly mixing the tungsten raw material liquid and the tellurium raw material liquid in the step S1 (the molar ratio of the tungsten raw material to the tellurium raw material is 1: 3.00), stirring for 30min, transferring into a 50ml centrifuge tube, centrifuging at the rotating speed of 3500rpm for 5min, and putting into a vacuum drying oven to dry for 7h at the temperature of 30 ℃.
S3, transferring the reaction mixture dried in the step S2 to a corundum crucible, covering, placing the corundum crucible in a tube furnace, introducing 400SCCM nitrogen to clean the furnace tube, vacuumizing to 0.10MPa, introducing 80SCCM nitrogen, sealing the furnace tube when the pressure is normal atmospheric pressure, stopping introducing the nitrogen, heating to 150 ℃, continuing introducing the nitrogen and opening an air outlet, then sealing the furnace tube, closing a gas valve, heating to 360 ℃, introducing the nitrogen, starting the furnace tube, continuing introducing the nitrogen and sealing the furnace tube, heating to 800 ℃, preserving the temperature for 12 hours, stopping heating, closing the nitrogen, and cooling the crucible to room temperature along with the furnace to obtain the tungsten ditelluride powder material with the giant magnetoresistance property.
Example 3
The embodiment of the invention provides a preparation method of tungsten ditelluride, which comprises the following steps:
s1, placing 1.19g of tungsten hexachloride in a 50ml beaker, dropwise adding 15ml of ethylenediamine into the beaker, stirring for 30min, and uniformly mixing to obtain a tungsten raw material solution; and (3) dropwise adding 15ml of ethylenediamine into a beaker filled with 2.641g of tellurium powder, stirring for 30min, and uniformly mixing to obtain a tellurium raw material solution.
S2, uniformly mixing the tungsten raw material liquid and the tellurium raw material liquid in the step S1 (the molar ratio of the tungsten raw material to the tellurium raw material is 1: 3.45), stirring for 30min, transferring into a 50ml centrifuge tube, centrifuging for 5min at the rotating speed of 4200rpm, and putting into a vacuum drying oven to dry for 7h at the temperature of 30 ℃.
S3, transferring the reaction mixture dried in the step S2 to a corundum crucible, covering, placing the corundum crucible in a tube furnace, introducing 400SCCM nitrogen to clean the furnace tube, vacuumizing to 0.10MPa, introducing 80SCCM nitrogen, sealing the furnace tube when the pressure is normal atmospheric pressure, stopping introducing the nitrogen, heating to 150 ℃, continuing introducing the nitrogen and opening an air outlet, then sealing the furnace tube, closing a gas valve, heating to 360 ℃, introducing the nitrogen, starting the furnace tube, continuing introducing the nitrogen and sealing the furnace tube, heating to 800 ℃, preserving the temperature for 12 hours, stopping heating, closing the nitrogen, and cooling the crucible to room temperature along with the furnace to obtain the tungsten ditelluride powder material with the giant magnetoresistance property.
Example 4
The embodiment of the invention provides a preparation method of tungsten ditelluride, which comprises the following steps:
s1, placing 2.38g of tungsten hexachloride in a 50ml beaker, dropwise adding 20ml of ethylenediamine into the beaker, stirring for 60min, and uniformly mixing to obtain a tungsten raw material solution; and (3) dropwise adding 20ml of ethylenediamine into a beaker filled with 4.60g of tellurium powder, stirring for 60min, and uniformly mixing to obtain a tellurium raw material solution.
S2, uniformly mixing the tungsten raw material liquid and the tellurium raw material liquid in the step S1, stirring for 60min, transferring into a 100ml centrifuge tube, centrifuging for 5min at the rotating speed of 4000rpm, and drying in a vacuum drying oven at 50 ℃ for 6 h.
S3, transferring the reaction mixture dried in the step S2 to a corundum crucible, covering, placing the corundum crucible in a tube furnace, introducing 400SCCM argon to clean the furnace tube, vacuumizing to 0.10MPa, introducing 80SCCM argon, sealing the furnace tube when the pressure is normal atmospheric pressure, stopping introducing the argon, heating to 160 ℃, continuing introducing the argon and opening an air outlet, then sealing the furnace tube, closing a gas valve, heating to 400 ℃, introducing the argon, starting the furnace tube, continuing introducing the argon and sealing the furnace tube, heating to 800 ℃, preserving the temperature for 16 hours, stopping heating, closing the argon, and cooling the crucible to room temperature along with the furnace to obtain the tungsten ditelluride powder material with the giant magnetoresistance property.
Example 5
The embodiment of the invention provides a preparation method of tungsten ditelluride, which comprises the following steps:
s1, placing 3.97g of tungsten powder into a 50ml beaker, dropwise adding 20ml of ethylenediamine into the beaker, stirring for 75min, and uniformly mixing to obtain a tungsten raw material solution; and (3) dropwise adding 20ml of ethylenediamine into a beaker filled with 4.79g of tellurium dioxide, stirring for 75min, and uniformly mixing to obtain a tellurium raw material solution.
S2, uniformly mixing the tungsten raw material liquid and the tellurium raw material liquid in the step S1, stirring for 75min, transferring into a 100ml centrifuge tube, centrifuging for 5min at the rotating speed of 4000rpm, and drying in a vacuum drying oven at 55 ℃ for 4.5 h.
S3, transferring the reaction mixture dried in the step S2 to a corundum crucible, covering, placing the corundum crucible in a tube furnace, introducing 400SCCM argon to clean the furnace tube, vacuumizing to 0.10MPa, introducing 80SCCM argon, sealing the furnace tube when the pressure is normal atmospheric pressure, stopping introducing the argon, heating to 180 ℃, continuing introducing the argon and opening an air outlet, then sealing the furnace tube, closing a gas valve, heating to 410 ℃, introducing the argon, starting the furnace tube, continuing introducing the argon and sealing the furnace tube, heating to 800 ℃, preserving the temperature for 16 hours, stopping heating, closing the argon, and cooling the crucible to room temperature along with the furnace to obtain the tungsten ditelluride powder material with the giant magnetoresistance property.
In the invention, the tungsten ditelluride powder material is a transition group metal compound formed by tungsten and tellurium in a chemical element ratio of 1:2, wherein the tungsten is +4 valence, and the tellurium is-2 valence.
As shown in figure 1, the X-ray diffraction patterns of the self-doped non-stoichiometric tungsten ditelluride prepared in examples 1-3 of the present invention, the figure shows, in order from bottom to top, a tungsten-doped non-stoichiometric tungsten ditelluride sample in example 1, a pure-phase tungsten ditelluride sample in example 2 and a tellurium-doped non-stoichiometric tungsten ditelluride sample in example 3, the diffraction peaks corresponding to tungsten being marked in the smaller font size in the XRD pattern of the tungsten-doped non-stoichiometric tungsten ditelluride sample in example 1, the diffraction peaks corresponding to tellurium being marked in the smaller font size in the XRD pattern of the tellurium-doped non-stoichiometric tungsten ditelluride sample in example 3, the diffraction peaks corresponding to tungsten ditelluride being marked in the larger font size in the X-ray diffraction pattern, the comparison with a standard map shows that the prepared tungsten ditelluride is a tungsten ditelluride material with [002] orientation.
Fig. 2 shows a raman spectrum when the stoichiometric pure-phase tungsten ditelluride prepared in example 2 of the present invention is excited by laser along the b-axis direction.
Finally, the above is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for preparing tungsten ditelluride, which is characterized by comprising the following steps: uniformly mixing a tungsten raw material solution consisting of a first solvent with a complexing effect and a tungsten raw material with a tellurium raw material solution consisting of a second solvent with a reducing effect and a tellurium raw material, centrifugally separating, drying at a low temperature in a vacuum drying oven, reacting for 10-20h at the temperature of 750-850 ℃ under the protection of inert gas, and cooling to obtain the complex compound;
the first solvent is ethylenediamine, the tungsten raw material is tungsten hexachloride and/or tungsten powder, the second solvent is ethylenediamine and/or hydrazine hydrate, and the tellurium raw material is tellurium powder and/or tellurium dioxide.
2. The production method according to claim 1,
the purity of the tungsten raw material is more than or equal to 99.5 percent;
and/or the purity of the tellurium raw material is more than or equal to 99.95 percent.
3. The production method according to claim 1,
the purity of the first solvent is more than or equal to 99.5%;
and/or the purity of the second solvent is greater than or equal to 99.5%.
4. The production method according to claim 1,
in the tungsten raw material liquid, the material-liquid ratio of the tungsten raw material to the first solvent is 1 g: 12-18 ml;
and/or in the tellurium raw material liquid, the material-liquid ratio of the tellurium raw material to the second solvent is 1 g: 6-15 ml.
5. The production method according to claim 1,
the inert gas is argon or nitrogen.
6. The production method according to claim 5,
the purity of the inert gas is more than or equal to 99.99 percent, and the flow rate of the inert gas is 10-400 SCCM.
7. The method for preparing the compound of claim 1, wherein the centrifugation speed is 3000-4500rpm, and the centrifugation time is 3-5 min.
8. The preparation method according to claim 1, wherein the drying temperature of the low-temperature drying is 29-55 ℃, and the drying time is 4.5-8.5 h.
9. The preparation method according to any one of claims 1 to 6, wherein the high temperature reaction process further comprises closing the furnace tube opening operation of the atmosphere furnace, specifically, introducing inert gas at 120 to 205 ℃, opening the gas outlet by loosening the rubber tube, keeping for 5 to 20min, not introducing inert gas, recovering the closing operation, introducing inert gas at 320 to 410 ℃, opening the gas outlet by loosening the rubber tube, keeping for 5 to 20min, not introducing inert gas, and recovering the closing operation.
10. The method for preparing a polymer according to any one of claims 1 to 6, comprising the steps of:
s1, dropwise adding a first solvent with a complexing effect into a tungsten raw material, uniformly mixing to obtain a tungsten raw material solution, simultaneously dropwise adding a second solvent with a reducing effect into a tellurium raw material, and uniformly mixing to obtain a tellurium raw material solution;
s2, uniformly mixing the tungsten raw material liquid and the tellurium raw material liquid in the step S1, performing centrifugal separation to obtain a reaction mixture, and then placing the reaction mixture in a vacuum drying oven for low-temperature drying;
s3, placing the dried reaction mixture in the step S2 in an atmosphere furnace, reacting at high temperature in an inert atmosphere, and cooling to obtain the catalyst.
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| CN104651940A (en) * | 2015-02-28 | 2015-05-27 | 安庆美晶新材料有限公司 | Method for growing tungsten ditelluride single crystals by using vapor transport process |
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| CN104651940A (en) * | 2015-02-28 | 2015-05-27 | 安庆美晶新材料有限公司 | Method for growing tungsten ditelluride single crystals by using vapor transport process |
Non-Patent Citations (2)
| Title |
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| The First Hexanuclear Tungsten Telluride Clusters [W6Te8L6]n- as Amine Complexes with L =Piperidine (n=0) and L = Pyridine (n = 1);Xiaobing Xie et al.;《Inorg. Chem.》;19961231;第35卷(第10期);第2713-2714页 * |
| Thin tungsten telluride layer preparation by thermal annealing;Wei Lu et al.;《Nanotechnology》;20160908;第27卷;第1-7页 * |
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