CN107541776A - A kind of growth apparatus and method of large scale gallium oxide single crystal - Google Patents
A kind of growth apparatus and method of large scale gallium oxide single crystal Download PDFInfo
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Abstract
The present invention relates to a kind of growth apparatus and method of large scale gallium oxide single crystal, including zirconium oxide insulating brick (1), quartz tube (2), water cooling copper electrode (3), Iridium Crucible (4), heat exchanger (6), infrared radiation thermometer (7), described Iridium Crucible (4) is placed in the crystal growing furnace furnace chamber of zirconium oxide insulating brick (1) formation, quartz tube (2) and water cooling copper electrode (3) are sequentially provided with the outside of zirconium oxide insulating brick (1), described heat exchanger (6) is placed in Iridium Crucible (4) bottom, described infrared radiation thermometer (7) connection Iridium Crucible (4), Iridium Crucible (4) is built with oxidation Gallium solution (8) and seed crystal (5).Compared with prior art, present invention heat-exchanging method is grown brilliant, improves efficiency, reduces production cost；Meanwhile the crystal mass that grows is excellent, stress is small, dislocation density is low, crystal perfection and optical homogeneity are good, can improve the utilization rate of gallium oxide material, simplifies procedure.
Description
Technical field
The present invention relates to a kind of growing method of gallium oxide single crystal and grower, specifically, be related to a kind of large scale,
High quality, the growing method of gallium oxide single crystal and grower, belong to technical field of crystal growth.
Background technology
Beta-gallium oxide (β-Ga2O3) monocrystalline is a kind of new broad stopband oxide semiconductor material, it can be used as high power member
Part, there is higher breakdown voltage and larger current density, but also can be used for LED chip, various sensor elements and take the photograph
Element etc..Wherein, β-Ga2O3Monocrystalline is the purposes being most expected as GaN backing material, and it combines leading for carborundum
Electrically and sapphire translucency, and (100) crystal face after surfaces nitrided reconstruct with the mismatch of GaN lattices zero.β-Ga2O3Tool
There is following advantage：(1) it is conductive, beneficial to the minimizing of device, integrated, it is adapted to the high-capacity LED for needing large-drive-current；
(2) cut-off absorption side wave length, it is seen that, ultraviolet light wave band transmitance up to more than 80%, be easy to the light extraction for sending LED chip
To outside；(3) (100) crystal face and GaN lattice mismatches are small, and matching completely can be achieved through surfaces nitrided reconstruct；(4) chemical property is steady
It is fixed, resistance to strong acid, highly basic, high mechanical strength.
Therefore, β-Ga2O3Monocrystalline is considered to be a kind of preferable GaN substrate material of alternative sapphire and carborundum.
β-Ga2O3Monocrystalline is a kind of novel transparent conductive substrate material, and market application potential is huge.Because its fusing point is higher
(1850 DEG C), there is cleavage characteristic, easily decompose and volatilize during melt method for growing, thus growing large-size (1 inch and with
On), the β-Ga of high quality2O3Monocrystalline is extremely difficult.β-Ga at present2O3Monocrystalline by float-zone method (FZ), czochralski method (CZ) and
EFG technique growth obtains, and float-zone method prepares β-Ga2O3Monocrystalline, crystalline size is smaller, can not meet the requirement of substrate base, Germany
Leibnitz research institute grown β-Ga with czochralski method generation work(2O3Crystal, but needed during growth using high pressure (7bar), greatly
The big equipment that improves is for high voltage bearing requirement, this control for equipment cost in industrialization from now on, and security
Control is all totally unfavorable.And it is unstable there is growing in crystal growing process, easily there is the problems such as spiral growth.Only
β-the Ga of EFG technique growth2O3Single-chip enters business application, and Chinese patent CN201310559528.8 discloses a kind of big chi
The growing method and grower of very little gallium oxide single crystal, this method include：Installed in single crystal growing furnace for heating and being incubated to be formed
Multiple thermal field components of thermal field, it is horizontal with center installation；The Iridium Crucible with cover for being embedded with iraurite mould is put into thermal field
The heart；By the β-Ga of specific orientation2O3Seed crystal is fixed on seed holder；Oxidation gallium material is put into Iridium Crucible, covers iraurite earthenware
Crucible lid；In gaseous mixture ratio Ar after vacuumizing:CO2=9:1~8:2 to be charged to furnace chamber pressure be 1.05~1.5MPa；Sensing heating
Oxidation gallium material is set to melt completely；Roasting seed crystal is inoculated with after 5~10 minutes；The seeding necking down after seed crystal and the abundant welding of melt, directly
1~2mm is contracted to seed crystal sectional dimension；Expand shoulder growth phase；The isodiametric growth stage；Crystal growth terminates to completely disengage mould
Stop lifting during top, be slowly dropped to room temperature, obtain the transparent completely high quality sheet gallium oxide single crystal without crystal boundary.This is exactly to adopt
Grown with EFG technique, and the inferior position of EFG technique is fairly obvious：EFG technique mould is generally greater than the liquid level in crucible, mould
When top reaches long brilliant temperature, melt temperature will be typically higher than tens degree of fusing point in crucible, and this exacerbates the decomposition of melt and waved
Hair；The long crystalline substance of EFG technique is needed by the long brilliant situation of observation window observation, and observation window is often covered and ineffective by volatile matter,
β-the Ga of EFG technique growth2O3Monocrystalline, the problems such as generally existing bubble, growth striation, cleavatge of crystals, polycrystalline, have a strong impact on crystal
Quality.
The content of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of large scale gallium oxide
The growth apparatus and method of monocrystalline.Crystalline substance is grown with heat-exchanging method, the shape of crystal is determined by the shape of crucible, effectively improves gallium oxide
Crystal preparation efficiency, reduce production cost；Meanwhile the crystal mass that grows is excellent, stress is small, dislocation density is low, crystal is complete
Whole property and optical homogeneity are good, can improve the utilization rate of gallium oxide material, simplify procedure.
The purpose of the present invention can be achieved through the following technical solutions：A kind of growth of large scale gallium oxide single crystal is set
It is standby, it is characterised in that including zirconium oxide insulating brick, quartz tube, water cooling copper electrode, Iridium Crucible, heat exchanger, infrared measurement of temperature
Instrument, described Iridium Crucible are placed in the crystal growing furnace furnace chamber of zirconium oxide insulating brick formation, on the outside of zirconium oxide insulating brick successively
Provided with quartz tube and water cooling copper electrode, described heat exchanger is placed in Iridium Crucible bottom, described infrared radiation thermometer connection iridium
Golden crucible, Iridium Crucible is built with oxidation Gallium solution and seed crystal.
Described Iridium Crucible interior bottom portion is provided with groove, for filling seed crystal；The Iridium Crucible has top drilling
Crucible cover.
Described Iridium Crucible inwall is in shrink mouth shape from top to bottom, and its inner wall section is in inverted trapezoidal.
Described Iridium Crucible inwall and horizontal plane angle a：30 degree<a<90 degree.
The mode of heating of described equipment is sensing heating；Supply frequency is 2.5-20khz.
Described Iridium Crucible side wall is provided with infrared measurement of temperature point, infrared measurement of temperature point connection infrared radiation thermometer, for monitoring
Temperature when crucible material and brilliant length.
Described heat exchanger helium injection gas cools down to crucible bottom seed crystal.
The method that large scale gallium oxide single crystal growth is carried out using equipment, it is characterised in that comprise the following steps：
Step S1：The oxidation gallium material of setting weight is fitted into Iridium Crucible, and loaded onto in Iridium Crucible bottom groove
Seed crystal；
Step S2：By crystal growth stove evacuation, vacuum is less than or equal to 10Pa；
Step S3：Control crystal growing furnace to be warming up to 1855~1860 DEG C by heater, make the gallium oxide melting sources be
Melt, the seed crystal of Iridium Crucible bottom can't melt due to there is the helium gas cooling being continually fed into or only part melted；
Step S4：By reduce heating power or increase helium gas flow make melt seed crystal face crystallize, until iraurite
Melt in crucible all crystallizes, and now crystal has grown up to the shape of crucible, and diameter dimension is identical with crucible internal diameter；
Step S5：Carry out the annealing of crystal, 1000~1200 DEG C of annealing temperature, 72~200h of annealing time；
Step S6：With 10~60 DEG C/h speed slow cooling；
Step S7：After in-furnace temperature is down to room temperature, crystal, processing are taken out.
The present invention is a kind of method and apparatus of growing large-size monocrystalline gallium oxide, selects high temperature resistant and senses heating
The iraurite of efficiency high is as crucible, by carrying out cone angle structure design to crucible shape, it is ensured that the crystal grown can be very easily
Take out without damaging crucible, crucible inner bottom part fluting is used for filling certain crystal orientation seed crystal, is provided with heat exchanger in crucible outer bottom, heat
Exchanger helium injection gas cools down to crucible bottom seed crystal, prevents seed crystal from melting, and take away latent heat, make melt seed crystal face after
Continuous growth, along with the decline of heating power, crystal also from it is small grow to it is big as crucible internal diameter, until melt is whole in crucible
Crystallization, entirely grow brilliant process and terminate.The crystal bar grown meets the requirement of LED industry, and growing method of the present invention is referred to as
Heat-exchanging method, it is the heat that crucible bottom is taken away by the helium being continually fed into, makes gallium oxide melt constantly cold in seed crystal face
But the method crystallized.
Compared with prior art, the present invention has the advantage that：Long brilliant temperature is close to fusing point, without the high overheat temperature of EFG technique
The problem of spending, raw material are entirely sealed in the crucible of lid --- and czochralski method crucible is no lid, and these can maximum journey
The volatilization and decomposition of melt are reduced on degree；The shape of crucible is exactly the shape of crystal, it is not necessary to the link of diameter control, long brilliant mistake
Journey can realize full-automation, save manpower.In addition heat-exchanging method inherently has following advantage.
1) for temperature gradient distribution with gravitational field on the contrary, crucible, crystal and heat exchanger neither move, crystal growth interface is steady
It is fixed, small without mechanical disturbance, Natural convection, eliminate due to mechanical movement and caused by crystal defect；
2) hot-zone is remained at after crystal growth, control helium gas flow can be such that temperature is slowly uniformly reduced by crystallization temperature,
In-situ annealing is realized, the defects of reducing the thermal stress and resulting crystal cleavage and dislocation of crystal；
3) solid liquid interface is in melt parcel, and thermal agitation can be reduced or even exclude before solid liquid interface is reached,
Uniform thermograde can be obtained on interface；
To sum up, gallium oxide crystal pole is grown with heat-exchanging method to be hopeful to obtain large scale, high quality gallium oxide single crystal.
Brief description of the drawings
Fig. 1 is the structural representation of present device；
Fig. 2 is the structural representation of Iridium Crucible.
Embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1
As shown in figure 1, a kind of growth apparatus of large scale gallium oxide single crystal, including zirconium oxide insulating brick 1, quartz tube 2, water
Cold copper electrode 3, Iridium Crucible 4, heat exchanger 6, infrared radiation thermometer 7, described Iridium Crucible 4 are placed in the shape of zirconium oxide insulating brick 1
Into crystal growing furnace furnace chamber in, the outside of zirconium oxide insulating brick 1 is sequentially provided with quartz tube 2 and water cooling copper electrode 3, described heat friendship
Parallel operation 6 is placed in the bottom of Iridium Crucible 4, and described infrared radiation thermometer 7 connects Iridium Crucible 4, and Iridium Crucible 4 is molten built with gallium oxide
Liquid 8 and seed crystal 5.The described side wall of Iridium Crucible 4 is provided with infrared measurement of temperature point, infrared measurement of temperature point connection infrared radiation thermometer 7, is used for
Monitor temperature when crucible material and brilliant length.The described helium injection gas of heat exchanger 6 cools down to crucible bottom seed crystal.
Wherein, the described interior bottom portion of Iridium Crucible 4 is provided with groove (as shown in Figure 2), for filling seed crystal 5；The iraurite
Crucible 4 has the crucible cover of top drilling.The described inwall of Iridium Crucible 4 is in shrink mouth shape from top to bottom, and its inner wall section is in
It is trapezoidal.The described inwall of Iridium Crucible 4 and horizontal plane angle a：80 degree.
The mode of heating of described equipment is sensing heating；Supply frequency is 2.5khz.
The method that large scale gallium oxide single crystal growth is carried out using the said equipment, is comprised the following steps：
Step S1：The oxidation gallium material of setting weight is fitted into Iridium Crucible 4, and filled in the bottom groove of Iridium Crucible 4
Upper seed crystal 5；
Step S2：By crystal growth stove evacuation, vacuum is less than or equal to 10Pa；
Step S3：Control crystal growing furnace to be warming up to 1855~1860 DEG C by heater, make the gallium oxide melting sources be
Melt, the seed crystal 5 of the bottom of Iridium Crucible 4 can't melt due to there is the helium gas cooling being continually fed into or only part melted；
Step S4：By reducing heating power or increase helium gas flow makes melt in the surface crystallization of seed crystal 5, until iraurite
Melt in crucible 4 all crystallizes, and now crystal has grown up to the shape of crucible, and diameter dimension is identical with crucible internal diameter；Such as Fig. 2 institutes
Show, control the in-furnace temperature of crystal growing furnace, growth interface I 51, growth interface II 52, growth can be formed on the surface of seed crystal 5
Interface III 53.
Step S5：Carry out the annealing of crystal, 1000~1200 DEG C of annealing temperature, 72~100h of annealing time；
Step S6：With 10~60 DEG C/h speed slow cooling；
Step S7：After in-furnace temperature is down to room temperature, crystal, processing are taken out.
Two inch oxidized gallium substrates of high quality are obtained using the above apparatus and method.
Embodiment 2
Described Iridium Crucible inwall and horizontal plane angle a：30 degree<a<90 degree.It can be set according to the needs of final products
Meter.
The mode of heating of described equipment is sensing heating；Supply frequency is 20khz.
Wherein, carry out the annealing of crystal, annealing time can be selected according to actual conditions other times such as 50h,
200h etc..
Remaining is the same as embodiment 1.
Claims (8)
1. a kind of growth apparatus of large scale gallium oxide single crystal, it is characterised in that including zirconium oxide insulating brick (1), quartz tube
(2), water cooling copper electrode (3), Iridium Crucible (4), heat exchanger (6), infrared radiation thermometer (7), described Iridium Crucible (4) are placed in
Be sequentially provided with the crystal growing furnace furnace chamber that zirconium oxide insulating brick (1) is formed, on the outside of zirconium oxide insulating brick (1) quartz tube (2) and
Water cooling copper electrode (3), described heat exchanger (6) are placed in Iridium Crucible (4) bottom, described infrared radiation thermometer (7) connection iridium
Golden crucible (4), Iridium Crucible (4) is built with oxidation Gallium solution (8) and seed crystal (5).
A kind of 2. growth apparatus of large scale gallium oxide single crystal according to claim 1, it is characterised in that described iraurite
Crucible (4) interior bottom portion is provided with groove, for filling seed crystal (5)；The Iridium Crucible (4) has the crucible cover of top drilling.
A kind of 3. growth apparatus of large scale gallium oxide single crystal according to claim 1, it is characterised in that described iraurite
Crucible (4) inwall is in shrink mouth shape from top to bottom, and its inner wall section is in inverted trapezoidal.
A kind of 4. growth apparatus of large scale gallium oxide single crystal according to claim 3, it is characterised in that described iraurite
Crucible (4) inwall and horizontal plane angle a：30 degree<a<90 degree.
A kind of 5. growth apparatus of large scale gallium oxide single crystal according to claim 1, it is characterised in that described equipment
Mode of heating be sensing heating；Supply frequency is 2.5-20khz.
A kind of 6. growth apparatus of large scale gallium oxide single crystal according to claim 1, it is characterised in that described iraurite
Crucible (4) side wall is provided with infrared measurement of temperature point, infrared measurement of temperature point connection infrared radiation thermometer (7), for monitoring crucible material and length
Temperature when brilliant.
A kind of 7. growth apparatus of large scale gallium oxide single crystal according to claim 1, it is characterised in that described heat friendship
Parallel operation (6) helium injection gas cools down to crucible bottom seed crystal.
8. a kind of according to the method that any described equipment carries out large scale gallium oxide single crystal growth in claim 1~7, it is special
Sign is, comprises the following steps：
Step S1：The oxidation gallium material of setting weight is fitted into Iridium Crucible (4), and filled in Iridium Crucible (4) bottom groove
Upper seed crystal (5)；
Step S2：By crystal growth stove evacuation, vacuum is less than or equal to 10Pa；
Step S3：Crystal growing furnace is controlled to be warming up to 1855~1860 DEG C by heater, it is melt to make gallium oxide melting sources,
The seed crystal (5) of Iridium Crucible (4) bottom can't melt due to there is the helium gas cooling being continually fed into or only part is melted；
Step S4：By reducing heating power or increase helium gas flow makes melt in seed crystal (5) surface crystallization, until iraurite earthenware
Melt in crucible (4) all crystallizes, and now crystal has grown up to the shape of crucible, and diameter dimension is identical with crucible internal diameter；
Step S5：Carry out the annealing of crystal, 1000~1200 DEG C of annealing temperature, 72~200h of annealing time；
Step S6：With 10~60 DEG C/h speed slow cooling；
Step S7：After in-furnace temperature is down to room temperature, crystal, processing are taken out.
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| CN114561701B (en) * | 2021-06-07 | 2022-08-19 | 浙江大学杭州国际科创中心 | Method for growing gallium oxide single crystal by casting method and semiconductor device containing gallium oxide single crystal |
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