CN105926039A - Method for synthesizing and growing titanium disulfide single crystal at high temperature - Google Patents
Method for synthesizing and growing titanium disulfide single crystal at high temperature Download PDFInfo
- Publication number
- CN105926039A CN105926039A CN201610482929.1A CN201610482929A CN105926039A CN 105926039 A CN105926039 A CN 105926039A CN 201610482929 A CN201610482929 A CN 201610482929A CN 105926039 A CN105926039 A CN 105926039A
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- CN
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- Prior art keywords
- titanium disulfide
- titanium
- monocrystalline
- high temperature
- 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
- C30B1/00—Single-crystal growth directly from the solid state
- C30B1/10—Single-crystal growth directly from the solid state by solid state reactions or multi-phase diffusion
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to a method for synthesizing and growing a titanium disulfide single crystal at a high temperature. The titanium disulfide single crystal can be prepared through mixing sponge-shaped titanium with sulfur, sealing the mixture and proper amount of an iodine block into a heat-resisting quartz tube and heating at the high temperature.
Description
Technical field
The method that the present invention relates to a kind of high-temperature nuclei growth titanium disulfide monocrystalline.
Background technology
Transient metal sulfide MS2(M can be the transition metal materials such as W, Mo, Ti) has occupied important ratio in two-dimensional material monocrystalline, it has the layer structure of similar graphite, combined by van der waals force between layers, can overcome to prepare few layer even nano material of monoatomic layer by extraneous factor easily.Wherein, titanium disulfide is a kind of brass flakey crystal, has metallic luster.At room temperature stable and stable to water, dilute sulfuric acid and hydrochloric acid, but nitric acid and concentrated sulphuric acid can make it decompose precipitation sulfur, thus destroy its structure.Since in recent years, because it is found that titanium disulfide has layer structure, the most each layer includes the interlayer of sulfur-titanium-sulfur, and by weak van der waals force contact between interlayer, therefore titanium disulfide monocrystalline can be as good two-dimensional material crystal raw material.Its method for monocrystal growth is numerous, can be by titanium silk heat growth in sulfur vapor, also can be synthesized by titanium tetrachloride and stink damp phase reaction, also can be prepared in hexane solution by titanium disulfide and n-BuLi, or prepared by electrochemical reaction, but the most defective existence of molybdenum bisuphide monocrystalline prepared by these methods, causes its optical property undesirable.It addition, titanium disulfide monocrystalline is in addition to having layer structure and become preferable two-dimensional material monocrystalline, or Li/TiS2 energy storage device or the basis of battery, thus attention.
Summary of the invention
In order to obtain the required high-purity monocrystalline titanium disulfide material used in optics, Experiments of Electricity, the method that the invention provides a kind of high-temperature nuclei growth titanium disulfide monocrystalline.
The technical solution adopted for the present invention to solve the technical problems is: takes titanium sponge and mixes with sulfur, together encloses in vitreosil pipe with appropriate iodine block, and at high temperature heating 5-7 days, can obtain titanium disulfide monocrystalline in one end of quartz ampoule.
The invention has the beneficial effects as follows: raw material easily obtains, step simply eliminates the synthesis step of titanium disulfide polycrystalline, operation safety, the titanium disulfide monocrystalline crystal purity height of acquisition.
Detailed description of the invention:
Embodiment one:1. weigh titanium sponge 0.30g, bright sulfur powder 0.40g, pure iodine block 65mg, pour internal diameter 13mm into, be about in one section of quartz ampoule of 10cm, and two seals.
2. being placed on by the quartz ampoule of good seal in single temperature-area tubular furnace, the thermocouple of one end and tube furnace of wherein placing medicine aligns.Within 3 hours, it is warming up to 850 degrees Celsius.
3. maintaining temperature in single temperature-area tubular furnace stove is 850 degrees Celsius, constant temperature 72 hours.
Temperature in tube furnace stove was down to room temperature in 4.12 hours, the titanium disulfide crystal of the lamellar of size about 4*5mm can be obtained in one end of quartz ampoule.
Embodiment two:1. weigh titanium sponge 0.50g, bright sulfur powder 0.67g, pure iodine block 65mg, pour internal diameter 13mm into, be about in one section of quartz ampoule of 15cm, and two seals.
2. being placed on by the quartz ampoule of good seal in single temperature-area tubular furnace, the thermocouple of one end and tube furnace of wherein placing medicine aligns.Within 3 hours, it is warming up to 880 degrees Celsius.
3. maintaining temperature in single temperature-area tubular furnace stove is 880 degrees Celsius, constant temperature 60 hours.
Temperature in tube furnace stove was down to room temperature in 4.12 hours, the 3*3mm titanium disulfide crystal of lamellar can be obtained in one end of quartz ampoule.
Claims (2)
1. the method for high-temperature nuclei growth titanium disulfide monocrystalline, it is characterised in that directly mix with sulfur with taking titanium sponge, and add appropriate iodine and grow lamellar titanium disulfide monocrystalline as transporting agent.
2. the method for high-temperature nuclei growth titanium disulfide monocrystalline, it is characterised in that eliminate the synthesis step of titanium disulfide polycrystalline, it is not necessary to by titanium and sulfur through high-temperature nuclei titanium disulfide polycrystalline, and use titanium sponge to mix direct growth titanium disulfide monocrystalline with sulfur.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610482929.1A CN105926039A (en) | 2016-06-28 | 2016-06-28 | Method for synthesizing and growing titanium disulfide single crystal at high temperature |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610482929.1A CN105926039A (en) | 2016-06-28 | 2016-06-28 | Method for synthesizing and growing titanium disulfide single crystal at high temperature |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105926039A true CN105926039A (en) | 2016-09-07 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610482929.1A Pending CN105926039A (en) | 2016-06-28 | 2016-06-28 | Method for synthesizing and growing titanium disulfide single crystal at high temperature |
Country Status (1)
| Country | Link |
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| CN (1) | CN105926039A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107447257A (en) * | 2017-09-04 | 2017-12-08 | 中国科学院地球化学研究所 | A kind of method for growing manganese spar monocrystalline at high temperature under high pressure |
| CN107675255A (en) * | 2017-09-04 | 2018-02-09 | 中国科学院地球化学研究所 | A kind of method for growing siderite monocrystalline at high temperature under high pressure |
| CN107675256A (en) * | 2017-09-04 | 2018-02-09 | 中国科学院地球化学研究所 | A kind of method for growing magnesite monocrystalline at high temperature under high pressure |
| CN112111788A (en) * | 2020-09-10 | 2020-12-22 | 吉林大学 | Method for preparing titanium disulfide crystal and product |
-
2016
- 2016-06-28 CN CN201610482929.1A patent/CN105926039A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107447257A (en) * | 2017-09-04 | 2017-12-08 | 中国科学院地球化学研究所 | A kind of method for growing manganese spar monocrystalline at high temperature under high pressure |
| CN107675255A (en) * | 2017-09-04 | 2018-02-09 | 中国科学院地球化学研究所 | A kind of method for growing siderite monocrystalline at high temperature under high pressure |
| CN107675256A (en) * | 2017-09-04 | 2018-02-09 | 中国科学院地球化学研究所 | A kind of method for growing magnesite monocrystalline at high temperature under high pressure |
| CN107675255B (en) * | 2017-09-04 | 2019-06-11 | 中国科学院地球化学研究所 | A method of growing siderite monocrystalline at high temperature under high pressure |
| CN107447257B (en) * | 2017-09-04 | 2019-06-11 | 中国科学院地球化学研究所 | A method of growing manganese spar monocrystalline at high temperature under high pressure |
| CN107675256B (en) * | 2017-09-04 | 2019-06-11 | 中国科学院地球化学研究所 | A method of growing magnesite monocrystalline at high temperature under high pressure |
| CN112111788A (en) * | 2020-09-10 | 2020-12-22 | 吉林大学 | Method for preparing titanium disulfide crystal and product |
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| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20160907 |
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| WD01 | Invention patent application deemed withdrawn after publication |