CN113026096B - Two-dimensional semiconductor material SnSe2Method for producing single crystal - Google Patents
Two-dimensional semiconductor material SnSe2Method for producing single crystal Download PDFInfo
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- CN113026096B CN113026096B CN202110146498.2A CN202110146498A CN113026096B CN 113026096 B CN113026096 B CN 113026096B CN 202110146498 A CN202110146498 A CN 202110146498A CN 113026096 B CN113026096 B CN 113026096B
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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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- 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
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/64—Flat crystals, e.g. plates, strips or discs
Abstract
The invention discloses a two-dimensional semiconductor material SnSe2The preparation method of the single crystal comprises the following steps: uniformly mixing Se powder and Sn powder, putting the mixture into a quartz tube, putting elementary iodine into the quartz tube, pumping the air pressure in the quartz tube to be less than or equal to 0.1mbar, and sealing the tube; putting the quartz tube into a double-temperature-zone tube furnace, placing one end filled with the raw materials in a high-temperature zone and the other end in a low-temperature zone, setting the temperature of the double-temperature zone at 560 ℃ and 600 ℃, and keeping the temperature constant for 1 day; then the temperature of the low temperature region is reduced to 550 ℃, the temperature of the high temperature region is kept at 560 ℃ and 600 ℃, and the temperature is kept for 5 to 7 days; cooling to room temperature, and maintaining the temperature difference between the high temperature region and the low temperature region at 10-50 deg.C to obtain flaky SnSe with large area and high quality2And (3) single crystal. The invention can prepare SnSe by one step2The single crystal is bright black and thin and flaky, has uniform components and smooth surface, is easy to mechanically peel, and is beneficial to the micro-processing technology such as photoetching on materials.
Description
Technical Field
The invention belongs to the field of two-dimensional materials, and relates to a two-dimensional semiconductor material SnSe2A preparation method of single crystal, in particular to a preparation method of large-area and high-quality two-dimensional intrinsic SnSe2A method of single crystal.
Background
Since the first report by Geim and Novoselov in 2004 that graphene is successfully prepared by a transparent tape stripping method, people are always trying to find two-dimensional materials and form a huge two-dimensional material family. Graphene has rich and peculiar physical properties, and has unique carrier characteristics and excellent electrical properties. The carriers in the graphene are dirac-fermi and have ultrahigh carrier mobility. However, perfect graphene is a zero-bandgap semiconductor, which hinders the application of graphene in semiconductor devices. A new two-dimensional material, two-dimensional semiconducting transition metal chalcogenides (TMDCs), has shown great potential in logic integration due to its appropriate bandgap (1-2eV), moderate carrier mobility, very high on-off current ratio, and good air stability and process compatibility. Meanwhile, the two-dimensional TMDCs have the advantages of integration over the traditional three-dimensional materials because the two-dimensional TMDCs have only a few atomic thicknesses. And the two-dimensional TMDCs do not have dangling bonds, the structure and the mobility are relatively stable, and the two-dimensional TMDCs become effective field effect tube channel materials due to the advantages, thereby showing potential application prospects in the fields of next generation of electronics and photoelectrons.
SnSe2As a novel two-dimensional semiconductor material, has the same structure as MoS2Similar structure. In addition, SnSe2Belongs to the group IVA-VIA, belongs to one of two-dimensional TMDCs, and SnSe2The method has the characteristics of abundant earth reserve resources, environmental friendliness, low cost and the like, and has obvious advantages in the fields of nano electronics and photoelectronics. Preparation of SnSe reported today2In the single crystal method, the product has defects due to the existence of inappropriate precursors or mixed products after the reaction, so that large-area and high-quality two-dimensional intrinsic SnSe cannot be obtained2Single crystals, further limiting their development in the field of optoelectronic devices.
Disclosure of Invention
The invention aims to: based on Chemical Vapor Transport (CVT), provides a two-dimensional semiconductor material SnSe which is beneficial to growing large area and high quality2A method for producing a single crystal.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
two-dimensional semiconductor material SnSe2A method for producing a single crystal, comprising the steps of:
step (1), uniformly mixing Se powder and Sn powder, putting the mixture into a quartz tube, adding a small amount of elemental iodine, pumping the air pressure in the quartz tube to be less than or equal to 0.1mbar, and sealing the tube;
step (2), placing the quartz tube into a double-temperature-zone tube furnace, placing one end filled with the raw materials in a high-temperature zone and the other end in a low-temperature zone, and setting the furnace temperature: the temperature of the two temperature areas is set to be 560-; then reducing the temperature of the low temperature region to 550 ℃, keeping the temperature of the high temperature region at 560 ℃ and 600 ℃, keeping the temperature difference between the high temperature region and the low temperature region at 10-50 ℃, and keeping the temperature difference for 5-7 days; then the temperature of the dual-temperature area is reduced to room temperature, the temperature difference between the high-temperature area and the low-temperature area is kept between 10 and 50 ℃ in the temperature reduction process, and the temperature difference between the high-temperature area and the low-temperature area is not required to be maintained after the low-temperature area is reduced to the room temperature;
step (3) taking out the quartz tube from the double-temperature-zone tube furnace to obtain the flaky SnSe2And (3) single crystal.
In the step (1), one end (namely the bottom) of the quartz tube is closed, the other end of the quartz tube is open, and Se powder, Sn powder and elementary iodine which are uniformly mixed are filled at the closed end of the quartz tube. When the tube is sealed, the quartz tube is inclined by 45 degrees, so that the height of the sealed end is lower than that of the open end, and the sample powder is prevented from being sucked backwards.
The operation of loading the uniformly mixed Se powder and Sn powder into a quartz tube is as follows: filling the uniformly mixed Se powder and Sn powder into the bottom of a quartz tube by using a paper cylindrical channel so as to prevent the raw materials from being adhered to the inner wall of the quartz tube; or the wall-hung powder is ultrasonically treated to the bottom of the quartz tube by an ultrasonic cleaning machine, and the ultrasonic treatment is generally carried out for 5-10 min.
The Se powder is elemental selenium powder, and the Sn powder is elemental tin powder. And uniformly mixing the Se powder and the Sn powder according to the molar ratio of 2: 1.
Specifically, Se powder and Sn powder are uniformly mixed in a grinding mode, and a mixed sample is gray black after grinding; the grinding time is about 10-15min, and the grinding time is not suitable for too long, so that the sample is prevented from being oxidized after being exposed in the air for a long time.
The elementary iodine is iodine balls (namely elementary iodine particles). The ratio of the weight of the iodine balls to the total weight of the Se powder and the Sn powder is (0.02-0.05): 1. The growth rate is influenced by the dosage of iodine, if the dosage is too large, the transport speed is too high, and the sample can grow into SnSe with smaller volume in a growth area (low-temperature area)2Crystal grains and flaky SnSe can not be obtained2Single crystal; if the iodine content is lower than the dosage requirement of the invention, the transmission speed is too slow, the sample can not grow in the growth region, or the obtained SnSe2Few single crystals; if elemental iodine is not used, the reaction cannot proceed.
Preferably, before packaging, the quartz tube is pre-vacuumized, argon gas is filled for washing until air is exhausted, and the air pressure in the quartz tube is pumped to be less than or equal to 0.1 mbar. After the tube is sealed, the quartz tube is kept in a vacuum state, oxygen is isolated, and oxide impurities are prevented from being generated in the reaction process.
Further preferably, the gas pressure in the quartz tube is evacuated by a molecular pump.
And (2) preferably, the temperature difference of the high-temperature area and the low-temperature area in the growth stage and the cooling stage is maintained at 10 ℃.
Preferably, the furnace temperature is set: the temperature of the double-temperature area is 560 ℃, and the double-temperature area is placed for 1 day at constant temperature; then the temperature of the low temperature area is reduced to 550 ℃, the temperature of the high temperature area is kept at 560 ℃, the temperature difference between the high temperature area and the low temperature area is kept at 10 ℃, and the temperature difference is kept for 5 days; then cooling to room temperature while maintaining the temperature difference between the high temperature region and the low temperature region at 10 ℃.
Further preferably, the furnace temperature is set: the double temperature zones are heated to 560 ℃ at the speed of 30 ℃/h and are placed for 1 day at constant temperature; the low temperature zone is reduced to 550 ℃ at the speed of 2 ℃/h, the high temperature zone is kept at 560 ℃, the temperature difference between the high temperature zone and the low temperature zone is kept at 10-50 ℃, and the temperature difference is kept for 5 days; and then, under the condition of keeping the temperature difference between the high-temperature area and the low-temperature area at 10 ℃, cooling the system to room temperature at the speed of 10 ℃/h, and slowly cooling to ensure that the reaction is fully carried out and the growth quality of the single crystal is ensured.
The invention has the beneficial effects that:
the invention adopts a chemical vapor transport method (CVT), a quartz tube which is filled with raw material powder and is packaged is placed into a double-temperature-zone tube furnace, under the action of temperature difference gradient of a high-temperature zone and a low-temperature zone, a small amount of iodine is used as a transport agent, Sn powder and Se powder in a source zone are transported to a low-temperature zone and grow in the low-temperature zone, and two-dimensional SnSe powder is prepared from powder elementary substance raw materials in one step2The single crystal is simple in equipment, easy to operate, easy to regulate and control experimental parameters, good in experimental repeatability, capable of directly growing to the single crystal in one step and effectively improving the preparation efficiency.
The two-dimensional SnSe obtained by the invention2The single crystal has semiconductor properties and is in a thin sheet shape, the thickness of the single crystal is close to that of paper and is about 0.05 mm; after the sample is characterized, the single crystal is found to have uniform components, flat surface and large enough areaThe mechanical stripping and transferring are easy, and the subsequent characterization is convenient; meanwhile, the method is also beneficial to the micromachining processes such as photoetching and the like on the material, and provides a simpler and easier preparation process for preparing the optoelectronic device.
Drawings
FIG. 1 shows Chemical Vapor Transport (CVT) growth of SnSe2A schematic view of a single crystal apparatus;
FIG. 2 shows SnSe obtained in example 12Sample pictures of the single crystal blocks (grid scale 5 mm).
FIG. 3 shows SnSe obtained in example 12An X-ray diffraction (XRD) pattern of the single crystal mass;
FIG. 4 shows SnSe obtained in example 12The Mapping mode atlas of the monocrystal block scanning electron microscope is as follows from left to right: the sample topography, the distribution of Se element and the distribution of Sn element.
FIG. 5 shows SnSe obtained in example 22Sample pictures of the single crystal blocks (grid scale 5 mm).
Detailed description of the invention
The technical solution of the present invention will be described below with reference to specific examples.
Example 1
Flaky two-dimensional SnSe easy to peel prepared based on Chemical Vapor Transport (CVT)2The single crystal preparation process includes the following steps:
step (1), weighing elemental selenium powder and elemental tin powder according to the molar ratio of Se powder to Sn powder of 2:1, wherein the total mass is 1 g; sequentially putting Sn powder and Se powder into a mortar according to the adhesiveness on weighing paper, and grinding for 10-15min in the mortar until the color is uniform gray black; the uniformly mixed powder sample is conveyed to a closed end (which can be called a source region) of a quartz tube (the size of the quartz tube is 300mm in length, 25mm in inner diameter and 100mm away from a quartz tube opening at a sealing position) through a paper cylinder channel;
adding a proper amount of iodine particles as a transmission agent into a quartz tube, wherein the dosage of 1g of sample iodine is generally 50mg, and the iodine particles are also arranged at the closed end of the quartz tube; because iodine is easy to deliquesce in the air, the iodine particles are filled in the iodine particles, the iodine particles are immediately pumped in vacuum by using a molecular pump, then argon is filled in the iodine particles, the quartz tube is cleaned for 2-3 times by using the argon, the air in the quartz tube is ensured to be exhausted, a sample cannot react with oxygen and the like to generate impurities, the air pressure of the quartz tube is kept less than or equal to 0.1mbar, and the quartz tube is packaged; during packaging, the quartz tube is inclined by 45 degrees, so that the height of the closed end is lower than that of the open end (end to be closed), and the sample powder is prevented from being sucked backwards.
Step (2), as shown in fig. 1, the packaged quartz tube is placed into a double-temperature-zone tube furnace, and the source area of the quartz tube is over against the high-temperature area of the double-temperature-zone tube furnace; setting the furnace temperature: double temperature zone (T)1,T2) Heating to 560 ℃ at the speed of 30 ℃/h, and placing the sample at constant temperature for 1 day; in the growth phase, a low temperature zone (T)1) Gradually decreases to 550 ℃ at a rate of 2 ℃/h, high temperature zone (T)2) Keeping the temperature at 560 ℃, keeping the temperature for 5 days, taking iodine as a transport agent in the state that the temperature difference between a high-temperature area and a low-temperature area is 10 ℃, transporting Sn powder and Se powder in the high-temperature area to the low-temperature area, and growing in the low-temperature area; then, the system is cooled at the speed of 10 ℃/h by keeping the temperature gradient (the temperature difference between the high-temperature area and the low-temperature area is 10 ℃), and the temperature difference between the high-temperature area and the low-temperature area does not need to be maintained after the low-temperature area is cooled to the room temperature; obtaining large-area flaky two-dimensional SnSe in low-temperature region2Single crystal, bright black;
and (3) taking out the quartz tube from the double-temperature-zone tube furnace.
SnSe obtained in the example2Single crystal characterization results were as follows:
FIG. 2 is photographed SnSe2Single crystal of SnSe2The single crystal area is large enough and the surface is flat.
FIG. 3 is a representation of an X-ray diffraction spectrometer showing sharp peaks, narrow peak widths, and high peaks, indicating SnSe2The single crystal has good crystallinity, high sample quality and few defects.
FIG. 4 is a Mapping mode map of a Scanning Electron Microscope (SEM), which shows that Sn and Se are uniformly distributed in a sample, and the surface of the sample is flat, thereby facilitating the subsequent peeling experiment.
Example 2
Referring to the method of example 1, only the growth stage, the temperature reduction stage and the high temperature region of step (2) were adjustedThe temperature difference was maintained at 20 ℃ and the temperature in the low temperature region was maintained at 550 ℃. The present example also enables the production of SnSe2Single crystal (see fig. 5).
SnSe obtained in example 12Compared with single crystal, the SnSe of the embodiment2The single crystal had a small area and the surface was inferior to that of SnSe obtained in example 12And (4) flattening the single crystal.
Claims (6)
1. Two-dimensional semiconductor material SnSe2A method for producing a single crystal, characterized in that: the method comprises the following steps:
uniformly mixing Se powder and Sn powder, putting the mixture into a quartz tube, putting elementary iodine into the quartz tube, pre-vacuumizing the quartz tube, filling argon for washing until air is exhausted, pumping the air pressure in the quartz tube to be less than or equal to 0.1mbar, and sealing the quartz tube; wherein the ratio of the weight of the elementary iodine to the total weight of the Se powder and the Sn powder is (0.02-0.05): 1;
step (2), placing the quartz tube into a double-temperature-zone tube furnace, placing one end filled with the raw materials in a high-temperature zone and the other end in a low-temperature zone, and setting the furnace temperature: the temperature of the double-temperature area is 560 ℃, and the double-temperature area is placed for 1 day at constant temperature; then the temperature of the low temperature area is reduced to 550 ℃, the temperature of the high temperature area is kept at 560 ℃, the temperature difference between the high temperature area and the low temperature area is kept at 10 ℃, and the temperature difference is kept for 5 days; then cooling the high-temperature area and the low-temperature area under the condition of keeping the temperature difference of 10 ℃;
step (3) taking out the quartz tube from the double-temperature-zone tube furnace to obtain the flaky SnSe2And (3) single crystal.
2. The method for preparing the two-dimensional semiconductor material SnSe2 single crystal according to claim 1, wherein: one end of the quartz tube is closed, the other end of the quartz tube is open, and Se powder, Sn powder and elementary iodine which are uniformly mixed are arranged at the closed end of the quartz tube.
3. The method for preparing the two-dimensional semiconductor material SnSe2 single crystal according to claim 1, wherein: in the step (1), Se powder and Sn powder are uniformly mixed according to the molar ratio of 2: 1.
4. Two-dimensional semiconductor material SnSe of claim 12A method for producing a single crystal, characterized in that: the Se powder is elemental selenium powder, and the Sn powder is elemental tin powder; the elementary iodine is iodine balls.
5. Two-dimensional semiconductor material SnSe of claim 12A method for producing a single crystal, characterized in that: in the step (1), when the tube is sealed, the quartz tube is inclined by 45 degrees, so that the height of the sealed end is lower than that of the open end.
6. Two-dimensional semiconductor material SnSe of claim 12A method for producing a single crystal, characterized in that: in the step (2), setting the furnace temperature: the double temperature zones are heated to 560 ℃ at the speed of 30 ℃/h and are placed for 1 day at constant temperature; the low temperature zone is reduced to 550 ℃ at the rate of 2 ℃/h, the high temperature zone is kept at 560 ℃, the temperature difference between the high temperature zone and the low temperature zone is kept at 10 ℃, and the temperature difference is kept for 5 days; then cooling at a speed of 10 ℃/h while keeping the temperature difference between the high-temperature area and the low-temperature area at 10 ℃.
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| CN114540944B (en) * | 2022-01-24 | 2023-05-12 | 天津理工大学 | Vertical CVT seed crystal method for preparing outer layer method for preparing crystalline metal oxide |
| CN114686986B (en) * | 2022-04-02 | 2023-03-28 | 齐齐哈尔大学 | SnSe 2 Method for producing single crystal |
| CN116575121B (en) * | 2023-05-09 | 2023-12-19 | 中国科学院宁波材料技术与工程研究所 | Monocrystalline Cr with high orientation 2 AlC material and preparation method thereof |
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| CN104962990A (en) * | 2015-07-23 | 2015-10-07 | 华中科技大学 | Preparation method of two-dimensional nano SnSe2 crystal material |
| CN112064116A (en) * | 2020-09-14 | 2020-12-11 | 中国科学院上海硅酸盐研究所 | Method for preparing InSeI single crystal |
| CN113410287A (en) * | 2020-03-17 | 2021-09-17 | 华中科技大学 | Two-dimensional SnSe-SnSe2P-n heterojunction and preparation method thereof |
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| CN104962990A (en) * | 2015-07-23 | 2015-10-07 | 华中科技大学 | Preparation method of two-dimensional nano SnSe2 crystal material |
| CN113410287A (en) * | 2020-03-17 | 2021-09-17 | 华中科技大学 | Two-dimensional SnSe-SnSe2P-n heterojunction and preparation method thereof |
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