CN116988159A - Antiferromagnetic topological semi-metal material EuSb 2 Single crystal and method for producing same - Google Patents
Antiferromagnetic topological semi-metal material EuSb 2 Single crystal and method for producing same Download PDFInfo
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- CN116988159A CN116988159A CN202310974832.2A CN202310974832A CN116988159A CN 116988159 A CN116988159 A CN 116988159A CN 202310974832 A CN202310974832 A CN 202310974832A CN 116988159 A CN116988159 A CN 116988159A
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- 239000013078 crystal Substances 0.000 title claims abstract description 69
- 230000005290 antiferromagnetic effect Effects 0.000 title claims abstract description 11
- 239000007769 metal material Substances 0.000 title claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- 239000002885 antiferromagnetic material Substances 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 8
- 239000010453 quartz Substances 0.000 claims description 30
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 30
- 239000002994 raw material Substances 0.000 claims description 19
- 239000002245 particle Substances 0.000 claims description 15
- 238000007789 sealing Methods 0.000 claims description 9
- 238000005303 weighing Methods 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- 238000010304 firing Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000002844 melting Methods 0.000 claims description 5
- 230000008018 melting Effects 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 238000005520 cutting process Methods 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 11
- 230000005291 magnetic effect Effects 0.000 abstract description 7
- 238000002360 preparation method Methods 0.000 abstract description 4
- 229910052716 thallium Inorganic materials 0.000 abstract description 4
- 229910052718 tin Inorganic materials 0.000 abstract description 4
- 238000002425 crystallisation Methods 0.000 abstract description 2
- 230000008025 crystallization Effects 0.000 abstract description 2
- 230000006911 nucleation Effects 0.000 abstract description 2
- 238000010899 nucleation Methods 0.000 abstract description 2
- 230000007704 transition Effects 0.000 abstract description 2
- 230000002349 favourable effect Effects 0.000 abstract 1
- 230000004907 flux Effects 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 206010010254 Concussion Diseases 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013590 bulk material Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000009514 concussion Effects 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000724 energy-dispersive X-ray spectrum Methods 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000000758 substrate 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
- C30B29/52—Alloys
-
- 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
- C30B9/00—Single-crystal growth from melt solutions using molten solvents
- C30B9/04—Single-crystal growth from melt solutions using molten solvents by cooling of the solution
- C30B9/08—Single-crystal growth from melt solutions using molten solvents by cooling of the solution using other solvents
- C30B9/12—Salt solvents, e.g. flux growth
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/0009—Antiferromagnetic materials, i.e. materials exhibiting a Néel transition temperature
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Power Engineering (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to an antiferromagnetic topological semi-metal material EuSb 2 A single crystal and a preparation method thereof belong to the technical field of single crystal materials. The unit cell parameters of the single crystal are as follows: a= 4.7680 a, b= 4.2990 a, c=8.97 a, α=γ=90°, β= 103.01 °. Tl-Sn is selected as a fluxing agent by adopting a fluxing agent method, and the addition of Tl and Sn elements is favorable for enabling Eu and Sb elements in the single crystal to be fused together more quickly and more uniformly, so that nucleation and crystallization are better. The material is an antiferromagnetic material, and the Neel temperature of the magnetic transition is 22.3K.
Description
Technical Field
The invention relates to an antiferromagnetic topological semi-metal material EuSb 2 A single crystal and a preparation method thereof belong to the technical field of single crystal materials.
Background
These non-bandgap points in momentum space cause many novel quantum transport phenomena in topological node semi-metals, dirac or halfcmetal. Theory predicts that the topology of the topological pitch line half-metal appears in the bulk and surface state quantum concussions. Thus, it is important to prepare a thin film or a single crystal having high mobility. On the other hand, when we consider spin-orbit coupling, many common node line materials are transformed into topological insulators orThe node is semi-metal. Therefore, a crystal structure that is not point-symmetric is necessary. CaSb 2 Is a novel topological pitch line semi-metal material, euSb with the same structure 2 On the basis of this unique crystal structure, a large magnetic moment is expected. In the past, in the 80 s of the 20 th century, there was a report of polycrystalline antiferromagnetic order, and in recent years, a study of transport properties of a single crystal thin film has been conducted. But the test results may be affected due to defects in the poly-crystal and thin film, and the thin film grown on the substrate. Therefore, in order to fully explore the intrinsic physical properties of the material, it is necessary to grow single crystal bulk materials, and only a single crystal bulk material sample is obtained, so that the subsequent quantum devices and future applications based on magnetic topology materials can be promoted. At present, the EuSb is not relevant 2 A single crystal and a method for producing the same.
Disclosure of Invention
In view of the above, the present invention aims to provide an antiferromagnetically topologically semimetal material EuSb 2 Single crystals and methods of making the same.
In order to achieve the above object, the technical scheme of the present invention is as follows.
Antiferromagnetic topological semi-metal material EuSb 2 Single crystal, the unit cell parameters of the single crystal are: a= 4.7680 a, b= 4.2990 a, c=8.97 a, α=γ=90°, β= 103.01 °.
The antiferromagnetic material EuSb 2 The preparation method of the monocrystal adopts a fluxing method which takes Tl-Sn binary compound as fluxing agent, and comprises the following steps:
(1) According to EuSb 2 The stoichiometric ratio with Tl-Sn is 1: 10-1: 40, weighing Eu blocks, tl particles, sb particles and Sn particles serving as raw materials respectively in an environment with water and oxygen content less than 0.1 ppm, loading the raw materials into a crucible, placing the crucible into a quartz tube, and vacuum-sealing the quartz tube;
the purity of the raw materials is more than or equal to 99.999 percent;
the vacuum degree of the vacuum seal is 1 multiplied by 10 -4 Pa or more;
(2) Placing the quartz tube subjected to the vacuum sealing in the step (1) into a muffle furnace for firing, wherein the furnace is set as follows: firstly, heating to 900-1100 ℃ from room temperature, keeping the temperature for more than 24 hours at constant temperature, then cooling to 400-600 ℃, opening a furnace door immediately, inversely placing a quartz tube into a centrifuge, and removing redundant products except single crystals;
(3) Opening a quartz tube, picking out single crystal slices, bonding some single crystal slices together due to fluxing agent, and cutting the single crystal slices along the crystal direction of single crystal growth by taking a blade to obtain independent single crystal slices, thereby obtaining the antiferromagnetic topological semi-metal material EuSb 2 And (3) single crystals.
Preferably, in the step (1), raw materials Eu blocks, tl particles, sb particles and Sn particles are respectively filled into a quartz tube, then the quartz tube is subjected to gas washing treatment by argon in a vacuum tube sealing system, and finally hydrogen with the pressure of more than 0.8 atmosphere is filled into the quartz tube, and the hydrogen is sealed in the quartz tube; the above raw materials were annealed at a temperature 50 ℃ below the respective melting points to remove the oxide layer on the surface.
Preferably, in the step (1), the vacuum degree of the vacuum seal is 3×10 -4 Pa~5×10 -4 Pa。
Preferably, in the step (1), the weighing error of the raw material is less than or equal to 0.01%.
Preferably, in the step (2), the quartz tube vacuum-sealed in the step (1) is put into a muffle furnace for firing, and the procedure is as follows: firstly, heating the quartz tube to 900-1100 ℃ from room temperature for 9-11 h, keeping the temperature for more than 24h at constant temperature, then cooling to 400-600 ℃ at a speed of 1-4 ℃/h, opening a furnace door immediately, inversely placing the quartz tube into a centrifuge, and separating redundant products except single crystals; during centrifugation, the quartz tube needs to be quickly removed from the furnace, otherwise the single crystal will solidify in the flux.
Advantageous effects
The invention provides an antiferromagnetic topological semi-metal material EuSb 2 The single crystal, the magneto-resistance result shows, is topological semi-metal. The single crystal is beneficial to subsequent quantum devices and future applications based on magnetic topology materials.
The invention provides an antiferromagnetic topological semi-metal material EuSb 2 Preparation of single crystalsAccording to the method, tl-Sn is selected as a fluxing agent, the melting points of Tl and Sn are low, and when binary compounds are generated by the Tl and Sn according to a certain proportion, the melting points are low, so that the two elements contained in the single crystal are fused together more quickly and more uniformly, and better nucleation crystallization is achieved. The parent phase EuSb in the present invention 2 The ratio to flux was chosen and validated after a number of other ratios were tried. The centrifugal temperature is very important, when the temperature exceeds 600 ℃, the single crystal is centrifuged along with the fluxing agent, and under 400 ℃, the fluxing agent and the single crystal are bonded together, so that the quantity of the obtained single crystal is small, and the quality is not high.
Drawings
FIG. 1 is an X-ray diffraction (XRD) spectrum of the single crystal described in example 1.
FIG. 2 is a Scanning Electron Microscope (SEM) photograph (a) and a corresponding Energy Dispersive Spectroscopy (EDS) map (b) of the single crystal described in example 1.
FIG. 3 is a graph showing the magnetic properties of the single crystal of example 1.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1
(1) According to the parent phase EuSb 2 : the stoichiometric ratio of the fluxing agent Tl-Sn=1:20, weighing raw materials respectively under the environment that the water content and the oxygen content are less than 0.1 ppm, wherein Eu blocks are 0.5334g, tl particles are 0.2870g, sb particles are 0.5128g and Sn particles are 1.6668g, putting the raw materials into a crucible with the diameter of 1cm, putting the crucible into a quartz tube after weighing, and vacuum sealing the quartz tube;
the raw materials are Sn, eu and Sb, and the purity of the raw materials is not less than 99.999%;
since the raw materials Tl and Sb are easily oxidized in air, in order to improve the electrical properties of the prepared single crystal, it is preferable that the raw materials are each packed in a quartz tube filled with hydrogen gas of 0.8 atm, and annealed at a temperature 50 ℃ lower than the melting point, respectively, to remove the oxidized layer on the surface;
preferably, the vacuum degree of the vacuum seal is 4×10 -4 Pa；
Preferably, the weighing errors of the raw materials are all 0.01%;
(2) Placing the quartz tube subjected to the vacuum sealing in the step (1) into a muffle furnace for firing, wherein the furnace is set as follows: heating to 1000 ℃ from room temperature for 10 hours, keeping at constant temperature for 24 hours, then cooling to 400 ℃ at the speed of 3.5 ℃/h, opening a furnace door, inversely placing a quartz tube into a centrifuge, and removing redundant products except single crystals;
(3) The quartz tube was opened and the single-crystal wafer was picked up.
The monocrystal prepared by the invention is strip-shaped, sheet-shaped and has metallic luster. The single crystal sample was first XRD characterized, and the result is shown in FIG. 1, which shows that the diffraction peaks of the single crystal are close to those of the standard spectrum (00) in comparison with the standard card (ICSD number: 98-001-0081)l) The crystal face, thereby confirming that the prepared single crystal sample is indeed EuSb 2 And the flakes present ab-facets. Analysis of the content of each element in the prepared single crystal was performed using EDS spectrum, and as a result, characteristic peaks of Eu and Sb appear as shown in fig. 2, and the content ratio of each element is 1:2. combining the characterization results of XRD and EDS, it was confirmed that the single crystal material of the invention is EuSb 2 。
The prepared single crystal samples were tested for magnetic properties at a temperature ranging from 300-1.8K. FIG. 3 shows the dependence of magnetization on temperature, demonstrating that the material is an antiferromagnetic material and that the Neel temperature of the magnetic transition is 22.3K.
Example 2
In this example, euSb 2 : the stoichiometric ratio of Tl-Sn was 1:10, with the remainder being as in example 1.
EuSb prepared in this example 2 The single crystal structure and properties were similar to those of example 1.
Example 3
In this example, euSb 2 : the stoichiometric ratio of Tl-Sn was 1:40, with the remainder being as in example 1.
EuSb prepared in this example 2 The single crystal structure and properties were similar to those of example 1.
Example 4
In this example, the temperature was lowered to 600℃in step (2), and the rest was the same as in example 1.
EuSb prepared in this example 2 The single crystal structure and properties were similar to those of example 1.
Comparative example 1
Changing the kind of flux, using Sn element as flux, when using EuSb as mother phase 2 And Sn according to 1:10 and 1:5 weighing the stoichiometric ratio, setting the muffle furnace procedure to grow to 1000 ℃ for 10 hours according to the growth step, stabilizing the temperature for more than one day, slowly cooling to 600 ℃, and centrifuging to obtain single crystals of Eu respectively 2 Sb 3 And EuSb single crystals.
In view of the foregoing, it will be appreciated that the invention includes but is not limited to the foregoing embodiments, any equivalent or partial modification made within the spirit and principles of the invention.
Claims (6)
1. Antiferromagnetic topological semi-metal material EuSb 2 Single crystal, the unit cell parameters of the single crystal are: a= 4.7680 a, b= 4.2990 a, c=8.97 a, α=γ=90°, β= 103.01 °.
2. An antiferromagnetic material EuSb as claimed in claim 1 2 A method for producing a single crystal, characterized by: the method comprises the following steps:
(1) According to EuSb 2 The stoichiometric ratio with Tl-Sn is 1: 10-1: 40, weighing Eu blocks, tl particles, sb particles and Sn particles serving as raw materials respectively in an environment with water and oxygen content less than 0.1 ppm, loading the raw materials into a crucible, placing the crucible into a quartz tube, and vacuum-sealing the quartz tube;
the purity of the raw materials is more than or equal to 99.999 percent;
the vacuum degree of the vacuum seal is 1 multiplied by 10 -4 Pa or more;
(2) Placing the quartz tube subjected to the vacuum sealing in the step (1) into a muffle furnace for firing, wherein the furnace is set as follows: firstly, heating to 900-1100 ℃ from room temperature, keeping the temperature for more than 24 hours at constant temperature, then cooling to 400-600 ℃, opening a furnace door immediately, inversely placing a quartz tube into a centrifuge, and removing redundant products except single crystals;
(3) Opening a quartz tube, picking out single crystal slices, bonding some single crystal slices together due to fluxing agent, and cutting the single crystal slices along the crystal direction of single crystal growth by taking a blade to obtain independent single crystal slices, thereby obtaining the antiferromagnetic topological semi-metal material EuSb 2 And (3) single crystals.
3. An antiferromagnetic material EuSb as claimed in claim 2 2 A method for producing a single crystal, characterized by: in the step (1), raw materials Eu blocks, tl particles, sb particles and Sn particles are respectively filled into a quartz tube, then the quartz tube is subjected to gas washing treatment by argon in a vacuum tube sealing system, and finally hydrogen with the pressure of more than 0.8 atmosphere is filled into the quartz tube, and the hydrogen is sealed in the quartz tube; the above raw materials were annealed at a temperature 50 ℃ below the respective melting points to remove the oxide layer on the surface.
4. An antiferromagnetic material EuSb as claimed in claim 2 2 A method for producing a single crystal, characterized by: in the step (1), the vacuum degree of the vacuum seal is 3×10 -4 Pa~5×10 -4 Pa。
5. An antiferromagnetic material EuSb as claimed in claim 2 2 A method for producing a single crystal, characterized by: in the step (1), the weighing error of the raw materials is less than or equal to 0.01%.
6. An antiferromagnetic material EuSb as claimed in claim 2 2 A method for producing a single crystal, characterized by: in the step (2), the quartz tube subjected to the vacuum sealing in the step (1) is put into a muffle furnace for firing, and the procedure is as follows: firstly, heating to 900-1100 ℃ from room temperature for 9-11 h, keeping the temperature for more than 24h at constant temperature, then cooling to 400-600 ℃ at the speed of 1-4 ℃/h, opening a furnace door, inversely placing a quartz tube into a centrifuge, and separating redundant products except single crystals.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310974832.2A CN116988159A (en) | 2023-08-04 | 2023-08-04 | Antiferromagnetic topological semi-metal material EuSb 2 Single crystal and method for producing same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310974832.2A CN116988159A (en) | 2023-08-04 | 2023-08-04 | Antiferromagnetic topological semi-metal material EuSb 2 Single crystal and method for producing same |
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| Publication Number | Publication Date |
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| CN116988159A true CN116988159A (en) | 2023-11-03 |
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| CN202310974832.2A Pending CN116988159A (en) | 2023-08-04 | 2023-08-04 | Antiferromagnetic topological semi-metal material EuSb 2 Single crystal and method for producing same |
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- 2023-08-04 CN CN202310974832.2A patent/CN116988159A/en active Pending
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