CN104386753A - Method for preparing molybdenum disulfide nanotube - Google Patents

Method for preparing molybdenum disulfide nanotube Download PDF

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CN104386753A
CN104386753A CN201410676448.5A CN201410676448A CN104386753A CN 104386753 A CN104386753 A CN 104386753A CN 201410676448 A CN201410676448 A CN 201410676448A CN 104386753 A CN104386753 A CN 104386753A
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nanotube
mos2
mos
molybdenum disulfide
carbon
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CN104386753B (en
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凤仪
刘文宏
钱刚
苗世顶
豆亚坤
黄晓晨
丁冬冬
汤海
张学斌
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Hefei University of Technology
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Hefei University of Technology
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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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • 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
    • C01P2004/13—Nanotubes

Abstract

The invention discloses a method for preparing a molybdenum-disulfide (MoS2) nanotube. The method is characterized by comprising the following steps of preparing a C-MoS2 coaxial nanotube wrapped by homogeneous MoS2 by taking a fibrous carbon (C) nanomaterial as a template, and calcining the C-MoS2 coaxial nanotube at a high temperature in a flowing CO2 atmosphere to remove C to obtain the MoS2 nanotube. The thickness of the wall of the MoS2 nanotube prepared by adopting the method can be controlled by changing the thickness of the MoS2 wrapping layer in the C-MoS2 coaxial nanotube. Because the raised surface or sharply bent part of the fibrous C nanomaterial can not be totally wrapped by MoS2, the prepared MoS2 nanotube has structure defects correspondingly, but the number of active spots on the edge of the MoS2 nanotube can be increased due to the structure defects so that the MoS2 nanotube has excellent optical and catalytic properties.

Description

A kind of preparation method of molybdenum disulfide nano tube
One, technical field
The present invention relates to a kind of preparation method of molybdenum disulfide nano tube.
Two, background technology
Molybdenumdisulphide is the lamellar compound of class Graphene, its structural unit is made up of three layers of atom, namely each Mo (IV) atom is in the center of triangular prism, and with six sulphur atom coordinations, sulphur atom layer is distributed in the both sides of Mo atomic shell with covalent bonds, forms the laminate structure being similar to sandwich.Unique laminate structure makes it can form the nanostructure of many novelties, Van der Waals force as faint in interlayer makes it be easy to be stripped into monodispersed multilayer even individual layer nanometer sheet, the inside of these nanometer sheet and the atomic bonding-valence at edge are different, inner atom is saturated, and the atom at edge is undersaturated, form dangling bonds, i.e. edge active position, in addition, thin layer molybdenumdisulphide is also very soft, be easy to bend, therefore the impact by external environment is easy to, its edge active position is cross-linked with each other and is formed stable and there is nano particle or the nanotube of fullerene structure.
In various configurations, MoS 2nanotube progressively receives the concern of scholar because of its potential application, and alumina formwork method can prepare MoS 2the array of nanotube, (Dongbo Yu, et al., Materials Research Bulletin 46 (2011) 1504-1509) but earning rate is too little, is difficult to apply on a large scale.The conversion method (Sifei Zhuo, et al., AngewandteChemie International Edition 125 (2013) 8764-8768) of presoma nano wire and C 60catalysis method (Maja Remskar et al., Science292 (2001) 479-481) also can prepare molybdenum disulfide nano tube, but these methods are also not suitable for preparing bending nanotube, and the wall thickness of nanotube is also difficult to control.Therefore, need a kind of method developing simple environmental protection to prepare the molybdenum disulfide nano tube of structure-controllable on a large scale.
Three, summary of the invention
The present invention is the weak point for avoiding existing for above-mentioned prior art, provides a kind of preparation method of molybdenum disulfide nano tube, and the technical barrier that overcome is the CO in flowing 2c-MoS is removed in atmosphere at high temperature calcining 2carbon component in Coaxial Nanotubes, obtains molybdenum disulfide nano tube
Technical solution problem of the present invention, adopts following technical scheme:
The preparation method of molybdenum disulfide nano tube of the present invention, its feature is: take fibrous carbon nanomaterials as template, obtains the C-MoS that the molybdenumdisulphide of homogeneous is coated 2coaxial Nanotubes; Then at the CO of flowing 2atmosphere at high temperature calcines the coated C-MoS of the molybdenumdisulphide of described homogeneous 2coaxial Nanotubes, to remove carbon component, obtains molybdenum disulfide nano tube;
Described CO 2purity be 80-100%, flow velocity is 1-10000mL/min;
The calcining temperature of described high-temperature calcination is 600 DEG C ~ 1500 DEG C, and calcination time is 1h ~ 96h.
The preparation method of molybdenum disulfide nano tube of the present invention, its feature is also: described fibrous carbon nanomaterials is carbon nanotube, carbon nano fiber, carbon nano wire, carbon containing polymer nano-wire or carbon containing macromolecule nano-tube.
The wall thickness of described molybdenum disulfide nano tube can by changing C-MoS 2moS in Coaxial Nanotubes 2coating thickness controls.
The C-MoS that in raw material of the present invention, the molybdenumdisulphide of homogeneous is coated 2co-axial nano tube preparation method is:
Molybdate (ammonium molybdate or Sodium orthomolybdate) is dissolved in distilled water, the ammoniacal liquor adding sulfide (sodium sulphite or ammonium sulfide) and mass concentration 28-30% reacts 2 hours at 50-90 DEG C, in 2-10 DEG C of standing crystallization 48 hours after reaction terminates, filter and Air drying, obtain four thio ammonium molybdate crystal.Polyoxyethylene glycol (PEG400) and four thio ammonium molybdate are dissolved in distilled water, add fibrous carbon nanomaterials again, ultrasonic disperse 1h, through centrifugal, washing and 60 DEG C of dryings after, namely obtain the C-MoS that the molybdenumdisulphide of homogeneous is coated after calcining 2h under 850 DEG C of hydrogen atmospheres 2coaxial Nanotubes.
The concrete preparation process of the present invention is as follows:
1, the preparation of four thio ammonium molybdate: molybdate is dissolved in the water, the ammoniacal liquor adding sulfide and mass concentration 28-30% reacts 2 hours at 50-90 DEG C, in 2-10 DEG C of standing crystallization 48 hours after reaction terminates, filters, Air drying, obtains four thio ammonium molybdate crystal; (preparation method is shown in patent application 200410039454.6)
2, the C-MoS that the molybdenumdisulphide of homogeneous is coated 2the preparation of Coaxial Nanotubes: polyoxyethylene glycol (PEG400) and four thio ammonium molybdate are dissolved in distilled water, add fibrous carbon nanomaterials again, ultrasonic disperse 1h, through centrifugal, washing after and after 60 DEG C of dryings, namely obtain the C-MoS that the molybdenumdisulphide of homogeneous is coated after calcining 2h under 850 DEG C of hydrogen atmospheres 2coaxial Nanotubes.(preparation method is shown in: Liu Wenhong et al., Electrochimica Acta 144 (2014) 119 – 126)
3, MoS 2the preparation of nanotube: by C-MoS coated for the molybdenumdisulphide of homogeneous 2coaxial Nanotubes puts into tube furnace, and in carbon dioxide atmosphere, this mixture of high-temperature calcination is to remove carbon template, namely obtains MoS 2nanotube.MoS 2the thickness of pipe of nanotube can by changing MoS 2coating thickness controls.
Compared with prior art, the invention has the advantages that:
1, the present invention is by the coated C-MoS of high-temperature calcination molybdenumdisulphide under carbon dioxide atmosphere 2coaxial Nanotubes, thus obtain molybdenum disulfide nano tube, the method environmental protection, can avoid the generation of waste water, it also avoid loaded down with trivial details last handling process;
2, the present invention finds under study for action, in fibrous carbon nanomaterials protrusion of surface or bending place, molybdenumdisulphide is coated there will be defect, the molybdenum disulfide nano tube formed thus also has many textural defect, these defects make it form more multiple edge active sites, have potential photoelectricity and catalytic performance;
The wall thickness of the molybdenum disulfide nano tube 3, prepared by the present invention can by changing MoS 2the thickness of coating layer controls, and preparation method is flexible and changeable.
Four, accompanying drawing explanation
Fig. 1 is the TEM figure of the embodiment of the present invention 1 gained molybdenum disulfide nano tube;
Fig. 2 is the HRTEM figure of the dissimilar indentation, there of the embodiment of the present invention 1 gained molybdenum disulfide nano tube, and wherein (a) is complete breach, and (b) is incomplete breach;
Fig. 3 is the XRD figure of the embodiment of the present invention 1 gained molybdenum disulfide nano tube;
Fig. 4 is the HRTEM figure of the molybdenum disulfide nano tube of the embodiment of the present invention 2 and embodiment 3 gained different wall, and wherein (a) is about the nanotube of 5nm for embodiment 2 gained thickness of pipe; B () is about the nanotube of 18nm for embodiment 3 gained thickness of pipe.
Five, embodiment
Embodiment 1:
The present embodiment prepares molybdenum disulfide nano tube as follows:
5g ammonium molybdate is dissolved in distilled water, add the ammoniacal liquor of 40mL ammonium sulfide solution and 20mL mass concentration 28-29%, react 2 hours at 60-70 DEG C, in 2-10 DEG C of standing crystallization 48 hours after reaction terminates, filter and Air drying, obtain four thio ammonium molybdate crystal;
3g four thio ammonium molybdate crystal and 2mL polyoxyethylene glycol are dissolved in 50mL distilled water successively and obtain mixed solution; then 0.5g carbon nanotube is added; ultrasonic disperse is centrifugal after 1 hour; use distilled water and absolute ethanol washing successively and in 60 DEG C of dryings; then calcine 2 hours in 850 DEG C under hydrogen shield, after being cooled to room temperature, obtain the C-MoS that the molybdenumdisulphide of homogeneous is coated 2coaxial Nanotubes.
By C-MoS coated for the molybdenumdisulphide of 2g homogeneous 2coaxial Nanotubes puts into tube furnace, is in the carbon dioxide atmosphere of 60mL/min at flow velocity, and 850 DEG C of calcining 20h, namely obtain MoS 2nanotube.
MoS prepared by the present embodiment 2respectively as depicted in figs. 1 and 2, as can be seen from the figure, nanotube is bending to TEM and the HRTEM figure of nanotube, and the breach that existence two kinds is different.Prepared MoS 2the XRD of nanotube is as shown in Figure 3, visible, and this nanotube is 2H type molybdenumdisulphide.
Embodiment 2:
The present embodiment prepares molybdenum disulfide nano tube as follows:
5g ammonium molybdate is dissolved in distilled water, add the ammoniacal liquor of 40mL ammonium sulfide solution and 20mL mass concentration 28-29%, react 2 hours at 60-70 DEG C, in 2-10 DEG C of standing crystallization 48 hours after reaction terminates, filter and Air drying, obtain four thio ammonium molybdate crystal;
0.5g four thio ammonium molybdate crystal and 2mL polyoxyethylene glycol are dissolved in 50mL water successively and obtain mixed solution; then 0.5g carbon nano fiber is added; ultrasonic disperse is centrifugal after 1 hour; use distilled water and absolute ethanol washing successively and in 60 DEG C of dryings; then calcine 2 hours in 850 DEG C under hydrogen shield, after being cooled to room temperature, obtain the C-MoS that the molybdenumdisulphide of homogeneous is coated 2coaxial Nanotubes.
By C-MoS coated for the molybdenumdisulphide of 4g homogeneous 2coaxial Nanotubes puts into tube furnace, is in the carbon dioxide atmosphere of 100mL/min at flow velocity, and 900 DEG C of calcining 85h, namely obtain MoS 2nanotube, its HRTEM is as shown in Fig. 4 (a), and as can be seen from the figure, the wall thickness of prepared molybdenum disulfide nano tube is 5nm.
Embodiment 3:
The present embodiment prepares molybdenum disulfide nano tube as follows:
5g ammonium molybdate is dissolved in distilled water, add the ammoniacal liquor of 40mL ammonium sulfide solution and 20mL mass concentration 28-29%, react 2 hours at 60-70 DEG C, in 2-10 DEG C of standing crystallization 48 hours after reaction terminates, filter and Air drying, obtain four thio ammonium molybdate crystal;
3g four thio ammonium molybdate crystal and 2mL polyoxyethylene glycol are dissolved in 50mL water successively and obtain mixed solution; then 0.5g carbon nano wire is added; ultrasonic disperse is centrifugal after 1 hour; use distilled water and absolute ethanol washing successively and in 60 DEG C of dryings; then calcine 2 hours in 850 DEG C under hydrogen shield, after being cooled to room temperature, obtain the C-MoS that the molybdenumdisulphide of homogeneous is coated 2coaxial Nanotubes.
By C-MoS coated for the molybdenumdisulphide of 4g homogeneous 2coaxial Nanotubes puts into tube furnace, is in the carbon dioxide atmosphere of 100mL/min at flow velocity, and 750 DEG C of calcining 86h, namely obtain MoS 2nanotube, its HRTEM is as shown in Fig. 4 (b), and as can be seen from the figure, the wall thickness of prepared molybdenum disulfide nano tube is 18nm.
Comparative example 2 and embodiment 3 known, the wall thickness of gained molybdenum disulfide nano tube of the present invention can by changing C-MoS 2moS in Coaxial Nanotubes 2coating thickness controls.
Embodiment 4:
The present embodiment prepares molybdenum disulfide nano tube as follows:
5g ammonium molybdate is dissolved in distilled water, add the ammoniacal liquor of 40mL ammonium sulfide solution and 20mL mass concentration 28-29%, react 2 hours at 60-70 DEG C, in 2-10 DEG C of standing crystallization 48 hours after reaction terminates, filter and Air drying, obtain four thio ammonium molybdate crystal;
3g four thio ammonium molybdate crystal and 2mL polyoxyethylene glycol are dissolved in 50mL water successively and obtain mixed solution; then 0.5g carbon nanotube is added; ultrasonic disperse is centrifugal after 1 hour; use distilled water and absolute ethanol washing successively and in 60 DEG C of dryings; then calcine 2 hours in 850 DEG C under hydrogen shield, after being cooled to room temperature, obtain the C-MoS that the molybdenumdisulphide of homogeneous is coated 2coaxial Nanotubes.
By C-MoS coated for the molybdenumdisulphide of 8g homogeneous 2coaxial Nanotubes puts into tube furnace, is in the carbon dioxide atmosphere of 10000mL/min at flow velocity, and 700 DEG C of calcining 46h, namely obtain MoS 2nanotube.

Claims (3)

1. a preparation method for molybdenum disulfide nano tube, is characterized in that: take fibrous carbon nanomaterials as template, obtains the C-MoS that the molybdenumdisulphide of homogeneous is coated 2coaxial Nanotubes; Then at the CO of flowing 2atmosphere at high temperature calcines the coated C-MoS of the molybdenumdisulphide of described homogeneous 2coaxial Nanotubes, to remove carbon component, obtains molybdenum disulfide nano tube;
Described CO 2purity be 80-100%, flow velocity is 1-10000mL/min;
The calcining temperature of described high-temperature calcination is 600 DEG C ~ 1500 DEG C, and calcination time is 1h ~ 96h.
2. preparation method according to claim 1, is characterized in that: described fibrous carbon nanomaterials is carbon nanotube, carbon nano fiber, carbon nano wire, carbon containing polymer nano-wire or carbon containing macromolecule nano-tube.
3. preparation method according to claim 1, is characterized in that: the wall thickness of described molybdenum disulfide nano tube can by changing C-MoS 2moS in Coaxial Nanotubes 2coating thickness controls.
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Cited By (8)

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CN104900867A (en) * 2015-05-25 2015-09-09 哈尔滨工业大学 Preparation method of CNT/Co/MoS2 composite material
CN105645471A (en) * 2016-04-08 2016-06-08 合肥工业大学 Method for preparing molybdenum disulfide nanotubes by vulcanizing nano fibrous polymolybdic acid material
CN106145190A (en) * 2016-06-15 2016-11-23 南开大学 The preparation method of a kind of molybdenum disulfide nano tube and the application in lithium ion battery thereof
CN106206034A (en) * 2016-07-01 2016-12-07 南京清辉新能源有限公司 A kind of multifunctional electrodes for Line of light electric flux device and preparation method thereof
CN106964362A (en) * 2017-04-10 2017-07-21 中国科学技术大学 Metal molybdate/carbon composite nano-fiber and preparation method thereof and composite and its application
CN108103766A (en) * 2017-12-29 2018-06-01 成都新柯力化工科技有限公司 A kind of molybdenum disulfide composite fibre photochemical catalyst and preparation method for sewage disposal
CN108745380A (en) * 2018-06-28 2018-11-06 合肥工业大学 A kind of preparation method carrying silver-colored molybdenum disulfide nano tube composite electro catalytic liberation of hydrogen material
CN109256546A (en) * 2018-09-03 2019-01-22 山西煤炭进出口集团科学技术研究院有限公司 A kind of molybdenum disulfide/graphene composite material and its preparation method and application

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104900867A (en) * 2015-05-25 2015-09-09 哈尔滨工业大学 Preparation method of CNT/Co/MoS2 composite material
CN104900867B (en) * 2015-05-25 2017-04-12 哈尔滨工业大学 Preparation method of CNT/Co/MoS2 composite material
CN105645471A (en) * 2016-04-08 2016-06-08 合肥工业大学 Method for preparing molybdenum disulfide nanotubes by vulcanizing nano fibrous polymolybdic acid material
CN105645471B (en) * 2016-04-08 2017-10-03 合肥工业大学 A kind of method that nanometer fibrous poly- molybdic acid class material cures prepare molybdenum disulfide nano tube
CN106145190A (en) * 2016-06-15 2016-11-23 南开大学 The preparation method of a kind of molybdenum disulfide nano tube and the application in lithium ion battery thereof
CN106206034A (en) * 2016-07-01 2016-12-07 南京清辉新能源有限公司 A kind of multifunctional electrodes for Line of light electric flux device and preparation method thereof
CN106964362A (en) * 2017-04-10 2017-07-21 中国科学技术大学 Metal molybdate/carbon composite nano-fiber and preparation method thereof and composite and its application
CN108103766A (en) * 2017-12-29 2018-06-01 成都新柯力化工科技有限公司 A kind of molybdenum disulfide composite fibre photochemical catalyst and preparation method for sewage disposal
CN108103766B (en) * 2017-12-29 2021-07-30 澄江市力点科技有限公司 Molybdenum disulfide composite fiber photocatalyst for sewage treatment and preparation method thereof
CN108745380A (en) * 2018-06-28 2018-11-06 合肥工业大学 A kind of preparation method carrying silver-colored molybdenum disulfide nano tube composite electro catalytic liberation of hydrogen material
CN109256546A (en) * 2018-09-03 2019-01-22 山西煤炭进出口集团科学技术研究院有限公司 A kind of molybdenum disulfide/graphene composite material and its preparation method and application

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