CN106435736A - Aluminum nitride crystal growing furnace - Google Patents

Aluminum nitride crystal growing furnace Download PDF

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Publication number
CN106435736A
CN106435736A CN201610822802.XA CN201610822802A CN106435736A CN 106435736 A CN106435736 A CN 106435736A CN 201610822802 A CN201610822802 A CN 201610822802A CN 106435736 A CN106435736 A CN 106435736A
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CN
China
Prior art keywords
crucible
aluminum nitride
nitride crystal
heater
temperature
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Pending
Application number
CN201610822802.XA
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Chinese (zh)
Inventor
吴亮
曹凯
王智昊
汪佳
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Suzhou Trend Optoelectronics Technology Co Ltd
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Suzhou Trend Optoelectronics Technology Co Ltd
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Priority to CN201610822802.XA priority Critical patent/CN106435736A/en
Publication of CN106435736A publication Critical patent/CN106435736A/en
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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
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10Inorganic compounds or compositions
    • C30B29/38Nitrides
    • 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

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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 an aluminum nitride crystal growing furnace. The aluminum nitride crystal growing furnace comprises a furnace body, a moving mechanism, a crucible, a multi-section heating mechanism, a heat insulation mechanism and a temperature measuring mechanism, wherein the moving mechanism vertically movably penetrates the bottom surface of the furnace body, the crucible is arranged at the top of the moving mechanism and arranged in the furnace body, the multi-section heating mechanism is arranged in the furnace body, vertically sequentially distributed and used for heating the crucible, the heat insulation mechanism is arranged on the outer side of the crucible, and the temperature measuring mechanism is arranged on the outer side of the furnace body and used for measuring the temperature of the crucible. The aluminum nitride crystal growing furnace has the advantages that the multi-section heating mechanism can provide a stable temperature field for aluminum nitride crystal growth; the three-way temperature measuring mechanism can accurately measure the temperature; the heat field in the growing furnace mainly adopts a tungsten heat screen and a boron nitride heat screen, a good heat insulation effect is achieved, the tungsten heat screen and the boron nitride heat screen can be demounted and replaced conveniently, and impurities can be effectively prevented from being introduced to cause crystal pollution.

Description

A kind of aluminum nitride crystal growth stove
Technical field
The present invention relates to a kind of aluminum nitride crystal growth stove.
Background technology
Aluminum-nitride single crystal, as third generation semiconductor material with wide forbidden band, has broad-band gap, high heat conductance, high carrier saturation Drift velocity simultaneously has high temperature resistant, high radiation preventing ability energy feature simultaneously, is making modern high power microelectronic component, photoelectron Field(As deep ultraviolet LED), the high-end sciemtifec and technical sphere such as high power electronic device and ultraviolet detection possess wide application prospect.Make For a kind of key national strategy material, now to be put into《Made in China 2025》Major fields Technology Roadmap.
Aluminum-nitride single crystal manufacturing process difficulty is very big, especially large-sized high quality single crystal piece.Prepare block nitrogen at present The best approach changing aluminum monocrystalline is physical vapor transport(PVT method), the method prepares monocrystalline and need to meet micro- low pressure, high temperature(Can Reach 2400 DEG C)Crystal growth condition, and to thermal field life-span and chemical stability etc. propose requirements at the higher level.Therefore grow size Greatly, defect is few, performance is good etc., and high-quality monocrystalline substrate material process specifications are very high.
Same category of device and its costliness in the world, domestic also do not have ready-made supply of equipment.And most of related equipment life The crystalline size that during long crystal, temperature field is unstable, intracavity impurity easily pollutes crystal, obtain is little, uniformity and concordance poor, Waiting not enough crack defect more.
Content of the invention
It is an object of the invention to provide a kind of aluminum nitride crystal growth stove, can provide stable for aluminum nitride crystal growth Temperature field.
For reaching above-mentioned purpose, the technical solution used in the present invention is:
A kind of aluminum nitride crystal growth stove, including:
Body of heater;
The up and down motion being arranged in described body of heater bottom surface;
Located at the crucible at described motion top, described crucible is in described body of heater;
Vertically be sequentially distributed in described body of heater for the multisection type heating arrangements that described crucible is heated;
Heat-shield mechanism outside described crucible;
The temperature measuring mechanism for measuring crucible temperature outside described body of heater.
Preferably, described multisection type heating arrangements are sensing heating mechanism, and described sensing heating mechanism includes being located on institute The epimere load coil state the heater outside crucible, being distributed up and down and hypomere load coil, described epimere sensing Heating coil and described hypomere load coil are all located between described heater and described inboard wall of furnace body.
It is highly preferred that described heat-shield mechanism include the first heat screen above described crucible, located at described crucible and The second heat screen between described motion, it is located on the 3rd heat screen outside described heater, is located on the described 3rd The 4th heat screen outside heat screen, described 4th heat screen adds located at described epimere load coil and the sensing of described hypomere The inner side of heat coil.
It is highly preferred that described sensing heating mechanism is also included located at described epimere load coil and the sensing of described hypomere Magnetic shielding device between heating coil.
It is highly preferred that described heater, described crucible and described motion are all made using tungsten.
Preferably, described multisection type heating arrangements are resistive heating mechanism, and described resistive heating mechanism includes two sections or two The above adding thermal resistance being distributed up and down of section, described adding thermal resistance is outside described crucible.
Preferably, described motion includes up and down being arranged in the support bar of described bottom of furnace body, located at described The support plate of support bar top.
Preferably, described temperature measuring mechanism include for measure described crucible top temperature the first measuring device, be used for measuring Second measuring device of described crucible middle portion temperature, the 3rd measuring device for measuring described crucible bottom temperature.
It is highly preferred that described first measuring device and described 3rd measuring device are high-temperature infrared temperature measurer.
It is highly preferred that described second measuring device is telescopic Wolfram rhenium heat electric couple.
Due to the utilization of technique scheme, the present invention compared with prior art has following advantages:A kind of nitrogen of the present invention Change aluminum crystal growing furnace, using multisection type heating arrangements, stable temperature field can be provided for aluminum nitride crystal growth;Using three Channel Temperature Measuring mechanism, can meet the accurate mensure of temperature;Thermal field in growth furnace mainly adopt tungsten heat screen and boron nitride every Heat shielding, high insulating effect, dismounting and change can be facilitated, and can effectively prevent introducing impurity from causing crystal contamination.
Brief description
Accompanying drawing 1 is the structural representation of apparatus of the present invention;
Accompanying drawing 2 is the structural representation in stove.
Wherein:1st, body of heater;2nd, motion;3rd, crucible;4th, heater;5th, epimere load coil;6th, hypomere sensing Heating coil;7th, the first heat screen;8th, the second heat screen;9th, the 3rd heat screen;10th, the 4th heat screen;11st, the first measuring device; 12nd, the second measuring device;13rd, the 3rd measuring device.
Specific embodiment
Come below in conjunction with the accompanying drawings technical scheme is further elaborated.
Referring to shown in Fig. 1-2, a kind of above-mentioned aluminum nitride crystal growth stove, including body of heater 1, in this body of heater 1 side wall, it is provided with use It is passed through the pipeline of cooling water in circulation.By being passed through cooling water in furnace wall, can prevent internal heterogeneity phantom from causing furnace wall temperature Spend height.
This aluminum nitride crystal growth stove also includes the up and down motion 2 being arranged on body of heater 1 bottom surface, detachable The crucible 3 located at this motion 2 top, this crucible 3 is inside body of heater 1.This crucible 3 shape can be designed as plane earthenware Crucible 3, taper crucible 3 or special-shaped crucible 3.In the present embodiment, this crucible 3 is used for two inches of aluminum nitride crystals of growth.Crucible 3 This motion 2 includes the up and down support bar being arranged on body of heater 1 bottom surface, the support plate located at this support bar top. This support plate is used for installing crucible 3.The rising or falling speed of this support bar can be adjusted within the scope of two, is 0.06- respectively 0.6mm/h(At a slow speed)And 0-750mm/h(Quickly).Slow-action is saved in long crystalline substance, and quick regulation is used for clearing up thermal field, conveniently tears open Repair.
This aluminum nitride crystal growth stove also include vertically being sequentially distributed in this body of heater 1 for crucible 3 The multisection type heating arrangements of heating, the heat-shield mechanism located at this crucible 3 outside.
In the present embodiment, this multisection type heating arrangements is sensing heating mechanism.By arranging multisection type heating arrangements, can With the temperature conditionss needed for the temperature of precise control crucible 3 upper-lower position, reasonable adjusting.This sensing heating mechanism includes being located on The heater 4 in crucible 3 outside, the epimere load coil 5 being distributed up and down and hypomere load coil 6, located at this epimere Magnetic shielding device between load coil 5 and this hypomere load coil 6.This magnetic shielding device is used for preventing two-route wire Circle inductive interference.This epimere load coil 5 and this hypomere load coil 6 are all located on this heater 4 and this body of heater 1 Between inwall.This heater 4 is in cylinder.Epimere load coil 5 and hypomere load coil 6 all twist windings Outside in heater 4.
Using two-part sensing heating mechanism, can be from main regulation two sections mode of heating.During the temperature rise period, Ke Yixian Heating crucible 3 top, then adjust heating crucible 3 bottom.For preventing the crystal growth initial stage, crucible 3 lid produces polycrystalline, Ke Yiti For stable temperature field, prevent crystal from producing thermal stress due to thermal expansion, cause crystal that crack defect occurs.During temperature-fall period, Hypomere load coil 6 can first be adjusted lower the temperature, epimere load coil 5 takes mitigation cooling, secondary to prevent Crystallization.This mode of heating, can the more efficient thermo parameters method ensureing crystal growth.
This heat-shield mechanism include the first heat screen 7 located at crucible 3 top, between crucible 3 and motion 2 the Two heat screens 8, it is located on the 3rd heat screen 9 in heater 4 outside, is located on the 4th heat screen 10 in the 3rd heat screen 9 outside. 4th heat screen 10 is located at the inner side of epimere load coil 5 and hypomere load coil 6.This first heat screen 7 He This second heat screen 8 is circle;3rd heat screen 9 and the 4th heat screen 10 are cylinder.By arrange first every Heat shielding 7, the second heat screen 8, the 3rd heat screen 9 and the 4th heat screen 10 can be thermally shielded to crucible 3 to a certain extent.The Three heat screens 9 have multilamellar, and multilamellar the 3rd heat screen 9, using separately hexagonal angle degree, staggered arrangement, is prevented effectively from magnetic induction.
Due to up to more than 3000 degrees Celsius of the fusing point of tungsten and boron nitride, it is not easily introduced impurity, surface reflectivity is high, insulation Effect is good.Therefore, in the present embodiment, the first heat screen 7, the second heat screen 8, the 3rd heat screen 9 are the tungsten that surface polishes Heat shielding;4th heat screen 10 is boron nitride heat shielding.Heater 4, crucible 3, support bar and support plate are all made using tungsten, have Effect prevents the impacts to crystal growth for the impurity such as oxygen and carbon in Conventional insulation graphite.
This multisection type heating arrangements can also be resistive heating mechanism, in another embodiment, this resistive heating mechanism Including about the three sections adding thermal resistances being distributed, this adding thermal resistance, outside crucible 3, is respectively used to heating crucible 3 top, middle part And bottom.
This aluminum nitride crystal growth stove also includes the temperature measuring mechanism for measuring crucible 3 temperature located at body of heater 1 outside.? In the present embodiment, this temperature measuring mechanism include for measure crucible 3 head temperature the first measuring device 11, be used for measuring in crucible 3 Second measuring device 12 of portion's temperature, the 3rd measuring device 13 for measuring crucible 3 bottom temp.This first measuring device 11 and this Three measuring devices 13 are high-temperature infrared temperature measurer, and its measurement range is 0-3000 DEG C, and precision is ± 0.3%+1 DEG C.This second measuring device 12 is telescopic Wolfram rhenium heat electric couple, and its measurement range is 0-2300 DEG C, in measurement, can be using measuring method in short-term, thermometric Retract immediately afterwards, prevent high temperature failure thermocouple.By this setting, can be with comprehensive monitor in real time temperature of thermal field.
Illustrate the work process of lower the present embodiment in detail below:
During work, the internal evacuation first to body of heater 1, being re-filled with mass ratio is 97%:3% nitrogen and hydrogen, by body of heater 1 Pressure is adjusted to 60kpa-100kpa.Crucible 3 thickness takes 2mm, and crucible 3 lid is using plane.To epimere load coil 5 He Hypomere load coil 6 is energized, vortex induction heater 4, and heater 4 radiant heat transfer is to crucible 3.Powder source is inside crucible 3 It is heated to 2200 DEG C, surveyed the temperature of crucible 3 top and bottom, the second survey by the first measuring device 11 and the 3rd measuring device 13 respectively Measuring device 12 measures the temperature of crucible 3 middle part of sliding channel.Epimere load coil 5 and hypomere sensing heating are adjusted according to measurement result Size of current in coil 6, makes crucible 3 be axially formed thermograde, and gas powder sublimes up into spontaneous nucleation crystallization at crucible 3 lid.
Above-described embodiment only technology design to illustrate the invention and feature, its object is to allow person skilled in the art Scholar will appreciate that present disclosure and is carried out, and can not be limited the scope of the invention with this, all according to the present invention Equivalence changes or modification that spirit is made, all should cover within the scope of the present invention.

Claims (10)

1. a kind of aluminum nitride crystal growth stove it is characterised in that:Described growth furnace includes:
Body of heater;
The up and down motion being arranged in described body of heater bottom surface;
Located at the crucible at described motion top, described crucible is in described body of heater;
Vertically be sequentially distributed in described body of heater for the multisection type heating arrangements that described crucible is heated;
Heat-shield mechanism outside described crucible;
The temperature measuring mechanism for measuring crucible temperature outside described body of heater.
2. a kind of aluminum nitride crystal growth stove according to claim 1 it is characterised in that:Described multisection type heating arrangements are Sensing heating mechanism, described sensing heating mechanism includes being located on heater outside described crucible, the epimere sense being distributed up and down Heating coil and hypomere load coil, described epimere load coil and the equal ring of described hypomere load coil is answered to set Between described heater and described inboard wall of furnace body.
3. a kind of aluminum nitride crystal growth stove according to claim 2 it is characterised in that:Described heat-shield mechanism include located at The first heat screen above described crucible, the second heat screen between described crucible and described motion, it is located on institute State the 3rd heat screen outside heater, be located on the 4th heat screen outside described 3rd heat screen, described 4th heat screen Inner side located at described epimere load coil and described hypomere load coil.
4. a kind of aluminum nitride crystal growth stove according to claim 2 it is characterised in that:Described sensing heating mechanism also wraps Include the magnetic shielding device between described epimere load coil and described hypomere load coil.
5. a kind of aluminum nitride crystal growth stove according to claim 2 it is characterised in that:Described heater, described crucible All made using tungsten with described motion.
6. a kind of aluminum nitride crystal growth stove according to claim 1 it is characterised in that:Described multisection type heating arrangements are Resistive heating mechanism, described resistive heating mechanism includes the adding thermal resistance that two or more are distributed up and down, described heating electricity Resistance is outside described crucible.
7. a kind of aluminum nitride crystal growth stove according to claim 1 it is characterised in that:Described motion includes up and down Activity be arranged in described bottom of furnace body support bar, located at described support bar top support plate.
8. a kind of aluminum nitride crystal growth stove according to claim 1 it is characterised in that:Described temperature measuring mechanism include for Measure the first measuring device of described crucible top temperature, be used for measuring the second measuring device of described crucible middle portion temperature, being used for surveying Measure the 3rd measuring device of described crucible bottom temperature.
9. a kind of aluminum nitride crystal growth stove according to claim 8 it is characterised in that:Described first measuring device and described 3rd measuring device is high-temperature infrared temperature measurer.
10. a kind of aluminum nitride crystal growth stove according to claim 8 it is characterised in that:Described second measuring device is to stretch Contracting formula Wolfram rhenium heat electric couple.
CN201610822802.XA 2016-09-14 2016-09-14 Aluminum nitride crystal growing furnace Pending CN106435736A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107460541A (en) * 2017-09-12 2017-12-12 中国电子科技集团公司第四十六研究所 The aluminum nitride crystal growth device controllable for raw material distillation and application method
WO2021138771A1 (en) * 2020-01-06 2021-07-15 奥趋光电技术(杭州)有限公司 Heating device and preparation method for mass preparation of high-quality aluminium nitride templates

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1570225A (en) * 2003-04-24 2005-01-26 奥克麦蒂克有限公司 Device and method for producing single crystals by vapor deposition
JP2009249202A (en) * 2008-04-02 2009-10-29 Fujikura Ltd Method for producing aluminum nitride single crystal
CN201711501U (en) * 2010-05-26 2011-01-19 丽达科技有限公司 Silicon electromagnet casting device
CN204714946U (en) * 2015-03-10 2015-10-21 深圳大学 The aluminum nitride crystal growth device that temperature field is controlled and technique
CN205990462U (en) * 2016-09-14 2017-03-01 苏州奥趋光电技术有限公司 A kind of aluminum nitride crystal growth stove

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1570225A (en) * 2003-04-24 2005-01-26 奥克麦蒂克有限公司 Device and method for producing single crystals by vapor deposition
JP2009249202A (en) * 2008-04-02 2009-10-29 Fujikura Ltd Method for producing aluminum nitride single crystal
CN201711501U (en) * 2010-05-26 2011-01-19 丽达科技有限公司 Silicon electromagnet casting device
CN204714946U (en) * 2015-03-10 2015-10-21 深圳大学 The aluminum nitride crystal growth device that temperature field is controlled and technique
CN205990462U (en) * 2016-09-14 2017-03-01 苏州奥趋光电技术有限公司 A kind of aluminum nitride crystal growth stove

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107460541A (en) * 2017-09-12 2017-12-12 中国电子科技集团公司第四十六研究所 The aluminum nitride crystal growth device controllable for raw material distillation and application method
WO2021138771A1 (en) * 2020-01-06 2021-07-15 奥趋光电技术(杭州)有限公司 Heating device and preparation method for mass preparation of high-quality aluminium nitride templates

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