CN104630892A - Method for growing molybdenum disulfide single crystal by vapor phase transportation method - Google Patents
Method for growing molybdenum disulfide single crystal by vapor phase transportation method Download PDFInfo
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- CN104630892A CN104630892A CN201510090506.0A CN201510090506A CN104630892A CN 104630892 A CN104630892 A CN 104630892A CN 201510090506 A CN201510090506 A CN 201510090506A CN 104630892 A CN104630892 A CN 104630892A
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- Prior art keywords
- molybdenumdisulphide
- monocrystalline
- polycrystalline
- molybdenum disulfide
- single crystal
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
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- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention provides a method for growing molybdenum disulfide single crystal by a vapor phase transportation method. The method comprises the following steps: by taking pure molybdenum powder and pure sulfur powder as raw materials, performing chemical reaction at a high temperature to obtain a polycrystal molybdenum disulfide material; putting molybdenum disulfide polycrystal and tantalum pentachloride into a furnace with three temperature regions to perform vapor phase transportation reaction, thereby obtaining high-purity molybdenum disulfide single crystal.
Description
Technical field
The present invention relates to a kind of method utilizing vapor transportation method to grow molybdenumdisulphide monocrystalline.
Background technology
As a kind of layer mineral, molybdenumdisulphide is widely used in lubricating area because of advantages such as its frictional coefficient is low, stable in properties.In recent years, class Graphene molybdenumdisulphide causes people's interest widely because of the microtexture of its uniqueness and optics, electrical properties.Class Graphene molybdenumdisulphide is all gathered around in various fields such as secondary cell, field effect transistor, sensor, electroluminescent and is had broad application prospects, and is expected to the two-dimensional stage becoming new electronics with Graphene side by side.
The preparation of monocrystal material, also referred to as the growth of crystal, is the reactant that the non-crystalline state of material, polycrystalline state maybe can be formed this material changes monocrystalline into process by the means of certain chemistry.The preparation method of monocrystalline usually can be divided into melt growth, solution growth and grow mutually.Melt growth is divided into again: flame melt method, crystal pulling method, zone melting method etc.; Solution growth is divided into again: sol-gel method, hydrothermal method etc.; Namely phase growth method refers to a kind of method of growing single-crystal from gas phase, is also called
vapor transportation method---be the important method that a kind of single crystal growing and material are purified.This is wherein divided into again: single-component system and multicomponent system grow these two kinds.Polycomponent vapor phase growth is generally used for epitaxial film growth, and epitaxy is that a kind of crystal is grown floating on water on another kind of crystal.Be mainly used in the production of the working element of the aspects such as electronic machine, Magnetic memory device and integrated optics.Single component vapor phase growth requires that gas phase possesses sufficiently high vapour pressure, utilizes in high-temperature zone vaporization distillation, grows in the principle of cold zone condensation growth.But this method application is wideless, and the crystal grown is mostly the single crystal of needle-like, sheet.
In two-dimensional semiconductor single crystal growth process, the method for general application namely
chemical vapor transportation method (CVT).In many instances, chemical vapor transportation and chemical vapor deposition (CVD) strict difference, and occasion and the reaction unit of just application are different.In general, chemical vapour deposition mainly refers to the preparation of film, and chemical vapor transportation then often refers to for occasions such as the synthesis of single crystal growing, new compound and the purifications of material.When utilizing chemical vapor transportation method to prepare the crystal of a kind of solid matter A, can add in system and transport agent B, substance A with transport agent B and react and generate volatile product C, and set up following chemical equilibrium: iA (s)+kB (g) ← → jC (g).Reactant is enclosed in quartz container, and is placed in the tube furnace of certain temperature gradient.Due at different temperature, the equilibrium constant of above-mentioned reaction is different, and when the gaseous substance C of generation is transported to the other end from one end of container, balance moves round about, and A is deposited.Substance A can be made in this way to obtain purifying, good crystal can also be obtained.Vapor transportation method has that equipment is simple, operational safety, controllability strong, synthetic product purity advantages of higher.
Summary of the invention
In order to obtain the required high purity monocrystalline molybdenumdisulphide material used in optics, Experiments of Electricity, the invention provides a kind of method utilizing vapor transportation method to grow molybdenumdisulphide monocrystalline.The technical solution adopted for the present invention to solve the technical problems is: with pure molybdenum powder and bright sulfur powder for starting material, at high temperature carry out chemical reaction and obtain polycrystalline molybdenumdisulphide material.Again molybdenumdisulphide polycrystalline and tantalum pentachloride are put into three-temperature-zone stove and carry out vapor transportation reaction, finally obtain highly purified molybdenumdisulphide monocrystalline crystal.
The invention has the beneficial effects as follows: starting material easily obtain, equipment is simple, operational safety, acquisition molybdenumdisulphide monocrystalline crystal purity high.
embodiment:
embodiment:1. take pure molybdenum powder 3g and bright sulfur powder 2g, pour in the one section of silica tube being about 15cm and seal.
2. the silica tube of good seal is placed in box-type furnace, heat up 3 little up to temperature be 750 degrees Celsius.
3. maintaining temperature in stove is 750 degrees Celsius, and after about 5 days, blow-on is inspected, and observes in closed quartz tube without stopping heating after tawny gas.Obtain molybdenumdisulphide Polycrystalline.
4. open silica tube, take 0.5g molybdenumdisulphide polycrystalline, be together sealed in one with 40mg tantalum pentachloride and be about in the silica tube of 23 centimetres.
5. the silica tube of good seal is put into three-temperature-zone stove, have one end of medicine to be placed on the centre of stove.
6. heat 3 hours, by temperature-raising region temperature raising to 1040 degree Celsius in the middle of the stove of three-temperature-zone, both sides temperature-raising region temperature raising to 1020 degree Celsius, and constant temperature 5 days.
7. three-temperature-zone stove is lowered the temperature 24 little of normal temperature, obtain the molybdenumdisulphide monocrystalline crystal born at the cold junction of silica tube.
Claims (3)
1. the method for a vapor transportation growth molybdenumdisulphide monocrystalline, it is characterized in that obtaining molybdenumdisulphide polycrystalline with pure molybdenum powder and bright sulfur powder for starting material carry out chemical reaction, carry out gas phase reactant transport with molybdenumdisulphide polycrystalline and tantalum pentachloride and obtain high purity molybdenumdisulphide monocrystalline.
2. the method for a kind of vapor transportation growth molybdenumdisulphide monocrystalline according to claim 1, molybdenumdisulphide polycrystalline is obtained by chemical reaction, be positioned in box-type furnace after it is characterized in that a certain proportion of pure molybdenum powder and bright sulfur powder are sealed in silica tube, be heated to complete reaction at 750 degrees c and obtain molybdenumdisulphide polycrystalline.
3. the method for a kind of vapor transportation growth molybdenumdisulphide monocrystalline according to claim 1, molybdenumdisulphide monocrystalline is obtained by reacting by vapor transportation, be positioned in the stove of three-temperature-zone after it is characterized in that a certain proportion of molybdenumdisulphide polycrystalline and tantalum pentachloride are sealed in silica tube, arrange after suitable thermostatic reacts a couple of days and obtain molybdenumdisulphide monocrystalline.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510090506.0A CN104630892A (en) | 2015-02-28 | 2015-02-28 | Method for growing molybdenum disulfide single crystal by vapor phase transportation method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510090506.0A CN104630892A (en) | 2015-02-28 | 2015-02-28 | Method for growing molybdenum disulfide single crystal by vapor phase transportation method |
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| CN104630892A true CN104630892A (en) | 2015-05-20 |
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| CN201510090506.0A Pending CN104630892A (en) | 2015-02-28 | 2015-02-28 | Method for growing molybdenum disulfide single crystal by vapor phase transportation method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109371468A (en) * | 2018-10-20 | 2019-02-22 | 南京大学 | A kind of high quality Cu2Se(1-x)AxThe growing method of crystal |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102892709A (en) * | 2010-03-10 | 2013-01-23 | 耶达研究与发展有限公司 | Nanostructures, their use and process for their production |
| CN103579419A (en) * | 2013-11-13 | 2014-02-12 | 苏州科技学院 | Grapheme/MoS2/Si heterojunction thin-film solar cell and manufacturing method thereof |
-
2015
- 2015-02-28 CN CN201510090506.0A patent/CN104630892A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102892709A (en) * | 2010-03-10 | 2013-01-23 | 耶达研究与发展有限公司 | Nanostructures, their use and process for their production |
| CN103579419A (en) * | 2013-11-13 | 2014-02-12 | 苏州科技学院 | Grapheme/MoS2/Si heterojunction thin-film solar cell and manufacturing method thereof |
Non-Patent Citations (1)
| Title |
|---|
| ANDREA PISONI, ET AL.: "The Role of Transport Agents in MoS2 Single Crystals", 《J. PHYS. CHEM. C》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109371468A (en) * | 2018-10-20 | 2019-02-22 | 南京大学 | A kind of high quality Cu2Se(1-x)AxThe growing method of crystal |
| CN109371468B (en) * | 2018-10-20 | 2020-05-05 | 南京大学 | High-quality Cu2Se(1-x)AxMethod for growing crystal |
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Application publication date: 20150520 |