CN115216845B - Co-based ternary insulator single crystal with centimeter-level size and preparation method thereof - Google Patents
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- 239000013078 crystal Substances 0.000 title claims abstract description 62
- 239000012212 insulator Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000000126 substance Substances 0.000 claims abstract description 8
- 239000010453 quartz Substances 0.000 claims description 29
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 29
- 238000007789 sealing Methods 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 14
- 238000005303 weighing Methods 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 6
- 229910052740 iodine Inorganic materials 0.000 claims description 6
- 239000011630 iodine Substances 0.000 claims description 6
- 238000000137 annealing Methods 0.000 claims description 5
- XSOKHXFFCGXDJZ-UHFFFAOYSA-N telluride(2-) Chemical compound [Te-2] XSOKHXFFCGXDJZ-UHFFFAOYSA-N 0.000 claims description 4
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical group II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
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- 239000000523 sample Substances 0.000 description 11
- 238000012360 testing method Methods 0.000 description 9
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- 230000000704 physical effect Effects 0.000 description 5
- 238000012552 review Methods 0.000 description 5
- 238000001228 spectrum Methods 0.000 description 5
- 238000001816 cooling Methods 0.000 description 3
- 238000000724 energy-dispersive X-ray spectrum Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000005641 tunneling Effects 0.000 description 3
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000001237 Raman spectrum Methods 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
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- 239000004332 silver Substances 0.000 description 2
- WKBPZYKAUNRMKP-UHFFFAOYSA-N 1-[2-(2,4-dichlorophenyl)pentyl]1,2,4-triazole Chemical compound C=1C=C(Cl)C=C(Cl)C=1C(CCC)CN1C=NC=N1 WKBPZYKAUNRMKP-UHFFFAOYSA-N 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 229910005642 SnTe Inorganic materials 0.000 description 1
- 229910004523 TaCo Inorganic materials 0.000 description 1
- 244000309464 bull Species 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
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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
-
- 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
- C30B1/02—Single-crystal growth directly from the solid state by thermal treatment, e.g. strain annealing
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Abstract
The invention discloses a Co-based ternary insulator monocrystal with a centimeter-level size and a preparation method thereof, wherein the chemical formula of the monocrystal material is Ta 1‑x Co 1‑y Te 2±z X, y, z is less than or equal to 0.1. The invention adopts chemical gas phase transportation method, mixes raw materials in air environment, and successfully prepares Co-based ternary insulator monocrystal TaCoTe with centimeter-level size by using simple equipment in relatively short time and relatively low temperature 2 A block body. TaCoTe in the invention 2 The single crystal belongs to monoclinic system, and the space group is P2 1 C, the lattice constants are a= 8.152 (4) a, b= 6.264 (9) a, c=7.794 (5) a, the sample is van der waals layered crystal, and the maximum single crystal size is about 1.3cm, and the sample is stable in air. Co-based ternary insulator TaCoTe prepared by the invention 2 Single crystal materials, electrical transport is manifested as insulator behavior, and low temperature, resistance-like saturation characteristics.
Description
Technical Field
The invention belongs to the field of material science, and particularly relates to a Co-based ternary insulator monocrystal with a centimeter-level size and a preparation method thereof.
Background
Insulator materials with novel properties will play an important role in future electronic devices and have received extensive attention from researchers for many years. For example, topologically protected metal surface states in topological insulators and topologically crystalline insulators have potential application advantages in future quantum computing and future electronics, so exploring and delving new insulator materials would have extraordinary significance for future quantum computing and electronics development and application. It has been found that insulators with novel properties do not contain magnetic elements unless doped with magnetic elements, such as Bi 2 Te 3 、Bi 2 Se 3 And Sb (Sb) 2 Te 3 (Nature Physics 5 , 438, 2009)，Bi 2+x Te 2-x Se(Physical Review B, 86, 165119, 2012)，SmB 6 (Physical Review B, 91(20), 205133, 2015)，SnTe (Nature Physics, 8, 800-803, 2012)、Pb 1-x Sn x Te(Nature Communication, 3, 1192, 2012)、Pb 1-x Sn x Se(Nature Materials, 11, 1023-1027, 2012)、Ta 2 Pd 3 Te 5 (Physical Review B, 104, L241408, 2021)，ThTaN 3 (Physical Review B, 97, 121104 (R), 2018), etc., which are detrimental to the development of basic and practical studies of intrinsic magnetic regulation with novel insulator properties. Therefore, research into the field of novel layered insulators containing magnetic elements, which have novel physical properties, and physical properties have been conducted, will greatly advance the research of such insulators. The research shows that the ternary compounds containing Ta, co and Te and the research on physical properties thereof are not reported in many cases. Ta 4 CoTe 4 The poly (Mater Res Bull 29,327 1994) and TaCo 2 Te 2 The single crystal (Advanced Functional Materials, 2108920, 2021) exhibits metallic appearance; taCoTe 2 Polycrystalline and use of TeCl 4 TaCoTe prepared by keeping temperature of 900 ℃ for 5 days (high temperature and long time) as transport agent 2 The single crystal has only crystal structure information and no physical property information (Inorganic Chemistry, 4829, 1993), and the raw materials need to be handled in a glove box and are not simple; recent theoretical calculation of monolayer TaCoTe 2 Dirac fermi (Physical Review B, 100, 205102, 2019) is present. Obviously, the current insulating single crystal materials containing Ta, co and Te and research thereof are still to be developed, so that the research of preparing Co-based ternary insulator single crystal materials, particularly in centimeter-level size, by using simple equipment at a relatively environment-friendly transport agent in a relatively short time and at a relatively low temperature is necessary, not only can enrich the family of insulators, but also provides a new research object for researching novel insulator properties, and in addition, the insulator single crystal containing the magnetic element is also a potential carrier for comparing the physical properties of topological materials with experimental results.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for preparing Co-based ternary insulator monocrystal with a centimeter-level size at a lower temperature in a shorter time and by using environment-friendly transport agent iodine.
In order to achieve the aim of the invention, the invention adopts the following technical scheme:
a preparation method of Co-based ternary insulator single crystals with centimeter-level size comprises the following steps:
1) Weighing raw materials and sealing
Weighing a Ta source, a Co source and a Te source as raw materials or polycrystalline powder which accords with the molar ratio as raw materials according to the molar ratio of Ta, co and Te of 1:1 (2-15), uniformly mixing the raw materials and a transport agent in an air environment, then filling the mixture into a high-purity quartz tube, and carrying out vacuum sealing on the quartz tube, wherein the pressure intensity in the quartz tube after sealing is less than or equal to 0.1Pa;
2) Heating and annealing process
Placing the sealed quartz tube in a temperature gradient furnaceSetting the low temperature end temperature to 550-750 ℃ and the high temperature end temperature to 650-850 ℃ in a single-temperature area or double-temperature area tube furnace, placing the raw material end at the high temperature end, and starting to set the programmed temperature: the high temperature end and the low temperature end are heated from room temperature to a set temperature at uniform speed for 12-60 hours, then are kept for at least 48 hours, the furnace is naturally cooled to room temperature after the heat preservation is finished, and the layered Ta is obtained at the low temperature end 1-x Co 1-y Te 2±z Single crystal, x, y, z +.0.1.
Further, in the step 1), the Ta source is a Ta simple substance or a telluride of Ta, the Co source is a Co simple substance or a telluride of Co, and the Te source is a Te simple substance.
Preferably, the pressure in the quartz tube is 10 -4 Pa ~0.1 Pa。
Further, in the step 1), the sealing length of the quartz tube is 5-50cm.
Further, the transporter iodine was weighed at (1-20) mg/mL in terms of the volume inside the quartz tube after sealing.
Ta produced by the foregoing method 1-x Co 1-y Te 2±z And (3) single crystals.
The Ta is 1-x Co 1-y Te 2±z The size of the single crystal is 0.1-1.3. 1.3 cm.
The invention takes a mixture of a Ta source, a Co source and a Te source or polycrystalline powder which accords with the molar ratio as a raw material and takes iodine which is friendly to the environment as a transport agent. The weighed raw materials are mixed in dry air and then are put into a high-purity quartz tube with special structure or other tubes which are not reacted with the raw materials and are similar to the quartz tube, and Co-based ternary insulator monocrystal TaCoTe with centimeter-level size is prepared at lower temperature and shorter time by utilizing the reversible chemical reaction principle and precisely controlling the temperature gradient 2 A block body. TaCoTe can be regulated by changing the preparation conditions 2 The elemental proportion of the single crystal, i.e. Ta 1-x Co 1-y Te 2±z (x,y,z<=0.1). The invention provides a Co-based ternary insulator TaCoTe with a growth centimeter-level size 2 The method of monocrystal with maximum length up to near cm level enriches the variety of Ta, co and Te compounds and expands the research range of layered insulator monocrystal materialThe method has the advantages of low cost, easy control, good repeatability, simple equipment and the like. The Co-based ternary insulator TaCoTe with the centimeter-level size 2 The monocrystal has good crystallization performance, no impurity phase, lamellar block, and can be cleaved into few layers and is stable in air. The electric transport of the material is represented by the behavior of an insulator, and the characteristic of resistance-like saturation appears at low temperature. The 5K scanning tunneling microscope spectrum shows the presence of a band gap.
Drawings
FIG. 1 shows TaCoTe according to example 1 of the present invention 2 The outline and the size of the single crystal (left) and the schematic diagram of the crystal structure (right);
FIG. 2 is TaCoTe according to example 1 of the present invention 2 EDS spectra of single crystals;
FIG. 3 is TaCoTe according to example 1 of the present invention 2 Powder X-ray diffraction pattern of single crystal;
FIG. 4 is TaCoTe according to example 1 of the present invention 2 A resistance temperature profile of the single crystal;
FIG. 5 is TaCoTe according to example 1 of the present invention 2 Raman spectrum of single crystal;
FIG. 6 is TaCoTe according to example 1 of the present invention 2 Single crystal 5K scanning tunneling microscope energy spectrum
FIG. 7 is TaCoTe according to example 2 of the present invention 2 EDS spectra of single crystals;
FIG. 8 is TaCoTe according to example 2 of the present invention 2 Powder X-ray diffraction pattern of single crystal, the illustration is crystal appearance and size;
FIG. 9 is TaCoTe according to example 3 of the present invention 2 EDS spectra of single crystals;
FIG. 10 is TaCoTe according to example 3 of the present invention 2 Single crystal X-ray diffraction pattern of single crystals.
Detailed Description
The present invention is further illustrated in detail below with reference to examples, which are not intended to limit the scope of the invention. Variations and advantages that would occur to those skilled in the art are included within the scope of the invention without departing from the inventive concept.
Example 1
Co-based ternary insulator with centimeter-level sizeTaCoTe 2 The preparation method comprises the following steps:
1. single crystal preparation
1) Weighing raw materials and sealing
0.7310g (4.04 mmol) of Ta powder, 0.2381g (4.04 mmol) of Co powder and 1.0310g (8.08 mmol) of Te powder are weighed, mixed, 0.10g of iodine is weighed, mixed and put into a high-purity cylindrical quartz tube (purity is more than 99.99%), the inner diameter of the quartz tube is 8mm, and the quartz tube is vacuumized to 10 -3 Pa; the sealing length of the quartz tube is about 10cm (the sealing of the propane flame gun, the same applies below), and the inner volume of the sealed quartz tube is about 5000 mm 3 。
2) Heating and annealing process
Placing the sealed quartz tube in a tube furnace with double temperature areas, placing a raw material end at a high temperature end, placing a growth end at a low temperature end, and starting to set a programmed temperature: raising the temperature of a low-temperature end (a growth end) from room temperature to 750 ℃ at constant speed, keeping the temperature for 100 hours for 24 hours; simultaneously, the temperature of a high temperature end (raw material end) is uniformly increased to 850 ℃ from room temperature, the time is 24 hours, and the temperature is kept for 100 hours; then naturally cooling to room temperature, obtaining the layered TaCoTe at the low temperature end 2 Single crystal bulk.
3) Electrode preparation: the resistance of the sample was measured by the four-probe method, so that TaCoTe obtained in step 2) was obtained 2 And sticking and pressing 4 In electrodes or silver paste electrodes on the single crystal along the c axis.
2. Crystal structure test
The crystal appearance is shown in figure 1 (left), the crystal size is between 0.2cm and 1.1cm, and the crystal structure diagram is shown in figure 1 (right); measuring element ratio of a small single crystal by using an energy spectrometer on a scanning electron microscope, wherein the sample contains elements shown in figure 2, and the element atomic ratio Ta, co and Te is 1.01:0.98:2; cutting a small block of single crystal, grinding into powder, testing data on X-ray powder diffractometer and analyzing (TOPAS fitting), XRD spectrum of sample is shown in figure 3, all diffraction peak positions and inorganic crystal database-73738 TaCoTe 2 The files are consistent. In the figure, black star lines are XRD experimental data, red lines are XRD theoretical fitting curves, and blue vertical lines are inorganic crystal database-73738 TaCoTe 2 Bragg diffraction peak position of documentThe green line is the fit error line. The perfect coincidence of the theoretical curve with the implementation curve and the small error line of the fit indicate that the fit is reliable and that the sample is pure phase. The experimental result proves that the proportion of single crystal elements is very close to the molecular formula TaCoTe 2 Monoclinic system, space group No. 14P 2 1 C, having a lattice constant of a= 8.152 (4) a, b= 6.264 (9) a, c=7.794 (5) a, substantially in accordance with lattice parameters reported in the literature (Inorganic Chemistry, 32, 4829-4833, 1993).
3. Electrical property test
1) Electrode preparation
Along the a-axis direction of the crystal, 4 electrodes or silver paste electrodes were stuck with In.
2) And (5) testing performance.
The electrical properties of the single crystals were tested using a PPMS system. The test ranges from 2K to 300K, and the results are shown in FIG. 4. As can be seen from FIG. 4, taCoTe 2 Single crystals exhibit pronounced insulator behavior and a tendency to saturate resistance at low temperatures (below 50K). A single crystal was selected to be horizontally placed on a raman bench and a room temperature raman spectrum of the sample was obtained by laser testing at 633nm, as shown in fig. 5, which shows that the sample was pure phase. Single crystals with a size greater than 2mm were selected and observed in a scanning tunneling microscope, as shown in FIG. 6, where the presence of a distinct band gap was seen at 5K.
Example 2
Co-based ternary insulator monocrystal TaCoTe with centimeter-level size 2 The preparation method comprises the following steps:
1. single crystal preparation
1) Weighing raw materials and sealing
Weighing TaCoTe with the mole ratio of Ta, co and Te being 1:1:2 2 1.5g of polycrystal powder, then weighing 0.06g of iodine, mixing, loading into a high-purity L-shaped quartz tube (purity is more than 99.99 percent), and vacuumizing the tube to the pressure of 10 percent -4 Pa; the inner diameter of the quartz tube is 10mm, the sealing length is about 15cm, and the inner volume of the sealed quartz tube is about 12000 mm 3 。
2) Heating and annealing process
Placing a sealed quartz tube inIn a double-temperature-zone tube furnace, placing a raw material end at a high temperature end, starting to set a programmed temperature, uniformly heating a low temperature end from room temperature to 650 ℃, keeping the temperature for 12 hours and preserving the heat for 72 hours; simultaneously, the high temperature end is uniformly heated to 750 ℃ from room temperature for 12 hours, and the temperature is kept for 72 hours; naturally cooling to room temperature to obtain layered TaCoTe 2 Single crystal bulk.
2. Crystal structure test
Measuring element ratio of a small single crystal by using an energy spectrometer on a scanning electron microscope, wherein the sample contains elements shown in figure 7, and the element atomic ratio Ta, co and Te is 0.98:1.01:2; an XRD spectrum of a sample obtained by cutting a small piece of single crystal and grinding into powder, testing and analyzing the data on an X-ray powder diffractometer is shown in FIG. 8, and is identical to that of example 1. The crystal size was 1.3cm at maximum, as shown in the inset of FIG. 8.
Example 3
Co-based ternary insulator monocrystal TaCoTe with centimeter-level size 2 The preparation method comprises the following specific steps:
1. single crystal preparation
1) Weighing raw materials and sealing
Mixing Ta powder, co powder and Te powder according to the molar ratio of Ta, co and Te of 1:1:5, weighing 0.16g of iodine granules, loading the mixture into a high-purity U-shaped quartz tube with the purity of more than 99.99%, and vacuumizing the tube to the pressure of 10 percent -1 Pa; the inner diameter of the quartz tube is 10mm, the sealing length is about 13cm, and the inner volume of the sealed quartz tube is about 11000 and 11000 mm 3 。
2) Heating and annealing process
Placing the sealed quartz tube in a double-temperature-zone tube furnace, placing the raw material end at the high temperature end, starting to set a programmed temperature, uniformly heating the low temperature end to 700 ℃ from room temperature, keeping the temperature for 86 hours for 10 hours; simultaneously, the high temperature end is uniformly heated to 800 ℃ from room temperature for 10 hours, and the temperature is kept for 86 hours; naturally cooling to room temperature to obtain layered TaCoTe 2 Single crystal bulk.
2. Crystal structure test
Measuring element ratio of a small single crystal by using an energy spectrometer on a scanning electron microscope, wherein the sample contains elements shown in figure 9, and the element atomic ratio Ta: co: te is 1.003:1.021:2.111; a small piece of single crystal was cut to cleave the fresh bright surface, and the data were tested and analyzed on an X-ray diffractometer, and the XRD spectrum of the single crystal sample is shown in FIG. 10.
Claims (3)
1. The preparation method of the Co-based ternary insulator monocrystal with the centimeter-level size is characterized by comprising the following steps of:
1) Weighing raw materials and sealing
The Ta source, the Co source and the Te source are weighed according to the mole ratio of 1:1 (2-15) to be used as raw materials or polycrystalline powder which accords with the mole ratio is used as raw materials, the raw materials and a transport agent are uniformly mixed in an air environment and then are filled into a high-purity quartz tube, the transport agent is iodine, then the quartz tube is vacuumized and sealed, and the pressure intensity in the sealed quartz tube is 10 percent -4 Pa-0.1 Pa; the Ta source is Ta simple substance or Ta telluride, the Co source is Co simple substance or Co telluride, and the Te source is Te simple substance; the sealing length of the quartz tube is 5-50cm;
2) Heating and annealing process
Placing the sealed quartz tube in a single-temperature zone or a double-temperature zone tube furnace of a temperature gradient furnace, setting the temperature of a low-temperature end to 550-750 ℃ and the temperature of a high-temperature end to 650-850 ℃, placing a raw material end at the high-temperature end, and starting to set the temperature programming: the high temperature end and the low temperature end are heated from room temperature to a set temperature at constant speed for 10 hours or 12-60 hours, then are insulated for 48-100 hours, the furnace is naturally cooled to room temperature after the insulation is finished, and the layered Ta is obtained at the low temperature end 1-x Co 1-y Te 2±z Single crystal, x, y, z +.0.1.
2. The method for producing a Co-based ternary insulator single crystal material of centimeter-scale size according to claim 1, wherein the transporter iodine is weighed at (1-20) mg/mL by the volume in the quartz tube after sealing.
3. The method for producing a Co-based ternary insulator single crystal material of centimeter-scale size according to claim 1, wherein the Ta 1-x Co 1-y Te 2±z The size of the single crystal is at0.1-1.3 cm。
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| 过渡金属三组元碲化物研究;黄金陵,黄宝泉;福州大学学报(自然科学版)(第01期);1-8 * |
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