CN114645326B - Preparation method of InTeI single crystal - Google Patents
Preparation method of InTeI single crystal Download PDFInfo
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- CN114645326B CN114645326B CN202011509550.8A CN202011509550A CN114645326B CN 114645326 B CN114645326 B CN 114645326B CN 202011509550 A CN202011509550 A CN 202011509550A CN 114645326 B CN114645326 B CN 114645326B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000013078 crystal Substances 0.000 title claims description 31
- 239000010453 quartz Substances 0.000 claims abstract description 68
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 68
- 239000000126 substance Substances 0.000 claims abstract description 23
- 238000010438 heat treatment Methods 0.000 claims abstract description 22
- 239000002994 raw material Substances 0.000 claims abstract description 18
- 238000001816 cooling Methods 0.000 claims abstract description 16
- 238000000137 annealing Methods 0.000 claims abstract description 13
- 238000004321 preservation Methods 0.000 claims abstract description 9
- 238000011065 in-situ storage Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 25
- 239000000843 powder Substances 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 14
- 238000006243 chemical reaction Methods 0.000 description 11
- 239000000047 product Substances 0.000 description 8
- 238000004140 cleaning Methods 0.000 description 7
- 239000008367 deionised water Substances 0.000 description 7
- 229910021641 deionized water Inorganic materials 0.000 description 7
- 239000012535 impurity Substances 0.000 description 7
- 238000002844 melting Methods 0.000 description 7
- 230000008018 melting Effects 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 238000005245 sintering Methods 0.000 description 6
- 238000002156 mixing Methods 0.000 description 5
- 238000007789 sealing Methods 0.000 description 4
- 238000005520 cutting process Methods 0.000 description 3
- 239000000155 melt Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000012856 weighed raw material Substances 0.000 description 1
Classifications
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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
- C30B29/12—Halides
-
- 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
- C30B28/04—Production of homogeneous polycrystalline material with defined structure from liquids
-
- 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
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/02—Heat treatment
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- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
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- Thermal Sciences (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to a preparation method of an InTeI monocrystal. The preparation method comprises the following steps: in the form of simple substances of In, te and I 2 Raw materials are mixed and placed in a quartz tube, and the quartz tube is vacuumized and sealed; placing the sealed quartz tube into a muffle furnace, heating to 475 ℃ and preserving heat for 10-30 hours, cooling to 192+/-5 ℃ and annealing in situ for 20-80 hours at the temperature; placing the annealed quartz tube in a double-temperature-zone tube furnace for heat preservation for 7-14 days, and cooling to obtain an InTeI monocrystal; wherein the temperature range of the tube furnace with the double temperature areas is 350-500 ℃.
Description
Technical Field
The invention relates to a preparation technology and a process of an InTeI single crystal, in particular to a method for preparing the InTeI single crystal by combining a melt method and a Physical Vapor Transport (PVT) method.
Background
The InTeI single crystal is a novel two-dimensional semiconductor material. The first principle calculation shows that the band gap of the single layer of the InTeI single crystal is 2.735eV, the band gap is related to the InTeI layer number, the band gap can be regulated and controlled by changing the layer number of the InTeI single crystal, and the anisotropic electron mobility is up to 12137.80cm 2 V -1 s -1 This shows the great potential of InTeI single crystals in nanoelectronics and optoelectronics, but InTeI single crystalsThe synthesis of crystals is also a problem.
In the conventional technology, in is adopted 2 Te 3 With InI 3 Chemical vapor transport reactions take place in a sealed container to obtain the InTeI single crystal. The method requires the synthesis of In 2 Te 3 And InI 3 The whole process for preparing the InTeI single crystal is complicated, and In is synthesized 2 Te 3 May have In the process of (C) 3 Te 4 、In 4 Te 7 And the generation of the impurities is difficult, the reaction process is not easy to control, and InTeI single crystals are not easy to obtain.
Disclosure of Invention
Based on the technical problems, the invention provides a simple and effective preparation method of an InTeI monocrystal, which comprises the following steps: in the form of simple substances of In, te and I 2 Raw materials are mixed and placed in a quartz tube, and the quartz tube is vacuumized and sealed; placing the sealed quartz tube into a muffle furnace, heating to 475 ℃ and preserving heat for 10-30 hours, cooling to 192+/-5 ℃ and annealing in situ for 20-80 hours at the temperature; placing the annealed quartz tube in a double-temperature-zone tube furnace for heat preservation for 7-14 days, and cooling to obtain an InTeI monocrystal; wherein the temperature range of the tube furnace with the double temperature areas is 350-500 ℃.
The invention mixes the raw materials and then places the mixed raw materials into a quartz tube, the quartz tube is vacuumized and then sealed, and the vacuum melting environment avoids introducing impurities. The sealed quartz tube is placed into a muffle furnace, and the temperature is raised to 475 ℃ or higher, so that the raw materials or the generated product InTeI (melting point 475 ℃) are all in a molten state. Then annealing at a certain temperature (192+ -5 ℃), during the melting or cooling process, inTeI is easily decomposed into In 2 Te 3 And InI 3 While annealing at 192.+ -. 5 ℃ for a long period of time enables the intermediate product In 2 Te 3 And InI 3 Can fully react to generate pure phase InTeI. Then placing the single crystal into a double-temperature zone tube furnace, and preserving the heat for 7-14 days at 350-500 ℃, thereby further preparing the single crystal by using PVT method and increasing the size of the single crystal.
The preparation process of the InTeI single crystal comprises complex thermodynamic and kinetic changes, and the reaction process can be summarized as follows:
the first stage reaction of In+Te- & gtIn occurs In a muffle furnace 2 Te 3 ，In+I→InI 3 ，In 2 Te 3 +InI 3 -InTeI (polycrystalline);
the second stage reaction, inTeI (polycrystalline) to InTeI (single crystal), takes place in a double-temperature zone tube furnace.
Preferably, the elements In, te and I 2 The molar ratio of (2) is 1:1 (1-1.05). The invention ensures no In by strictly controlling the component molar ratio In: te=1:1 In the preparation process and annealing at a certain temperature after cooling 3 Te 4 、In 4 Te 7 And generating impurities.
Preferably, the elements In, te and I 2 The molar ratio of (2) is 1:1:1.02.I 2 The simple substance is slightly excessive because it needs to act as a transport agent and compensate for I 2 The volatilization of the simple substance, especially the volatilization in the high temperature tube sealing process.
The simple substances of In, te and I 2 The purity of the product is above 99.99%. High-purity raw materials are adopted, so that impurities are prevented from being introduced from the source.
Preferably, the elements In, te and I 2 Selected from powders having an average particle size of 0.5-5 μm, can ensure adequate mixing of the raw materials.
Preferably, the length of the quartz tube is about 15-25cm and the inner diameter is about 15-25mm.
Preferably, the quartz tube is placed into a muffle furnace, the temperature is raised to 500-550 ℃, and the heat preservation time is 12-24 hours. The temperature range is set to 475 ℃ or higher of the melting point of InTeI, so that InTeI polycrystal can be generated from the raw material, and if the temperature is too high or low, inTeI polycrystal cannot be generated.
Preferably, the annealing temperature is 192+/-5 ℃ and the annealing time is 24-72 hours.
Preferably, the temperature rising rate of the muffle furnace is set to be 0.5-2 ℃/min. Preferably, the quartz tube is placed into a double-temperature-zone tube furnace for heating, the temperature difference of two ends is set to 80-120 ℃, the temperature is kept for 7-14 days, and the quartz tube naturally falls to room temperature after the temperature is kept.
The beneficial effects are that:
the invention is thatThree high purity simple substances of In, te and I 2 The method comprises the steps of mixing and heating raw materials to a temperature above the melting point of InTeI by a melt method, annealing at a certain temperature to obtain InTeI polycrystal material, and preparing InTeI monocrystal by a physical vapor transmission method instead of polycrystal and impurity-free phase.
Drawings
Fig. 1 shows the single crystal of InTeI prepared in example 1, and it can be seen from fig. 1 that the single crystal has a regular geometry.
Fig. 2 shows the single crystal of InTeI prepared in example 2, and it can be seen from fig. 2 that the single crystal has a regular geometry.
Fig. 3 shows the single crystal of InTeI prepared in example 3, and it can be seen from fig. 3 that the single crystal has a regular geometry.
Fig. 4 shows the profile of the sample of example 1 measured by a powder X-ray diffractometer, and according to the bragg equation, four peaks of the measured substance are completely coincident with the corresponding peaks along the (X0 0) plane in the PDF #83-1788 card, and the sample is seen to be an InTeI single crystal.
Figure 5 shows the XRD pattern of the product obtained in comparative example 1, which shows that the sample obtained is the InTeI polycrystalline phase.
FIG. 6 shows the XRD pattern of the product obtained In comparative example 2, showing that In addition to InTeI, there is In the sample obtained 2 Te 3 And (5) generating.
FIG. 7 shows the XRD pattern of the product obtained In comparative example 3, showing that In addition to InTeI, there is In the obtained sample 1.33 Te 2 And In 7 Te 10 。
Detailed Description
The invention will be further described with reference to the accompanying drawings and the following embodiments, it being understood that the following embodiments are only illustrative of the invention and not limiting thereof.
The invention provides a preparation method of an InTeI monocrystal. The method uses In, te and I 2 The method comprises the steps of uniformly mixing raw materials, heating the mixture to above the melting point of InTeI (above 475 ℃), preferably 500-550 ℃ by a melt method, annealing at the decomposition temperature of InTeI (192+/-5 ℃), and growing by a physical vapor transport method to obtain InTeI single crystals.
The following illustrates an exemplary method for preparing the InTeI single crystal provided by the invention.
The invention uses micron-sized In, te and I with purity not lower than 99.99% 2 The three simple substances are used as raw materials and are uniformly mixed. When the raw materials are selected, powder can be selected as the raw materials for ensuring the full mixing of the raw materials, and the average particle size can be 0.5-5 mu m. Due to the simple substance I 2 Is easy to volatilize, especially the volatilization is faster in the high-temperature tube sealing process, and when the raw materials are selected, a small excess amount of I should be selected 2 Simple substances, e.g. In, te, I 2 The ratio of the three elements can be 1:1:1 (1-1.05), preferably 1:1:1.02.
Transferring the weighed raw materials into a clean quartz tube, and sequentially ultrasonically cleaning the fired quartz tube by using acetone and deionized water for 0.5-2 hours to ensure that the quartz tube is free of impurities and moisture. The raw materials are fully and uniformly mixed, then the air in the quartz tube is pumped to vacuum by using a vacuum pump, and finally the tube is sealed by using an oxyhydrogen mixing flame (safety is required during tube sealing).
And (3) placing the quartz tube subjected to tube sealing in a muffle furnace, heating to above the InTeI melting point (475 ℃), wherein the heating rate is 0.5-2 ℃/min, and in order to ensure that the quartz tube is heated sufficiently and save heating time, the quartz tube can be preferably heated at 500-550 ℃, kept for 12-24 hours, then annealed at 192+/-5 ℃ for 24-72 hours, and naturally cooled to room temperature after the annealing is finished.
And placing the annealed quartz tube in a double-temperature-zone tube furnace, taking attention to placing the raw materials at a high-temperature end, setting the temperature of the double-temperature-zone tube furnace to 350-500 ℃, keeping the temperature difference between two ends at 80-120 ℃, and preserving the heat for 7-14 days. Naturally cooling to room temperature. After the reaction is completed, the quartz tube is cut, and the obtained reddish brown sheet is the InTeI monocrystal.
The present invention will be further illustrated by the following examples. It is also to be understood that the following examples are given solely for the purpose of illustration and are not to be construed as limitations upon the scope of the invention, as many insubstantial modifications and variations are within the scope of the invention as would be apparent to those skilled in the art in light of the foregoing disclosure.
Example 1
And cleaning the quartz tube for 0.5h by using acetone and deionized water in sequence, and drying. In, te and I with the mol ratio of 1:1:1.02 are mixed 2 The three single substances are put into a quartz tube and are uniformly mixed. The air in the quartz tube was evacuated using a vacuum pump. And sintering with mixed flame composed of hydrogen and oxygen to seal. Then the quartz tube is horizontally placed in a muffle furnace, and is heated to 500 ℃, the heating rate is 1 ℃/min, the heat is preserved for 720min, and then the quartz tube is preserved for one day at 192 ℃ and is cooled to room temperature. And then the quartz tube is taken out and placed in a double-temperature-zone tube furnace for heating. Setting a high temperature region of 500 ℃ and a low temperature region of 400 ℃. After the heat preservation is carried out for 8 days, naturally cooling to room temperature, and after the reaction is finished, cutting a quartz tube, wherein the reddish brown sheet-shaped object is the InTeI single crystal. As can be seen from FIG. 4, according to the Bragg equation, the four peaks of the measured substance are completely matched with the corresponding peaks along the (x 0 0) plane in the PDF#83-1788 card, so that the measured substance is an InTeI single crystal.
Example 2
And cleaning the quartz tube for 0.5h by using acetone and deionized water in sequence, and drying. In, te and I with the mol ratio of 1:1:1.02 are mixed 2 The three single substances are put into a quartz tube and are uniformly mixed. The air in the quartz tube was evacuated using a vacuum pump. And sintering with mixed flame composed of hydrogen and oxygen to seal. Then horizontally placing the quartz tube in a muffle furnace, raising the temperature to 500 ℃, keeping the temperature at a heating rate of 5-10 ℃/min for 720min, keeping the temperature at 192 ℃ for one day, and cooling to room temperature. And then the quartz tube is taken out and placed in a double-temperature-zone tube furnace for heating. The high temperature region is set at 450 ℃ and the low temperature region is set at 350 ℃. After the heat preservation is carried out for 8 days, naturally cooling to room temperature, and after the reaction is finished, cutting a quartz tube, wherein the reddish brown sheet-shaped object is the InTeI single crystal. Both the test procedure and the analysis of the results were the same as in example 1.
Example 3
And cleaning the quartz tube for 0.5h by using acetone and deionized water in sequence, and drying. In, te and I with the mol ratio of 1:1:1.05 are added into the catalyst 2 The three single substances are put into a quartz tube and are uniformly mixed. The air in the quartz tube was evacuated using a vacuum pump. And sintering with mixed flame composed of hydrogen and oxygen to seal. Then horizontally placing the quartz tube in a muffle furnace, heating to 500 ℃, heating up to 1 ℃/min, preserving heat for 720min, and then heating up to 192 DEG CPreserving heat for one day, and cooling to room temperature. And then the quartz tube is taken out and placed in a double-temperature-zone tube furnace for heating. Setting a high temperature region of 500 ℃ and a low temperature region of 400 ℃. After the heat preservation is carried out for 8 days, naturally cooling to room temperature, and after the reaction is finished, cutting a quartz tube, wherein the reddish brown sheet-shaped object is the InTeI single crystal. Both the test procedure and the analysis of the results were the same as in example 1.
Comparative example 1
And cleaning the quartz tube for 0.5h by using acetone and deionized water in sequence, and drying. In, te and I with the mol ratio of 1:1:1.02 are mixed 2 The three single substances are put into a quartz tube and are uniformly mixed. The air in the quartz tube was evacuated using a vacuum pump. And sintering with mixed flame composed of hydrogen and oxygen to seal. Then the quartz tube is horizontally placed in a muffle furnace, and is heated to 500 ℃, the heating rate is 1 ℃/min, the heat is preserved for 720min, and then the quartz tube is preserved for one day at 192 ℃ and is cooled to room temperature. The resulting product was selected and tested by XRD (XRD pattern see FIG. 5) to give InTeI polycrystals.
Comparative example 2
And cleaning the quartz tube for 0.5h by using acetone and deionized water in sequence, and drying. In, te and I with the mol ratio of 1:1:1.02 are mixed 2 The three single substances are put into a quartz tube and are uniformly mixed. The air in the quartz tube was evacuated using a vacuum pump. And sintering with mixed flame composed of hydrogen and oxygen to seal. Then the quartz tube is horizontally placed in a muffle furnace, the temperature is raised to 500 ℃, the heating rate is 1 ℃/min, the heat is preserved for 720min, and then the quartz tube is preserved for one day at 180 ℃ and is cooled to the room temperature. And then the quartz tube is taken out and placed in a high-temperature zone of the double-temperature zone tube furnace for heating. Setting a high temperature region of 500 ℃ and a low temperature region of 400 ℃. After 8 days of heat preservation, naturally cooling to room temperature. After the reaction was completed, the quartz tube was cut, and XRD test (XRD pattern see FIG. 6) was performed, and the test product found that the obtained InTeI product was impure and had In 2 Te 3 And generating impurities.
Comparative example 3
And cleaning the quartz tube for 0.5h by using acetone and deionized water in sequence, and drying. The three simple substances of In, te and I2 with the molar ratio of 1:1:1.02 are put into a quartz tube and uniformly mixed. The air in the quartz tube was evacuated using a vacuum pump. And sintering with mixed flame composed of hydrogen and oxygen to seal. However, the method is thatThen the quartz tube is horizontally placed in a muffle furnace, the temperature is raised to 500 ℃, the heating rate is 1 ℃/min, the heat is preserved for 720min, and then the quartz tube is preserved for one day at 200 ℃ and is cooled to the room temperature. And then the quartz tube is taken out and placed in a high-temperature zone of the double-temperature zone tube furnace for heating. Setting a high temperature region of 500 ℃ and a low temperature region of 400 ℃. After 8 days of heat preservation, naturally cooling to room temperature. After the reaction was completed, the quartz tube was cut and XRD (XRD pattern, see FIG. 7) was tested to find that the InTeI was impure and had In 1.33 Te 2 And In 7 Te 10 And generating impurities.
Claims (7)
1. A method for preparing an InTeI single crystal, comprising:
in the form of simple substances of In, te and I 2 Raw materials are mixed and placed in a quartz tube, and the quartz tube is vacuumized and sealed;
placing the sealed quartz tube into a muffle furnace, heating to 500-550 ℃ for 10-30 hours, cooling to 192+/-5 ℃ and annealing in situ for 20-80 hours at the temperature;
placing the annealed quartz tube in a double-temperature-zone tube furnace for heat preservation for 7-14 days, and cooling to obtain an InTeI monocrystal;
wherein the temperature range of the tube furnace with the double temperature areas is 350-500 ℃, and the temperature difference between two ends is set to 80-120 ℃.
2. The method according to claim 1, wherein the simple substances In, te and I 2 The molar ratio of (2) is 1:1 (1-1.05).
3. The method according to claim 1, wherein the simple substances In, te and I 2 The purity of the product is above 99.99%.
4. The method according to claim 1, wherein the simple substances In, te and I 2 Selected from powders having an average particle size of 0.5-5 μm.
5. The method according to claim 1, wherein the quartz tube has a length of 15-25cm and an inner diameter of 15-25mm.
6. The preparation method according to claim 1, wherein the quartz tube is placed in a muffle furnace, heated to 500-550 ℃, and kept for 12-24 hours; the annealing temperature is 192+/-5 ℃ and the annealing time is 24-72 hours.
7. The method according to any one of claims 1 to 6, wherein the muffle is set to a temperature increase rate of 0.5-2 ℃/min.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2292853A1 (en) * | 1998-12-21 | 2000-06-21 | Pirelli Cavi E Sistemi S.P.A. | Process and apparatus for synthesizing and growing crystals |
| CN101550586A (en) * | 2009-03-27 | 2009-10-07 | 上海应用技术学院 | Growing technique of ZnTe monocrystal |
| WO2012079439A1 (en) * | 2010-12-14 | 2012-06-21 | 北京天科合达蓝光半导体有限公司 | Process for growing silicon carbide single crystal by physical vapor transport method and annealing silicon carbide single crystal in situ |
| 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 |
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|---|---|---|---|---|
| CN111979581B (en) * | 2019-05-22 | 2022-05-31 | 清华大学 | MnBi2Te4Method for producing bulk single crystal |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2292853A1 (en) * | 1998-12-21 | 2000-06-21 | Pirelli Cavi E Sistemi S.P.A. | Process and apparatus for synthesizing and growing crystals |
| CN101550586A (en) * | 2009-03-27 | 2009-10-07 | 上海应用技术学院 | Growing technique of ZnTe monocrystal |
| WO2012079439A1 (en) * | 2010-12-14 | 2012-06-21 | 北京天科合达蓝光半导体有限公司 | Process for growing silicon carbide single crystal by physical vapor transport method and annealing silicon carbide single crystal in situ |
| 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 |
Non-Patent Citations (2)
| Title |
|---|
| Jiang, SJ 等.InTeI: a novel wide-bandgap 2D material with desirable stability and highly anisotropic carrier mobility.NANOSCALE.2020,第12卷(第10期),5888-5897. * |
| 周玄 等.InSeI 单晶的制备及其结构与性能研究.人工晶体学报.2020,第49卷(第12期),2252-2255. * |
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