CN108396375A - A kind of crucible device of isoepitaxial growth aluminum-nitride single crystal - Google Patents

A kind of crucible device of isoepitaxial growth aluminum-nitride single crystal Download PDF

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Publication number
CN108396375A
CN108396375A CN201810269548.4A CN201810269548A CN108396375A CN 108396375 A CN108396375 A CN 108396375A CN 201810269548 A CN201810269548 A CN 201810269548A CN 108396375 A CN108396375 A CN 108396375A
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China
Prior art keywords
crucible
seed crystal
kuppe
single crystal
aluminium nitride
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CN201810269548.4A
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Inventor
吴亮
贺广东
雷丹
黄嘉丽
王智昊
王琦琨
龚加玮
黄毅
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Suzhou Trend Optoelectronics Technology Co Ltd
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Suzhou Trend Optoelectronics Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B23/00Single-crystal growth by condensing evaporated or sublimed materials
    • C30B23/02Epitaxial-layer growth
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10Inorganic compounds or compositions
    • C30B29/40AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
    • C30B29/403AIII-nitrides

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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

The invention discloses a kind of crucible devices of isoepitaxial growth aluminum-nitride single crystal, it is used to place the crucible body of aluminium nitride seed crystal, the crucible cover at the top of crucible body, the fixed mechanism for being fixed on aln raw material above aluminium nitride seed crystal in crucible body including bottom, crucible device further includes being set to kuppe between aln raw material and aluminium nitride seed crystal, and kuppe is along close to the direction of aluminium nitride seed crystal gradual radial contraction downwards.A kind of crucible device of isoepitaxial growth aluminum-nitride single crystal of the present invention, it will be placed directly in crucible bottom for the aluminium nitride seed crystal of growing aluminum nitride monocrystalline, aln raw material is placed on crucible middle and upper part, it is inverted raw material area and vitellarium, avoiding the adhesive layer that traditional seed crystal technique for sticking is brought has the shortcomings that bubble, seed crystal face pollution;By the way that kuppe is arranged in crucible body, mass transfer direction in crucible body is optimized, the rate of aluminium nitride seed crystal epitaxial growth has been greatly facilitated.

Description

A kind of crucible device of isoepitaxial growth aluminum-nitride single crystal
Technical field
The present invention relates to a kind of crucible devices of isoepitaxial growth aluminum-nitride single crystal.
Background technology
Aluminium nitride(AlN)Typical material of the crystal as third generation semiconductor has broad-band gap, high resistivity highly thermally conductive Rate and high electronic drifting rate, while also there is good ultraviolet permeability, high disruptive field intensity.It is manufacture high temperature, height Frequently, the ideal material of radioresistance and high power device.In addition AlN crystal is also as III race such as epitaxial growth GaN, AlGaN The best substrate material of nitride, compared with common SiC substrate, Sapphire Substrate, the lattice mismatch of AlN and GaN, thermal mismatching are all It is relatively smaller.The preparation method of AlN crystal mainly has physical vapor transport at present(PVT), hydride vapour phase epitaxy method (HVPE), metal organic chemical compound vapor deposition method(MOCVD)Deng.Wherein physical vapor transport(PVT)It is that current growth is big The most common method of size high quality aluminum nitride crystal, basic process are to make aln raw material by being heated in crucible Its decompose distillation, then again low-temperature space depositing crystalline at aluminum nitride crystal.
Method is by continuing to develop, now more often using the crystal grain obtained with spontaneous nucleation by cutting, chemical machinery The chip made after polishing is that seed crystal carries out isoepitaxial growth.Carrying out isoepitaxial growth with AlN substrates can effectively prepare Go out that dislocation is few, the small high quality single crystal of stress.Existing grower is that aln raw material is placed on crucible bottom mostly, Aluminium nitride seed crystal is bonded at crucible cover, crucible is heated to grow aluminum-nitride single crystal.
This grower is very high to the processing requirement of seed crystal, and the surface damage layer of seed crystal after treatment can cause Crystal dislocation increases when epitaxial growth, and the stomata caused by the bonding agent that seed crystal bonding uses can be also transmitted in epitaxial growth It grows in crystal, causes crystal hole or crackle occur, it is often to lead to isoepitaxial growth failure that seed crystal, which is bonded improper, The technology of main cause, seed crystal bonding has become the technical barrier for hindering related scientific research unit.Therefore it is same PVT methods how to be solved Seed crystal bonding problem in matter epitaxial growth aluminum-nitride single crystal, which becomes, restricts downstream aluminium nitride related electronic devices industry development Key factor.
Invention content
The object of the present invention is to provide a kind of crucible devices of isoepitaxial growth aluminum-nitride single crystal, can effectively avoid The problems such as seed crystal caused by aluminium nitride seed crystal bonding pollutes during aluminium nitride isoepitaxial growth, growth crystal quality is poor, energy Enough prepare the large-sized aluminum-nitride single crystal of high quality.
In order to achieve the above objectives, the technical solution adopted by the present invention is:
A kind of crucible device of isoepitaxial growth aluminum-nitride single crystal, including bottom are used to place the crucible sheet of aluminium nitride seed crystal Body, is used to aln raw material being fixed on institute the crucible cover at the top of the crucible body in the crucible body The fixed mechanism above aluminium nitride seed crystal is stated, the crucible device further includes being set to the aln raw material and the aluminium nitride seed Kuppe between crystalline substance, the kuppe, along the direction gradual radial contraction downwards close to the aluminium nitride seed crystal.
Preferably, the fixed mechanism includes bonding agent, and the aln raw material is by the adhesive bonds described The lower surface of crucible cover.
It is highly preferred that the fixed mechanism includes separation net, the aln raw material is placed on the separation net, described The first step for placing the separation net is equipped in crucible body.
It is further preferred that the aperture of the separation net is 0.5-10mm, the thickness of the separation net is 0.1-5mm.
Preferably, the second step being located at below the first step is equipped in the crucible body, the kuppe Upper end edge its be circumferentially with the extension for being placed on the second step.
Preferably, the kuppe is in the downward taper of cone angle.
It is highly preferred that the kuppe is distributed with the crucible body coaxial inner conductor, the aluminium nitride seed crystal is located at described On the axial line of kuppe.
Preferably, the crucible cover is sheathed in the crucible body, inside circumference and the crucible of the crucible cover The distance between outside circumference of ontology is 0.01-1mm.
Preferably, the thickness of the kuppe is 0.1-3mm.
Preferably, the distance between the bottom of the kuppe and aluminium nitride seed crystal upper surface are 0-50mm.
Due to the application of the above technical scheme, the present invention has following advantages compared with prior art:It is of the invention a kind of same The crucible device of matter epitaxial growth aluminum-nitride single crystal will be placed directly in crucible bottom for the aluminium nitride seed crystal of growing aluminum nitride monocrystalline Aln raw material is placed on crucible middle and upper part, is inverted raw material area and vitellarium, avoids what traditional seed crystal technique for sticking was brought by portion Adhesive layer has the shortcomings that bubble, seed crystal face pollution;By the way that kuppe is arranged in crucible body, optimize in crucible body Mass transfer direction has greatly facilitated the rate of aluminium nitride seed crystal epitaxial growth.
Description of the drawings
Attached drawing 1 is the structural schematic diagram of apparatus of the present invention;
Attached drawing 2 is the structural schematic diagram of separation net;
Attached drawing 3 is the structural schematic diagram of kuppe.
Wherein:1, crucible body;2, crucible cover;3, aln raw material;4, aluminium nitride seed crystal;5, kuppe;6, separation net; 7, first step;8, second step;9, extension.
Specific implementation mode
The technical solution of the present invention will be further described below with reference to the accompanying drawings.
Referring to shown in Fig. 1-3, a kind of above-mentioned crucible device of isoepitaxial growth aluminum-nitride single crystal, including bottom are used to put It sets the crucible body 1 of aluminium nitride seed crystal 4, be used to fix set on the crucible cover 2 at 1 top of crucible body, in crucible body 1 The fixed mechanism of aln raw material 3, aln raw material 3 are located at the top of aluminium nitride seed crystal 4.It will be for growing aluminum nitride monocrystalline Aluminium nitride seed crystal 4 is placed directly in crucible bottom, and aln raw material 3 is placed on crucible middle and upper part, is inverted raw material area and vitellarium, energy The adhesive layer that traditional seed crystal technique for sticking is brought enough is avoided to have the shortcomings that bubble, seed crystal face pollution.
Fixed mechanism can only include bonding agent, and aln raw material 3 is by adhesive bonds in the lower surface of crucible cover 2.
In the present embodiment, fixed mechanism only includes separation net 6, and aln raw material 3 is placed on separation net 6, crucible sheet The first step 7 for placing separation net 6 is equipped in body 1.The first step 7 can be convexly equipped on the madial wall of crucible body 1, It can also be recessed in the madial wall of crucible body 1;In the present embodiment, first step 7 is convexly equipped in the madial wall of crucible body 1 On, the distance of protrusion is 1.5mm.Separation net 6 is rounded, and the aperture with the coaxial distribution of crucible body 1, separation net 6 is 0.5- The thickness of 10mm, separation net 6 are 0.1-5mm.In the present embodiment, the aperture of mesh is 5mm in separation net 6, and thickness is 0.5mm, the gas phase transmission that appropriately sized mesh contributes to aln raw material 3 to distil carry out crystal life at aluminium nitride seed crystal 4 Long, it is uniform that relatively thin thickness also contributes to raw material area heterogeneity phantom.
Fixed mechanism can also include bonding agent and separation net 6 simultaneously, and the upper surface of aln raw material 3 is viscous by bonding agent It closes on crucible cover 2, the lower surface of aln raw material 3 contradicts on separation net 6, by dual fixation, is risen to aln raw material 3 Better fixed effect is arrived.
Crucible device further includes the kuppe 5 being set between aln raw material 3 and aluminium nitride seed crystal 4, and kuppe 5 is along close The direction of aluminium nitride seed crystal 4 gradual radial contraction downwards.The second step for being located at 7 lower section of first step is equipped in crucible body 1 8, the upper end edge of kuppe 5 its be circumferentially with the extension 9 for being placed on second step 8.The extension 9 in a ring, edge Horizontal direction extends.The second step 8 can be convexly equipped on the madial wall of crucible body 1, can also be recessed in crucible body 1 In madial wall;In the present embodiment, second step 8 is convexly equipped on the madial wall of crucible body 1, and the distance of protrusion is 1.5mm.
In the present embodiment, kuppe 5 is in the downward conical distribution of cone angle.Kuppe 5 and 1 coaxial inner conductor of crucible body point Cloth, aluminium nitride seed crystal 4 are located on the axial line of kuppe 5, by this setting, can improve mass-transfer efficiency.The thickness of kuppe 5 Degree is 0.1-3mm;The distance between bottom and 4 upper surface of aluminium nitride seed crystal of kuppe 5 are 0-50mm.In the present embodiment, The cone angle of kuppe 5 is 60 °, and the distance between aluminium nitride seed crystal 4 is 20mm, is conducive to lead top raw material area distillation gas phase It is streamed to 4 surface of aluminium nitride seed crystal, reaches preferable degree of supersaturation, promotes crystal growth.
Crucible cover 2 is sheathed in crucible body 1, and the inside circumference of crucible cover 2 is with the outside circumference of crucible body 1 along crucible The distance between 1 radial direction of ontology is 0.01-1mm.In the present embodiment, which is 0.5mm, and smaller gap can ensure earthenware There is good air-tightness between crucible ontology 1 and crucible cover 2.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art Scholar cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all according to the present invention Equivalent change or modification made by Spirit Essence, should be covered by the protection scope of the present invention.

Claims (10)

1. a kind of crucible device of isoepitaxial growth aluminum-nitride single crystal, it is characterised in that:Including bottom for placing aluminium nitride The crucible body of seed crystal, is used in the crucible body by aluminium nitride the crucible cover at the top of the crucible body Raw material is fixed on the fixed mechanism above the aluminium nitride seed crystal, the crucible device further include be set to the aln raw material and Kuppe between the aluminium nitride seed crystal, the kuppe, along gradually radial downwards close to the direction of the aluminium nitride seed crystal It shrinks.
2. a kind of crucible device of isoepitaxial growth aluminum-nitride single crystal according to claim 1, it is characterised in that:It is described Fixed mechanism includes bonding agent, and the aln raw material is by the adhesive bonds in the lower surface of the crucible cover.
3. a kind of crucible device of isoepitaxial growth aluminum-nitride single crystal according to claim 1 or 2, it is characterised in that: The fixed mechanism includes separation net, and the aln raw material is placed on the separation net, is equipped with and uses in the crucible body In the first step for placing the separation net.
4. a kind of crucible device of isoepitaxial growth aluminum-nitride single crystal according to claim 3, it is characterised in that:It is described The aperture of separation net is 0.5-10mm, and the thickness of the separation net is 0.1-5mm.
5. a kind of crucible device of isoepitaxial growth aluminum-nitride single crystal according to claim 1, it is characterised in that:It is described Be equipped with the second step being located at below the first step in crucible body, the upper end edge of the kuppe its be circumferentially with and be used for The extension being placed on the second step.
6. a kind of crucible device of isoepitaxial growth aluminum-nitride single crystal according to claim 1, it is characterised in that:It is described Kuppe is in the downward taper of cone angle.
7. a kind of crucible device of isoepitaxial growth aluminum-nitride single crystal according to claim 6, it is characterised in that:It is described Kuppe is distributed with the crucible body coaxial inner conductor, and the aluminium nitride seed crystal is located on the axial line of the kuppe.
8. a kind of crucible device of isoepitaxial growth aluminum-nitride single crystal according to claim 1, it is characterised in that:It is described Crucible cover is sheathed in the crucible body, between the inside circumference of the crucible cover and the outside circumference of the crucible body Distance is 0.01-1mm.
9. a kind of crucible device of isoepitaxial growth aluminum-nitride single crystal according to claim 1, it is characterised in that:It is described The thickness of kuppe is 0.1-3mm.
10. a kind of crucible device of isoepitaxial growth aluminum-nitride single crystal according to claim 1, it is characterised in that:Institute It is 0-50mm to state the distance between bottom and aluminium nitride seed crystal upper surface of kuppe.
CN201810269548.4A 2018-03-29 2018-03-29 A kind of crucible device of isoepitaxial growth aluminum-nitride single crystal Withdrawn CN108396375A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110886018A (en) * 2019-12-03 2020-03-17 中国电子科技集团公司第四十六研究所 Growth method of large-size high-quality aluminum nitride single crystal
CN112126975A (en) * 2020-09-18 2020-12-25 山东国晶电子科技有限公司 Silicon carbide single crystal growth device
CN113337886A (en) * 2021-06-04 2021-09-03 哈尔滨科友半导体产业装备与技术研究院有限公司 Thermal field device and method for high-quality single crystal growth by PVT (physical vapor transport) method
CN113622030A (en) * 2021-08-18 2021-11-09 福建北电新材料科技有限公司 Method for preparing silicon carbide single crystal

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Publication number Priority date Publication date Assignee Title
JPH06183897A (en) * 1992-12-16 1994-07-05 Nisshin Steel Co Ltd Method for growing silicon carbide single crystal
CN205223407U (en) * 2015-11-24 2016-05-11 北京华进创威电子有限公司 Growth aluminum nitride crucible for single crystal
CN107723788A (en) * 2017-10-20 2018-02-23 苏州奥趋光电技术有限公司 A kind of crucible device for aluminum-nitride single crystal growth
CN107829134A (en) * 2017-11-22 2018-03-23 北京大学 A kind of aluminum-nitride single crystal grower and method without seed crystal adhesive technology
CN208151521U (en) * 2018-03-29 2018-11-27 苏州奥趋光电技术有限公司 A kind of crucible device of isoepitaxial growth aluminum-nitride single crystal

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06183897A (en) * 1992-12-16 1994-07-05 Nisshin Steel Co Ltd Method for growing silicon carbide single crystal
CN205223407U (en) * 2015-11-24 2016-05-11 北京华进创威电子有限公司 Growth aluminum nitride crucible for single crystal
CN107723788A (en) * 2017-10-20 2018-02-23 苏州奥趋光电技术有限公司 A kind of crucible device for aluminum-nitride single crystal growth
CN107829134A (en) * 2017-11-22 2018-03-23 北京大学 A kind of aluminum-nitride single crystal grower and method without seed crystal adhesive technology
CN208151521U (en) * 2018-03-29 2018-11-27 苏州奥趋光电技术有限公司 A kind of crucible device of isoepitaxial growth aluminum-nitride single crystal

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110886018A (en) * 2019-12-03 2020-03-17 中国电子科技集团公司第四十六研究所 Growth method of large-size high-quality aluminum nitride single crystal
CN112126975A (en) * 2020-09-18 2020-12-25 山东国晶电子科技有限公司 Silicon carbide single crystal growth device
CN113337886A (en) * 2021-06-04 2021-09-03 哈尔滨科友半导体产业装备与技术研究院有限公司 Thermal field device and method for high-quality single crystal growth by PVT (physical vapor transport) method
CN113622030A (en) * 2021-08-18 2021-11-09 福建北电新材料科技有限公司 Method for preparing silicon carbide single crystal

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