CN101880061A - Method for preparing inorganic fullerene molybdenum disulphide - Google Patents

Method for preparing inorganic fullerene molybdenum disulphide Download PDF

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CN101880061A
CN101880061A CN2009101382623A CN200910138262A CN101880061A CN 101880061 A CN101880061 A CN 101880061A CN 2009101382623 A CN2009101382623 A CN 2009101382623A CN 200910138262 A CN200910138262 A CN 200910138262A CN 101880061 A CN101880061 A CN 101880061A
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hexanaphthene
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mos
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王齐华
张俊鹏
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Lanzhou Institute of Chemical Physics LICP of CAS
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Lanzhou Institute of Chemical Physics LICP of CAS
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Abstract

The invention discloses a method for preparing inorganic fullerene molybdenum disulphide. In the method, a precursor MoS3 is prepared by a micro emulsion method and then subjected to heat treatment in an atmosphere of N2 and H2 to form the inorganic fullerene molybdenum disulphide. By characterization of a HRTEM (high-resolution transmission electron microscope), the prepared molybdenum disulphide has a fullerene structure, and the average grain size is about 100 nanometers.

Description

A kind of preparation method of inorganic fullerene molybdenum disulphide
Technical field
The present invention relates to a kind of preparation method of inorganic fullerene molybdenum disulphide.
Background technology
Molybdenumdisulphide has a wide range of applications in solid lubrication and lubricating oil additive as a kind of typical laminate structure, and experiment shows that nano level molybdenumdisulphide has excellent lubricating properties more than micron-sized molybdenumdisulphide.But because the molybdenumdisulphide of nano lamellar has a large amount of edge dangling bonds, easily oxidized under oxygen enrichment and hot environment, limited its application.(inorganic fullerene-like, IF) molybdenumdisulphide has enclosed construction to the inorganic fullerene shape, so its chemical stability is higher, and can introduce rolling resistance mechanism, has excellent lubricating property more.
IF-MoS 2The preparation method mainly contain gas-phase reaction method, laser splash method, electron irradiation method, solution method etc.Adopt gas-phase fluidized bed technology to produce IF-MoS 2Its output is limited.
At present, Chinese invention patent publication number CN1752020A discloses and has added polyoxyethylene glycol (PEG) in the employing solution and prepare precursor MoS as dispersion agent 3, in argon gas atmosphere, prepare the method for IF-MoS2 then with the hydrogen desulfurization; Also there is the dry ammonium thiomolybdate solution of the spray-drying process of employing to obtain precursor MoS 3(CN1752023), thermal treatment prepares IF-MoS then 2But adopt microemulsion method to prepare presoma MoS3, then at N 2/ H 2Thermal treatment prepares IF-MoS in the atmosphere 2Method do not appear in the newspapers as yet.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of inorganic fullerene molybdenum disulphide.
The present invention adopts microemulsion method to prepare presoma MoS 3, then at N 2And H 2In the atmosphere to presoma MoS 3Heat-treat preparation IF-MoS 2
A kind of preparation method of inorganic fullerene molybdenum disulphide is characterized in that this method may further comprise the steps:
A, preparation contain the water solution A of Sodium orthomolybdate and thioacetamide, preparation contains the mixture B of Value 3608 (TX-10), cetyl trimethylammonium bromide (CTAB), hexanaphthene and n-hexyl alcohol, A is joined among the B, stir and form microemulsion;
B, in microemulsion, add micro-formic acid, become scarlet to liquid, reacted under the room temperature 8～14 hours.By centrifugal, separate obtaining precursor MoS 3Throw out through washing and vacuum drying treatment, obtains precursor MoS again 3Powder;
C, with precursor MoS 3Powder is at 500～1000 ℃ N 2And H 2Thermal treatment is 30～300 minutes in the atmosphere, obtains inorganic fullerene molybdenum disulphide.
In step a, the concentration of Sodium orthomolybdate is 0.01～0.07mol/L in the water solution A, and the concentration of thioacetamide is 0.042～0.294mol/L.
In step a, the mol ratio of Value 3608 and cetyl trimethylammonium bromide is 10: 1～3 among the mixture B, the mol ratio of n-hexyl alcohol and Value 3608 is 10: 1～4, and the mol ratio of Value 3608 and hexanaphthene is 1～5: 100.
In step a, the volume ratio of water solution A and hexanaphthene is 0.25～2.5: 10.
N in step c 2With H 2Volume ratio be 9: 1.
The presoma MoS of the present invention's preparation 3With respect to the MoS for preparing in the aqueous solution 3Have following characteristics:
Its particle diameter is between 10～100 nanometers, and the surface is coated with tensio-active agent; Characterize the sphere that MoS3 is a rule through transmission electron microscope, present monodispersity.Characterize through high-resolution-ration transmission electric-lens, the molybdenumdisulphide that makes has fullerene structure, and median size is about 100 nanometers.
Embodiment
Embodiment 1: preparation contains the water solution A of Sodium orthomolybdate and thioacetamide, and the concentration of Sodium orthomolybdate is 0.01mol/L, and the concentration of thioacetamide is 0.042mol/L.Preparation contains cetyl trimethylammonium bromide (CTAB), Value 3608 (TX-10), n-hexyl alcohol, the mixture B of hexanaphthene, wherein cetyl trimethylammonium bromide is 0.4657g, Value 3608 is 4.657g, and n-hexyl alcohol is 3.105g, and hexanaphthene is 20ml.Mixture B was stirred 30 minutes.The water solution A of 1ml is joined among the mixture B, stirred 30 minutes, form microemulsion.In above-mentioned microemulsion, add micro-formic acid, become scarlet to liquid, reacted 8 hours.By centrifugal, separate obtaining precursor MoS 3Throw out, again through washing, and vacuum drying treatment, obtain precursor MoS 3Powder.With precursor MoS 3Powder is at 600 ℃ N 2/ H 2Thermal treatment is 60 minutes in (9: 1) atmosphere, obtains inorganic fullerene molybdenum disulphide.
Embodiment 2: preparation contains the water solution A of Sodium orthomolybdate and thioacetamide, and the concentration of Sodium orthomolybdate is 0.03mol/L, and the concentration of thioacetamide is 0.126mol/L.Preparation Value 3608 (TX-10), cetyl trimethylammonium bromide (CTAB), hexanaphthene, the mixture B of n-hexyl alcohol, wherein cetyl trimethylammonium bromide is 0.4657g, Value 3608 is 4.657g, n-hexyl alcohol is 3.105g, and hexanaphthene is 20ml.Mixture B was stirred 30 minutes.Among the mixture B that the water solution A of 1ml is joined, stirred 30 minutes, form microemulsion.In above-mentioned microemulsion, add micro-formic acid, become scarlet to liquid, reacted 8 hours.By centrifugal, separate obtaining precursor MoS 3Throw out, again through washing, and vacuum drying treatment, obtain precursor MoS 3Powder.With precursor MoS 3Powder is at 600 ℃ N 2/ H 2Thermal treatment is 60 minutes in (9: 1) atmosphere, obtains inorganic fullerene molybdenum disulphide.
Embodiment 3: preparation contains the water solution A of Sodium orthomolybdate and thioacetamide, and the concentration of Sodium orthomolybdate is 0.07mol/L, and the concentration of thioacetamide is 0.294mol/L.Preparation Value 3608 (TX-10), cetyl trimethylammonium bromide (CTAB), hexanaphthene, the mixture B of n-hexyl alcohol, wherein cetyl trimethylammonium bromide is 0.4657g, Value 3608 is 4.657g, n-hexyl alcohol is 3.105g, and hexanaphthene is 20ml.Mixture B was stirred 30 minutes.The water solution A of 1ml is joined among the mixture B, stirred 30 minutes, form microemulsion.In above-mentioned microemulsion, add micro-formic acid, become scarlet to liquid, reacted 8 hours.By centrifugal, separate obtaining precursor MoS 3Throw out, again through washing, and vacuum drying treatment, obtain precursor MoS 3Powder.With precursor MoS 3Powder is at 600 ℃ N 2/ H 2Thermal treatment is 60 minutes in (9: 1) atmosphere, obtains inorganic fullerene molybdenum disulphide.
Embodiment 4: preparation contains the water solution A of Sodium orthomolybdate and thioacetamide, and the concentration of Sodium orthomolybdate is 0.03mol/L, and the concentration of thioacetamide is 0.126mol/L.Preparation Value 3608 (TX-10), cetyl trimethylammonium bromide (CTAB), hexanaphthene, the mixture B of n-hexyl alcohol, wherein cetyl trimethylammonium bromide is 0.9314g, Value 3608 is 4.657g, n-hexyl alcohol is 3.105g, and hexanaphthene is 20ml.Mixture B was stirred 30 minutes.The water solution A of 1ml is joined among the mixture B, stirred 30 minutes, form microemulsion.In above-mentioned microemulsion, add micro-formic acid, become scarlet to liquid, reacted 8 hours.By centrifugal, separate obtaining precursor MoS 3Throw out, again through washing, and vacuum drying treatment, obtain precursor MoS3 powder.With the N of precursor MoS3 powder at 600 ℃ 2/ H 2Thermal treatment is 60 minutes in (9: 1) atmosphere, obtains inorganic fullerene molybdenum disulphide.
Embodiment 5: preparation contains the water solution A of Sodium orthomolybdate and thioacetamide, and the concentration of Sodium orthomolybdate is 0.03mol/L, and the concentration of thioacetamide is 0.126mol/L.Preparation Value 3608 (TX-10), cetyl trimethylammonium bromide (CTAB), hexanaphthene, the mixture B of n-hexyl alcohol, wherein cetyl trimethylammonium bromide is 1.3971g, Value 3608 is 4.657g, n-hexyl alcohol is 3.105g, and hexanaphthene is 20ml.Mixture B was stirred 30 minutes.The water solution A of 1ml is joined among the mixture B, stirred 30 minutes, form microemulsion.In above-mentioned microemulsion, add micro-formic acid, become scarlet to liquid, reacted 8 hours.By centrifugal, separate obtaining precursor MoS 3Throw out, again through washing, and vacuum drying treatment, obtain precursor MoS 3Powder.With precursor MoS 3Powder is at 600 ℃ N 2/ H 2Thermal treatment is 60 minutes in (9: 1) atmosphere, obtains inorganic fullerene molybdenum disulphide.
Embodiment 6: preparation contains the water solution A of Sodium orthomolybdate and thioacetamide, and the concentration of Sodium orthomolybdate is 0.03mol/L, and the concentration of thioacetamide is 0.126mol/L.Preparation Value 3608 (TX-10), cetyl trimethylammonium bromide (CTAB), hexanaphthene, the mixture B of n-hexyl alcohol, wherein cetyl trimethylammonium bromide is 0.4657g, Value 3608 is 4.657g, n-hexyl alcohol is 3.105g, and hexanaphthene is 20ml.Mixture B was stirred 30 minutes.The water solution A of 2ml is joined among the mixture B, stirred 30 minutes, form microemulsion.In above-mentioned microemulsion, add micro-formic acid, become scarlet to liquid, reacted 8 hours.By centrifugal, separate obtaining precursor MoS 3Throw out, again through washing, and vacuum drying treatment, obtain precursor MoS 3Powder.With precursor MoS 3Powder is at 600 ℃ N 2/ H 2Thermal treatment is 60 minutes in (9: 1) atmosphere, obtains inorganic fullerene molybdenum disulphide.
Embodiment 7: preparation contains the water solution A of Sodium orthomolybdate and thioacetamide, and the concentration of Sodium orthomolybdate is 0.03mol/L, and the concentration of thioacetamide is 0.126mol/L.Preparation Value 3608 (TX-10), cetyl trimethylammonium bromide (CTAB), hexanaphthene, the mixture B of n-hexyl alcohol, wherein cetyl trimethylammonium bromide is 0.4657g, Value 3608 is 4.657g, n-hexyl alcohol is 3.105g, and hexanaphthene is 20ml.Mixture B was stirred 30 minutes.The water solution A of 3ml is joined among the mixture B, stirred 30 minutes, form microemulsion.In above-mentioned microemulsion, add micro-formic acid, become scarlet to liquid, reacted 8 hours.By centrifugal, separate obtaining precursor MoS 3Throw out, again through washing, and vacuum drying treatment, obtain precursor MoS 3Powder.With precursor MoS 3Powder is at 600 ℃ N 2/ H 2Thermal treatment is 60 minutes in (9: 1) atmosphere, obtains inorganic fullerene molybdenum disulphide.
Embodiment 8: preparation contains the water solution A of Sodium orthomolybdate and thioacetamide, and the concentration of Sodium orthomolybdate is 0.01mol/L, and the concentration of thioacetamide is 0.042mol/L.Preparation Value 3608 (TX-10), cetyl trimethylammonium bromide (CTAB), hexanaphthene, the mixture B of n-hexyl alcohol, wherein cetyl trimethylammonium bromide is 0.4657g, Value 3608 is 4.657g, n-hexyl alcohol is 4.657g, and hexanaphthene is 20ml.Mixture B was stirred 30 minutes.The water solution A of 3ml is joined among the mixture B, stirred 30 minutes, form microemulsion.In above-mentioned microemulsion, add micro-formic acid, become scarlet to liquid, reacted 8 hours.By centrifugal, separate obtaining precursor MoS 3Throw out, again through washing, and vacuum drying treatment, obtain precursor MoS 3Powder.With precursor MoS 3Powder is at 600 ℃ N 2/ H 2Thermal treatment is 60 minutes in (9: 1) atmosphere, obtains inorganic fullerene molybdenum disulphide.
Embodiment 9: preparation contains the water solution A of Sodium orthomolybdate and thioacetamide, and the concentration of Sodium orthomolybdate is 0.03mol/L, and the concentration of thioacetamide is 0.126mol/L.Preparation Value 3608 (TX-10), cetyl trimethylammonium bromide (CTAB), hexanaphthene, the mixture B of n-hexyl alcohol, wherein cetyl trimethylammonium bromide is 0.4657g, Value 3608 is 4.657g, n-hexyl alcohol is 3.105g, and hexanaphthene is 30ml.Mixture B was stirred 30 minutes.The water solution A of 3ml is joined among the mixture B, stirred 30 minutes, form microemulsion.In above-mentioned microemulsion, add micro-formic acid, become scarlet to liquid, reacted 8 hours.By centrifugal, separate obtaining precursor MoS 3Throw out, again through washing, and vacuum drying treatment, obtain precursor MoS 3Powder.With precursor MoS 3Powder is at 600 ℃ N 2/ H 2Thermal treatment is 60 minutes in (9: 1) atmosphere, obtains inorganic fullerene molybdenum disulphide.
Embodiment 10: preparation contains the water solution A of Sodium orthomolybdate and thioacetamide, and the concentration of Sodium orthomolybdate is 0.03mol/L, and the concentration of thioacetamide is 0.124mol/L.Preparation Value 3608 (TX-10), cetyl trimethylammonium bromide (CTAB), hexanaphthene, the mixture B of n-hexyl alcohol, wherein cetyl trimethylammonium bromide is 0.4657g, Value 3608 is 4.657g, n-hexyl alcohol is 3.105g, and hexanaphthene is 20ml.Said mixture was stirred 30 minutes.The water solution A of 3ml is joined among the mixture B, stirred 30 minutes, form microemulsion.In above-mentioned microemulsion, add micro-formic acid, become scarlet to liquid, reacted 10 hours.By centrifugal, separate obtaining precursor MoS 3Throw out, again through washing, and vacuum drying treatment, obtain precursor MoS 3Powder.With precursor MoS 3Powder is at 600 ℃ N 2/ H 2Thermal treatment is 60 minutes in (9: 1) atmosphere, obtains inorganic fullerene molybdenum disulphide.
Embodiment 11: preparation contains the water solution A of Sodium orthomolybdate and thioacetamide, and the concentration of Sodium orthomolybdate is 0.03mol/L, and the concentration of thioacetamide is 0.126mol/L.Preparation Value 3608 (TX-10), cetyl trimethylammonium bromide (CTAB), hexanaphthene, the mixture B of n-hexyl alcohol, wherein cetyl trimethylammonium bromide is 0.4657g, Value 3608 is 4.657g, n-hexyl alcohol is 3.105g, and hexanaphthene is 20ml.Said mixture was stirred 30 minutes.The water solution A of 3ml is joined among the mixture B, stirred 30 minutes, form microemulsion.In above-mentioned microemulsion, add micro-formic acid, become scarlet to liquid, reacted 12 hours.By centrifugal, separate obtaining precursor MoS 3Throw out, again through washing, and vacuum drying treatment, obtain precursor MoS 3Powder.With precursor MoS 3Powder is at 600 ℃ N 2/ H 2Thermal treatment is 60 minutes in (9: 1) atmosphere, obtains inorganic fullerene molybdenum disulphide.
Embodiment 12: preparation contains the water solution A of Sodium orthomolybdate and thioacetamide, and the concentration of Sodium orthomolybdate is 0.03mol/L, and the concentration of thioacetamide is 0.126mol/L.Preparation Value 3608 (TX-10), cetyl trimethylammonium bromide (CTAB), hexanaphthene, the mixture B of n-hexyl alcohol, wherein cetyl trimethylammonium bromide is 0.4657g, Value 3608 is 4.657g, n-hexyl alcohol is 3.105g, and hexanaphthene is 20ml.Said mixture was stirred 30 minutes.The water solution A of 3ml is joined among the mixture B, stirred 30 minutes, form microemulsion.In above-mentioned microemulsion, add micro-formic acid, become scarlet to liquid, reacted 12 hours.By centrifugal, separate obtaining precursor MoS 3Throw out, again through washing, and vacuum drying treatment, obtain precursor MoS 3Powder.With precursor MoS 3Powder is at 700 ℃ N 2/ H 2Thermal treatment is 60 minutes in (9: 1) atmosphere, obtains inorganic fullerene molybdenum disulphide.
Embodiment 13: preparation contains the water solution A of Sodium orthomolybdate and thioacetamide, and the concentration of Sodium orthomolybdate is 0.03mol/L, and the concentration of thioacetamide is 0126mol/L.Preparation Value 3608 (TX-10), cetyl trimethylammonium bromide (CTAB), hexanaphthene, the mixture B of n-hexyl alcohol, wherein cetyl trimethylammonium bromide is 0.4657g, Value 3608 is 4.657g, n-hexyl alcohol is 3.105g, and hexanaphthene is 20ml.Said mixture was stirred 30 minutes.The water solution A of 3ml is joined among the mixture B, stirred 30 minutes, form microemulsion.In above-mentioned microemulsion, add micro-formic acid, become scarlet to liquid, reacted 12 hours.By centrifugal, separate obtaining precursor MoS 3Throw out, again through washing, and vacuum drying treatment, obtain precursor MoS 3Powder.With precursor MoS 3Powder is at 800 ℃ N 2/ H 2Thermal treatment is 60 minutes in (9: 1) atmosphere, obtains inorganic fullerene molybdenum disulphide.
Embodiment 14: preparation contains the water solution A of Sodium orthomolybdate and thioacetamide, and the concentration of Sodium orthomolybdate is 0.03mol/L, and the concentration of thioacetamide is 0.126mol/L.Preparation Value 3608 (TX-10), cetyl trimethylammonium bromide (CTAB), hexanaphthene, the mixture B of n-hexyl alcohol, wherein cetyl trimethylammonium bromide is 0.4657g, Value 3608 is 4.657g, n-hexyl alcohol is 3.105g, and hexanaphthene is 20ml.Said mixture was stirred 30 minutes.The water solution A of 3ml is joined among the mixture B, stirred 30 minutes, form microemulsion.In above-mentioned microemulsion, add micro-formic acid, become scarlet to liquid, reacted 12 hours.By centrifugal, separate obtaining precursor MoS 3Throw out, again through washing, and vacuum drying treatment, obtain precursor MoS 3Powder.With precursor MoS 3Powder is at 900 ℃ N 2/ H 2Thermal treatment is 60 minutes in (9: 1) atmosphere, obtains inorganic fullerene molybdenum disulphide.
Embodiment 15: preparation contains the water solution A of Sodium orthomolybdate and thioacetamide, and the concentration of Sodium orthomolybdate is 0.03mol/L, and the concentration of thioacetamide is 0.126mol/L.Preparation Value 3608 (TX-10), cetyl trimethylammonium bromide (CTAB), hexanaphthene, the mixture B of n-hexyl alcohol, wherein cetyl trimethylammonium bromide is 0.4657g, Value 3608 is 4.657g, n-hexyl alcohol is 3.105g, and hexanaphthene is 20ml.Said mixture was stirred 30 minutes.The water solution A of 3ml is joined among the mixture B, stirred 30 minutes, form microemulsion.In above-mentioned microemulsion, add micro-formic acid, become scarlet to liquid, reacted 12 hours.By centrifugal, separate obtaining precursor MoS 3Throw out, again through washing, and vacuum drying treatment, obtain precursor MoS 3Powder.With precursor MoS 3Powder is at 700 ℃ N 2/ H 2Thermal treatment is 100 minutes in (9: 1) atmosphere, obtains inorganic fullerene molybdenum disulphide.
Embodiment 16: preparation contains the water solution A of Sodium orthomolybdate and thioacetamide, and the concentration of Sodium orthomolybdate is 0.03mol/L, and the concentration of thioacetamide is 0.126mol/L.Preparation Value 3608 (TX-10), cetyl trimethylammonium bromide (CTAB), hexanaphthene, the mixture B of n-hexyl alcohol, wherein cetyl trimethylammonium bromide is 0.4657g, Value 3608 is 4.657g, n-hexyl alcohol is 3.105g, and hexanaphthene is 20ml.Said mixture was stirred 30 minutes.The water solution A of 3ml is joined among the mixture B, stirred 30 minutes, form microemulsion.In above-mentioned microemulsion, add micro-formic acid, become scarlet to liquid, reacted 12 hours.By centrifugal, separate obtaining precursor MoS 3Throw out, again through washing, and vacuum drying treatment, obtain precursor MoS 3Powder.With precursor MoS 3Powder is at 700 ℃ N 2/ H 2Thermal treatment is 150 minutes in (9: 1) atmosphere, obtains inorganic fullerene molybdenum disulphide.
Embodiment 17: preparation contains the water solution A of Sodium orthomolybdate and thioacetamide, and the concentration of Sodium orthomolybdate is 0.03mol/L, and the concentration of thioacetamide is 0.126mol/L.Preparation Value 3608 (TX-10), cetyl trimethylammonium bromide (CTAB), hexanaphthene, the mixture B of n-hexyl alcohol, wherein cetyl trimethylammonium bromide is 0.4657g, Value 3608 is 4.657g, n-hexyl alcohol is 3.105g, and hexanaphthene is 20ml.Said mixture was stirred 30 minutes.The water solution A of 3ml is joined among the mixture B, stirred 30 minutes, form microemulsion.In above-mentioned microemulsion, add micro-formic acid, become scarlet to liquid, reacted 12 hours.By centrifugal, separate obtaining precursor MoS 3Throw out, again through washing, and vacuum drying treatment, obtain precursor MoS 3Powder.With precursor MoS 3Powder is at 700 ℃ N 2/ H 2Thermal treatment is 180 minutes in (9: 1) atmosphere, obtains inorganic fullerene molybdenum disulphide.
Embodiment 18: preparation contains the water solution A of Sodium orthomolybdate and thioacetamide, and the concentration of Sodium orthomolybdate is 0.03mol/L, and the concentration of thioacetamide is 0.126mol/L.Preparation Value 3608 (TX-10), cetyl trimethylammonium bromide (CTAB), hexanaphthene, the mixture B of n-hexyl alcohol, wherein cetyl trimethylammonium bromide is 0.4657g, Value 3608 is 4.657g, n-hexyl alcohol is 3.105g, and hexanaphthene is 20ml.Said mixture was stirred 30 minutes.The water solution A of 3ml is joined among the mixture B, stirred 30 minutes, form microemulsion.In above-mentioned microemulsion, add micro-formic acid, become scarlet to liquid, reacted 12 hours.By centrifugal, separate obtaining precursor MoS 3Throw out, again through washing, and vacuum drying treatment, obtain precursor MoS 3Powder.With precursor MoS 3Powder is at 800 ℃ N 2Thermal treatment is 60 minutes in/H2 (9: the 1) atmosphere, obtains inorganic fullerene molybdenum disulphide.

Claims (4)

1. the preparation method of an inorganic fullerene molybdenum disulphide is characterized in that this method may further comprise the steps:
A, preparation contain the water solution A of Sodium orthomolybdate and thioacetamide, and preparation contains the mixture B of Value 3608, cetyl trimethylammonium bromide, hexanaphthene and n-hexyl alcohol, and A is joined among the B, stir to form microemulsion;
B, in microemulsion, add micro-formic acid, become scarlet to liquid, reacted under the room temperature 8～14 hours.By centrifugal, separate obtaining precursor MoS 3Throw out through washing and vacuum drying treatment, obtains precursor MoS again 3Powder;
C, with precursor MoS 3Powder is at 500～1000 ℃ N 2And H 2Thermal treatment is 30～300 minutes in the atmosphere, obtains inorganic fullerene molybdenum disulphide.
2. the method for claim 1, it is characterized in that: in step a, the mol ratio of Value 3608 and cetyl trimethylammonium bromide is 10: 1～3 among the mixture B, the mol ratio of n-hexyl alcohol and Value 3608 is 10: 1～4, and the mol ratio of Value 3608 and hexanaphthene is 1～5: 100.
3. the method for claim 1, it is characterized in that: in step a, the volume ratio of water solution A and hexanaphthene is 0.25～2.5: 10.
4. the method for claim 1 is characterized in that: N in step c 2With H 2Volume ratio be 9: 1.
CN2009101382623A 2009-05-08 2009-05-08 Method for preparing inorganic fullerene molybdenum disulphide Pending CN101880061A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104962340A (en) * 2015-07-17 2015-10-07 合肥工业大学 Inorganic fullerene molybdenum disulfide/graphene composite lubricant and preparation method thereof
CN105347401A (en) * 2015-11-19 2016-02-24 常州大学 Method used for controllable preparation of monodisperse mesoporous molybdenum disulfide nanospheres
CN105731542A (en) * 2014-12-10 2016-07-06 中国科学院大连化学物理研究所 A method of preparing molybdenum disulfide microspheres in a reversed-phase microemulsion system
CN105731543A (en) * 2016-01-04 2016-07-06 济南大学 Laser rapid preparation method of inorganic molybdenum disulfide microsphere with fullerene like structure

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105731542A (en) * 2014-12-10 2016-07-06 中国科学院大连化学物理研究所 A method of preparing molybdenum disulfide microspheres in a reversed-phase microemulsion system
CN105731542B (en) * 2014-12-10 2018-09-04 中国石油天然气股份有限公司 A method of preparing mos2 microsphere in Reverse Microemulsion System
CN104962340A (en) * 2015-07-17 2015-10-07 合肥工业大学 Inorganic fullerene molybdenum disulfide/graphene composite lubricant and preparation method thereof
CN104962340B (en) * 2015-07-17 2017-06-16 合肥工业大学 Inorganic fullerene molybdenum disulfide/Graphene compounded lubricant and preparation method thereof
CN105347401A (en) * 2015-11-19 2016-02-24 常州大学 Method used for controllable preparation of monodisperse mesoporous molybdenum disulfide nanospheres
CN105731543A (en) * 2016-01-04 2016-07-06 济南大学 Laser rapid preparation method of inorganic molybdenum disulfide microsphere with fullerene like structure
CN105731543B (en) * 2016-01-04 2018-03-27 济南大学 A kind of laser fast preparation method of inorganic fullerene molybdenum disulfide microballoon

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