CN105350075A - Method for preparing high-purity topological insulator YbB6 single crystal - Google Patents

Method for preparing high-purity topological insulator YbB6 single crystal Download PDF

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Publication number
CN105350075A
CN105350075A CN201510849964.8A CN201510849964A CN105350075A CN 105350075 A CN105350075 A CN 105350075A CN 201510849964 A CN201510849964 A CN 201510849964A CN 105350075 A CN105350075 A CN 105350075A
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ybb
single crystal
seed crystal
zone
charge bar
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CN105350075B (en
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张忻
刘洪亮
王杨
李录录
江浩
张久兴
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Beijing University of Technology
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Beijing University of Technology
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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
    • 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
    • C30B13/00—Single-crystal growth by zone-melting; Refining by zone-melting

Abstract

The invention discloses a method for preparing a high-purity topological insulator YbB6 single crystal, and belongs to the technical field of topological insulator materials. At present, preparation and study on the high-purity topological insulator YbB6 single crystal are rarely carried out, the preparation process is complex, and the single crystal is poor in quality, low in purity and small in size, and can hardly be actually applied. The method of combining plasma activated sintering and suspension zone melting is adopted, and the high-quality, high-purity and large-size YbB6 single crystal is prepared in the high vacuum environment. High-purity YbB6 powder is adopted as initial raw materials, the prepared YbB6 single crystal is a cylinder with phi of 4.5 mm*20 mm, and it is shown through the testing result of a single-crystal diffractometer that the quality of the single crystal is good.

Description

A kind of high purity topological insulator YbB 6the preparation method of single crystal
Technical field
The invention belongs to topological insulator material technical field, be specifically related to one and utilize optical region smelting process to prepare YbB 6the method of single crystal material.
Background technology
Topological insulator is a kind of brand-new quantum physical form.Under strong Effect of Spin-orbit Coupling, its physical efficiency state is isolator, and surface is then metallic.This surface state without energy gap by Time-reversal symmetry protect, the electronic state of spinning resolving, and described by the dirac equation without quality.These unusual features make topological insulator have important application prospect in the field such as spintronics and quantum calculation in future.In recent years, research finds SmB 6and YbB 6monocrystalline is the important three-dimensional topology isolator of a class, thus is subject to increasing attention.Yb element is widely used as a kind of important rare earth element, and high purity YbB 6the preparation of single crystal is less.
At present, usually adopt al solvent legal system for rare-earth boride YbB 6single crystal, but the single crystal size that this method is prepared is less, and impurity aluminum element is easily brought in preparation process, reduce monocrystalline purity, have impact on its topological performance, limit its practical application.
Summary of the invention
The object of the invention is to the problem solving prior art, and a kind of high purity YbB is provided 6the preparation method of single crystal topological insulator.Method provided by the present invention can improve quality and the purity of single crystal, and XRF tests purity can reach 100%, is conducive to large-scale commercial production and application.
The method that the present invention adopts plasma activated sintering to combine with floating zone melting prepares high purity, high quality YbB 6single crystal, concrete steps are as follows:
1) by YbB 6load after the mixing of powder ball milling in graphite jig; Mould is placed in the sintering cavity of plasma activated sintering machine, sinters under the vacuum condition of total gas pressure lower than 5Pa; Be warming up to 1300 ~ 1400 DEG C with the temperature rise rate of 80 ~ 120 DEG C/min, insulation 10 ~ 15min, cools to room temperature with the furnace, obtains YbB 6polycrystalline rod;
2) adopting optical region smelting furnace, is the YbB of 5 ~ 10mm with diameter 6polycrystalline rod is that seed crystal and charge bar carry out first time zone-refine; After equipment is evacuated to below 1Pa, pour flowing H 2volume content is the H of 5% 2/ Ar reduction gas mixture rises to 0.2MPa to air pressure, gas flow rate is 1.5 ~ 2L/min, 20min zone melting furnace power is increased to seed crystal and charge bar and melts and formed and stablize melting zone, in order to make melting zone more even, by seed crystal and charge bar reverse rotation, rotating speed is 25rpm, and crystalline growth velocity unit 15 ~ 20mm/h, enters step 3 after growing to 2-5cm length);
3) optical region smelting furnace is adopted, with the YbB of a zone-refine 6for charge bar, with step 1) YbB that sinters 6polycrystalline rod be seed crystal carry out second time district melt; After equipment is evacuated to below 1Pa, 20min zone melting furnace power is increased to seed crystal and charge bar and melts and formed and stablize melting zone, in order to make melting zone more even, by seed crystal and charge bar reverse rotation, rotating speed is 25rpm, and crystalline growth velocity unit 6 ~ 8mm/h, grows to 2-5cm length.
Wherein, step 1) described in plasma activated sintering unit type be SPS-3.20MK-V; Step 2) described in optical region smelting furnace model be FZ-T-12000-S-BU-PC.
Compared with existing technology of preparing, the present invention has following beneficial effect:
YbB prepared by the present invention 6single crystal purity is high, quality is high, and single crystal is columnar block.
Accompanying drawing explanation
The YbB of Fig. 1, embodiment 1 preparation 6the photo in kind of single crystal.
The YbB of Fig. 2, embodiment 1 preparation 6the single crystal diffraction low Loran PRR photo of single crystal.
The YbB of Fig. 3, embodiment 2 preparation 6single crystal is along c-axis direction of growth Laue photo.
The YbB of Fig. 4, embodiment 2 preparation 6the low temp. electric performance map of single crystal.
Below in conjunction with the drawings and specific embodiments, the invention will be further described, but protection scope of the present invention is not limited to following embodiment.
Embodiment
Embodiment 1
1) by YbB 6load after the mixing of powder ball milling in graphite jig; Mould is placed in the sintering cavity of plasma activated sintering machine, sinters under the vacuum condition of total gas pressure lower than 5Pa; Be warming up to 1300 DEG C with the temperature rise rate of 80 DEG C/min, insulation 15min, cools to room temperature with the furnace, obtains YbB 6polycrystalline rod;
2) adopting optical region smelting furnace, take diameter as the YbB of 5mm 6polycrystalline rod is that seed crystal and charge bar carry out first time zone-refine; After equipment is evacuated to below 1Pa, pour flowing H 2content (volume content, as follows) is the H of 5% 2/ Ar reduction gas mixture rises to 0.2MPa to air pressure, gas flow rate is 1.5L/min, 20min zone melting furnace power is increased to seed crystal and charge bar and melts and formed and stablize melting zone, in order to make melting zone more even, by seed crystal and charge bar reverse rotation, rotating speed is 25rpm, and crystalline growth velocity unit 15mm/h, grows to 2cm length;
3) optical region smelting furnace is adopted, with the YbB of a zone-refine 6for charge bar, with step 1) YbB that sinters 6polycrystalline rod be seed crystal carry out second time district melt; After equipment is evacuated to below 1Pa, 20min zone melting furnace power is increased to seed crystal and charge bar and melts and formed and stablize melting zone, in order to make melting zone more even, by seed crystal and charge bar reverse rotation, rotating speed is 25rpm, and crystalline growth velocity unit 6mm/h, grows to 2cm length.
Embodiment 2
1) by YbB 6load after the mixing of powder ball milling in graphite jig; Mould is placed in the sintering cavity of plasma activated sintering machine, sinters under the vacuum condition of total gas pressure lower than 5Pa; Be warming up to 1350 DEG C with the temperature rise rate of 100 DEG C/min, insulation 12min, cools to room temperature with the furnace, obtains YbB 6polycrystalline rod;
2) adopting optical region smelting furnace, take diameter as the YbB of 8mm 6polycrystalline rod is that seed crystal and charge bar carry out first time zone-refine; After equipment is evacuated to below 1Pa, pour flowing H 2content is the H of 5% 2/ Ar reduction gas mixture rises to 0.2MPa to air pressure, gas flow rate is 1.8L/min, 20min zone melting furnace power is increased to seed crystal and charge bar and melts and formed and stablize melting zone, in order to make melting zone more even, by seed crystal and charge bar reverse rotation, rotating speed is 25rpm, and crystalline growth velocity unit 18mm/h, grows to 3cm length;
3) optical region smelting furnace is adopted, with the YbB of a zone-refine 6for charge bar, with step 1) YbB that sinters 6polycrystalline rod be seed crystal carry out second time district melt; After equipment is evacuated to below 1Pa, 20min zone melting furnace power is increased to seed crystal and charge bar and melts and formed and stablize melting zone, in order to make melting zone more even, by seed crystal and charge bar reverse rotation, rotating speed is 25rpm, and crystalline growth velocity unit 8mm/h, grows to 3cm length.
Embodiment 3
1) by YbB 6load after the mixing of powder ball milling in graphite jig; Mould is placed in the sintering cavity of plasma activated sintering machine, sinters under the vacuum condition of total gas pressure lower than 5Pa; Be warming up to 1100 DEG C with the temperature rise rate of 120 DEG C/min, insulation 10min, cools to room temperature with the furnace, obtains YbB 6polycrystalline rod;
2) adopting optical region smelting furnace, take diameter as the YbB of 10mm 6polycrystalline rod is that seed crystal and charge bar carry out first time zone-refine; After equipment is evacuated to below 1Pa, pour flowing H 2content is the H of 5% 2/ Ar reduction gas mixture rises to 0.2MPa to air pressure, gas flow rate is 1.8L/min, 20min zone melting furnace power is increased to seed crystal and charge bar and melts and formed and stablize melting zone, in order to make melting zone more even, by seed crystal and charge bar reverse rotation, rotating speed is 25rpm, and crystalline growth velocity unit 20mm/h, grows to 5cm length;
3) optical region smelting furnace is adopted, with the YbB of a zone-refine 6for charge bar, with step 1) YbB that sinters 6polycrystalline rod be seed crystal carry out second time district melt; After equipment is evacuated to below 1Pa, 20min zone melting furnace power is increased to seed crystal and charge bar and melts and formed and stablize melting zone, in order to make melting zone more even, by seed crystal and charge bar reverse rotation, rotating speed is 25rpm, and crystalline growth velocity unit 10mm/h, grows to 5cm length.
The YbB of preparation in embodiment 1 6single crystal is light blue, and as shown in Figure 1, sample even thickness, smooth surface, does not find the vestige that gas and impurity overflow.Fig. 2 is YbB prepared by embodiment 1 6the single crystal diffractometer low Loran PRR photo of single crystal, diffraction spot is complete, does not occur that the phenomenon interpret sample such as splitting hangover are monocrystalline and quality is good.Fig. 3 is YbB prepared by embodiment 2 6single crystal is along c-axis direction of growth Laue photo.Fig. 4 is YbB prepared by embodiment 2 6the low temp. electric performance map of single crystal, shows that sample has topological insulator characteristic.Show that growth parameter(s) still can prepare high-quality single crystal after changing.3 embodiments have extremely similar the above results, and interpret sample is monocrystalline and quality is good, avoids repeating so do not provide too many similar figure.

Claims (1)

1. a high purity topological insulator YbB 6the preparation method of single crystal, is characterized in that, comprises the following steps:
1) by YbB 6load after the mixing of powder ball milling in graphite jig; Mould is placed in the sintering cavity of plasma activated sintering machine, sinters under the vacuum condition of total gas pressure lower than 5Pa; Be warming up to 1300 ~ 1400 DEG C with the temperature rise rate of 80 ~ 120 DEG C/min, insulation 10 ~ 15min, cools to room temperature with the furnace, obtains YbB 6polycrystalline rod;
2) adopting optical region smelting furnace, is the YbB of 5 ~ 10cm with diameter 6polycrystalline rod is that seed crystal and charge bar carry out first time zone-refine; After equipment is evacuated to below 1Pa, pour flowing H 2volume content is the H of 5% 2/ Ar reduction gas mixture rises to 0.2MPa to air pressure, gas flow rate is 1.5 ~ 2L/min, 20min zone melting furnace power is increased to seed crystal and charge bar and melts and formed and stablize melting zone, then by seed crystal and charge bar reverse rotation, rotating speed is 25rpm, crystalline growth velocity unit 15 ~ 20mm/h, enters step 3 after growing to 2-5cm length);
3) optical region smelting furnace is adopted, with the YbB of a zone-refine 6for charge bar, with step 1) YbB that sinters 6polycrystalline rod be seed crystal carry out second time district melt; After equipment is evacuated to below 1Pa, 20min zone melting furnace power is increased to seed crystal and charge bar and melts and formed and stablize melting zone, and then by seed crystal and charge bar reverse rotation, rotating speed is 25rpm, and crystalline growth velocity unit 6 ~ 8mm/h, grows to 2-5cm length.
CN201510849964.8A 2015-11-29 2015-11-29 A kind of high-purity topological insulator YbB6The preparation method of monocrystal Expired - Fee Related CN105350075B (en)

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CN106012011A (en) * 2016-05-11 2016-10-12 合肥工业大学 Preparation method for LaB6-ZrB2 eutectic composite material
CN106007728A (en) * 2016-05-19 2016-10-12 航天材料及工艺研究所 Thermal-shock-resistant ultrahigh-temperature ceramic and preparation method thereof

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CN106007728B (en) * 2016-05-19 2019-01-25 航天材料及工艺研究所 A kind of anti-thermal shock superhigh temperature ceramics and preparation method thereof

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