CN109336069A - A kind of preparation of two telluride molybdenum nano-material and two telluride molybdenum nano-materials - Google Patents
A kind of preparation of two telluride molybdenum nano-material and two telluride molybdenum nano-materials Download PDFInfo
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- CN109336069A CN109336069A CN201811292957.2A CN201811292957A CN109336069A CN 109336069 A CN109336069 A CN 109336069A CN 201811292957 A CN201811292957 A CN 201811292957A CN 109336069 A CN109336069 A CN 109336069A
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- molybdenum
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
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- 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
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
Abstract
The invention discloses a kind of preparation of two telluride molybdenum nano-materials and two telluride molybdenum nano-materials, silica/silicon piece is substrate, molybdenum powder and tellurium powder are raw material, carry out the growth of two telluride molybdenum nano wires using chemical vapour deposition technique in the silica face of the substrate；The growing container of the two telluride molybdenum nano wire is quartz ampoule, and the mixed gas of argon gas and hydrogen is passed through in quartz ampoule；Quartz test tube is also set up in the quartz ampoule, the sealing end of quartz test tube is opposite with simulation model for mixing gases flows direction, and quartz test tube is used to place the substrate for carrying out chemical vapor deposition；The flow of argon gas is 100sccm；The flow of hydrogen is 5~30sccm；The reaction temperature of chemical vapor deposition is 600~800 DEG C.Simple process and low cost, two telluride molybdenum Nanowire Qualities are high.
Description
Technical field
The invention belongs to field of nanometer material technology, are related to the preparation and two telluride molybdenum nanometers of a kind of two telluride molybdenum nano-materials
Wire material.
Background technique
Two telluride molybdenums are the important members of Transition-metal dichalcogenide TMDs family, are a kind of novel two-dimensional materials,
Because of its unique electrical and optical performance, rapidly by extensive concern, two telluride molybdenum of stratiform is made of three atomic layers, and centre is molybdenum
Atomic layer, upper layer and lower layer are tellurium atom layer, and intermediate molybdenum atom layer is clipped between two tellurium atoms up and down, collectively form sandwich
Structure, in layer, molybdenum atom and six tellurium atoms are combined by too strong covalent bond.Two telluride molybdenum semimetals belong to big band gap
Quantum Spin Hall insulator, can be used for field effect transistor, additionally due to energy band and fermi level overlapping, have excellent electricity
Chemical property can be used as the electrode material of supercapacitor and be widely studied.Two telluride molybdenums are to belong to transition metal sulfur family
Unique stratified material of object is closed, the preparation of two telluride molybdenums is divided into physical method and chemical method, such as: mechanical stripping, chemical gaseous phase
It transports.Wherein chemical vapour deposition technique is the preparation method of most promising two telluride molybdenum generally acknowledged at present.Have at present
Researcher is engaged in the preparation of two-dimensional two telluride molybdenum material and achieves certain achievement, but the two of non-synthesizing one-dimensional structure
Telluride molybdenum nano wire.
Summary of the invention
The present invention provides a kind of preparation of two telluride molybdenum nano-materials and two telluride molybdenum nano-materials.This experiment work
Skill process is simple, and raw material, which obtains, to be easy, and the two telluride molybdenum Nanowire Qualities prepared are good.
In order to achieve the above objectives, the technical solution that the present invention takes includes:
A kind of preparation method of two telluride molybdenum nano-material, silica/silicon piece are substrate, and molybdenum powder and tellurium powder are original
Material carries out the growth of two telluride molybdenum nano wires in the silica face of the substrate using chemical vapour deposition technique；
The growing container of the two telluride molybdenum nano wire is quartz ampoule, and the gaseous mixture of argon gas and hydrogen is passed through in quartz ampoule
Body；
Quartz test tube, sealing end and the simulation model for mixing gases flows direction phase of quartz test tube are also set up in the quartz ampoule
Right, quartz test tube is used to place the substrate for carrying out chemical vapor deposition；
The flow of argon gas is 100sccm；The flow of hydrogen is 5~30sccm；The reaction temperature of chemical vapor deposition is 600
~800 DEG C.
Optionally, the silica/silicon piece substrate has two panels, the silica of two silica/silicon piece substrates
Face is opposite to be stacked, and folds up molybdenum powder and tellurium powder stacking interlayer.
Optionally, the molar ratio of the molybdenum powder and tellurium powder is 1:1~20, the gross mass of the molybdenum powder and tellurium powder be 1mg~
4mg。
Optionally, NaCl is adulterated between molybdenum powder and tellurium powder, the doping of NaCl is 0.1mg~0.5mg.
Optionally, the heating rate of hydrogen is 20~50 DEG C/min.
Optionally, the molybdenum powder and the molar ratio of tellurium powder mixing are 1:1~20.
Optionally, the growth time of the two telluride molybdenum nano wire is 4~15min.
Optionally, it specifically includes:
(1) silica/silicon substrate is cut into the sheet of 1cm*3cm, and molybdenum powder and tellurium powder are mixed in proportion as mixed powder；
(2) mixed powder is placed on the silica face of a silica/silicon substrate, and adds sodium chloride；Another
The silica face of silica/silicon substrate, which tips upside down on, to be placed on the silica/silicon substrate of mixed powder；
(3) two silica/silicon substrate shiftings are placed in quartz test tube, quartz test tube is placed in quartz ampoule, stone
The sealing end of English test tube is opposite with simulation model for mixing gases flows direction, and heating carries out the change of two telluride molybdenum nano wires in tube-type atmosphere furnace
Learn vapor deposition.
A kind of two telluride molybdenum nano-materials, including silica/silicon substrate, are adopted on the silica/silicon substrate
The growth of two telluride molybdenum nano wires is carried out with method of the present invention.
Two more uniform telluride molybdenum nano wires of size are being prepared in present invention success, and preparation process is simple.
Detailed description of the invention
Fig. 1 is that the experiment of embodiment and comparative example in the present invention prepares schematic diagram；
Fig. 2 is the optical microscope photograph of embodiment 1 in the present invention；
Fig. 3 is the Raman map of embodiment 1 in the present invention；
Fig. 4 is the optical microscope photograph of embodiment 2 in the present invention；
Fig. 5 is the Raman map of embodiment 2 in the present invention；
Fig. 6 is the optical microscope photograph of comparative example 1 in the present invention；
The present invention is illustrated below in conjunction with specification drawings and specific embodiments.
Specific embodiment
Two telluride molybdenum nano-material prepared by the present invention, using chemical vapour deposition technique directly in silica/silicon
It is grown on substrate.By the ratio of reaction source, reaction temperature, the factors such as reaction time obtain two telluride molybdenum nano-material works
Skill is simple, low in cost.
In order to which objects and advantages of the present invention are more clearly understood, the present invention is carried out below in conjunction with drawings and examples
It is further described, and by embodying advantage of the invention to the analysis of comparative example.It should be appreciated that tool described herein
Body embodiment is only used to explain the present invention, is not intended to limit the present invention.
Embodiment one:
The present embodiment provides a kind of method that two telluride molybdenum nano wires are prepared on silica/silicon substrate, including following
Step:
Step 1: silica/silicon substrate is cut into the sheet of 1cm*3cm and is blown off with air gun；
Step 2: being that 1:4 ratio is ground by molybdenum powder and tellurium powder in molar ratio, is uniformly mixed, by the mixed-powder of 2mg
It is placed on silica/silicon substrate, and adds the sodium chloride of 0.1mg；By another silica/silicon substrate, SiO2It faces
Under, it tips upside down on the silicon wafer；
Step 3: two silica/silicon substrates being moved and are placed in the quartz ampoule that internal diameter is the single-ended sealing of 1.2mm, will
The quartz ampoule of single-ended sealing is placed in tube-type atmosphere furnace heated center position, and single-ended sealing quartz ampoule opening is towards exhaust outlet one
Side, as shown in Figure 1a.
Step 4: the argon gas of 100sccm, duration of ventilation 30min, to thoroughly remove residual oxygen in pipe are passed through.Then
Continue the hydrogen for being passed through 10sccm, and tube-type atmosphere furnace is heated to 750 DEG C, the rate of heat addition is 37.5 DEG C/min, heat preservation
15min.It is then turned off heater, cooled to room temperature, the two telluride molybdenum nano wires obtained at this time are as shown in Fig. 2, Raman light
Spectrum is as shown in Figure 3.
Illustrate that the material synthesized is nanowire structure by Fig. 2 optical photograph, Fig. 3 illustrates that the material of synthesis has two telluride molybdenums
Raman characteristic peak, show synthesis material be two telluride molybdenums.
Embodiment two:
The present embodiment provides a kind of method that two telluride molybdenum nano wires are prepared on silica/silicon substrate, including following
Step:
Step 1: silica/silicon substrate is cut into the sheet of 1cm*3cm and is blown off with air gun；
Step 2: being that 1:12 ratio is ground by molybdenum powder and tellurium powder in molar ratio, is uniformly mixed, by the mixed powder of 3mg
End is placed on silica/silicon substrate, and adds the sodium chloride of 0.2mg；By another silica/silicon substrate, SiO2Face
Downward, it tips upside down on the silicon wafer；
Step 3: two silica/silicon substrates being moved and are placed in the quartz ampoule that internal diameter is the single-ended sealing of 1.2mm, will
The quartz ampoule of single-ended sealing is placed in tube-type atmosphere furnace heated center position, and single-ended sealing quartz ampoule opening is towards exhaust outlet one
Side, as shown in Figure 1a.
Step 4: the argon gas of 100sccm, duration of ventilation 30min, to thoroughly remove residual oxygen in pipe are passed through.Then
Continue the hydrogen for being passed through 20sccm, and tube-type atmosphere furnace is heated to 700 DEG C, the rate of heat addition is 35 DEG C/min, keeps the temperature 4min.With
After close heater, cooled to room temperature, the two telluride molybdenum nano wires obtained at this time are as shown in figure 4, Raman spectrum such as Fig. 5 institute
Show.
Illustrate that the material synthesized is nanowire structure by Fig. 4 optical photograph, Fig. 5 illustrates that the material of synthesis has two telluride molybdenums
Raman characteristic peak, show synthesis material be two telluride molybdenums.
Comparative example 1:
This comparative example provides a kind of quartz ampoule without using single-ended sealing come the method for preparing material, includes the following steps,
Step 1: same as Example 1；
Step 2: same as Example 1；
Step 3: two silica/silicon substrates are directly placed at and are placed in tube-type atmosphere furnace heated center position, such as
Shown in Fig. 1 b.
Step 4: same as Example 1, the result obtained at this time is as shown in Figure 6.
Comparison can be shown, do not used the quartz ampoule of single-ended sealing as cavity, in the case that other conditions are constant, served as a contrast
The material synthesized on bottom is microparticle, does not form nanowire structure.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (9)
1. a kind of preparation method of two telluride molybdenum nano-materials, which is characterized in that silica/silicon piece is substrate, molybdenum powder and
Tellurium powder is raw material, carries out the growth of two telluride molybdenum nano wires using chemical vapour deposition technique in the silica face of the substrate；
The growing container of the two telluride molybdenum nano wire is quartz ampoule, and the mixed gas of argon gas and hydrogen is passed through in quartz ampoule；
Quartz test tube is also set up in the quartz ampoule, the sealing end of quartz test tube is opposite with simulation model for mixing gases flows direction, stone
English test tube is used to place the substrate for carrying out chemical vapor deposition；
The flow of argon gas is 100sccm；The flow of hydrogen is 5~30sccm；The reaction temperature of chemical vapor deposition be 600~
800℃。
2. the preparation method of two telluride molybdenum nano-material according to claim 1, which is characterized in that the titanium dioxide
Silicon/silicon chip substrate has two panels, and the silica face of two silica/silicon piece substrates is opposite to be stacked, and folds up molybdenum stacking interlayer
Powder and tellurium powder.
3. the preparation method of two telluride molybdenum nano-material according to claim 2, which is characterized in that the molybdenum powder and tellurium
The molar ratio of powder is 1:1~20, and the gross mass of the molybdenum powder and tellurium powder is 1mg~4mg.
4. the preparation method of two telluride molybdenum nano-material according to claim 3, which is characterized in that in molybdenum powder and tellurium powder
Between adulterate NaCl, the doping of NaCl is 0.1mg~0.5mg.
5. the preparation method of two telluride molybdenum nano-material according to claim 1,2,3 or 4, which is characterized in that hydrogen
Heating rate be 20~50 DEG C/min.
6. the preparation method of two telluride molybdenum nano-material according to claim 1 or 2, which is characterized in that the molybdenum powder
Molar ratio with the mixing of tellurium powder is 1:1~20.
7. the preparation method of two telluride molybdenum nano-material according to claim 1 or 2, which is characterized in that two tellurium
The growth time for changing molybdenum nano wire is 4~15min.
8. the preparation method of two telluride molybdenum nano-material according to claim 1 or 2, which is characterized in that specifically include:
(1) silica/silicon substrate is cut into the sheet of 1cm*3cm, and molybdenum powder and tellurium powder are mixed in proportion as mixed powder；
(2) mixed powder is placed on the silica face of a silica/silicon substrate, and adds sodium chloride；Another dioxy
SiClx/silicon substrate silica face, which tips upside down on, to be placed on the silica/silicon substrate of mixed powder；
(3) two silica/silicon substrate shiftings are placed in quartz test tube, quartz test tube is placed in quartz ampoule, quartz examination
The sealing end of pipe is opposite with simulation model for mixing gases flows direction, and heating carries out the chemical gas of two telluride molybdenum nano wires in tube-type atmosphere furnace
Mutually deposit.
9. a kind of two telluride molybdenum nano-materials, which is characterized in that including silica/silicon substrate, in the silica/silicon
The growth of two telluride molybdenum nano wires is carried out on substrate using method described in claim 1-8 any claim.
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| CN201811292957.2A CN109336069B (en) | 2018-11-01 | 2018-11-01 | Preparation of molybdenum ditelluride nanowire material and molybdenum ditelluride nanowire material |
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| CN111403475A (en) * | 2020-03-06 | 2020-07-10 | 华中科技大学 | Two-dimensional molybdenum ditelluride vertical heterojunction and preparation method and application thereof |
| CN113173562A (en) * | 2021-05-17 | 2021-07-27 | 福州大学 | Preparation method of metallic ditelluride |
| CN113839044A (en) * | 2021-11-29 | 2021-12-24 | 广东工业大学 | Lithium-sulfur battery positive electrode, preparation method thereof and lithium-sulfur battery |
| CN115404460A (en) * | 2022-09-02 | 2022-11-29 | 西北工业大学宁波研究院 | One-dimensional MoS 2 Nanotube material and method for preparing same |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111403475A (en) * | 2020-03-06 | 2020-07-10 | 华中科技大学 | Two-dimensional molybdenum ditelluride vertical heterojunction and preparation method and application thereof |
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| CN113173562A (en) * | 2021-05-17 | 2021-07-27 | 福州大学 | Preparation method of metallic ditelluride |
| CN113173562B (en) * | 2021-05-17 | 2022-10-21 | 福州大学 | Preparation method of metallic ditelluride |
| CN113839044A (en) * | 2021-11-29 | 2021-12-24 | 广东工业大学 | Lithium-sulfur battery positive electrode, preparation method thereof and lithium-sulfur battery |
| CN113839044B (en) * | 2021-11-29 | 2022-03-18 | 广东工业大学 | Lithium-sulfur battery positive electrode, preparation method thereof and lithium-sulfur battery |
| CN115404460A (en) * | 2022-09-02 | 2022-11-29 | 西北工业大学宁波研究院 | One-dimensional MoS 2 Nanotube material and method for preparing same |
| CN115404460B (en) * | 2022-09-02 | 2023-08-08 | 西北工业大学宁波研究院 | One-dimensional MoS 2 Nanotube material and method for preparing same |
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