CN104818519A - Method for improving properties of nonlinear optical crystal of ZnGeP2 - Google Patents
Method for improving properties of nonlinear optical crystal of ZnGeP2 Download PDFInfo
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- CN104818519A CN104818519A CN201510189486.2A CN201510189486A CN104818519A CN 104818519 A CN104818519 A CN 104818519A CN 201510189486 A CN201510189486 A CN 201510189486A CN 104818519 A CN104818519 A CN 104818519A
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- magnetic field
- zngep
- crystal
- zngep2
- directional solidification
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Abstract
The invention discloses a method for improving the properties of a nonlinear optical crystal of ZnGeP2. The method comprises directionally growing synthesized ZnGeP2 polycrystalline materials into a superconducting magnet uniform magnetic field and a gradient magnetic field, specifically, increasing the temperature slowly to 1070 DEG C, and after the polycrystalline materials are melt, performing heat preservation for 8 h and then performing directional solidification, wherein the crystal growth speed is 0.5 mu m/s; after the polycrystalline materials grow for 40 h, reducing the temperature slowly to obtain monocrystalline ZnGeP2 with intact appearance and few cracks. The method for improving the properties of the nonlinear optical crystal of ZnGeP2 can obviously improve the optical and electrical properties of the monocrystalline ZnGeP2 compared with methods without the magnetic fields.
Description
Technical field
The present invention relates to a kind of growing method improving crystal mass, under specifically relating to a kind of high-intensity magnetic field, grow the method for non-linear optic crystal.Belong to optical crystal preparing technical field.
Background technology
ZnGeP
2crystal is ternary II-IV-V
2race's chalcopyrite based semiconductor, has the large and far infrared of nonlinear optical coefficients through advantages such as wide wavebands, therefore ZnGeP
2crystal is considered to the best middle infrared nonlinear optical crystal of over-all properties.But difficulty maximum is at present difficult to obtain excellent performance, large-sized infrared nonlinear optical crystal.The nearly more than ten years, high-intensity magnetic field is applied to the study hotspot that process of setting has become new in material electromagnetic treatment research field.High-intensity magnetic field is applied to the process such as preparation, processing, process of material by people, different from ordinary electromagnetic field action, the energy of high strength contactlessly can be delivered to the atomic scale of material by it, change the behaviors such as the arrangement of atom, coupling and migration, thus realize the control of material technology process and the improvement of structure and properties.The present invention proposes to grow non-linear optic crystal ZnGeP under high-intensity magnetic field
2, based on the effect alleviating flowing under the effect of the magnetic brake melt of static magnetic field and gradient magnetic, improve growth quality and the performance of crystal.
Summary of the invention
One of the present invention improves non-linear optic crystal ZnGeP
2the method of performance, is characterized in that having following process and step:
A. by ZnGeP
2polycrystal raw material is sealed in and vacuumizes in silica tube, then in the uniform magnetic field and upper gradient magnetic of high-intensity magnetic field, carries out directional solidification growth, ZnGeP
2crystalline growth velocity is 0.5 μm/s, after directional freeze 40h, obtains complete appearance, ZnGeP that crackle is few
2single crystal, and the infrared transmittivity of crystal and electrical property are significantly improved;
B. described ZnGeP
2polycrystal raw material need carry out directional solidification growth in the even strong region of high-intensity magnetic field 6T;
Or described ZnGeP c.
2polycrystal raw material need carry out directional solidification growth in the upper gradient magnetic of high-intensity magnetic field (magnetic field center weakens gradually to magneticstrength B direction, and gradient is-145 T/m).
Directional solidification growth ZnGeP under a kind of high-intensity magnetic field of the present invention
2crystal unit, it is the multipurpose plant that tradition is commonly used, and includes: thermal insulation layer, carborunbum tube, superconduction kicker magnet, pull system, alundum tube, polycrystalline specimen and corundum sheet.
Accompanying drawing explanation
Fig. 1 is directional solidification growth ZnGeP under high-intensity magnetic field of the present invention
2crystal unit schematic diagram.Wherein, 1 thermal insulation layer, 2 carborunbum tubes, 3 superconduction kicker magnets, 4 pull System's composition, 5 alundum tubes, 6 polycrystalline specimens, 7 corundum sheets.
Fig. 2 is the ZnGeP grown under different magnetic field condition of the present invention
2monocrystalline and crystal medium position wafer.Wherein, (a) is without magnetic field, (b) uniform magnetic field, (c) upper gradient magnetic.
Fig. 3 is ZnGeP of the present invention
2crystal infrared through spectrum.
Embodiment
By synthetic ZnGeP
2polycrystal raw material vacuumizes sealing, and the monocrystal growing furnace being placed in improvement grows, simultaneously at list
Crystals growth stove outside applies a longitudinal high-intensity magnetic field, and requires that this magnetic field can provide a steady magnetic field and upper gradient magnetic (magneticstrength and gradient magnetic amass maximum) herein.Under high-intensity magnetic field, device for directionally solidifying is made up of (see accompanying drawing 1) thermal insulation layer 1, heating element carborunbum tube 2, superconduction kicker magnet 3 and pull system 4, alundum tube 5 is fixed on above pull system 4, alundum tube is driven to move, by products material ZnGeP by the orientation movement of drawing device
2be sealed in the silica tube that vacuumizes, and it is inner to be placed on alundum tube 5; Polycrystalline specimen 6 also will along with drawing device generation orientation movement; Corundum sheet 7 can effectively reduce furnace temperature rangeability in addition, ensures that in sample grown process, furnace temperature keeps stable.
embodiment one
In the present embodiment, under adopting 6T uniform magnetic field condition, grow ZnGeP
2crystal, sample is placed in superconduction kicker magnet mid-way, and magneticstrength is adjusted to 6T magneticstrength, then sample is slowly heated to 1070 DEG C, directional freeze is carried out after constant temperature 8h, pulling rate is 0.5 μm/s, and the directional freeze time is 40h, and in process of growth, sample is in uniform magnetic field region all the time.Compare with without the crystal grown under magnetic field, the crystal outward appearance grown under uniform magnetic field be brighter, crackle less (see accompanying drawing 2); And the infrared transmittivity of crystal is 1000cm in wave number
-1place reaches 28%, is significantly improved (see accompanying drawing 3) compared with without 9% under magnetic field; Room temperature resistivity 4.44 × 10
6ohmcm, compared with without 7.017 × 10 under magnetic field
6ohmcm reduces; Crystal mass is improved significantly.
embodiment two
The present embodiment and embodiment difference are: in the present embodiment, and polycrystalline specimen position is in 11.5cm place, superconduction kicker magnet top, and magneticstrength and gradient magnetic amass maximum herein.Compare with without the crystal grown under magnetic field, the crystal outward appearance grown under upper gradient magnetic be brighter, crackle less (see accompanying drawing 2); And the infrared transmittivity of crystal is 4000 cm in wave number
-1and 1000cm
-1place reaches 22% and 16% respectively, is significantly improved (see accompanying drawing 3) compared with without 4% under magnetic field and 9%; Room temperature resistivity 3.394 × 10
6ohmcm, compared with without 7.017 × 10 under magnetic field
6ohmcm reduces; Crystal mass is improved significantly.
Claims (2)
1. one kind is improved non-linear optic crystal ZnGeP
2the method of performance, is characterized in that having following process and step:
A. by ZnGeP
2polycrystal raw material is sealed in the silica tube that vacuumizes, then in the uniform magnetic field and upper gradient magnetic of high-intensity magnetic field, carries out directional solidification growth, ZnGeP
2crystalline growth velocity is 0.5 μm/s, after directional freeze 40h, obtains complete appearance, ZnGeP that crackle is few
2single crystal, and the infrared transmittivity of crystal and electrical property are significantly improved;
B. described ZnGeP
2polycrystal raw material carries out directional solidification growth in the even strong region of high-intensity magnetic field 6T;
Or described ZnGeP c.
2polycrystal raw material need carry out directional solidification growth in the upper gradient magnetic of high-intensity magnetic field (magnetic field center weakens gradually to magneticstrength B direction, and gradient is-145 T/m).
2. the device of directional solidification growth ZnGeP2 crystal under a high-intensity magnetic field, it is the multipurpose plant that tradition is commonly used, and includes: thermal insulation layer (1), heating element carborunbum tube (2), superconduction kicker magnet (3), pull system (4), alundum tube (5), polycrystalline specimen (6) and corundum sheet (7).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510189486.2A CN104818519A (en) | 2015-04-21 | 2015-04-21 | Method for improving properties of nonlinear optical crystal of ZnGeP2 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510189486.2A CN104818519A (en) | 2015-04-21 | 2015-04-21 | Method for improving properties of nonlinear optical crystal of ZnGeP2 |
Publications (1)
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| CN104818519A true CN104818519A (en) | 2015-08-05 |
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Family Applications (1)
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|---|---|---|---|
| CN201510189486.2A Pending CN104818519A (en) | 2015-04-21 | 2015-04-21 | Method for improving properties of nonlinear optical crystal of ZnGeP2 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106835046A (en) * | 2017-02-15 | 2017-06-13 | 苏州思创源博电子科技有限公司 | A kind of ZnGeP2The preparation method of semiconductor material film |
| CN107268070A (en) * | 2017-06-10 | 2017-10-20 | 中国科学院合肥物质科学研究院 | A kind of method of low absorption phosphorus germanium zinc crystal growth |
| CN110042461A (en) * | 2019-04-30 | 2019-07-23 | 哈尔滨工业大学 | A kind of growing method increasing heat transmitting large scale zinc-germanium phosphide crystal |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1088634A (en) * | 1992-12-19 | 1994-06-29 | 中国科学院金属研究所 | Floating zone meling single crystal (or directional freeze) material preparation method in the electromagnetic field |
| CN2715885Y (en) * | 2004-07-08 | 2005-08-10 | 上海大学 | Gradient strong magnetic field unidirectional solidification crystallization apparatus |
| CN204491024U (en) * | 2015-01-04 | 2015-07-22 | 广东电网有限责任公司电力科学研究院 | A kind of device controlling superalloy oriented freezing organization |
-
2015
- 2015-04-21 CN CN201510189486.2A patent/CN104818519A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1088634A (en) * | 1992-12-19 | 1994-06-29 | 中国科学院金属研究所 | Floating zone meling single crystal (or directional freeze) material preparation method in the electromagnetic field |
| CN2715885Y (en) * | 2004-07-08 | 2005-08-10 | 上海大学 | Gradient strong magnetic field unidirectional solidification crystallization apparatus |
| CN204491024U (en) * | 2015-01-04 | 2015-07-22 | 广东电网有限责任公司电力科学研究院 | A kind of device controlling superalloy oriented freezing organization |
Non-Patent Citations (1)
| Title |
|---|
| GUODONG ZHANG ET AL.: "Growth and thermal annealing effect on infrared transmittance of ZnGeP2 single crystal", 《JOURNAL OF CRYSTAL GROWTH》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106835046A (en) * | 2017-02-15 | 2017-06-13 | 苏州思创源博电子科技有限公司 | A kind of ZnGeP2The preparation method of semiconductor material film |
| CN107268070A (en) * | 2017-06-10 | 2017-10-20 | 中国科学院合肥物质科学研究院 | A kind of method of low absorption phosphorus germanium zinc crystal growth |
| CN110042461A (en) * | 2019-04-30 | 2019-07-23 | 哈尔滨工业大学 | A kind of growing method increasing heat transmitting large scale zinc-germanium phosphide crystal |
| CN110042461B (en) * | 2019-04-30 | 2021-06-08 | 哈尔滨工业大学 | Growth method of large-size zinc germanium phosphide crystal for increasing heat transfer |
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Application publication date: 20150805 |