CN105887198B - Air bubble apparatus and sweep-out method in a kind of removing sapphire crystal melt material - Google Patents
Air bubble apparatus and sweep-out method in a kind of removing sapphire crystal melt material Download PDFInfo
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- CN105887198B CN105887198B CN201610425152.5A CN201610425152A CN105887198B CN 105887198 B CN105887198 B CN 105887198B CN 201610425152 A CN201610425152 A CN 201610425152A CN 105887198 B CN105887198 B CN 105887198B
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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
- C30B29/20—Aluminium 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
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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
- C30B15/34—Edge-defined film-fed crystal-growth using dies or slits
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- Crystallography & Structural Chemistry (AREA)
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- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The present invention relates to air bubble apparatus and the methods removed with the device in a kind of removing sapphire crystal melt material, and described device includes a crucible, mold, crucible cover, bubble trap and high frequency pumping device；It further include a support component, the support component is set to crucible bottom end, and the device for removing bubble in sapphire crystal melt material is fixed in crystal growing furnace by the support component, and the bubble on bubble trap is quickly and effectively forced to be detached from the bubble formation resonance effects on bubble trap using high-frequency vibration.The present invention has the advantages that air bubble apparatus in removing sapphire crystal melt material of the invention quickly and effectively forces the bubble on bubble trap to be detached from using high-frequency vibration to the bubble formation resonance effects on bubble trap, and float to above melt liquid level；Bubble in raw material can be effectively removed, the gas content of melt in crucible is reduced, utmostly ensures that raw material cleans in crucible, and then improve crystal final product quality.
Description
Technical field
The invention belongs to technical field of crystal growth, it is related to air bubble apparatus in a kind of removing sapphire crystal melt material, it is special
Be not related to it is a kind of using high-frequency vibration remove sapphire crystal melt material in air bubble apparatus, further relate to the remove device remove indigo plant
The method of bubble in gem crystal melt material.
Background technique
Sapphire group becomes aluminium oxide (Al2O3), it is by three oxygen atoms and two aluminium atoms with the combination of covalent bond pattern
It forms, crystal structure is hexagonal lattice structure.Since sapphire has the high velocity of sound, high temperature resistant, anticorrosive, high rigidity, height thoroughly
The features such as photosensitiveness, fusing point high (2045 DEG C), therefore often it is used as the material of photoelectric cell.At present super brightness it is white/blue light
The quality of LED depends on the material quality of epitaxial layer of gallium nitride (GaN), and epitaxial layer of gallium nitride quality is then precious with used indigo plant
Stone lining bottom surface processing quality is closely bound up.Due to sapphire (monocrystalline Al2O3) face c and III-V and II-VI race's deposition film it
Between lattice constant mismatch rate it is small, while meeting requirement resistant to high temperature in GaN epitaxy processing procedure, so that sapphire wafer becomes production
The critical material of white/blue green light LED.
There are many kinds of methods at present for the growing method of sapphire crystal material, mainly have: kyropoulos (i.e. Kyropolos
Method, abbreviation Ky method), EFG technique (i.e. edge defined film-fed growth techniques method, abbreviation EFG method, belong to
In one kind of TPS method), heat-exchanging method (i.e. heat exchange method method, abbreviation HEM method), Bridgman method (i.e.
Bridgman method or Bridgman-Stockbarger method), czochralski method (i.e. Czochralski, abbreviation Cz method) etc..But different crystal growth side
Method is designed for sapphire different purposes.Currently, being used for the above-mentioned sapphire of sapphire growing method of LED field
There are two types of the growing method of crystal is common:
1, the long crystallization of kelvin (Kyropoulos method), abbreviation KY method, also known as kyropoulos.Its principle and Chai Shi crystal pulling
Method (Czochralski method) is similar, and fusing forms melt after first heating the raw material to fusing point, then with the seed crystal of monocrystalline
(SeedCrystal) bath surface is touched, starts growth and seed crystal phase allomeric knot in solid liquid interface of the seed crystal with melt
The monocrystalline of structure, seed crystal are up drawn high with extremely slow speed, but up crystal pulling is for a period of time to form brilliant neck in seed crystal, to melt
After stablizing with the solidification rate at seed crystal interface, seed crystal is just no longer drawn high, and also rotating, is only come in a manner of cooling rate by controlling
Solidify monocrystalline gradually down from top, it is final solidified at an entire monocrystalline crystalline substance heavy stone used as an anchor.Then, using stick processing is drawn, along vertical axis
To the crystal bar for drawing standard LED processed.Its effective rate of utilization generally 30% or so, limits the cost of LED substrate piece.
2, EFG technique (also referred to as Edge-Defined Film feed method, EFG method), is mainly used for growing thin material.It is utilized
Melt is imported the top of mold by capillary principle, is then lifted this part melt with seed crystal and is generated single-chip.Then using drawing
Piece processing, draws the workprint for producing LED one by one.With the increase of the market demand, the sapphire product grown using EFG technique
Size is continuously increased, specifically a kind of big if Chinese patent CN201010147683.5 is related to the manufacturing technology of sapphire crystal
The growing method of size flakes sapphire crystal；And more sapphire products are disposably grown using guided mode general laws, such as China
Patent CN201310371528.5 is related to a kind of more forming sapphire crystallization devices.
On the one hand, traditional EFG method or Ky method, select material density to be less than crystalline density, and reason is that raw material includes
There is stomata, is to wait by prolonged it is expected in heat for putting into the bubble of the molten package of impurity, raw material of raw material in crucible
Run its course during balance, the energy not only wasted increases cost and effect is undesirable, and crystals are often coated with
The optical defects such as bubble and impurity.
On the other hand, no matter EFG large-size sapphire growth or EFG multi-disc sapphire growth, disposable inventory it is bright
It is aobvious to limit crystalline size or amount of crystals, it is necessary to it takes and constantly puts into new raw material in technical process, and newly put into
Bubble and impurity are introduced when melting sources again.
Therefore, bubble in raw material can effectively be removed by researching and developing one kind, utmostly ensure that raw material cleans in crucible, and improve
Bubble in the removing sapphire crystal melt material of crystal final product quality
Device and sweep-out method are necessary.
Summary of the invention
The technical problem to be solved in the present invention is to provide one kind can effectively remove bubble in raw material,
Utmostly ensure that raw material cleans in crucible, and in the removing sapphire crystal melt material of raising crystal final product quality
Air bubble apparatus also provides a kind of method for removing bubble in sapphire crystal melt material using the remove device.
In order to solve the above technical problems, the technical solution of the present invention is as follows: a kind of bubble in removing sapphire crystal melt material
Device, innovative point are: described device includes a crucible, mold, crucible cover, bubble trap and high frequency pumping device；
The crucible cover is set to the top of crucible, and the gap of 1mm-200mm is kept with crucible；The rotation of the crucible cover
The rotational symmetry overlapping of axles of symmetry axis and crucible, and also there is a charging through-hole on the crucible cover of the side；The mold is set
It sets at the center of crucible cover, and its lower end is located in crucible, a capillary channel is additionally provided on the symmetry axis of the mold；Institute
The lowermost end that crucible interior is arranged in bubble trap is stated, the high frequency pumping device is arranged in crucible bottom center, and high frequency
Exciting bank passes through crucible and connect with bubble trap；
Described device further includes a support component, and the support component is set to crucible bottom end, and will by the support component
The device for removing bubble in sapphire crystal melt material is fixed in crystal growing furnace.
Further, the bubble trap is made of the reticular structure that several layers refractory metal silk weaves, and several
From top to bottom, mesh is sequentially reduced layer reticular structure；The dendritic support of refractory metal silk is additionally provided between each lamina reticularis
Reticular structure.
Further, the minimum dimension of the mesh is 0.5mm-5mm, and the dendritic angle is 30 ° -120 °.
Further, the refractory metal is molybdenum, tungsten, tungsten-molybdenum alloy or tungsten-rhenium alloy.
A kind of sweep-out method with air bubble apparatus in above-mentioned removing sapphire crystal melt material, innovative point are: described
Sweep-out method includes the following steps:
(1) when the melt off-capacity stored in molybdenum crucible is with continued growth sapphire crystal, make mold together with crucible
Lid is separated with the melt in crucible together, and reduces heter temperature value to 2000 DEG C or less；(2) the high pure oxygen that will be cleaned up
Change aluminum feedstock, is put into crucible by the charging through-hole on crucible cover；(3) control crystal growing furnace is warming up to 2000-2100
DEG C, aluminum feedstock to be oxidized is fused into melt in bubble trap；(4) starting high frequency pumping is passed to high frequency into bubble trap
The microbubble discharged in melting process of raw material is removed in vibration, and lasting charging is so that obtain sufficient melt in crucible；(5) make mold
Melt material is contacted, and implements long brilliant operation, repeats S1 to S4 until crystal product meets the requirements.
Further, the step (4) includes at least 3 adjustment parameters, i.e. power, frequency and waveform；The power is logical
Often in 1W/cm2-1KW/ cm2, for the frequency usually in 1KHz-10MHz, the waveform is usually sine wave or square wave.
The present invention has the advantages that
(1) method for removing bubble in sapphire crystal melt material of the invention, using high-frequency vibration to bubble trap
On bubble formation resonance effects, quickly and effectively force the bubble on bubble trap to be detached from, and float on melt liquid level
Side；Meanwhile frequency vibration reduces the waiting time for eliminating bubble, saves material power, can effectively remove bubble in raw material, reduces
The gas content of melt in crucible utmostly ensures that raw material cleans in crucible, and then improves crystal final product quality；And the present invention
Alumina raw material is used in method, allows its density lower, and cellular alumina raw material is made to guarantee not increasing bubble in crystal
Under the premise of reached requirement, reduce feedstock processing cost；
(2) bubble trap removed in sapphire crystal melt material in air bubble apparatus of the invention, is by several layers
The reticular structure of refractory metal silk braiding is constituted, and can effectively increase the contact area of alumina raw material and heat source, is improved
Melting efficiency prevents raw material collision metal device or causes smelt splashes, and quickly collects the gas in melt, reduces bubble
Nucleation energy barrier surface potential barrier reduces the risk that gas forms bubble in crystals.
Detailed description of the invention
The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.
Fig. 1 is the structural schematic diagram that the present invention removes air bubble apparatus in sapphire crystal melt material.
Fig. 2 is that the three-layer network shape structure of bubble trap in air bubble apparatus in present invention removing sapphire crystal melt material is bowed
Depending on schematic diagram.
Fig. 3 is that the three-layer network shape structure of bubble trap in air bubble apparatus in present invention removing sapphire crystal melt material is bowed
Enlarged diagram is supported depending on schematic diagram and weaving dendroid tungsten-rhenium wire.
Specific embodiment
The following examples can make professional and technical personnel that the present invention be more fully understood, but therefore not send out this
It is bright to be limited among the embodiment described range.
Embodiment
The present embodiment removes air bubble apparatus in sapphire crystal melt material, as shown in Figure 1, the device includes a cylindrical molybdenum
Crucible 3 is equipped with a disk in the top of cylindrical molybdenum crucible 3 and fills molybdenum crucible lid 2, and keeps the gap of 1mm-200mm with crucible；
And the rotational symmetry overlapping of axles of disk dress 2 rotation axes of symmetry of molybdenum crucible lid and cylindrical molybdenum crucible 3, molybdenum crucible lid 2 is filled in disk
Left side be additionally provided with a charging through-hole；And a molybdenum mold 1,1 lower end of molybdenum mold are equipped at the center of disk dress molybdenum crucible lid 2
In cylindrical molybdenum crucible 3, a capillary channel is additionally provided on the symmetry axis of molybdenum mold 1.
Lowermost end in cylindrical 3 inner cavity of molybdenum crucible is additionally provided with bubble trap 7, as shown in Fig. 2, bubble trap 7 is
Three-layer network shape structure, is formed by tungsten-rhenium alloy weaving filaments, and three-layer network shape structure is from top to bottom, and mesh is sequentially reduced, most bottom
Layer mesh is 2mm, as shown in figure 3, there is dendroid tungsten-rhenium wire weaving structural support between stratum reticulare, tungsten-rhenium wire weaves alternate angle
Degree is 30 °, while the gap that support construction ensures to have 2cm or more between stratum reticulare.
After sapphire ball material is fallen on bubble trap 7, since alumina balls material has certain whereabouts kinetic energy, and bubble
The multilayered structure of the tungsten-rhenium wire support of collector 7 cooperates porous structure simultaneously, and eyelet is sequentially reduced from top to bottom, one side energy
It is enough effectively to ensure that ball material is smoothly fallen into bubble trap 7, ball material on the other hand can be effectively prevent to collect directly through bubble
Device 7 prevents ball material from falling directly into crucible, and it is bubble trap 7 that ball material, which falls on bubble trap 7 and effectively converts ball material kinetic energy,
Elastic potential energy prevents ball material whereabouts collision crucible or causes smelt splashes.
As shown in Figure 1, a high frequency pumping device is additionally provided in cylindrical 3 bottom center of molybdenum crucible, 6, and the high frequency pumping
Device 6 passes through cylindrical molybdenum crucible 3 and connect with bubble trap 7；Air bubble apparatus also wraps in the removing sapphire crystal melt material
A support component 5 is included, which is set to 3 bottom end of cylindrical molybdenum crucible, and will remove sapphire by the support component 5
The device of bubble is fixed in crystal growing furnace in crystal melt material.
Air bubble apparatus in the removing sapphire crystal melt material of the present embodiment, using high-frequency vibration on bubble trap
Bubble formation resonance effects quickly and effectively forces the bubble on bubble trap to be detached from, and floats to above melt liquid level；It can
Bubble in raw material is effectively removed, the gas content of melt in crucible is reduced, utmostly ensures that raw material cleans in crucible, Jin Erti
High crystal final product quality.
After ball material melted by heat, gas contained by ball material stomata is dissolved in alumina melt, is flowed through bubble in melt and is collected
When device 7, since its special dendroid tungsten-rhenium wire is staggeredly placed structure, according to formula [1] and [2]:
ΔG = [4πR2σ – 4/3πR3(Po + 2σ/R + Pv)] * Γ(θ, α) [1]
Γ(θ, α) = [1-sin(θ + α/2)]/4sin(α/2) * {2sin(α/2) – cos[1 + sin(θ +
α/2)]} [2]
Wherein, Δ G is this free energy of the jeep of bubble, and R is the size of bubble, and σ is the surface tension of alumina melt, Po
It is pressure, the P of bubble present positionvIt is the saturated vapor pressure of alumina melt, Euler integral of the second kind is shape function, and θ is that aluminium oxide is molten
The infiltration angle of body and tungsten-rhenium wire, α are the angles that 7 dendroid tungsten-rhenium wire of bubble trap is staggeredly placed.The value of infiltration angle θ exists
10 ° to 50 °, when α is 30 ° to 120 °, acquiring shape function Γ has minimum, and branch alternate angle α is optimal corner.
If melt, without bubble trap 7, shape function Γ takes 1, and oversaturated gaseous solute can not be precipitated, but
In crystal growing process, when rising to by die end the top of mold with melt, in the capillary channel or mold of mold
Surface bubble, and crystals are entered with crystallization process, become the mass defect in crystal.
If melt flows through bubble trap 7, and adjusts its dendroid tungsten-rhenium wire angle of cut α to optimal corner, shape letter can be made
Close to 0, then the bubble Gibbs free energy aoxidized in aluminum melt significantly reduces number Γ, fast in collector dendroid staggered place
Rapid-result core, after nucleation around bubble solute concentration reduction force nearby gaseous solute flowed to nucleation area, realize fast and effective gas
Bubble is collected.
For bubble adhesion after collection after the nucleation of tungsten-rhenium wire staggered place, gas and minute bubbles are constantly close to nucleation area, at
Bubble size is slowly increased at core, buoyancy be often not enough to leave tungsten-rhenium wire staggered place in the quite long waiting time and on
Melt liquid level is floated to until being discharged into ambiance.It is the original of subsequent addition to make the bubble after collecting leave tungsten-rhenium wire
Material provides the nucleation core of supersaturated gas, and the resonance caused by high frequency pumping is needed to be detached from bubble.
The vibration of not any frequency all can excite bubble resonance by bubble absorption.Resonant frequency is by addition to being added
The factors such as the density and internal porosity size of raw material influence, and additionally depend on the size of bubble.Free energy Δ G determines into nuclei air bubble
Size, while high frequency pumping starting opportunity difference, all affect the size of bubble.It is determined by parameters such as bubble size R
Resonant frequency ωr, see formula [3]:
ωr = 1/R [3γ/ρ (2σ/R + Po) - 2σ/ρR]0.5 [3]
Wherein, R is the size of bubble, and σ is the surface tension of alumina melt, PoIt is the pressure of bubble present position, ωr
It is resonant frequency, ρ is sapphire fusant density, and γ is the ratio that isobaric and constant volume specific heat is held.The size of R usually at more than ten microns extremely
Between several hundred microns, then estimated by sapphire parameters, resonant frequency is usually in 100KHz to 1MHz.
At this time using higher-order of oscillation excitation nucleation area's bubble of certain frequency, bubble boundary absorbs excitation energy, interface energy
Increase so that adsorption capacity is not enough to keep bubble to rest on original tungsten-rhenium wire reports to the leadship after accomplishing a task place, final bubble is to floating to liquid level.Gas
It is expanded in bubble floating-upward process because ambient pressure constantly reduces, until to release all kinds of gases contained by ball material miscellaneous for melt liquid level rupture
Matter, and gas contained by melt in crucible, decline to a great extent if CO, Ar equal size.
The high frequency wave excitation acoustic pressure of the present embodiment takes 3 subharmonic to optimize formula [4]:
PA = Psin(ωt) + P1sin(ωt + φ1) +P2sin(ωt + φ2) [4]
Wherein, PAIt is high frequency pumping acoustic pressure, it is harmonic pressure, φ respectively that ω, which is equal to higher frequency multiplied by 2 π, P, P1 and P2,1
And φ2It is the phase difference of harmonic wave.
Although having formula [3] and formula [4], technological parameter seems that comparison is clear, as long as being applied with resonant frequency to bubble
Larger sound pressure forces bubble quickly to absorb energy expansion collapse.But in actual conditions, sapphire items constant coefficient is such as viscous
Stagnant coefficient, vapour pressure and surface tension are related with practicable process temperature, so operating process is many and diverse.
The present embodiment is by 1 group of Optimal Parameters group and 3 contrast groups, and to show difference, design parameter is as follows:
| Parameter name | High frequency power | Motivate acoustic pressure (PA) | Frequency (π of ω/2) | Phase difference (φ1,φ2) |
| Contrast groups 1 | 0 | ? | ? | ? |
| Contrast groups 2 | 5w/cm2 | 0.12MPa | 0.05MHz | ? |
| Contrast groups 3 | 5w/cm2 | 0.25MPa | 0.02MHz | ? |
| Optimization group | 5w/cm2 | 0.25MPa | 0.02MHz | π/4, π/6 |
Wherein, contrast groups 1 does not start high frequency pumping；Contrast groups 2 motivate acoustic pressure pressure close at bubble, and frequency selection is altogether
Vibration frequency is slightly larger than frequency (0.04MHz)；Contrast groups 3, motivate acoustic pressure 2 times of pressure close at bubble, and frequency is close to resonant frequency
0.5 times；Optimization group motivates acoustic pressure 2 times of pressure close at bubble, and frequency selects its phase of 3 subharmonic close to 0.5 times of resonant frequency
Potential difference is π/4 and π/6 respectively.
The method that the present embodiment removes bubble in sapphire melt, according to above-mentioned experimental design thinking, specific steps are such as
Under:
Step S1: when 4 off-capacity of melt stored in molybdenum crucible 3 is with continued growth sapphire crystal, make molybdenum mold 1
Separate that (melt solidification shrinkage draws mold if touching mold, makes molybdenum die deformation with molybdenum crucible 3 together with molybdenum crucible lid 2
Even tilt), and heter temperature value is reduced to 2000 DEG C or less；
Step S2: the high purity aluminium oxide ball material that will be cleaned up is put into crucible；
Step S3: control crystal growing furnace is warming up to 2000-2100 DEG C, and aluminium ball material to be oxidized melts in bubble trap 7
Change；
The step S4 and S5 of contrast groups 1 are as follows:
Step S4: according to embodiment mentality of designing contrast groups 1, not starting high frequency pumping 6, and lasting charging in crucible so that obtain
Sufficient melt material is obtained, waits reach thermal balance within 2 hours；
Step S5: making mold contact melt 4 again, and implements long brilliant operation.
The step S4 and S5 of contrast groups 2 are as follows:
Step S4: according to embodiment mentality of designing contrast groups 2, start high frequency pumping 6, power 5w/cm2, pressure
0.12MPa, frequency 0.05MHz, no harmonic wave, lasting charging is so that obtain sufficient melt material in crucible；
Step S5: making mold contact melt material, and implements long brilliant operation.
The step S4 and S5 of contrast groups 3 are as follows:
Step S4: according to embodiment mentality of designing contrast groups 3, start high frequency pumping 6, power 5w/cm2, pressure
0.25MPa, frequency 0.02MHz, no harmonic wave, lasting charging is so that obtain sufficient melt material in crucible；
Step S5: making mold contact melt material, and implements long brilliant operation.
The step S4 and S5 of optimization group are as follows:
Step S4: according to embodiment mentality of designing optimization group, start high frequency pumping 6, power 5w/cm2, pressure 0.25MPa,
Frequency 0.02MHz, harmonic phase difference are not π/4 and π/6, and lasting charging is so that obtain sufficient melt material in crucible；
Step S5: making mold contact melt material, and implements long brilliant operation, until long crystalline substance terminates.
In colourless transparent crystal obtained by the present embodiment, crystal obtained by contrast groups 1-3 is respectively present different degrees of bubble,
Middle 2 bubble of contrast groups is at most maximum, and contrast groups 1 are better than contrast groups 2 close to contrast groups 3, and crystal quality obtained by optimization group is best,
There is no the macroscopic bubbles for being greater than 50 microns.
Basic principles and main features and advantages of the present invention of the invention have been shown and described above.The skill of the industry
Art personnel it should be appreciated that the present invention is not limited to the above embodiments, the above embodiments and description only describe
The principle of the present invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these
Changes and improvements all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and
Its equivalent thereof.
Claims (5)
1. air bubble apparatus in a kind of removing sapphire crystal melt material, it is characterised in that: described device include a crucible, mold,
Crucible cover, bubble trap and high frequency pumping device；The crucible cover is set to the top of crucible, and keeps 1mm- with crucible
The gap of 200mm；The rotation axes of symmetry of the crucible cover and the rotational symmetry overlapping of axles of crucible, and on the crucible cover of the side
Also there is a charging through-hole；The mold is arranged at the center of crucible cover, and its lower end is located in crucible, pair of the mold
Claim to be additionally provided with a capillary channel on axis；The lowermost end of crucible interior, the high frequency pumping dress is arranged in the bubble trap
It installs in crucible bottom center, and high frequency pumping device passes through crucible and connect with bubble trap；Described device further includes one
Support component, the support component is set to crucible bottom end, and will remove gas in sapphire crystal melt material by the support component
The device of bubble is fixed in crystal growing furnace；The reticular structure structure that the bubble trap is woven by several layers refractory metal silk
At, and several layers reticular structure is from top to bottom, mesh is sequentially reduced；Refractory metal silk is additionally provided between each lamina reticularis
Dendritic support net structure.
2. air bubble apparatus in removing sapphire crystal melt material according to claim 1, it is characterised in that: the mesh
Minimum dimension is 0.5mm-5mm, and the dendritic angle is 30 ° -120 °.
3. air bubble apparatus in removing sapphire crystal melt material according to claim 1, it is characterised in that: the resistance to height
Warm metal is molybdenum, tungsten, tungsten-molybdenum alloy or tungsten-rhenium alloy.
4. the sweep-out method of air bubble apparatus in a kind of removing sapphire crystal melt material described in claim 1, it is characterised in that:
The sweep-out method includes the following steps:
(1) when the melt off-capacity stored in molybdenum crucible is with continued growth sapphire crystal, make mold together with crucible cover one
It rises and is separated with the melt in crucible, and reduce heter temperature value to 2000 DEG C or less；
(2) the high purity aluminium oxide raw material that will be cleaned up is put into crucible by the charging through-hole on crucible cover；
(3) control crystal growing furnace is warming up to 2000-2100 DEG C, and aluminum feedstock to be oxidized is fused into melt in bubble trap；
(4) starting high frequency pumping is passed to high-frequency vibration into bubble trap, removes the microbubble discharged in melting process of raw material,
Lasting charging is so that obtain sufficient melt in crucible；
(5) so that mold is contacted melt material, and implement long brilliant operation, repeat (1) to (4) until crystal product conforms to
It asks.
5. the sweep-out method according to claim 4 for removing air bubble apparatus in sapphire crystal melt material, feature exist
In: the step (4) includes at least the adjusting of power, frequency and waveform parameter；The power is usually in 1W/cm2-1KW/
cm2, for the frequency usually in 1KHz-10MHz, the waveform is usually sine wave or square wave.
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| CN201610425152.5A CN105887198B (en) | 2016-06-16 | 2016-06-16 | Air bubble apparatus and sweep-out method in a kind of removing sapphire crystal melt material |
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| CN105887198B true CN105887198B (en) | 2019-01-11 |
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| AT16098U1 (en) * | 2017-05-03 | 2019-01-15 | Plansee Se | Glass melting component |
| CN108754611A (en) * | 2018-06-13 | 2018-11-06 | 江苏星特亮科技有限公司 | Crystalline material melting method and melting unit |
| CN115074828A (en) * | 2022-06-30 | 2022-09-20 | 徐州鑫晶半导体科技有限公司 | Crucible assembly, silicon crystal preparation device and preparation method of silicon crystal |
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