CN105970297A - Growth method of rhenium disulfide monocrystal - Google Patents

Growth method of rhenium disulfide monocrystal Download PDF

Info

Publication number
CN105970297A
CN105970297A CN201610494152.0A CN201610494152A CN105970297A CN 105970297 A CN105970297 A CN 105970297A CN 201610494152 A CN201610494152 A CN 201610494152A CN 105970297 A CN105970297 A CN 105970297A
Authority
CN
China
Prior art keywords
rhenium disulfide
rhenium
disulfide
polycrystalline
temperature
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201610494152.0A
Other languages
Chinese (zh)
Inventor
邱俊
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nanjing Anjing Terahertz Optoelectronics Technology Co Ltd
Original Assignee
Nanjing Anjing Terahertz Optoelectronics Technology Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Nanjing Anjing Terahertz Optoelectronics Technology Co Ltd filed Critical Nanjing Anjing Terahertz Optoelectronics Technology Co Ltd
Priority to CN201610494152.0A priority Critical patent/CN105970297A/en
Publication of CN105970297A publication Critical patent/CN105970297A/en
Pending legal-status Critical Current

Links

Classifications

    • 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
    • C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
    • 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
    • C30B28/00—Production of homogeneous polycrystalline material with defined structure
    • C30B28/02—Production of homogeneous polycrystalline material with defined structure directly from the solid state
    • 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

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The invention provides a growth method of rhenium disulfide monocrystal, including: mixing and placing rhenium trisulfide and excessive sulfur powder according to a ratio into a quartz tube, vacuumizing, holding a temperature of 400 DEG C for one to two days, grinding obtained powder, burning on an alcohol burner, and removing redundant sulfur to obtain high-purity rhenium disulfide polycrystal; mixing the obtained desulfurized rhenium disulfide polycrystal with a transport agent bromine, sealing in a quartz tube, vacuumizing, placing in a multi-temperature furnace, and growing rhenium disulfide monocrystal by a chemical gaseous transport method.

Description

A kind of growing method of rhenium disulfide monocrystalline
Technical field
The present invention relates to the growing method of a kind of rhenium disulfide monocrystalline.
Background technology
Transient metal sulfide MS2(M can be the transition metal materials such as W, Mo, Re) has occupied important ratio in two-dimensional material monocrystalline, as the important member of two-dimensional atomic crystal material family, rhenium disulfide (ReS2) there is structure and the character being different from conventional two-dimensional material: low lattice symmetry result in anisotropic optical and electrical properties in the two-dimensional surface that rhenium disulfide is unique, such that it is able to the aspects such as scene effect transistor, photodetector and new ideas device have very big using value, therefore rhenium disulfide also becomes the active material of current two-dimensional material research direction.But, it being stranded by this material structure and character particularity, the preparation of this material bulk still suffers from problems.First being to prepare the rhenium source needed for this material, its valence state is various, causes growing uncontrollable；And the fusing point of simple substance rhenium is up to 3180 DEG C, boiling point is more up to 5900 DEG C, thus causes its growth efficiency the lowest；Particularly ReS2Low lattice symmetry and weak interlayer coupling make the growth behavior of this material bulk more complicated than the growth of conventional two-dimensional material, the acquisition of material is more difficult to relative to other two-dimensional material bulks, this also hinder its optically and electrically aspect deeper into research.
Summary of the invention
In order to obtain the required high-purity rhenium disulfide monocrystal material used in an experiment, the invention provides the growing method of a kind of rhenium disulfide monocrystalline.
The technical solution adopted for the present invention to solve the technical problems is: takes a certain proportion of rhenium trioxide and mix with the sulfur powder of excess and put in quartz ampoule also evacuation, one it is incubated to two days later at 400 DEG C, it is placed on calcination on alcohol burner after finely ground for the powder obtained, remove unnecessary sulfur, obtain the rhenium disulfide polycrystalline that purity is higher.Rhenium disulfide polycrystalline after the desulfuration that will obtain with transport after agent bromine mixes, put into furnace with mutiple temperature regions after enclosing quartz ampoule evacuation, utilize chemical vapor transportation method to grow rhenium disulfide monocrystalline.
The invention has the beneficial effects as follows: the rhenium disulfide monocrystalline crystal of high-purity, high-quality can be obtained.
Detailed description of the invention:
Embodiment:
1. weigh rhenium trioxide 0.936g, amount appropriate for bright sulfur powder 0.28g(is 0.256g), pour internal diameter 13mm into, be about in one section of quartz ampoule of 15cm, and after evacuation, two seals.
2. the quartz ampoule of good seal is placed in batch-type furnace, within 2 hours, is warming up to 400 degrees Celsius.
3. maintaining temperature in single temperature-area tubular furnace stove is 400 degrees Celsius, constant temperature 24 hours.
4. take out synthesis powder, finely ground after, be placed on calcination more than 15 minutes on alcohol burner, to remove unnecessary sulfur.
5. by powder remaining after calcination, pour internal diameter 13mm into, be about in one section of quartz ampoule of 20cm, and after adding 40mg bromine, evacuation, and two seals.
6. quartz ampoule is put into three-temperature-zone stove, and the one end equipped with sample is placed on warm area in the middle of the stove of three-temperature-zone, and with 12 hours, centre warm area temperature is risen to 960 degrees Celsius, both sides warm area temperature is risen to 920 degrees Celsius, constant temperature 4-5 days.
Three warm areas of three-temperature-zone stove were down to room temperature in 7.12 hours, the rhenium disulfide platy-monocrystal that size is 4mm can be obtained in one end of quartz ampoule.

Claims (3)

1. the growing method of a rhenium disulfide monocrystalline, after it is characterized in that taking a certain proportion of rhenium trioxide prepares rhenium disulfide polycrystalline with excessive sulfur powder, it is placed on calcination desulfuration on alcohol burner after finely ground for the powder obtained, and after the desulfuration that will obtain rhenium disulfide polycrystalline with transport after agent bromine mixes, utilize chemical vapor transportation method to grow rhenium disulfide monocrystalline.
The growing method of a kind of rhenium disulfide monocrystalline the most according to claim 1, during it is characterized in that preparing rhenium disulfide polycrystalline, uses the sulfur powder of excess, and removes unnecessary sulfur after obtaining rhenium disulfide polycrystalline by the way of calcination.
The growing method of a kind of rhenium disulfide monocrystalline the most according to claim 1, it is characterized in that by rhenium disulfide polycrystalline with transport after agent bromine mixes, the temperature of vapor transportation is 960 degrees Celsius, high-temperature region, low-temperature space 920 degrees Celsius, and transport time is 4-5 days.
CN201610494152.0A 2016-06-30 2016-06-30 Growth method of rhenium disulfide monocrystal Pending CN105970297A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610494152.0A CN105970297A (en) 2016-06-30 2016-06-30 Growth method of rhenium disulfide monocrystal

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610494152.0A CN105970297A (en) 2016-06-30 2016-06-30 Growth method of rhenium disulfide monocrystal

Publications (1)

Publication Number Publication Date
CN105970297A true CN105970297A (en) 2016-09-28

Family

ID=57020924

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610494152.0A Pending CN105970297A (en) 2016-06-30 2016-06-30 Growth method of rhenium disulfide monocrystal

Country Status (1)

Country Link
CN (1) CN105970297A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108642563A (en) * 2018-06-27 2018-10-12 电子科技大学 A kind of VSe applied to ethanol sensor2The preparation method of monocrystal thin films
CN112593291A (en) * 2020-11-23 2021-04-02 南京理工大学 Preparation method of rhenium disulfide or rhenium diselenide crystal
CN114892277A (en) * 2022-04-20 2022-08-12 苏州科技大学 Preparation method of ferromagnetic two-dimensional material with strong room temperature

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108642563A (en) * 2018-06-27 2018-10-12 电子科技大学 A kind of VSe applied to ethanol sensor2The preparation method of monocrystal thin films
CN108642563B (en) * 2018-06-27 2020-06-16 电子科技大学 VSe applied to ethanol sensor2Method for preparing single crystal film
CN112593291A (en) * 2020-11-23 2021-04-02 南京理工大学 Preparation method of rhenium disulfide or rhenium diselenide crystal
CN114892277A (en) * 2022-04-20 2022-08-12 苏州科技大学 Preparation method of ferromagnetic two-dimensional material with strong room temperature
CN114892277B (en) * 2022-04-20 2023-11-14 苏州科技大学 Preparation method of two-dimensional material with strong room temperature ferromagnetism

Similar Documents

Publication Publication Date Title
Uecker et al. Large-lattice-parameter perovskite single-crystal substrates
CN105970297A (en) Growth method of rhenium disulfide monocrystal
Erdei Growth of oxygen deficiency-free YVO4 single crystal by top-seeded solution growth technique
CN101476156B (en) Gadolinium, yttrium, scandium and gallium doped garnet, gadolinium-yttrium-scandium-gallium-aluminum garnet and crystal growth method by melt method
CN103710755A (en) Rare earth co-doping activated yttrium-aluminum-scandium garnet luminescent material and melt crystal growth method thereof
CN105603517A (en) Method for growing monocrystal black phosphorus based on solid-source chemical vapor deposition method
Triboulet et al. “Cold travelling heater method”, a novel technique of synthesis, purification and growth of CdTe and ZnTe
CN103708463A (en) Preparation method of kilogram-grade high-purity silicon carbide powder
Mu et al. Solid–liquid interface optimization and properties of ultra-wide bandgap β-Ga 2 O 3 grown by Czochralski and EFG methods
CN102560672A (en) Semi-insulating silicon carbide single crystal material
CN109706520A (en) Black arsenic phosphorus crystal and preparation method thereof
CN105926039A (en) Method for synthesizing and growing titanium disulfide single crystal at high temperature
CN108118394A (en) A kind of method of nitrogen impurity content in reduction single-crystal silicon carbide
CN102560627B (en) N-type czochralski silicon with uniform doping resistivity and preparation method thereof
CN113430650A (en) Middle and far infrared crystal LiGaGe2Se6Polycrystalline raw material synthesis method and single crystal growth method thereof
Saint-Martin et al. Single-crystal growth of Mg-and Ni-doped chain compound SrCuO2 by the traveling-solvent floating-zone method and chain breaking effect induced by the dopants
Zheng et al. A new approach to single crystal growth of CuO
Wang et al. Single‐crystal growth: From new borates to industrial semiconductors
Mikkelsen Jr Bridgman-Stockbarger crystal growth of Li2Ti3O7
CN105714376B (en) High/low temperature phase strontium borate cadmium crystal and preparation method and purposes
An et al. Single crystal growth of apatite-type Al-doped neodymium silicates by the floating zone method
Yu et al. Crystal growth and spectroscopic properties of MoO3 and WO3 doped Bi4Ge3O12 by optical floating zone method
CN103305912A (en) Cr, Tm, Ho-doped LaVO4 luminescent material and melting crystal growth method thereof
CN103305913A (en) Tm-doped ScVO4 luminescent material and melting crystal growth method thereof
CN110129878A (en) A kind of SnSe crystal and its growing method and application with high carrier concentration

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
WD01 Invention patent application deemed withdrawn after publication
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20160928