CN1821090A - Dimolybdenum trisulfide nano material and its preparing method and obtained lubricant thereof - Google Patents
Dimolybdenum trisulfide nano material and its preparing method and obtained lubricant thereof Download PDFInfo
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- CN1821090A CN1821090A CN 200610031190 CN200610031190A CN1821090A CN 1821090 A CN1821090 A CN 1821090A CN 200610031190 CN200610031190 CN 200610031190 CN 200610031190 A CN200610031190 A CN 200610031190A CN 1821090 A CN1821090 A CN 1821090A
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Abstract
The present invention discloses a kind of nanometer Mo2O3 material, its preparation process and lubricant with nanometer Mo2O3 as material. Geometrically, the nanometer Mo2O3 material is one-dimensional nanometer material with diameter smaller than 50 nm, length greater than 500 nm and length/diameter ratio greater than 10. Chemically, the nanometer Mo2O3 material has S/Mo atom ratio of 3 to 2, monoclinic crystal structure, space group P21/m and unit cell parameters of a=6.086 angstrom, b=3.204 angstrom, c=8.623 angstrom, and beta=102.44 deg. The nanometer Mo2O3 as material has novel structure and simple preparation, and is suitable for industrial production. The lubricant with nanometer Mo2O3 as material has excellent wear resisting and lubricating performance and may find wide application in space engine, fuel oil and other fields.
Description
Technical field
The present invention relates to a kind of Dimolybdenum trisulfide nano material and preparation method thereof, and be the lubricant that raw material obtains with the nanometer molybdic sulfide.
Background technology
Metallic sulfide can be used as uses such as lubricant, catalyzer, electrode materials, intercalation compound and energy and material, has wide prospect in industrial application and is worth with exploitation.Molybdenumdisulphide, tungsten disulfide large size material have mainly been studied in patent of having authorized and former studies work, its deficiency is that millimeter lubricated granules of magnitude yardstick damages working positions such as gear surface easily, therefore its addition in auxiliary grease is very low, has limited its practical application.Therefore the moly-sulfide lubricant that develops Nano grade is imperative.
In the world seldom about nanometer material molybdenum sulfide preparation method's report, mainly be included in the High Temperature High Pressure synthetic technology under the hydrothermal condition, shortcoming is that impurity is many in the product, wear no resistance, reason is that the raw material of hydro-thermal reaction can only adopt the raw material of non-variable compounds such as molybdic oxide and moly-sulfide, therefore disproportionation, network and etc. the activation energy of reaction too high, the inevitable residual reaction raw materials that exists as impurity is so product purity is low.Other researchists report and use hydrogen sulfide original position sulfuration molybdenum trioxide nano line (rod), thereby generate the moly-sulfide nano material.The problem of this technology is that operational path is loaded down with trivial details, must be divided into preparation molybdenum oxide nano wire and two steps of vulcanization reaction and carry out, and has therefore improved the technology cost, and product is of a size of submillimeter, is not nano material.
Summary of the invention
The objective of the invention is deficiency at above-mentioned prior art existence, a kind of Dimolybdenum trisulfide nano material that can be used for lubricant and preparation method thereof is provided and is the lubricant of raw material with this Dimolybdenum trisulfide nano material, lubricant that is obtained and existing moly-sulfide lubricant have higher lubricity.
Realize that the technical scheme that the object of the invention adopts is:
A kind of Dimolybdenum trisulfide nano material, its geometric properties are nano level, and diameter or lateral cross section be less than 50 nanometers or 2000 square nanometers, and length is greater than 500 nanometers, and length-to-diameter ratio is greater than 10 monodimension nanometer material; Chemical feature is the sulphur of nano wire: molybdenum atom is 3: 2; Crystalline structure is a monoclinic crystal, and spacer is P21/m, and cell parameter is the a=6.086 dust, b=3.204 dust, c=8.623 dust, β=102.44 degree.
The production method of described Dimolybdenum trisulfide nano material is the molybdenum source with the Ammonium paramolybdate tetrahydrate, and the porous molybdic oxide is a solid support material, is the molybdic oxide crystal by heating pyrolyze converted in-situ Ammonium paramolybdate tetrahydrate in the molybdenum oxide duct; At last, be in 800 ℃ of-1100 ℃ of high-temperature cracking furnaces in temperature, introduce hydrogen sulfide, participate in reaction, under the restriction in molybdenum oxide duct, generate Dimolybdenum trisulfide nano material.
In above-mentioned production method, also can add gold/iron thin film catalyzer.
Described catalyzer can adopt on silicon (111) substrate with vacuum evaporation or sputter-deposition technology preparation.
Adopt the nano lubricating agent of Dimolybdenum trisulfide nano material preparation, it is directly to add Dimolybdenum trisulfide nano material in grease, just can obtained performance lubricant preferably.
Preparing preferably, nano lubricating agent is the 5-8 Dimolybdenum trisulfide nano material doubly that adds relative traditional macro size moly-sulfide powder in grease.
Dimolybdenum trisulfide nano material yardstick of the present invention is a nanometer scale, novel structure, its preparation method is simple, raw materials used extensively inexpensive, technology is simple and easy to do, is fit to industrial mass manufacture.Lubricant with the Dimolybdenum trisulfide nano material preparation has excellent wear-resisting, lubricity.Dimolybdenum trisulfide nano material can be used as the needed base mateiral of lubricant of nano level yardstick, has widespread use at military affairs such as airspace engine, fuel oil, civil area.
Embodiment
[embodiment one]
Nanometer molybdic sulfide provided by the invention, its geometric properties are to be of a size of Nano grade, and diameter or lateral cross section be less than 50 nanometers or 2000 square nanometers, and length is greater than 500 nanometers, and length-to-diameter ratio is greater than 10 monodimension nanometer material; Chemical feature is the sulphur of nano wire: molybdenum atom is 3: 2; Crystalline structure is a monoclinic crystal, and spacer is P21/m, and cell parameter is the a=6.086 dust, b=3.204 dust, c=8.623 dust, β=102.44 degree.
[embodiment two]
The preparation method of Dimolybdenum trisulfide nano material of the present invention: at first, be the molybdenum source with the Ammonium paramolybdate tetrahydrate, the porous molybdic oxide is a solid support material, is light green molybdic oxide crystal by heating pyrolyze converted in-situ Ammonium paramolybdate tetrahydrate in the molybdenum oxide duct; Add gold/iron thin film catalyzer, catalyzer is by preparing with vacuum evaporation or sputter-deposition technology on silicon (111) substrate; In temperature is in 800 ℃ of-1100 ℃ of high-temperature cracking furnaces, introduces hydrogen sulfide, participates in reaction, generates the nanometer molybdic sulfide under the restriction in molybdenum oxide duct.
[embodiment three]
In the production method of embodiment two
(1) formulation vehicle and molybdenum source compound material: 12.36 gram Ammonium Molybdate Tetrahydrates are dissolved in 70 ml distilled waters, stir, and add the γ type porous molybdic oxide of 3 gram specific surface areas greater than 200 meters squared per gram, continue to stir 2 hours;
(2) preparation catalyst metal film: the iron/gold thin film that adopts vacuum evaporation, sputtering sedimentation or plasma coating technology preparation 100-300 rice on the silicon substrate of (111) orientation.
(3) the thermal transition of preparation in the step (1), temperature is 350-450 ℃, and soaking time is that 3-7 hour compound molybdenum source/molybdenum oxide material adds in process furnace.It is molybdic oxide that the purpose of this step is to transform ammonium molybdate, is characterized as the light green crystal.
(4) molybdic oxide/molybdenum oxide material of putting step (3) conversion is placed on the silica tube middle part together on the silicon substrate of metallizing catalyst film, and the heating furnace temperature is to 870-950 ℃, and temperature rise rate is 40 ℃ of per minutes, is incubated 30 minutes.Feed hydrogen sulfide in this step, flow is 200sccm.
(5) treat the furnace temperature naturally cooling, collect the pewter product on the silicon substrate.
[embodiment four]
A kind of nano lubricating agent that adopts the preparation of nanometer molybdic sulfide: nanometer molybdic sulfide material and auxiliary grease are formed nano lubricating agent, the 5-8 of the moly-sulfide powder that its addition in auxiliary grease is the traditional macro size doubly, so lubricant effect is greatly improved.
Claims (7)
1, a kind of Dimolybdenum trisulfide nano material is characterized in that its geometric properties is a nano level, and diameter or lateral cross section be less than 50 nanometers or 2000 square nanometers, and length is greater than 500 nanometers, and length-to-diameter ratio is greater than 10 monodimension nanometer material; Chemical feature is the sulphur of nano wire: molybdenum atom is 3: 2; Crystalline structure is a monoclinic crystal, and spacer is P21/m, and cell parameter is the a=6.086 dust, b=3.204 dust, c=8.623 dust, β=102.44 degree.
2, a kind of production method of Dimolybdenum trisulfide nano material is characterized in that with the Ammonium paramolybdate tetrahydrate being the molybdenum source, and the porous molybdic oxide is a solid support material, is the molybdic oxide crystal by heating pyrolyze converted in-situ Ammonium paramolybdate tetrahydrate in the molybdenum oxide duct; At last, be in 800 ℃ of-1100 ℃ of high-temperature cracking furnaces in temperature, introduce hydrogen sulfide, participate in reaction, under the restriction in molybdenum oxide duct, generate Dimolybdenum trisulfide nano material.
3, the production method of Dimolybdenum trisulfide nano material as claimed in claim 2 is characterized in that adding gold/iron thin film catalyzer.
4, the production method of Dimolybdenum trisulfide nano material as claimed in claim 3 is characterized in that catalyzer adopts on silicon (111) substrate with vacuum evaporation or sputter-deposition technology preparation.
5, the production method of Dimolybdenum trisulfide nano material according to claim 4 is characterized in that:
(1) formulation vehicle and molybdenum source compound material: 12.36 gram Ammonium Molybdate Tetrahydrates are dissolved in 70 ml distilled waters, stir, and add the γ type porous molybdic oxide of 3 gram specific surface areas greater than 200 meters squared per gram, continue to stir 2 hours;
(2) preparation catalyst metal film: the iron/gold thin film that adopts vacuum evaporation, sputtering sedimentation or plasma coating technology preparation 100-300 rice on the silicon substrate of (111) orientation;
(3) the thermal transition of preparation in the step (1), temperature is 350-450 ℃, and soaking time is that 3-7 hour compound molybdenum source/molybdenum oxide material adds in process furnace, and it is molybdic oxide that the purpose of this step is to transform ammonium molybdate, is characterized as the light green crystal;
(4) molybdic oxide/molybdenum oxide material of putting step (3) conversion is placed on the silica tube middle part together on the silicon substrate of metallizing catalyst film, and the heating furnace temperature is to 870-950 ℃, and temperature rise rate is 40 ℃ of per minutes, is incubated 30 minutes.Feed hydrogen sulfide in this step, flow is 200sccm;
(5) treat the furnace temperature naturally cooling, collect the pewter product on the silicon substrate.
6, a kind of nano lubricating agent that adopts the Dimolybdenum trisulfide nano material preparation is characterized in that adding Dimolybdenum trisulfide nano material in grease.
7, nano lubricating agent according to claim 5 is characterized in that in grease adding the 5-8 nanometer molybdic sulfide material doubly of relative traditional macro size moly-sulfide powder.
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| CN 200610031190 CN1821090A (en) | 2006-01-24 | 2006-01-24 | Dimolybdenum trisulfide nano material and its preparing method and obtained lubricant thereof |
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| CN 200610031190 CN1821090A (en) | 2006-01-24 | 2006-01-24 | Dimolybdenum trisulfide nano material and its preparing method and obtained lubricant thereof |
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