CN104651940A - Method for growing tungsten ditelluride single crystals by using vapor transport process - Google Patents
Method for growing tungsten ditelluride single crystals by using vapor transport process Download PDFInfo
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- CN104651940A CN104651940A CN201510090508.XA CN201510090508A CN104651940A CN 104651940 A CN104651940 A CN 104651940A CN 201510090508 A CN201510090508 A CN 201510090508A CN 104651940 A CN104651940 A CN 104651940A
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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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- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention provides a method for growing tungsten ditelluride single crystals by using a vapor transport process. The method comprises the following step: by taking tungsten ditelluride polycrystalline powder with the purity over 3N as a raw material, putting tungsten ditelluride polycrystallines and a transfer agent (I2 or TeCl4 and the like) in a three-temperature-region furnace for vapor transport reaction so as to obtain high purity tungsten ditelluride single crystals.
Description
Technical field
The present invention relates to a kind of method utilizing vapor transportation method to grow two telluride tungsten monocrystalline.
Background technology
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.
Summary of the invention
Problem solved by the invention is to provide a kind of method utilizing vapor transportation method to grow two telluride tungsten monocrystalline.Concrete steps are as follows: (1) is got two telluride tungsten polycrystal powders and transfer agent powder to make mixing medicine powder for subsequent use.
(2) mixed powder made is loaded in the silica tube closed one end.
(3) vacuum pump is started, (1*10 after being vacuumized by silica tube
-1below pa), the opening end of closed quartz tube, forms the closed at both ends vitreosil pipe that a section is equipped with mixing medicine powder.
(4) by close after silica tube, be placed in furnace with mutiple temperature regions, one end that medicine is housed of silica tube be placed in the high-temperature part of furnace with mutiple temperature regions, the other end is placed in the low temperature part of furnace with mutiple temperature regions, start vapor transportation.
(5) furnace with mutiple temperature regions is risen to required temperature in the mode of ladder-elevating temperature, after maintaining this temperature certain hour, within 24 hours, slow cooling is to normal temperature.
(6) take out closed at both ends vitreosil pipe, the two telluride tungsten monocrystalline crystal being attached to silica tube inwall can be obtained.
Wherein, described step (1) use raw material for 3N(and purity be 99.9%) above powder stock or be 99.999% by 5N(and purity) compound powder powder stock synthesized by elemental powders raw material.
Beneficial effect: the two telluride tungsten monocrystalline that purity is higher can be grown.
Embodiment: the invention provides a kind of method utilizing vapor transportation method to grow two telluride tungsten monocrystalline.
Embodiment one: (1) gets two telluride tungsten polycrystal powders and transfer agent TeCl
4it is for subsequent use that powder makes mixing medicine powder.
(2) mixed powder made is loaded in the silica tube closed one end.
(3) vacuum pump is started, (1*10 after being vacuumized by silica tube
-1below pa), the opening end of closed quartz tube, forms the closed at both ends vitreosil pipe that a section is equipped with mixing medicine powder.
(4) by close after silica tube, be placed in furnace with mutiple temperature regions, one end that medicine is housed of silica tube be placed in the high-temperature part of furnace with mutiple temperature regions, the other end is placed in the low temperature part of furnace with mutiple temperature regions, start vapor transportation.
(5) by furnace with mutiple temperature regions high-temperature zone in the mode of ladder-elevating temperature, within 4 hours, rise to 1040 DEG C, cold zone, in the mode of ladder-elevating temperature, rises to 980 DEG C in 4 hours, and the temperature maintaining each warm area is after 5 days, and within 24 hours, slow cooling is to normal temperature.
(6) take out closed at both ends vitreosil pipe, the two telluride tungsten monocrystalline crystal being attached to silica tube inwall can be obtained.
Embodiment two: (1) gets two telluride tungsten polycrystal powders and transfer agent I
2it is for subsequent use that powder makes mixing medicine powder.
(2) mixed powder made is loaded in the silica tube closed one end.
(3) vacuum pump is started, (1*10 after being vacuumized by silica tube
-1below pa), the opening end of closed quartz tube, forms the closed at both ends vitreosil pipe that a section is equipped with mixing medicine powder.
(4) by close after silica tube, be placed in furnace with mutiple temperature regions, one end that medicine is housed of silica tube be placed in the high-temperature part of furnace with mutiple temperature regions, the other end is placed in the low temperature part of furnace with mutiple temperature regions, start vapor transportation.
(5) by furnace with mutiple temperature regions high-temperature zone in the mode of ladder-elevating temperature, within 3 hours, rise to 750 DEG C, cold zone, in the mode of ladder-elevating temperature, rises to 720 DEG C in 3 hours, and the temperature maintaining each warm area is after 6 days, and within 12 hours, slow cooling is to normal temperature.
(6) take out closed at both ends vitreosil pipe, the two telluride tungsten monocrystalline crystal being attached to silica tube inwall can be obtained.
Claims (3)
1. utilize vapor transportation method to grow a method for two telluride tungsten monocrystalline, the method concrete steps are as follows: (1) is got two telluride tungsten polycrystal powders and transfer agent powder to make mixing medicine powder for subsequent use; (2) mixed powder made is loaded in the silica tube closed one end; (3) vacuum pump is started, (1*10 after being vacuumized by silica tube
-1below pa), the opening end of closed quartz tube, forms the closed at both ends vitreosil pipe that a section is equipped with mixing medicine powder; (4) by close after silica tube, be placed in furnace with mutiple temperature regions, one end that medicine is housed of silica tube be placed in the high-temperature part of furnace with mutiple temperature regions, the other end is placed in the low temperature part of furnace with mutiple temperature regions, start vapor transportation; (5) furnace with mutiple temperature regions is risen to required temperature in the mode of ladder-elevating temperature, after maintaining this temperature certain hour, within 24 hours, slow cooling is to normal temperature; (6) take out closed at both ends vitreosil pipe, the two telluride tungsten monocrystalline crystal being attached to silica tube inwall can be obtained.
2. according to a kind of method utilizing vapor transportation method to grow two telluride tungsten monocrystalline described in claim 1, it is characterized in that, described step (1) use raw material for 3N(and purity be 99.9%) above powder stock or the compound powder powder stock synthesized by 5N elemental powders raw material.
3. according to a kind of method utilizing vapor transportation method to grow two telluride tungsten monocrystalline described in claim 1, it is characterized in that the furnace with mutiple temperature regions in described step (5), use tellurium tetrachloride to be rise to 1040 DEG C in 4 hours as high-temperature part temperature during transfer agent, low temperature portion temperature is rise to 980 DEG C in 4 hours; Use iodine to be rise to 750 DEG C in 3 hours as high-temperature part temperature during transfer agent, low temperature portion temperature is rise to 720 DEG C in 3 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510090508.XA CN104651940A (en) | 2015-02-28 | 2015-02-28 | Method for growing tungsten ditelluride single crystals by using vapor transport process |
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| CN201510090508.XA CN104651940A (en) | 2015-02-28 | 2015-02-28 | Method for growing tungsten ditelluride single crystals by using vapor transport process |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107620123A (en) * | 2016-07-13 | 2018-01-23 | 清华大学 | A kind of preparation method of the semi metallic compound of metal platinum |
| CN107868981A (en) * | 2016-09-28 | 2018-04-03 | 清华大学 | A kind of semi metallic compound of metal platinum and preparation method thereof |
| CN107868982A (en) * | 2016-09-28 | 2018-04-03 | 清华大学 | A kind of preparation method of the semi metallic compound of metal platinum |
| CN109295496A (en) * | 2018-09-18 | 2019-02-01 | 中国科学院合肥物质科学研究院 | A kind of synthetic method of binary phosphorus family compound-material |
| CN109516444A (en) * | 2018-12-12 | 2019-03-26 | 北京工业大学 | A kind of preparation method of two telluride tungsten |
| CN113247973A (en) * | 2021-06-28 | 2021-08-13 | 河南工程学院 | Preparation method of sulfur group magnetic compound of transition metal Cr intercalation |
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 CN201510090508.XA patent/CN104651940A/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 (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107620123A (en) * | 2016-07-13 | 2018-01-23 | 清华大学 | A kind of preparation method of the semi metallic compound of metal platinum |
| CN107620123B (en) * | 2016-07-13 | 2020-09-08 | 清华大学 | Preparation method of semimetal compound of metal platinum |
| CN107868981A (en) * | 2016-09-28 | 2018-04-03 | 清华大学 | A kind of semi metallic compound of metal platinum and preparation method thereof |
| CN107868982A (en) * | 2016-09-28 | 2018-04-03 | 清华大学 | A kind of preparation method of the semi metallic compound of metal platinum |
| CN107868981B (en) * | 2016-09-28 | 2020-09-29 | 清华大学 | Semi-metallic compound of metal platinum and preparation method thereof |
| CN109295496A (en) * | 2018-09-18 | 2019-02-01 | 中国科学院合肥物质科学研究院 | A kind of synthetic method of binary phosphorus family compound-material |
| CN109295496B (en) * | 2018-09-18 | 2020-08-25 | 中国科学院合肥物质科学研究院 | Synthesis method of binary phosphorus compound material |
| CN109516444A (en) * | 2018-12-12 | 2019-03-26 | 北京工业大学 | A kind of preparation method of two telluride tungsten |
| CN109516444B (en) * | 2018-12-12 | 2020-06-26 | 北京工业大学 | Preparation method of tungsten ditelluride |
| CN113247973A (en) * | 2021-06-28 | 2021-08-13 | 河南工程学院 | Preparation method of sulfur group magnetic compound of transition metal Cr intercalation |
| CN113247973B (en) * | 2021-06-28 | 2023-04-18 | 河南工程学院 | Preparation method of sulfur group magnetic compound of transition metal Cr intercalation |
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Application publication date: 20150527 |