CN100339309C - Preparation method of inorganic fullerene structured molybdenium disulfide - Google Patents
Preparation method of inorganic fullerene structured molybdenium disulfide Download PDFInfo
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- CN100339309C CN100339309C CNB2005100286743A CN200510028674A CN100339309C CN 100339309 C CN100339309 C CN 100339309C CN B2005100286743 A CNB2005100286743 A CN B2005100286743A CN 200510028674 A CN200510028674 A CN 200510028674A CN 100339309 C CN100339309 C CN 100339309C
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Abstract
The present invention relates to a preparation method of inorganic molybdenum disulfide in a fullerene structure in the technical field of materials. Ammonium molybdenum sulfide is used as a raw material, and an aqueous solution of the ammonium molybdenum sulfide is dried by a spray drying method to prepare superfine precursor grains of molybdenum trisulfide. Then, the molybdenum trisulfide grains are heated in the environment of the mixed gas of hydrogen gas and argon gas, and molybdenum trisulfide is reduced to molybdenum disulfide grains in a fullerene structure. In the present invention, a large number of inorganic fullerene molybdenum disulfide grains are prepared through a simple and effective chemosynthesis method; the method is simple and rapid, the grain size is convenient to control, and the present invention provides the possibility for the wide application in tribology and in other aspects.
Description
Technical field
The present invention relates to the preparation method in a kind of material technology field, specifically, relate to preparation method with a kind of inorganic fullerene structured molybdenium disulfide.
Background technology
As everyone knows, for example graphite, transient metal sulfide MX of the solid lubricant with better tribological property
2(M=W or Mo, X=S or Se) has great science importance under the environment that can't use such as liquid lubricants such as space technology, ultrahigh vacuum(HHV) or automotive trannsmission systems.Therefore these materials have extremely low shear-stress owing to reactive force (Van der Waals force) between its laminate structure and layer and the layer is very little.Although these materials have outstanding anti-attrition performance and very long life-span under vacuum, but because the undersaturated dangling bonds of its crystal edge have chemically reactive, in friction process, adhere to metallic surface and oxidized easily, make that its tribological property under wet condition or oxygen atmosphere is very poor, therefore limited their science in atmospheric environment and used.Inorganic fullerene structural transition metallic sulfide has excellent tribological property with its particular structure and good chemical stability as solid lubricant, has the potential application prospect aspect tribology.The inorganic fullerene structured material is compared with 2H laminate structure phase material, and major advantage is the spherical of it and does not have unsaturated suspension to be good for (fringing effect).The granularity of inorganic fullerene structural transition nano metal sulfide particulate is general＞100nm, and this is enough to prevent the uneven surface contact between contact surface.Ideally, the sphere of inorganic fullerene particulate can be used as the molecular ball bearing and makes it that rolling resistance take place between contact surface in friction process.Therefore in addition, because the inorganic fullerene hollow structure makes nanoparticle have certain elasticity, opposing inelastic deformation and reduced waste of energy in process of friction and wear makes frictional surface temperature reduce.In addition,, make this particulate that very high chemical stability be arranged,, and can under atmospheric environment, be extensive use of so particle is not easy to cling contact surface or adhered to one another owing to there is not unsaturated suspension strong.
Find through literature search prior art, Chen Weixiang, be coated with river equality, reported in " the synthetic and Tribological Applications progress of inorganic fullerene transient metal sulfide nano material " that the 76-80 page or leaf is delivered in lubricating oil, to add a spot of inorganic fullerene WS in " tribology journal " 2003 the 23rd the 1st phase of volume
2Can greatly improve its tribological property, in lubricating oil, add a spot of inorganic fullerene WS
2Can make the life-span of motor car engine improve 5 ~ 6 times, make oil consumption reduce by 1/2 ~ 1/3.Inorganic fullerene MoS with the arc discharge method preparation
2Film has extremely excellent tribological property, and its frictional coefficient only is 0.006, and still shows good tribological property in humidity is 45% nitrogen atmosphere.
But up to the present, the method for preparing inorganic fullerene sulfide is also very limited, has therefore also limited it greatly in tribology and otherwise widespread use.For MoS
2, up to the present, effective means is the method HS with the sulfuration bed
2The corresponding oxide particle that reduces prepares the mineral-type richness and reins in MoS
2Nano particle, but output is still more limited.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of preparation method of inorganic fullerene structured molybdenium disulfide is provided, make it prepare the inorganic fullerene molybdenum disulfide particle of magnanimity by simple and effective chemical synthesis process, method is simply quick, granularity is convenient to control, for it provides possibility in tribology and otherwise widespread use.
The present invention is achieved by the following technical solutions, the present invention's four thio ammonium molybdate is a raw material, with the four thio ammonium molybdate aqueous solution with spray-dired method drying, make the ultra-fine forerunner's particle of three aluminium sulfides, then the molybdenum trisulfide particle is heated under the environment of hydrogen and argon gas mixed gas, molybdenum trisulfide is reduced to fullerene structure molybdenumdisulphide particle.
Described four thio ammonium molybdate, the concentration of its aqueous solution are 0.01mol/L ~ 0.1mol/L, and the four thio ammonium molybdate raw material is commercially available or mixed according to chemical dosage ratio with the aqueous solution of ammonium molybdate and ammonium sulfide.
Described spraying drying, 220 ℃ of sample inlet temperature, 120 ℃ of temperature outs.
The ultra-fine forerunner's particle of described molybdenum trisulfide, granularity is between 0.1 ~ 5 μ m.
Described heating is specially: under argon gas and hydrogen gas mixture air-flow, be heated to 850 ℃ in silica tube, heated 5 hours, then furnace cooling.
The mixed gas of described hydrogen and argon gas, wherein the content of argon gas is 85% ~ 95%.
Described fullerene structure molybdenumdisulphide particle, granularity and all are hollow ball shell between 0.1 ~ 5 μ m, and the thickness of spherical shell is about tens nanometers.Whole particle is class pomegranate shape, and the spherical shell internal surface has been assembled the inorganic fullerene molybdenum disulfide small-particle of a large amount of granularities in 100nm.By the XRD test shows, this particle interfloor distance has the expansion of percentum than commercially available common laminate structure (2H) molybdenumdisulphide.
The present invention by improving drying process with atomizing or adopting more advanced spray drying device, can obtain more homogeneous granules of littler particle and granularity in the inorganic fullerene molybdenum disulfide granules preparation process of magnanimity.Used silica tube (commercially available) and supporting jet system thereof require to have good resistance to air loss (can not leak into air), the argon gas of only discharging in the heat-processed to be led to and the mixed gas of hydrogen.
Embodiment
With following example the present invention is prepared inorganic fullerene molybdenum disulfide particulate specific embodiments and be further described, will help the understanding of the present invention.But not as to the qualification of protection scope of the present invention, and protection scope of the present invention is decided by the spirit and the scope of claim.
Embodiment 1
(purity 99.8% 0.1mol), is made into the 1L aqueous solution, and concentration is 0.1mol/L, with the solution spray-drier of packing into, with the solution drying to get the 28.88g four thio ammonium molybdate.Spray-drier gas velocity 150m/s, 220 ℃ of inlet temperatures, 120 ℃ of temperature outs.The molybdenum trisulfide grain graininess of gained is between 0.2 ~ 5 μ m.The molybdenum trisulfide particle is put into silica tube, in tube furnace, be heated to 850 ℃, be incubated 5 hours, then furnace cooling.The mixed gas of a straight-through argon gas and hydrogen (argon gas 90%) in the silica tube.The molybdenumdisulphide grain graininess of gained still between 0.2 ~ 5 μ m, is the fullerene structure particle.
Embodiment 2
(purity 99.8% 0.01mol), is made into the 1L aqueous solution, and concentration is 0.01mol/L, with the solution spray-drier of packing into, with the solution drying to get the 2.9g four thio ammonium molybdate.Spray-drier gas velocity 150m/s, 220 ℃ of inlet temperatures, 120 ℃ of temperature outs.The molybdenum trisulfide grain graininess of gained is between 0.2 ~ 5 μ m.The molybdenum trisulfide particle is put into silica tube, in tube furnace, be heated to 850 ℃, be incubated 5 hours, then furnace cooling.The mixed gas of a straight-through argon gas and hydrogen (argon gas 85%) in the silica tube.Still between 0.2 ~ 5 μ m, just spherical shell shape particulate thickness decreases the molybdenumdisulphide grain graininess of gained.
Embodiment 3
(purity 99.8% 0.05mol), is made into the 1L aqueous solution, and concentration is 0.05mol/L, with the solution spray-drier of packing into, with the solution drying to get the 14.4g four thio ammonium molybdate.Spray-drier gas velocity 150m/s, 220 ℃ of inlet temperatures, 120 ℃ of temperature outs.The molybdenum trisulfide grain graininess of gained is between 0.2 ~ 5 μ m.The molybdenum trisulfide particle is put into silica tube, in tube furnace, be heated to 850 ℃, be incubated 5 hours, then furnace cooling.The mixed gas of a straight-through argon gas and hydrogen (argon gas 95%) in the silica tube.The molybdenumdisulphide grain graininess of gained is still between 0.2 ~ 5 μ m.
Embodiment 4
Working method and condition thereof are similar substantially to 1, and when being spray-dired, the spray-drier gas velocity increases to 200m/s.The molybdenumdisulphide grain graininess that the result obtains is reduced to 0.1 ~ 3 μ m, still is the fullerene structure particle.
Embodiment 5
Working method and condition thereof are similar substantially to 2, and when being spray-dired, the spray-drier gas velocity increases to 200m/s.The molybdenumdisulphide grain graininess that the result obtains is reduced to 0.1 ~ 3 μ m, still is the fullerene structure particle.
Embodiment 6
Working method and condition thereof are similar substantially to 3, and when being spray-dired, the spray-drier gas velocity increases to 200m/s.The molybdenumdisulphide grain graininess that the result obtains is reduced to 0.1 ~ 3 μ m, still is the fullerene structure particle.
Claims (6)
1, a kind of preparation method of inorganic fullerene structured molybdenium disulfide, it is characterized in that, with four thio ammonium molybdate is raw material, with the four thio ammonium molybdate aqueous solution with spray-dired method drying, make the molybdenum trisulfide forerunner particle of granularity between 0.1-5 μ m, then molybdenum trisulfide forerunner particle is heated under the environment of hydrogen and argon gas mixed gas, molybdenum trisulfide is reduced to fullerene structure molybdenumdisulphide particle; Described spraying drying, 220 ℃ of sample inlet temperature, 120 ℃ of temperature outs.
2, the preparation method of inorganic fullerene structured molybdenium disulfide according to claim 1, it is characterized in that, described four thio ammonium molybdate, the concentration of its aqueous solution is 0.01mol/L-0.1mol/L, and the four thio ammonium molybdate raw material is commercially available or mixed according to chemical dosage ratio with the aqueous solution of ammonium molybdate and ammonium sulfide.
3, the preparation method of inorganic fullerene structured molybdenium disulfide according to claim 1 is characterized in that, described heating is specially: under argon gas and hydrogen gas mixture air-flow, be heated to 850 ℃ in silica tube, heated 5 hours, then furnace cooling.
4, according to the preparation method of claim 1 or 3 described inorganic fullerene structured molybdenium disulfides, it is characterized in that, the mixed gas of described hydrogen and argon gas, wherein the content of argon gas is 80%-95%.
5, the preparation method of inorganic fullerene structured molybdenium disulfide according to claim 1 is characterized in that, described fullerene structure molybdenumdisulphide particle, and granularity is between 0.1-5 μ m.
6, the preparation method of inorganic fullerene structured molybdenium disulfide according to claim 1 is characterized in that, described spraying drying, spray-drier gas velocity are 150m/s or 200m/s.
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102616854B (en) * | 2011-01-31 | 2014-11-05 | 中国科学院过程工程研究所 | Preparation method of monodisperse spherical MoS2 ultrafine powder |
| CN102267724A (en) * | 2011-07-07 | 2011-12-07 | 金堆城钼业股份有限公司 | Method for preparing ammonium molybdate |
| CN105140518B (en) * | 2015-09-18 | 2017-08-18 | 河南师范大学 | A kind of nanocage hollow fullerene-like molybdenum disulfide and its preparation method and application |
| 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 |
| CN106379940B (en) * | 2016-11-24 | 2018-05-29 | 厦门理工学院 | A kind of two-dimensional nano molybdenum disulfide and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4081520A (en) * | 1976-03-19 | 1978-03-28 | Erco Industries Limited | High efficiency production of chlorine dioxide by solvay process |
| CN1519204A (en) * | 2003-01-20 | 2004-08-11 | 中国科学院金属研究所 | Method for mass producing material in nano structure of fullereneoid of molybdenum disulfide |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4081520A (en) * | 1976-03-19 | 1978-03-28 | Erco Industries Limited | High efficiency production of chlorine dioxide by solvay process |
| CN1519204A (en) * | 2003-01-20 | 2004-08-11 | 中国科学院金属研究所 | Method for mass producing material in nano structure of fullereneoid of molybdenum disulfide |
Non-Patent Citations (3)
| Title |
|---|
| Template Synthesis of Near-MonodisperseMicroscale Nanofibers and Nanotubules of MoS2 Catherine M. Zelenski and Peter K. Dorhout*.,J.Am.Chem.Soc.,Vol.120 No.4 1998 * |
| Thermogravimetric-differential thermal analysis ofthesolid-state decomposition of ammoniumtetrathiomolybdate during heating in argon Wang HW,Skeldon P,Thompson GE,Materials Science,Multidisciplinary,Vol.33 No.12 1998 * |
| 均匀沉淀法制备纳米二硫化钼粉末的研究 沃恒洲，胡献国，胡淑丽，赵业松，合肥工业大学学报（自然科学版），第26卷第4期 2003 * |
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