CN106048723A - Solid-liquid interface control method for growing gallium oxide crystal by utilization of pulling method - Google Patents
Solid-liquid interface control method for growing gallium oxide crystal by utilization of pulling method Download PDFInfo
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- CN106048723A CN106048723A CN201610615338.7A CN201610615338A CN106048723A CN 106048723 A CN106048723 A CN 106048723A CN 201610615338 A CN201610615338 A CN 201610615338A CN 106048723 A CN106048723 A CN 106048723A
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- auxiliary heater
- crystal
- shouldering
- height
- gallium oxide
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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
- C30B29/16—Oxides
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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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/20—Controlling or regulating
- C30B15/22—Stabilisation or shape controlling of the molten zone near the pulled crystal; Controlling the section of the crystal
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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 solid-liquid interface control method for growing a gallium oxide crystal by utilization of a pulling method. The method comprises the following steps that an auxiliary heater is arranged in a single crystal furnace body as a second heat source, and is connected with a pulling device through a fixing bracket; the position of the auxiliary heater is lifted to the top part of the single crystal furnace body in a primary stage of seeding and shouldering; the position of the auxiliary heater is descended in a growth stage of shouldering and diameter equalizing; the ascending or descending height of the auxiliary heater is calculated by the following steps that before the crystal is drawn, an initial height of a melt liquid surface is calculated according to the feeding amount of a Ga2O3 raw material, and the height position of the auxiliary heater is set according to a thermal field system structure. By utilization of the method disclosed by the invention, the thermal field distribution and heat dissipation condition can be improved, and a general cambered crystallization interface is converted into a planar crystallization interface. The method disclosed by the invention has the advantages that the thermal field system is obviously better than a conventional thermal field system, different parts can be separately heated according to different Cz (Czochralski) crystal pulling stages, the method is more suitable for growing a low-dislocation single crystal, and the crystal forming rate is improved.
Description
Technical field
The present invention relates to single crystal preparation technology, particularly relate to a kind of solid-liquid circle using Czochralski grown gallium oxide crystal
Face control method.
Background technology
Czochralski method (being called for short Cz method, again for czochralski method) is a kind of melt method crystal being most widely used at present
Growing method.In Cz method crystal growing process, the raw material of crystal growth is placed in crucible and adds heat fusing, it is thus achieved that certain mistake
Temperature.The seed crystal being fixed on crystal pulling rod is immersed melt from bath surface, after generating unit fractional melting, the most upwards lifts seed
Crystalline style, and pass through seed rod and shoulder to function of environment heat emission.First the melt contacted with seed crystal obtains certain degree of supercooling, and occurs
Crystallization.Constantly lift seed rod, make crystallization process be carried out continuously, thus realize continuous print crystal growth.
Monocline gallium oxide (Ga2O3) it is a kind of semiconductor material with wide forbidden band (energy gap Eg=4.9 eV), there is good thing
Physical chemistry characteristic, it is expected to for making the Novel Optoelectronic Device that wavelength is shorter.Ga2O3Material has a multiple phase structure, but only β phase
Can be at low temperature to high temperature stable existence.Being in the starting stage about gallium oxide single crystal growth the most both at home and abroad, Cz method is for giving birth to
The standard method of this crystal long.
The gallium oxide single crystal substrate with fabricating low-defect-density is the basic demand preparing high-performance novel photoelectric device.For
Cz method Ga2O3Crystal Growth Technique, it is thus achieved that the solid-liquid interface shape of plane or dimpling is effective way of growth low-dislocation-density monocrystalline
Footpath.
The macro morphology of crystalizing interface depends primarily on the heat-flux conditions of near interface.Raw at currently used Cz stove crystal
In growth device, the hot-fluid near crystalizing interface specifically includes that crystal radiant heat, melt convection are conducted heat by sidewall of crucible, plane of crystal
To environmental radiation and heat loss through convection, crystal is by seed rod heat loss through conduction.The above two are hot-fluid input items, and latter two is hot-fluid output
?.Under the conditions of the furnace binding designed, crucible structure, the thermal field of Cz method crystal growth is maintained substantially to determine, therefore,
In above-mentioned four hot-fluid items, in addition to convective term, other three heat flow densities produced are difficult to be adjusted by process conditions
Joint；But, if using traditional method change melt convection heat transfer item by changing crucible rotation or crystal rotation, can be certain
Degree improves solid-liquid interface shape, but also easily causes the change of Convection states, thus produces attached to the uniformity of crystal doping
The adverse effect added.Therefore, fundamentally thermal field is optimized be only solve the problems referred to above key.
Summary of the invention
In view of prior art present situation and the technical problem of existence, the present invention provides a kind of and uses Czochralski grown gallium oxide brilliant
The solid liquid interface control method of body.
The present invention adopts the technical scheme that: a kind of solid liquid interface controlling party using Czochralski grown gallium oxide crystal
Method, it is characterised in that this control method is be provided with as the tapered shape of Secondary Heat Source and center drilling in monocrystalline body of heater auxiliary
Helping heater, auxiliary heater cone angle angle of inclination is consistent with crystal shouldering angle, and auxiliary heater is connected to by fixed mount
On pulling apparatus, in the growth seeding of gallium oxide crystal, the shouldering starting stage, auxiliary heater position is risen to monocrystalline body of heater top
Portion, heats seed rod, in the growth shouldering of gallium oxide crystal, the isodiametric growth stage, is declined auxiliary heater position,
Heating position near shouldering, the computational methods of the height that auxiliary heater rises or falls are: before drawing crystal,
By Ga2O3Raw material inventory calculates melt liquid level elemental height, according to thermal field system configuration settings auxiliary heater height position
Putting, auxiliary heater height and position calculates according to equation below: H=H0-h-D/2/tan(theta)
In formula: H represents auxiliary heater height and position, unit: mm；
H0Represent bushing position, unit: mm, Cz control system directly read；
H represents the melt liquid level elemental height calculated, unit: mm；
D represents drawing crystal diameter；Unit: mm；
Theta represents the half of crystal shouldering angle.
At Ga2O3In Crystal Growth Technique, owing to Cz body of heater longitudinal direction gradient is relatively big, atmosphere convection current is strong.At Cz growth technique
In, seed rod rate of heat dispation is basically unchanged, and along with crystalline size expands, shouldering position heat-sinking capability is gradually strengthened, therefore solid
Liquid interface configuration will be progressively changed into the recessed interface in later stage by the Raised key axis at initial stage.Nonplanar crystalizing interface, easily generates height
The gallium oxide single crystal of dislocation density.
As it is shown in figure 1, the present invention proposes a kind of novel C z method solid-liquid interface shape optimization method, i.e. design in Cz body of heater
Adding an auxiliary heater, this structure material is iraurite material.This material, under induction coil the action of a magnetic field, produces faradic current
And generate heat, can be as Secondary Heat Source.As in figure 2 it is shown, the tapered shape of auxiliary heater structure and center drilling, perforate is used for passing through
Seed crystal lifting bar and the crystal ingot of drawing.Auxiliary heater cone angle angle of inclination is consistent with crystal shouldering angle, generally 90 degree.
Auxiliary heater is connected on pulling apparatus by fixed mount, it is achieved auxiliary heater rise and fall process (this pulling apparatus
Structure can refer to the seed crystal lifting device of Cz single crystal growing furnace).
The beneficial effect comprise that: use this method, heterogeneity phantom and heat radiation can be improved
Condition, is changed into plane crystalizing interface by general curved surface crystalizing interface.This thermal field system is substantially better than the thermal field of routine
System, and respectively different parts can be heated according to Cz crystal pulling different phase, it is more suitable for growing low dislocation monocrystalline and raising
Crystal forming rate.
Accompanying drawing explanation
Fig. 1 is that system arranges schematic diagram in the single crystal growing furnace of gallium oxide crystal growth；
Fig. 2 is the schematic top plan view that in Fig. 1, auxiliary heater amplifies.
Detailed description of the invention
Below in conjunction with accompanying drawing, the invention will be further described:
Seeing figures.1.and.2, this control method is to be provided with in monocrystalline body of heater 1 as the tapered shape of Secondary Heat Source and center drilling
Auxiliary heater 4, auxiliary heater 4 cone angle angle of inclination consistent with crystal shouldering angle (generally 90 degree), auxiliary heating
Device 4 is connected on pulling apparatus by fixed mount 3, in the growth seeding of gallium oxide crystal, the shouldering starting stage, auxiliary is heated
Device 4 position rises to monocrystalline body of heater 1 top, heats seed rod 2, on the growth shouldering of gallium oxide crystal, isodiametric growth rank
Section, declines auxiliary heater 4 position, heats position near shouldering, the height that auxiliary heater 4 rises or falls
Computational methods are: before drawing crystal, by Ga2O3Raw material inventory calculates melt liquid level elemental height, according to thermal field system
System configuration settings auxiliary heater 4 height and position, auxiliary heater 4 height and position calculates according to equation below: H=H0-h-
D/2/tan(theta)
In formula: H represents auxiliary heater height and position, unit: mm；
H0Represent bushing position, unit: mm, Cz control system directly read；
H represents the melt liquid level elemental height calculated, unit: mm；
D represents drawing crystal diameter；Unit: mm；
Theta represents the half of crystal shouldering angle.
Note: auxiliary heater pulling apparatus position coordinates keeps consistent with Cz control system position coordinates, coordinate positive direction
Downwards.When, in crystal continued growth, seed rod 2 lifting process, auxiliary heater 4 promotes with identical speed sync.
Auxiliary heater 4 material of this control method design is iraurite material, and purity is 99.95-99.999%.Auxiliary adds
Fixed mount 3 material of hot device is Mo.
Embodiment: preparationGa 2 O 3 Crystal, a diameter of 50.8mm.Design assistant heater chip thickness 1.5mm, cone-shaped bottom is opened
Mouth internal diameter is 120mm, and central upper portion perforate internal diameter is that 60mm(is more than preparationGa 2 O 3 The diameter 50.8mm of crystal).Specifically take
Following steps:
(1) with reference to traditional handicraft, the inspection of Cz furnace equipment is carried out；
(2) by Ga2O3Raw material loads crucible, is warming up to melting sources；
(3) control auxiliary heater 4 by pulling apparatus, make auxiliary heater 4 position be promoted to peak position；
(4) in seeding, shouldering starting stage, auxiliary heater 4 position is constant at peak, and auxiliary heater 4 surface is to seed crystal
Bar 2 heats；
(5) in shouldering, isodiametric growth stage, reduce auxiliary heater position, make auxiliary heater 4 lower end be in shouldering position
Sustained height；In subsequent crystallographic growth course, auxiliary heater 4 rises with constant speed, climbing speed and seed crystal lifting speed
Rate is consistent；
(6) crystal growth is complete, and traditional etching process can be used to obtain crystal growth interface striped.By striped clearly not
With the Curvature varying situation of the solid liquid interface 5 of growth stage, it is simultaneously available for the height optimizing auxiliary heater 4 in different phase
Position and the rate of pulling.
In crystal growing process, auxiliary heater is equivalent to face light (hot) source and produces the radiant heat of orientation, in addition its
Height and position can accurately regulate, and is therefore accurately controlled the position of heated member.Great many of experiments shows, at Cz method crystal growth
Seeding and shouldering initial stage, crystal solid liquid interface in being convex to melt structure, and shouldering latter stage and isodiametric growth stage in
Concave towards melt structure.Therefore, in the shouldering stage, auxiliary heater position is risen to monocrystalline body of heater top, seed rod is added
Heat, slows down seed rod heat conducting and radiating, thus reduces germ nucleus rate of heat dispation, makes the interface curvature being convex to melt reduce；?
In the isometrical stage, auxiliary heater position is reduced, now position near shouldering is heated, i.e. compensate shouldering position to environment
Heat radiation, i.e. weaken crystal in heat radiation radially, form axial one dimensional heat transfer state, it is easy to control by matrix crystalizing interface to
Plane crystalizing interface changes.Before drawing crystal, by Ga2O3Raw material inventory calculates melt liquid level elemental height, thus
According to system structure, specify auxiliary heater height and position H.
Claims (3)
1. the solid liquid interface control method using Czochralski grown gallium oxide crystal, it is characterised in that this control method is
Being provided with as the tapered shape of Secondary Heat Source and the auxiliary heater of center drilling in monocrystalline body of heater, auxiliary heater cone angle tilts
Angle is consistent with crystal shouldering angle, and auxiliary heater is connected on pulling apparatus by fixed mount, at growth gallium oxide crystal
Seeding, the shouldering starting stage, auxiliary heater position is risen to monocrystalline body of heater top, seed rod is heated, growth
The shouldering of gallium oxide crystal, isodiametric growth stage, auxiliary heater position is declined, position near shouldering is heated, auxiliary
The computational methods helping the height that heater rises or falls are: before drawing crystal, by Ga2O3Raw material inventory calculates
Melt liquid level elemental height, according to thermal field system configuration settings auxiliary heater height and position, auxiliary heater height and position is pressed
Calculate according to equation below: H=H0-h-D/2/tan(theta)
In formula: H represents auxiliary heater height and position, unit: mm；
H0Represent bushing position, unit: mm, Cz control system directly read；
H represents the melt liquid level elemental height calculated, unit: mm；
D represents drawing crystal diameter；Unit: mm；
Theta represents the half of crystal shouldering angle.
A kind of solid liquid interface control method using Czochralski grown gallium oxide crystal the most according to claim 1, it is special
Levying and be, described auxiliary heater material is iraurite material, and purity is 99.95-99.999%.
A kind of solid liquid interface control method using Czochralski grown gallium oxide crystal the most according to claim 2, it is special
Levying and be, the fixed mount material of auxiliary heater is Mo.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610615338.7A CN106048723A (en) | 2016-08-01 | 2016-08-01 | Solid-liquid interface control method for growing gallium oxide crystal by utilization of pulling method |
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| CN201610615338.7A CN106048723A (en) | 2016-08-01 | 2016-08-01 | Solid-liquid interface control method for growing gallium oxide crystal by utilization of pulling method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107541776A (en) * | 2017-08-14 | 2018-01-05 | 同济大学 | A kind of growth apparatus and method of large scale gallium oxide single crystal |
| CN111719180A (en) * | 2020-07-21 | 2020-09-29 | 江苏利泷半导体科技有限公司 | Growth equipment suitable for gallium oxide crystal |
| WO2020220766A1 (en) * | 2019-04-29 | 2020-11-05 | 上海新昇半导体科技有限公司 | Semiconductor crystal growth method and apparatus |
| CN112795982A (en) * | 2020-12-31 | 2021-05-14 | 杭州光学精密机械研究所 | Mold for growing large-size gallium oxide crystal by guided mode method and growing method |
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| JPH05279172A (en) * | 1991-04-20 | 1993-10-26 | Komatsu Denshi Kinzoku Kk | Method and apparatus for growing crystal |
| CN1197128A (en) * | 1997-03-21 | 1998-10-28 | 瓦克硅电子半导体材料股份公司 | Device and method for pulling single crystal |
| CN1738930A (en) * | 2002-11-12 | 2006-02-22 | Memc电子材料有限公司 | Crystal puller and method for growing a monocrystalline ingot |
| CN103668441A (en) * | 2013-12-23 | 2014-03-26 | 英利集团有限公司 | Vertical-pull method for silicon single crystal rod and prepared silicon single crystal rod employing same |
| CN204570091U (en) * | 2015-03-20 | 2015-08-19 | 江苏盎华光伏工程技术研究中心有限公司 | There is the single crystal growing furnace mending warm guide shell |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05279172A (en) * | 1991-04-20 | 1993-10-26 | Komatsu Denshi Kinzoku Kk | Method and apparatus for growing crystal |
| CN1197128A (en) * | 1997-03-21 | 1998-10-28 | 瓦克硅电子半导体材料股份公司 | Device and method for pulling single crystal |
| CN1738930A (en) * | 2002-11-12 | 2006-02-22 | Memc电子材料有限公司 | Crystal puller and method for growing a monocrystalline ingot |
| CN103668441A (en) * | 2013-12-23 | 2014-03-26 | 英利集团有限公司 | Vertical-pull method for silicon single crystal rod and prepared silicon single crystal rod employing same |
| CN204570091U (en) * | 2015-03-20 | 2015-08-19 | 江苏盎华光伏工程技术研究中心有限公司 | There is the single crystal growing furnace mending warm guide shell |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107541776A (en) * | 2017-08-14 | 2018-01-05 | 同济大学 | A kind of growth apparatus and method of large scale gallium oxide single crystal |
| WO2020220766A1 (en) * | 2019-04-29 | 2020-11-05 | 上海新昇半导体科技有限公司 | Semiconductor crystal growth method and apparatus |
| US12000060B2 (en) | 2019-04-29 | 2024-06-04 | Zing Semiconductor Corporation | Semiconductor crystal growth method and device |
| CN111719180A (en) * | 2020-07-21 | 2020-09-29 | 江苏利泷半导体科技有限公司 | Growth equipment suitable for gallium oxide crystal |
| CN112795982A (en) * | 2020-12-31 | 2021-05-14 | 杭州光学精密机械研究所 | Mold for growing large-size gallium oxide crystal by guided mode method and growing method |
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Application publication date: 20161026 |