CN1803632A - Method for preparing nanometer metallic sulfide - Google Patents
Method for preparing nanometer metallic sulfide Download PDFInfo
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- CN1803632A CN1803632A CN 200610031191 CN200610031191A CN1803632A CN 1803632 A CN1803632 A CN 1803632A CN 200610031191 CN200610031191 CN 200610031191 CN 200610031191 A CN200610031191 A CN 200610031191A CN 1803632 A CN1803632 A CN 1803632A
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Abstract
The invention discloses a preparation method for nano molybdenum disulfide and tungsten sulfide. Wherein, with ammonium molybdate/tungstate hydrate as molybdenum/tungsten source and porous molybdenum trioxide/tungsten oxide as carrier, thermal cracking to original converse into molybdenum trioxide/tungsten oxide crystal in carrier pore channel; in high-temperature cracking furnace of 800-1100Deg, leading H2S gas and H2 gas with 8-20% partial pressure/H2S gas to generate the final product on limit of pore carrier channel.
Description
Technical field
The invention belongs to the preparation method of nano metal sulphide, be specifically related to its preparation method of a kind of nano molybdenum disulfide material and nanometer tungsten 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, a kind of preparation method who can be used for the nano metal sulphide of lubricant is provided at above-mentioned prior art existence.This method is compared with traditional method, and the preparation method is simple, raw materials used extensively inexpensive, technology is simple and easy to do, is fit to industrial mass manufacture.
Realize that the technical scheme that the object of the invention adopts is:
As the production method of the molybdenum disulfide nano material of nano metal sulfide material, be to be the molybdenum source with the Ammonium paramolybdate tetrahydrate, 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 and hydrogen simultaneously, the dividing potential drop that makes hydrogen is 8%-20%, can generate the molybdenum disulfide nano material under the restriction in molybdenum oxide duct.
The production method of described molybdenum disulfide nano material also can add gold/iron thin film catalyzer.Catalyzer can adopt on silicon (111) substrate with vacuum evaporation or sputter-deposition technology preparation.
As the production method of the tungsten sulfide nano material of nano metal sulfide material, also be to be the tungsten source with the tungstic acid hydrate ammonium, porous tungsten oxide is a solid support material, is the Tungsten oxide 99.999 crystal by heating pyrolyze converted in-situ tungstic acid hydrate ammonium in the Tungsten oxide 99.999 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 Tungsten oxide 99.999 duct, generate the tungsten sulfide nano material.
The production method of described tungsten sulfide nano material can add gold/iron thin film catalyzer.Catalyzer can adopt on silicon (111) substrate with vacuum evaporation or sputter-deposition technology preparation.
The inventive method is compared with traditional method, and the preparation method is simple, raw materials used extensively inexpensive, technology is simple and easy to do, is fit to industrial mass manufacture.
Embodiment
[embodiment one]
The production method of molybdenum disulfide nano material is to be 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; Add gold/iron thin film catalyzer, catalyzer can adopt on silicon (111) substrate with vacuum evaporation or sputter-deposition technology preparation; At last, be in 800 ℃ of-1100 ℃ of high-temperature cracking furnaces in temperature, introduce hydrogen sulfide and hydrogen simultaneously, the dividing potential drop that makes hydrogen is 8%-20%, can generate the molybdenum disulfide nano material under the restriction in molybdenum oxide duct.
[embodiment two]
The further production method of molybdenum disulfide nano material:
(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 and hydrogen gas mixture in this step, flow is 200sccm, and wherein hydrogen partial pressure is 8%, also feeds the nitrogen carrier gas of 1000sccm simultaneously.
(5) treat the furnace temperature naturally cooling, collect the pewter product on the silicon substrate.
[embodiment three]
The production method of tungsten sulfide nano material also is to be the tungsten source with the tungstic acid hydrate ammonium, and porous tungsten oxide is a solid support material, is the Tungsten oxide 99.999 crystal by heating pyrolyze converted in-situ tungstic acid hydrate ammonium in the Tungsten oxide 99.999 duct; Add gold/iron thin film catalyzer, catalyzer can adopt on silicon (111) substrate with vacuum evaporation or sputter-deposition technology preparation; At last, be in 800 ℃ of-1100 ℃ of high-temperature cracking furnaces in temperature, introduce hydrogen sulfide, participate in reaction, under the restriction in Tungsten oxide 99.999 duct, generate the tungsten sulfide nano material.
[embodiment four]
The further production method of tungsten sulfide nano material:
(1) be the inorganic salt of corresponding tungsten with changing the raw material Ammonium Molybdate Tetrahydrate in embodiment two steps (1), consumption changes according to being equal to molar equivalent.
(2) other steps are with embodiment two, and products therefrom is the tungsten sulfide series material.
Claims (7)
1, a kind of preparation method of nano metal sulphide, nano metal sulphide is the molybdenum disulfide nano material, it is characterized in that with the Ammonium paramolybdate tetrahydrate being the molybdenum source, 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 and hydrogen simultaneously, the dividing potential drop that makes hydrogen is 8%-20%, can generate the molybdenum disulfide nano material under the restriction in molybdenum oxide duct.
2, the preparation method of nano metal sulphide as claimed in claim 1 is characterized in that adding gold/iron thin film catalyzer.
3, the preparation method of nano metal sulphide as claimed in claim 2 is characterized in that catalyzer adopts on silicon (111) substrate with vacuum evaporation or sputter-deposition technology preparation.
4, the preparation method of nano metal sulphide according to claim 3 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.It is molybdic oxide that the purpose of this step is to transform ammonium molybdate, is characterized as the light green crystal;
(4) put the molybdic oxide/molybdenum oxide material of step (3) conversion on the silicon substrate of metallizing catalyst film, be placed on the silica tube middle part together, the heating furnace temperature is to 870-950 ℃, temperature rise rate is 40 ℃ of per minutes, be incubated 30 minutes, feed hydrogen sulfide and hydrogen gas mixture in this step, flow is 200sccm, wherein hydrogen partial pressure is 8%, also feeds the nitrogen carrier gas of 1000sccm simultaneously;
(5) treat the furnace temperature naturally cooling, collect the pewter product on the silicon substrate.
5, a kind of preparation method of nano metal sulphide, nano metal sulphide is the tungsten sulfide nano material, it is characterized in that with the tungstic acid hydrate ammonium be the tungsten source, porous tungsten oxide is a solid support material, is the Tungsten oxide 99.999 crystal by heating pyrolyze converted in-situ tungstic acid hydrate ammonium in the Tungsten oxide 99.999 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 Tungsten oxide 99.999 duct, generate the tungsten sulfide nano material.
6, the preparation method of nano metal sulphide as claimed in claim 4 is characterized in that adding gold/iron thin film catalyzer.
7, the preparation method of nano metal sulphide as claimed in claim 5 is characterized in that catalyzer adopts on silicon (111) substrate with vacuum evaporation or sputter-deposition technology preparation.
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| CN 200610031191 CN1803632A (en) | 2006-01-24 | 2006-01-24 | Method for preparing nanometer metallic sulfide |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100408471C (en) * | 2006-08-25 | 2008-08-06 | 南京大学 | Preparation method of nanometer metal sulfide |
| CN103771518A (en) * | 2014-01-27 | 2014-05-07 | 金堆城钼业股份有限公司 | Porous molybdenum disulfide particle preparation method |
| CN104310485A (en) * | 2014-10-20 | 2015-01-28 | 安徽工业大学 | Tungsten disulfide nano powder material with aluminum sulfide shell, and preparation method of tungsten disulfide nano powder material |
| CN104386766A (en) * | 2014-10-20 | 2015-03-04 | 安徽工业大学 | Nickel sulfide nanometer powdered material with aluminium sulfide casing and preparation method thereof |
| CN105344309A (en) * | 2015-12-01 | 2016-02-24 | 宁波诺丁汉新材料研究院有限公司 | Mercury removal agent with nano laminated structure |
| CN105742080A (en) * | 2016-04-07 | 2016-07-06 | 东南大学 | Preparation method for one-dimensional ordered titanium dioxide nanorod array composite material |
| CN106379940A (en) * | 2016-11-24 | 2017-02-08 | 厦门理工学院 | Two-dimensional nano-molybdenum disulfide and preparation method thereof |
| CN106645308A (en) * | 2016-10-11 | 2017-05-10 | 南京工业大学 | Method for manufacturing acetone gas sensor based on alloy molybdenum disulfide tungsten nanosheets |
| CN107384530A (en) * | 2017-07-26 | 2017-11-24 | 深圳市威勒科技股份有限公司 | A kind of engine extreme pressure anti-wear additives and preparation method thereof |
| CN109046390A (en) * | 2018-07-19 | 2018-12-21 | 中国科学院大学 | The derivative molybdenum base complex sulfide catalysis material of houghite is in H2S and CO2Concerted catalysis converts the application in carbonyl sulfur processed |
| CN114560502A (en) * | 2020-11-27 | 2022-05-31 | 国电南瑞科技股份有限公司 | Three-dimensional nano molybdenum-based lithium ion battery cathode material and preparation method thereof |
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2006
- 2006-01-24 CN CN 200610031191 patent/CN1803632A/en active Pending
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100408471C (en) * | 2006-08-25 | 2008-08-06 | 南京大学 | Preparation method of nanometer metal sulfide |
| CN103771518A (en) * | 2014-01-27 | 2014-05-07 | 金堆城钼业股份有限公司 | Porous molybdenum disulfide particle preparation method |
| CN103771518B (en) * | 2014-01-27 | 2015-03-04 | 金堆城钼业股份有限公司 | Porous molybdenum disulfide particle preparation method |
| CN104310485A (en) * | 2014-10-20 | 2015-01-28 | 安徽工业大学 | Tungsten disulfide nano powder material with aluminum sulfide shell, and preparation method of tungsten disulfide nano powder material |
| CN104386766A (en) * | 2014-10-20 | 2015-03-04 | 安徽工业大学 | Nickel sulfide nanometer powdered material with aluminium sulfide casing and preparation method thereof |
| CN104310485B (en) * | 2014-10-20 | 2015-12-09 | 安徽工业大学 | A kind of Wolfram disulfide nano powdered material with aluminium sulfide shell and preparation method thereof |
| CN105344309A (en) * | 2015-12-01 | 2016-02-24 | 宁波诺丁汉新材料研究院有限公司 | Mercury removal agent with nano laminated structure |
| CN105742080B (en) * | 2016-04-07 | 2018-02-02 | 东南大学 | A kind of preparation method of one-dimensional titanic oxide nanorod array composite in order |
| CN105742080A (en) * | 2016-04-07 | 2016-07-06 | 东南大学 | Preparation method for one-dimensional ordered titanium dioxide nanorod array composite material |
| CN106645308A (en) * | 2016-10-11 | 2017-05-10 | 南京工业大学 | Method for manufacturing acetone gas sensor based on alloy molybdenum disulfide tungsten nanosheets |
| CN106645308B (en) * | 2016-10-11 | 2020-09-29 | 南京工业大学 | Method for manufacturing acetone gas sensor based on alloy molybdenum disulfide tungsten nanosheets |
| CN106379940A (en) * | 2016-11-24 | 2017-02-08 | 厦门理工学院 | Two-dimensional nano-molybdenum disulfide and preparation method thereof |
| 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 |
| CN107384530B (en) * | 2017-07-26 | 2020-07-07 | 深圳市威勒科技股份有限公司 | Extreme pressure antiwear agent for engine and preparation method thereof |
| CN107384530A (en) * | 2017-07-26 | 2017-11-24 | 深圳市威勒科技股份有限公司 | A kind of engine extreme pressure anti-wear additives and preparation method thereof |
| CN109046390A (en) * | 2018-07-19 | 2018-12-21 | 中国科学院大学 | The derivative molybdenum base complex sulfide catalysis material of houghite is in H2S and CO2Concerted catalysis converts the application in carbonyl sulfur processed |
| CN109046390B (en) * | 2018-07-19 | 2020-12-22 | 中国科学院大学 | Hydrotalcite-like compound derived molybdenum-based composite sulfide catalytic material in H2S and CO2Application of concerted catalytic conversion in preparation of carbonyl sulfide |
| CN114560502A (en) * | 2020-11-27 | 2022-05-31 | 国电南瑞科技股份有限公司 | Three-dimensional nano molybdenum-based lithium ion battery cathode material and preparation method thereof |
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