CN109205677B - A kind of one-dimensional MoS2The preparation method of nanobelt - Google Patents

A kind of one-dimensional MoS2The preparation method of nanobelt Download PDF

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CN109205677B
CN109205677B CN201811454026.8A CN201811454026A CN109205677B CN 109205677 B CN109205677 B CN 109205677B CN 201811454026 A CN201811454026 A CN 201811454026A CN 109205677 B CN109205677 B CN 109205677B
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CN109205677A (en
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黄寒
施姣
刘金鑫
陈凤鸣
吴迪
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Central South University
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G39/00—Compounds of molybdenum
    • C01G39/06—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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • 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
    • C01P2004/17—Nanostrips, nanoribbons or nanobelts, i.e. solid nanofibres with two significantly differing dimensions between 1-100 nanometer

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Abstract

The present invention relates to technical field of nano material, more particularly to a kind of preparation method of one-dimensional molybdenum sulfide nanobelt, the present invention respectively heats sulphur and molybdenum oxide, under the current-carrying effect of nitrogen stream, sulphur steam is contacted with molybdenum oxide steam, molybdenum oxide steam forms gaseous molybdenum oxide in the environment of sulphur steam content few (i.e. a lack of sulfur) by sulphur steam reduction, these gaseous molybdenum oxides deposit to form MoOxS2‑x, in more (i.e. sulfur-rich) environment of sulphur steam content, MoOxS2‑xMolybdenum sulfide is formed by further vulcanization.Embodiment the result shows that, molybdenum sulfide nanobelt can be prepared in method provided by the invention, and method time-consuming provided by the invention is short, and do not use catalyst under conditions of can be completed.

Description

A kind of one-dimensional MoS2The preparation method of nanobelt
Technical field
The present invention relates to technical field of nano material more particularly to a kind of one-dimensional MoS2The preparation method of nanobelt.
Background technique
As one of the member of Transition-metal dichalcogenide (TMDs), two-dimentional MoS2Material due to its unique physics and Chemical property is widely used in the fields such as catalysis, sensor, solar battery and photoelectric device preparation.Theoretical research table It is bright, work as MoS2Dimension when being down to one-dimensional from two dimension, zigzag molybdenum sulfide nanobelt is changed by nonmetal character and nonferromagnetic Metallicity and magnetism, magnetic atom are mainly provided by the Mo atom at edge.
Currently, preparing one-dimensional MoS2The method of nanobelt is mainly as follows: 1. electrochemistry/chemical method, specifically comprises the processes of: it uses Molybdenum dioxide nano wire is electrodeposited at the step of highly oriented pyrolytic graphite as presoma by galvanoplastic, is then in temperature 800~900 DEG C and H2Molybdenum sulfide nanobelt can be obtained in annealing a few hours under S atmosphere；2. the chemical vapor deposition of catalyst auxiliary Method: MoO is used3With S as reaction raw materials, MoS is grown in substrate under the catalysis of NaCl2Nanobelt, principle are NaCl and MoO3Reaction forms NaMoO drop, and the NaMoO drop of melting promotes MoS under the atmosphere of sulfur vapor with reptile fashion2 The growth of nanobelt.
But the above method has the following problems: electrochemical process needs the time above for 24 hours could complete cure；Catalyst The chemical vapour deposition technique needs of auxiliary carry out under catalyst, but the presence of catalyst is equivalent to and has been mostly used a kind of material, It is likely to influence sample purity, and then influences sample quality.
Summary of the invention
In view of the above-mentioned problems in the prior art, the present invention provides a kind of one-dimensional MoS2The preparation side of nanobelt Method, the preparation method used time provided by the invention is short, and without using catalyst in preparation process.
The present invention provides a kind of one-dimensional MoS2The preparation method of nanobelt, comprising the following steps:
Under conditions of being continually fed into nitrogen, to S and MoO3Aumospheric pressure cvd is carried out, one-dimensional MoS is obtained2Nanometer Band；
The S and MoO3Separated, the S is placed on the first warm area, the MoO3It is placed on the second warm area；
The circulating direction of the nitrogen is to flow to MoO by S3；
The aumospheric pressure cvd successively includes six stages, specially first stage, second stage, third rank Section, fourth stage, the 5th stage and the 6th stage,
In the first stage, to MoO3Heating treatment is carried out, initial temperature is room temperature, and final temperature is 280~320 DEG C, heating rate is 13~17 DEG C/min；Constant temperature processing is carried out to S, temperature is 78~82 DEG C；
In the second stage, to MoO3Constant temperature processing is carried out, temperature is 280~320 DEG C；Constant temperature processing, temperature are carried out to S Degree is 78~82 DEG C；The time of the second stage is 28~32 min；
In the phase III, to MoO3Heating treatment is carried out, initial temperature is 280~320 DEG C, final temperature 730 ~770 DEG C, heating rate is 10~15 DEG C/min；Constant temperature processing is carried out to S, temperature is 78~82 DEG C；
In the fourth stage, to MoO3Constant temperature processing is carried out, temperature is 730~770 DEG C, and the time is 10~14min；? Preceding 5~7min of fourth stage carries out constant temperature processing to S, and temperature is 78~82 DEG C, in rear 5~7min of fourth stage, to S Heating treatment is carried out, heating rate is 23~27 DEG C/min；
In the 5th stage, cooling processing is carried out to the second warm area, initial temperature is 730~770 DEG C, final temperature It is 530~570 DEG C, rate of temperature fall is 8~12 DEG C/min；Constant temperature processing is carried out to the first warm area, temperature is 200~250 DEG C；
In the 6th stage, cooling processing is carried out to second warm area, initial temperature is 530~570 DEG C, is terminated Temperature is room temperature, and rate of temperature fall is 20~25 DEG C/min；Cooling processing is carried out to first warm area, rate of temperature fall is 20~25 DEG C/min, final temperature is room temperature；
During aumospheric pressure cvd, without using catalyst.
Preferably, in the first stage and second stage, the nitrogen be passed through speed independently be 300~ 500cm3/min；25~50cm independently is in the speed that is passed through of the phase III and fourth stage, the nitrogen3/min；? The speed that is passed through in the 5th stage, the nitrogen is 25~50cm3/min；In the 6th stage, the nitrogen is passed through Speed is 400~600cm3/min。
Preferably, the S and MoO3Mass ratio be 28~32:1.
Preferably, the S is provided in the form of S block；The MoO3With MoO3The form of powder provides.
Preferably, the aumospheric pressure cvd is carried out in substrate surface, and the substrate is placed on MoO3Top.
Preferably, the material of the substrate includes sapphire and/or silicon wafer.
Preferably, the aumospheric pressure cvd carries out in CVD tube furnace, the S and MoO3It is individually positioned in The different warm areas of CVD tube furnace.
Preferably, six stages of the aumospheric pressure cvd are successively are as follows:
In the first stage, to MoO3Heating treatment is carried out, initial temperature is room temperature, and final temperature is 300 DEG C, heating Rate is 15 DEG C/min；Constant temperature processing is carried out to S, temperature is 80 DEG C；
In the second stage, to MoO3Constant temperature processing is carried out, temperature is 300 DEG C；Constant temperature processing is carried out to S, temperature is 80℃；The time of second stage is 30min；
In the phase III, to MoO3Heating treatment is carried out, initial temperature is 300 DEG C, and final temperature is 750 DEG C, is risen Warm rate is 13 DEG C/min；Constant temperature processing is carried out to S, temperature is 80 DEG C；
In the fourth stage, to MoO3Constant temperature processing is carried out, temperature is 750 DEG C, time 12min；In fourth stage Preceding 6min, constant temperature processing is carried out to S, temperature is 80 DEG C, in the rear 6min of fourth stage, carries out heating treatment, heating speed to S Rate is 25 DEG C/min；
In the 5th stage, cooling processing is carried out to the second warm area, initial temperature is 750 DEG C, final temperature 550 DEG C, rate of temperature fall is 10 DEG C/min；Constant temperature processing is carried out to the first warm area, temperature is 230 DEG C；
In the 6th stage, cooling processing is carried out to the second warm area, initial temperature is 550 DEG C, and final temperature is room temperature, Rate of temperature fall is 25 DEG C/min；Cooling processing is carried out to the first warm area, rate of temperature fall is 20~25 DEG C/min, and final temperature is room Temperature.
The present invention provides a kind of one-dimensional MoS2The preparation method of nanobelt, the present invention is respectively to S and MoO3It is heated, Under the current-carrying effect of nitrogen stream, S steam and MoO3Steam contact, MoO3Steam is few (i.e. in S steam content by S steam reduction A lack of sulfur) environment in form gaseous MoO3-x, these gaseous MoO3-xDeposition forms MoOxS2-x, more in S steam content In the environment of (i.e. sulfur-rich), MoOxS2-xMoS is formed by further vulcanization2。
The present invention in the first stage, preceding 5~7min of second stage, phase III and fourth stage, the temperature of S compared with It is low, and MoO3Temperature it is higher so that in the process, sulphur supply is insufficient, in the case where this lack of sulfur, S steam and MoO3Steam Form one-dimensional MoOxS2-x；It is increased in the temperature of rear 5~7min of fourth stage, S, forms a large amount of sulfur vapors, it is sulfur-rich herein In environment, one-dimensional MoOxS2-xIt cures to form MoS2Nanobelt, with the progress of reaction, all one-dimensional MoOxS2-xQuilt entirely Vulcanization forms one-dimensional MoS2Nanobelt.Embodiment the result shows that, MoS can be prepared in method provided by the invention2Nanobelt, And method time-consuming provided by the invention is short, and can be completed under conditions of not using catalyst.
Detailed description of the invention
Fig. 1 is substrate and MoO3Positional relationship；
Fig. 2 is the optical microscope for the product that the embodiment of the present invention 1 is prepared；
Fig. 3 is the atomic force microscopy diagram for the product that the embodiment of the present invention 1 is prepared；
Fig. 4 is the Raman spectrum and Raman mapping figure for the product that the embodiment of the present invention 1 is prepared；
Fig. 5 is the fluorescence spectrum and fluorescence mapping figure for the product that the embodiment of the present invention 1 is prepared；
Fig. 6 is the optical microscope for the product that the embodiment of the present invention 2 is prepared；
Fig. 7 is the atomic force microscopy diagram for the product that the embodiment of the present invention 2 is prepared；
Fig. 8 is the Raman spectrogram for the product that the embodiment of the present invention 2 is prepared.
Specific embodiment
The present invention provides a kind of one-dimensional MoS2The preparation method of nanobelt, comprising the following steps:
Under conditions of being continually fed into nitrogen, to S and MoO3Aumospheric pressure cvd is carried out, one-dimensional MoS is obtained2Nanometer Band；
The S and MoO3It is separated；
The circulating direction of the nitrogen is to flow to MoO by S3；
The aumospheric pressure cvd successively includes six stages, specially first stage, second stage, third rank Section, fourth stage, the 5th stage and the 6th stage,
In the first stage, to MoO3Heating treatment is carried out, initial temperature is room temperature, and final temperature is 280~320 DEG C, heating rate is 13~17 DEG C/min；Constant temperature processing is carried out to S, temperature is 78~82 DEG C；
In the second stage, to MoO3Constant temperature processing is carried out, temperature is 280~320 DEG C；Constant temperature processing, temperature are carried out to S Degree is 78~82 DEG C；The time of the second stage is 28~32 min；
In the phase III, to MoO3Heating treatment is carried out, initial temperature is 280~320 DEG C, final temperature 730 ~770 DEG C, heating rate is 10~15 DEG C/min；Constant temperature processing is carried out to S, temperature is 78~82 DEG C；
In the fourth stage, to MoO3Constant temperature processing is carried out, temperature is 730~770 DEG C, and the time is 10~14min；? Preceding 5~7min of fourth stage carries out constant temperature processing to S, and temperature is 78~82 DEG C, in rear 5~7min of fourth stage, to S Heating treatment is carried out, heating rate is 23~27 DEG C/min；
In the 5th stage, cooling processing is carried out to the second warm area, initial temperature is 730~770 DEG C, final temperature It is 530~570 DEG C, rate of temperature fall is 8~12 DEG C/min；Constant temperature processing is carried out to the first warm area, temperature is 200~250 DEG C；
In the 6th stage, cooling processing is carried out to the second warm area, initial temperature is 530~570 DEG C, final temperature For room temperature, rate of temperature fall is 20~25 DEG C/min；Cooling processing is carried out to the first warm area, rate of temperature fall is 20~25 DEG C/min, Final temperature is room temperature；
During aumospheric pressure cvd, without using catalyst.
The present invention is under conditions of being continually fed into nitrogen, to S and MoO3Aumospheric pressure cvd is carried out, is obtained one-dimensional MoS2Nanobelt.
In the present invention, the circulating direction of the nitrogen is to flow to MoO by S3, it is then discharged out reaction system.In the present invention In, the nitrogen plays transmission sulphur steam, makes sulphur steam and MoO as current-carrying gas3Steam contacts with each other, and then forms MoS2 Nanobelt；Meanwhile nitrogen plays the role of providing inert environments as protective gas.
In the present invention, the S and MoO3Mass ratio be preferably 28~32:1, further preferably 30:1.The present invention Size, MoO to S block3Partial size and S and MoO3Source do not specially require, using commercial goods.
In the present invention, the aumospheric pressure cvd preferably carries out in CVD tube furnace.In the present invention, the S And MoO3It is separated, the S and MoO3It is preferably disposed respectively the different warm areas of CVD tube furnace.In the present invention, the S and MoO3It is preferably positioned in different quartz boats, then will contain S and MoO3Different quartz boats be individually positioned in CVD tube furnace Different warm areas.
In the present invention, the aumospheric pressure cvd is preferably carried out in substrate surface, and the material of the substrate is preferred Including sapphire and/or silicon wafer.In the present invention, the substrate is preferably positioned at MoO3Top, the substrate and MoO3Placement Mode is as shown in Figure 1, wherein Fig. 1 a is MoO3With the top view of substrate modes of emplacement, Fig. 1 b is MoO3With substrate modes of emplacement Side view.
The present invention preferably successively uses deionized water, acetone, isopropanol and hydrogen peroxide before aumospheric pressure cvd Substrate is cleaned in ultrasonator, is then dried up substrate with spare with nitrogen gun.In the present invention, when the substrate is preferred When for sapphire substrates, the present invention is preferably according to holding MoO3Quartz boat size, along the sapphire face C, i.e. (0001) Sapphire substrates are cut into suitable size strip by face；When the substrate is preferably silicon wafer substrate, the present invention preferably basis Hold MoO3Quartz boat size, silicon wafer is cut into the shape of suitable size.
In the present invention, the aumospheric pressure cvd successively includes six stages, specially first stage, second-order Section, phase III, fourth stage, the 5th stage and the 6th stage,
In the first stage, to MoO3Heating treatment is carried out, initial temperature is room temperature, and final temperature is 280~320 DEG C, preferably 290~310 DEG C, more preferably 300 DEG C, heating rate be 13~17 DEG C/min, preferably 14~16 DEG C/min, More preferably 15 DEG C/min；Constant temperature processing is carried out to S, temperature is 78~82 DEG C, preferably 79~81 DEG C, more preferably 80 DEG C；
In the second stage, to MoO3Carry out constant temperature processing, temperature be 280~320 DEG C, preferably 290~310 DEG C, More preferably 300 DEG C；Constant temperature processing is carried out to S, temperature is 78~82 DEG C, preferably 79~81 DEG C, more preferably 80 DEG C；Institute The time for stating second stage is 28~32min, preferably 29~31min, more preferably 30min；
In the phase III, to MoO3Carry out heating treatment, initial temperature be 280~320 DEG C, preferably 290~ 310 DEG C, more preferably 300 DEG C, final temperature are 730~770 DEG C, preferably 740~760 DEG C, more preferably 750 DEG C, heating Rate is 10~15 DEG C/min, preferably 12~14 DEG C/min, more preferably 13 DEG C/min；Constant temperature processing, temperature are carried out to S It is 78~82 DEG C, preferably 79~81 DEG C, more preferably 80 DEG C；
In the fourth stage, to MoO3Carry out constant temperature processing, temperature be 730~770 DEG C, preferably 740~760 DEG C, More preferably 750 DEG C, the time is 10~14min, preferably 11~13min, more preferably 12min；In the fourth stage Preceding 5~7min, preferably 6min, to S carry out constant temperature processing, temperature be 78~82 DEG C, preferably 79~81 DEG C, more preferably 80℃；In rear 5~7min of the fourth stage, preferably 6min, heating treatment carried out to S, heating rate is 23~27 DEG C/ Min, preferably 24~26 DEG C/min, more preferably 25 DEG C/min；
In the 5th stage, cooling processing carried out to the second warm area, initial temperature is 730~770 DEG C, preferably 740 ~760 DEG C, more preferably 750 DEG C, final temperature are 530~570 DEG C, preferably 540~560 DEG C, more preferably 550 DEG C, drop Warm rate is 8~12 DEG C/min, preferably 9~11 DEG C/min, more preferably 10 DEG C/min；First warm area is carried out at constant temperature Reason, temperature are 200~250 DEG C, preferably 210~240 DEG C, more preferably 220~230 DEG C；
In the 6th stage, cooling processing carried out to the second warm area, initial temperature is 530~570 DEG C, preferably 540 ~560 DEG C, more preferably 550 DEG C, final temperature are room temperature, and rate of temperature fall is 20~25 DEG C/min, preferably 20 DEG C/min, 22 DEG C/min, 24 DEG C/min or 25 DEG C/min；Cooling processing is carried out to the first warm area, rate of temperature fall is 20~25 DEG C/min, preferably For 20 DEG C/min, 22 DEG C/min, 24 DEG C/min or 25 DEG C/min；Final temperature is room temperature.
In six stages of aumospheric pressure cvd, the nitrogen to be passed through speed preferred are as follows:
It is independently preferably 300~500cm in the speed that is passed through of the first stage and second stage, the nitrogen3/ Min, more preferably 350~450cm3/min；
It is independently preferably 25~50cm in the speed that is passed through of the phase III and fourth stage, the nitrogen3/ Min, preferably 30~45cm3/ min, more preferably 35~40cm3/min；
In the 5th stage, the speed that is passed through of the nitrogen is preferably 25~50cm3/ min, further preferably 30~ 45cm3/ min, more preferably 35~40cm3/min；
In the 6th stage, the speed that is passed through of the nitrogen is preferably 400~600cm3/ min, further preferably 450~550cm3/ min, more preferably 500cm3/min。
The present invention is respectively to S and MoO3It is heated, under the current-carrying effect of nitrogen stream, S steam and MoO3Steam contact, MoO3Steam forms gaseous MoO in the environment of S steam content few (i.e. a lack of sulfur) by S steam reduction3-x, these are gaseous MoO3-xDeposition forms MoOxS2-x, in more (i.e. sulfur-rich) environment of S steam content, MoOxS2-xIt is formed by further vulcanization MoS2。
The present invention 5~7min before the first stage, second stage, phase III and fourth stage, the temperature of S Spend lower, and MoO3Temperature it is higher so that in the process, sulphur supply is insufficient, in the case where this lack of sulfur, S steam and MoO3 Steam forms one-dimensional MoOxS2-x；It is increased in the temperature of rear 5~7min of the fourth stage, S, forms a large amount of sulfur vapors, In this sulfur-rich environment, one-dimensional MoOxS2-xIt cures to form MoS2Nanobelt, with the progress of reaction, all is one-dimensional MoOxS2-xIt cures to form one-dimensional MoS entirely2Nanobelt.MoS can be prepared in method provided by the invention2Nanobelt, and Method time-consuming provided by the invention is short, and can be completed under conditions of not using catalyst.
Below in conjunction with the embodiment in the present invention, the technical solution in the present invention is clearly and completely described.
Embodiment 1
(1) first with glass cutter by the face C (0001) sapphire along the substrate of its crystal orientation cut growth bar shaped, use deionization Water, acetone, isopropanol and hydrogen peroxide clean substrate in ultrasonator respectively, and each process time is 15min, use nitrogen Rifle dries up substrate with spare.
(2) load weighted 600mg sulphur-cake is put into No. 1 quartz boat, 20mg MoO3Powder is put into No. 2 quartz boats, by substrate It is placed in MoO3Right above powder, wherein the top of No. 2 quartz boats is not completely covered for substrate.
(3) MoO will be housed3Powder and the quartzy Noah's ark of substrate are placed in right warm area (the i.e. second temperature of dual temperature area CVD tube furnace Area), and sapphire substrates is made to be located at right warm area center, No. 1 quartz boat equipped with S block is put into left warm area (i.e. the first warm area) Center, then seal tube furnace lead to N2Make current-carrying gas and protective gas.
(4) be arranged growth procedure, right warm area with the rate of 15 DEG C/min by room temperature to 300 DEG C, nitrogen is passed through flow velocity For 400cm3/min；In 300 DEG C of holding 30min, while continuing with 400cm3The speed of/min is passed through nitrogen；Then with 13 DEG C/ The speed of min is warming up to 750 DEG C, and the speed that is passed through of nitrogen is 40cm3/min；In 750 DEG C of holding 12min, at the same continue with 40cm3The speed of/min is passed through nitrogen；Then temperature is cooled down into 20min with the cooling velocity of 10 DEG C/min, this stage nitrogen Being passed through speed is 25cm3/min；Finally being passed through speed in nitrogen is 500cm3It under the conditions of/min, is rapidly cooled to room temperature, cooling speed Rate is 25 DEG C/min；
In addition, No. 1 quartz boat containing S block to be placed in the upstream at left warm area center, left area is temperature programmed as follows: temperature 80 DEG C are always held at, the 6min after right warm area temperature reaches 750 DEG C, right warm area is just with the heating rate liter of 25 DEG C/min To 210 DEG C, 20min is kept.
The preceding 6min for being 750 DEG C in right warm area, since sulphur supply is insufficient when growth course starts, i.e., in the environment of a lack of sulfur One-dimensional MoO will be formedxS2-x, after then in left side, temperature region starts to warm up and introduces a large amount of sulfur vapors, sulfur-rich environment will be one-dimensional MoOxS2-xVulcanization is to form MoS2Nanobelt, as reaction carries out, all one-dimensional MoOxS2-xCrystal is all sulfided into one-dimensional MoS2It receives Then rice band is opened stove and is rapidly cooled to room temperature, can obtain one-dimensional highly directional MoS in substrate at this time2Nanobelt.
Embodiment 2
It is tested according to the method for embodiment 1, difference is, substrate is silicon wafer.
Performance detection
The one-dimensional highly directional MoS that embodiment 1 is obtained2Nanobelt is characterized using optical microscopy, as a result such as Fig. 2 institute Show.As shown in Figure 2, MoS2The direction of growth of nanobelt concentrates on the direction of 0 ° He ± 60 °, and the three times of display are symmetrically and MoS2It is single It is brilliant consistent.
The one-dimensional highly directional MoS that embodiment 1 is obtained2Nanobelt is characterized using atomic force microscope, as a result such as Fig. 3 It is shown.From the figure 3, it may be seen that the MoS that the present invention is prepared2The distribution of nanobelt high uniformity.
The Raman spectrum and Raman mapping for the product that embodiment 1 obtains are schemed as shown in figure 4, wherein Fig. 4 a is Raman light Spectrum, Fig. 4 b are Raman mapping figure.As shown in Figure 4, the Raman spectrum of nanobelt and nano flake has corresponding MoS in product2's Two characteristic peaks, should be the result shows that the ingredient of the nanobelt and nano flake that are prepared be MoS2；Raman mapping figure Show MoS2Nanobelt has high degree of crystallinity.
The fluorescence spectrum and fluorescence mapping for the product that embodiment 1 obtains are schemed as shown in figure 5, wherein Fig. 5 a is fluorescence light Spectrum, Fig. 5 b are fluorescence mapping figure.As shown in Figure 5, the characteristic peak of the fluorescence spectrum of nanobelt and nano flake exists in product 1.8 or so, this feature peak corresponds to MoS2Band gap, Fig. 5 can further demonstrate that the ingredient of nanobelt and nano flake is MoS2。
The one-dimensional highly directional MoS that embodiment 2 is obtained2Nanobelt is characterized using optical microscopy, as a result such as Fig. 6 institute Show.It will be appreciated from fig. 6 that MoS2The direction of growth of nanobelt concentrates on the direction of 0 ° He ± 60 °, and the three times of display are symmetrically and MoS2It is single It is brilliant consistent.
The one-dimensional highly directional MoS that embodiment 2 is obtained2Nanobelt is characterized using atomic force microscope, as a result such as Fig. 7 It is shown.As shown in Figure 7, the MoS that the present invention is prepared2The distribution of nanobelt high uniformity.
Product that embodiment 2 obtains carries out Raman Characterization, as a result as shown in figure 8, Fig. 8 include nano strip product, The Raman spectrum of laminar product and single layer molybdenum sulfide.By Fig. 8 it is found that in product nanobelt, nano flake two features Peak is corresponding with the characteristic peak of single layer molybdenum sulfide, should be the result shows that the ingredient of the nanobelt and nano flake that are prepared is MoS2。
In conclusion one-dimensional MoS can be prepared in method provided by the invention2Nanobelt, method provided by the invention It is time-consuming short, and method provided by the invention under catalyst without that can carry out.
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 (8)

1. a kind of one-dimensional MoS2The preparation method of nanobelt, comprising the following steps:
Under conditions of being continually fed into nitrogen, to S and MoO3Aumospheric pressure cvd is carried out, one-dimensional MoS is obtained2Nanobelt；
The S and MoO3Separated, the S is placed on the first warm area, the MoO3It is placed on the second warm area；
The circulating direction of the nitrogen is to flow to MoO by S3；
The aumospheric pressure cvd successively includes six stages, specially first stage, second stage, phase III, Four stages, the 5th stage and the 6th stage,
In the first stage, to MoO3Heating treatment is carried out, initial temperature is room temperature, and final temperature is 280~320 DEG C, heating Rate is 13~17 DEG C/min；Constant temperature processing is carried out to S, temperature is 78~82 DEG C；
In the second stage, to MoO3Constant temperature processing is carried out, temperature is 280~320 DEG C；Constant temperature processing is carried out to S, temperature is 78~82 DEG C；The time of the second stage is 28~32min；
In the phase III, to MoO3Heating treatment is carried out, initial temperature is 280~320 DEG C, and final temperature is 730~770 DEG C, heating rate is 10~15 DEG C/min；Constant temperature processing is carried out to S, temperature is 78~82 DEG C；
In the fourth stage, to MoO3Constant temperature processing is carried out, temperature is 730~770 DEG C, and the time is 10~14min；The 4th Preceding 5~the 7min in stage carries out constant temperature processing to S, and temperature is 78~82 DEG C, in rear 5~7min of fourth stage, is carried out to S Heating treatment, heating rate are 23~27 DEG C/min；
In the 5th stage, cooling processing is carried out to second warm area, initial temperature is 730~770 DEG C, and final temperature is 530~570 DEG C, rate of temperature fall is 8~12 DEG C/min；Constant temperature processing is carried out to first warm area, temperature is 200~250 DEG C；
In the 6th stage, cooling processing is carried out to second warm area, initial temperature is 530~570 DEG C, and final temperature is Room temperature, rate of temperature fall are 20~25 DEG C/min；Cooling processing carried out to first warm area, rate of temperature fall is 20~25 DEG C/ Min, final temperature are room temperature；
During aumospheric pressure cvd, without using catalyst.
2. preparation method according to claim 1, which is characterized in that in the first stage and second stage, the nitrogen The speed that is passed through of gas independently is 300~500cm3/min；In the phase III and fourth stage, the nitrogen is passed through speed Degree independently is 25~50cm3/min；In the 5th stage, the speed that is passed through of the nitrogen is 25~50cm3/min；Institute Stated for the 6th stage, the speed that is passed through of the nitrogen is 400~600cm3/min。
3. preparation method according to claim 1, which is characterized in that the S and MoO3Mass ratio be 28~32:1.
4. preparation method according to claim 1 or 3, which is characterized in that the S is provided in the form of S block；The MoO3 With MoO3The form of powder provides.
5. preparation method according to claim 1 or 3, which is characterized in that the aumospheric pressure cvd is in substrate table Face carries out, and the substrate is placed on MoO3Top.
6. preparation method according to claim 5, which is characterized in that the material of the substrate includes sapphire and/or silicon Piece.
7. preparation method according to claim 1, which is characterized in that the aumospheric pressure cvd is in CVD tube furnace Middle progress, the S and MoO3It is individually positioned in the different warm areas of CVD tube furnace.
8. preparation method according to claim 1, which is characterized in that six stages of the aumospheric pressure cvd according to It is secondary are as follows:
In the first stage, to MoO3Heating treatment is carried out, initial temperature is room temperature, and final temperature is 300 DEG C, heating rate For 15 DEG C/min；Constant temperature processing is carried out to S, temperature is 80 DEG C；
In the second stage, to MoO3Constant temperature processing is carried out, temperature is 300 DEG C；Constant temperature processing is carried out to S, temperature is 80 DEG C； The time of second stage is 30min；
In the phase III, to MoO3Heating treatment is carried out, initial temperature is 300 DEG C, and final temperature is 750 DEG C, heating rate For 13 DEG C/min；Constant temperature processing is carried out to S, temperature is 80 DEG C；
In the fourth stage, to MoO3Constant temperature processing is carried out, temperature is 750 DEG C, time 12min；Before fourth stage 6min carries out constant temperature processing to S, and temperature is 80 DEG C, in the rear 6min of fourth stage, carries out heating treatment to S, heating rate is 25℃/min；
In the 5th stage, cooling processing is carried out to the second warm area, initial temperature is 750 DEG C, and final temperature is 550 DEG C, drop Warm rate is 10 DEG C/min；Constant temperature processing is carried out to the first warm area, temperature is 230 DEG C；
In the 6th stage, cooling processing is carried out to the second warm area, initial temperature is 550 DEG C, and final temperature is room temperature, cooling Rate is 25 DEG C/min；Cooling processing is carried out to the first warm area, rate of temperature fall is 25 DEG C/min, and final temperature is room temperature.
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