CN105350075B - A kind of high-purity topological insulator YbB6The preparation method of monocrystal - Google Patents

A kind of high-purity topological insulator YbB6The preparation method of monocrystal Download PDF

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Publication number
CN105350075B
CN105350075B CN201510849964.8A CN201510849964A CN105350075B CN 105350075 B CN105350075 B CN 105350075B CN 201510849964 A CN201510849964 A CN 201510849964A CN 105350075 B CN105350075 B CN 105350075B
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ybb
seed crystal
charge bar
purity
monocrystal
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CN105350075A (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

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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)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

A kind of high-purity topological insulator YbB6The preparation method of monocrystal belongs to topological insulator material technical field.At present, high-purity YbB6The preparation of monocrystalline is seldom with research, and preparation technology is complicated, and monocrystal is second-rate, and purity is low, and size is small, is difficult to realize practical application.The method that the present invention is combined using plasma activated sintering and floating zone melting, high quality, high-purity, large-sized YbB are prepared under high vacuum environment6Monocrystal.With high-purity YbB6Powder is the YbB that initial feed is prepared6Monocrystalline is φ 4.5mm × 20mm cylinder, and single crystal diffractometer test result shows that monocrystalline quality is good.

Description

A kind of high-purity topological insulator YbB6The preparation method of monocrystal
Technical field
The invention belongs to topological insulator material technical field, and in particular to be prepared to one kind using optical region smelting process YbB6The 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 Insulator, surface is then metallicity.The surface state of this no energy gap is protected by Time-reversal symmetry, spinned The electronic state of resolution, and as described by the Dirac equation of massless.These unusual features cause topological insulator in future Spintronics and the field such as quantum calculation have important application prospect.In recent years, research finds SmB6And YbB6Monocrystalline is one The important three-dimensional topology insulator of class, so as to more and more be paid attention to.Yb elements are as a kind of important rare earth element quilt Extensive use, and high-purity YbB6The preparation of monocrystal is less with studying.
At present, generally use al solvent method prepares rare-earth boride YbB6Monocrystal, but the monocrystal that the method is prepared Size is smaller, and easily brings impurity aluminium element into preparation process, reduces monocrystalline purity, have impact on its topological performance, limitation Its practical application.
The content of the invention
It is an object of the invention to solve problem of the prior art, and provide a kind of high-purity YbB6Monocrystal topology is absolutely The preparation method of edge body.Method provided by the present invention can improve the quality and purity of monocrystal, and XRF tests purity is reachable 100%, be advantageous to large-scale industrial production and application.
The present invention prepares high-purity, high quality using plasma activated sintering with the method that floating zone melting is combined YbB6Monocrystal, comprise the following steps that：
1) by YbB6Powder ball milling is fitted into graphite jig after mixing；Mould is placed in the sintering of plasma activated sintering machine In cavity, sintered under vacuum condition of the total gas pressure less than 5Pa；1300 are warming up to 80~120 DEG C/min heating rate~ 1400 DEG C, 10~15min is incubated, room temperature is cooled to the furnace, obtains YbB6Polycrystalline rod；
2) optical region smelting furnace is used, with a diameter of 5~10mm YbB6Polycrystalline rod is that seed crystal and charge bar carry out first Secondary zone-refine；After equipment is evacuated to below 1Pa, flowing H is poured2Volume content is 5% H2/ Ar reduces gaseous mixture to gas Pressure rises to 0.2MPa, and gas flow rate is 1.5~2L/min, and 20min zone melting furnace power increases to seed crystal and charge bar melts and formed Stable melting zone, in order that melting zone is more uniform, seed crystal and charge bar are reversely rotated, rotating speed 25rpm, rate of crystalline growth list 15~20mm/h of position, enters step 3) after growing to 2-5cm length；
3) optical region smelting furnace is used, with the YbB of a zone-refine6For charge bar, the YbB sintered with step 1)6Polycrystalline Rod is that second of area of seed crystal progress melts；After equipment is evacuated to below 1Pa, 20min zone melting furnace power increases to seed crystal and charge bar Melt and form stable melting zone, in order that melting zone is more uniform, seed crystal and charge bar are reversely rotated, rotating speed 25rpm, crystal life Long 6~8mm/h of speed unit, grows to 2-5cm length.
Wherein, the plasma activated sintering unit type described in step 1) is SPS-3.20MK-V；Light described in step 2) School district domain smelting furnace model FZ-T-12000-S-BU-PC.
Compared with existing technology of preparing, the invention has the advantages that：
YbB prepared by the present invention6Single crystal purity is high, quality is high, and monocrystal isColumn block Body.
Brief description of the drawings
YbB prepared by Fig. 1, embodiment 16The photo in kind of monocrystal.
YbB prepared by Fig. 2, embodiment 16The single crystal diffraction slow scanning photo of monocrystal.
YbB prepared by Fig. 3, embodiment 26Monocrystal is along c-axis direction of growth Laue photo.
YbB prepared by Fig. 4, embodiment 26The low temperature electric performance map of monocrystal.
Below in conjunction with the drawings and specific embodiments, the invention will be further described, but protection scope of the present invention is not It is limited to following embodiments.
Embodiment
Embodiment 1
1) by YbB6Powder ball milling is fitted into graphite jig after mixing；Mould is placed in the sintering of plasma activated sintering machine In cavity, sintered under vacuum condition of the total gas pressure less than 5Pa；1300 DEG C are warming up to 80 DEG C/min heating rate, insulation 15min, cool to room temperature with the furnace, obtain YbB6Polycrystalline rod；
2) optical region smelting furnace is used, with a diameter of 5mm YbB6Polycrystalline rod is that seed crystal and charge bar carry out first time area Molten purification；After equipment is evacuated to below 1Pa, flowing H is poured2Content (volume content, as follows) is 5% H2/ Ar is reduced Gaseous mixture to air pressure rises to 0.2MPa, and gas flow rate 1.5L/min, 20min zone melting furnace power increases to seed crystal and charge bar melts Change and form stable melting zone, in order that melting zone is more uniform, seed crystal and charge bar are reversely rotated, rotating speed 25rpm, crystal growth Speed unit 15mm/h, grow to 2cm length；
3) optical region smelting furnace is used, with the YbB of a zone-refine6For charge bar, the YbB sintered with step 1)6Polycrystalline Rod is that second of area of seed crystal progress melts；After equipment is evacuated to below 1Pa, 20min zone melting furnace power increases to seed crystal and charge bar Melt and form stable melting zone, in order that melting zone is more uniform, seed crystal and charge bar are reversely rotated, rotating speed 25rpm, crystal life Long speed unit 6mm/h, grows to 2cm length.
Embodiment 2
1) by YbB6Powder ball milling is fitted into graphite jig after mixing；Mould is placed in the sintering of plasma activated sintering machine In cavity, sintered under vacuum condition of the total gas pressure less than 5Pa；1350 DEG C are warming up to 100 DEG C/min heating rate, is protected Warm 12min, cools to room temperature with the furnace, obtains YbB6Polycrystalline rod；
2) optical region smelting furnace is used, with a diameter of 8mm YbB6Polycrystalline rod is that seed crystal and charge bar carry out first time area Molten purification；After equipment is evacuated to below 1Pa, flowing H is poured2Content is 5% H2/ Ar reduction gaseous mixture to air pressure rises to 0.2MPa, gas flow rate 1.8L/min, 20min zone melting furnace power increases to seed crystal and charge bar melts and forms stable melting zone, In order that melting zone is more uniform, seed crystal and charge bar are reversely rotated, rotating speed 25rpm, rate of crystalline growth unit 18mm/h, it is raw Grow to 3cm length；
3) optical region smelting furnace is used, with the YbB of a zone-refine6For charge bar, the YbB sintered with step 1)6Polycrystalline Rod is that second of area of seed crystal progress melts；After equipment is evacuated to below 1Pa, 20min zone melting furnace power increases to seed crystal and charge bar Melt and form stable melting zone, in order that melting zone is more uniform, seed crystal and charge bar are reversely rotated, rotating speed 25rpm, crystal life Long speed unit 8mm/h, grows to 3cm length.
Embodiment 3
1) by YbB6Powder ball milling is fitted into graphite jig after mixing；Mould is placed in the sintering of plasma activated sintering machine In cavity, sintered under vacuum condition of the total gas pressure less than 5Pa；1100 DEG C are warming up to 120 DEG C/min heating rate, is protected Warm 10min, cools to room temperature with the furnace, obtains YbB6Polycrystalline rod；
2) optical region smelting furnace is used, with a diameter of 10mm YbB6Polycrystalline rod is that seed crystal and charge bar carry out first time area Molten purification；After equipment is evacuated to below 1Pa, flowing H is poured2Content is 5% H2/ Ar reduction gaseous mixture to air pressure rises to 0.2MPa, gas flow rate 1.8L/min, 20min zone melting furnace power increases to seed crystal and charge bar melts and forms stable melting zone, In order that melting zone is more uniform, seed crystal and charge bar are reversely rotated, rotating speed 25rpm, rate of crystalline growth unit 20mm/h, it is raw Grow to 5cm length；
3) optical region smelting furnace is used, with the YbB of a zone-refine6For charge bar, the YbB sintered with step 1)6Polycrystalline Rod is that second of area of seed crystal progress melts；After equipment is evacuated to below 1Pa, 20min zone melting furnace power increases to seed crystal and charge bar Melt and form stable melting zone, in order that melting zone is more uniform, seed crystal and charge bar are reversely rotated, rotating speed 25rpm, crystal life Long speed unit 10mm/h, grows to 5cm length.
The YbB prepared in embodiment 16Monocrystal is light blue, as shown in figure 1, sample even thickness, surface is smooth, does not have It is found the vestige that gas and impurity overflow.Fig. 2 is YbB prepared by embodiment 16The single crystal diffractometer slow scanning of monocrystal Photo, diffraction spot is complete, do not occur splitting hangover phenomena such as illustrate sample for monocrystalline and quality it is good.Fig. 3 is embodiment 2 YbB prepared6Monocrystal is along c-axis direction of growth Laue photo.Fig. 4 is YbB prepared by embodiment 26The low temperature of monocrystal is electrical It can scheme, show that sample has topological insulator characteristic.Show that growth parameter(s) can still prepare the monocrystalline of high quality after changing Body.3 embodiments have extremely similar the above results, illustrate that sample is monocrystalline and quality is good, avoid repeating so not having Similar figure too much is provided.

Claims (1)

  1. A kind of 1. high-purity topological insulator YbB6The preparation method of monocrystal, it is characterised in that comprise the following steps：
    1) by YbB6Powder ball milling is fitted into graphite jig after mixing；Mould is placed in the sintering cavity of plasma activated sintering machine In, sintered under vacuum condition of the total gas pressure less than 5Pa；1300~1400 are warming up to 80~120 DEG C/min heating rate DEG C, 10~15min is incubated, room temperature is cooled to the furnace, obtains YbB6Polycrystalline rod；
    2) optical region smelting furnace is used, with a diameter of 5~10cm YbB6Polycrystalline rod is that seed crystal and charge bar carry out first time area and melted Purification；After equipment is evacuated to below 1Pa, flowing H is poured2Volume content is 5% H2/ Ar reduction gaseous mixture to air pressure rises to 0.2MPa, gas flow rate are 1.5~2L/min, and 20min zone melting furnace power increases to seed crystal and charge bar melts and formed stable molten Area, then seed crystal and charge bar are reversely rotated, rotating speed 25rpm, rate of crystalline growth 15~20mm/h of unit, grow to 2- Enter step 3) after 5cm length；
    3) optical region smelting furnace is used, with the YbB of a zone-refine6For charge bar, the YbB sintered with step 1)6Polycrystalline rod is Seed crystal carries out second of area and melted；After equipment is evacuated to below 1Pa, 20min zone melting furnace power increases to seed crystal and charge bar fusing And stable melting zone is formed, then seed crystal and charge bar are reversely rotated, rotating speed 25rpm, rate of crystalline growth 6~8mm/h of unit, Grow 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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CN106012011B (en) * 2016-05-11 2018-05-18 合肥工业大学 A kind of LaB6-ZrB2The preparation method of eutectic composites
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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