CN105887198A - Device and method for clearing away bubbles in sapphire crystal melt material - Google Patents
Device and method for clearing away bubbles in sapphire crystal melt material Download PDFInfo
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- CN105887198A CN105887198A CN201610425152.5A CN201610425152A CN105887198A CN 105887198 A CN105887198 A CN 105887198A CN 201610425152 A CN201610425152 A CN 201610425152A CN 105887198 A CN105887198 A CN 105887198A
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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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Abstract
The invention relates to a device for clearing away bubbles in a sapphire crystal melt material and a method for clearing away the bubbles in the sapphire crystal melt material through the device. The device comprises a crucible, a die, a crucible cover, a bubble collector and a high frequency excitation device; the device further comprises a supporting assembly, the supporting assembly is arranged at the bottom end of the crucible, the device for clearing away the bubbles in the sapphire crystal melt material is fixed into a crystal growing furnace through the supporting assembly, a resonance effect is generated on the bubbles on the bubble collector through high frequency vibration, and the bubbles on the bubble collector are forced to break away rapidly and effectively. The device for clearing away the bubbles in the sapphire crystal melt material has the advantages that the resonance effect is generated on the bubbles on the bubble collector through high frequency vibration, and the bubbles on the bubble collector are forced to break away rapidly and effectively and float upward above the liquid level of melt; the bubbles in the raw material can be effectively cleared away, the content of gas in the melt in the crucible is lowered, cleanliness of the raw material in the crucible is guaranteed to the maximum extent, and furthermore quality of finished crystals is improved.
Description
Technical field
The invention belongs to technical field of crystal growth, relate to air bubble apparatus in a kind of removing sapphire crystal melt material, utilize dither to remove air bubble apparatus in sapphire crystal melt material particularly to one, further relate to remove the method for bubble in sapphire crystal melt material with this removing device.
Background technology
Sapphire consist of aluminium oxide (Al2O3), it is to be combined into covalent bond pattern by three oxygen atoms and two aluminum atoms, its crystal structure is hexagonal lattice structure.Owing to sapphire has the feature such as the high velocity of sound, high temperature resistant, anticorrosive, high rigidity, high light transmittance, fusing point high (2045 DEG C), the most often it is used as the material of photoelectric cell.At present super brightness white/quality of blue-ray LED depends on the material quality of epitaxial layer of gallium nitride (GaN), epitaxial layer of gallium nitride quality is then closely bound up with the sapphire substrate surface processing quality used.Due to sapphire (monocrystalline Al2O3) lattice constant mismatch rate between c face and III-V and II-VI race deposition thin film is little, meets resistant to elevated temperatures requirement in GaN epitaxy processing procedure so that sapphire wafer becomes the critical material making white/blue green light LED simultaneously.
The growing method of sapphire crystal material existing a variety of methods at present, mainly have: kyropoulos (i.e. Kyropolos method, be called for short Ky method), EFG technique (i.e. edge defined film-fed growth techniques method, it is called for short EFG method, belong to the one of TPS method), heat-exchanging method (i.e. heat exchange method method, be called for short HEM method), Bridgman method (i.e. Bridgman method, or Bridgman-Stockbarger method), czochralski method (i.e. Czochralski, be called for short Cz method) etc..But different growing methods designs for sapphire different purposes.What the growing method of the above-mentioned sapphire crystal of sapphire growing method being presently used for LED field was commonly used has two kinds:
1, the long crystallization of kelvin (Kyropoulos method), is called for short KY method, also known as kyropoulos.Its principle is similar with Chai Shi crystal pulling method (Czochralski method), after raw material is first heated to fusing point, fusing forms melt, bath surface is touched again with the seed crystal (SeedCrystal) of monocrystalline, the seed crystal solid liquid interface with melt starts growth and the monocrystalline of seed crystal same crystal structure, seed crystal up draws high with pole speed slowly, but in seed crystal up crystal pulling a period of time to form brilliant neck, after melt is stable with the freezing rate at seed crystal interface, seed crystal the most no longer draws high, the most do not rotate, only monocrystalline is made the most down to solidify from top in control cooldown rate mode, final set becomes a whole monocrystalline crystalline substance heavy stone used as an anchor.Then, utilize and draw rod processing, draw the crystal bar of standard LED processed along vertical axial.Its effective rate of utilization, typically about 30%, limits the cost of LED substrate sheet.
2, EFG technique (also referred to as Edge-Defined Film feed method, EFG method), is mainly used in growing thin material.It make use of capillary principle, melt imports the top of mould, then with seed crystal, the lifting of this part melt is generated single-chip.Then utilize and draw sheet processing, draw the workprint making LED one by one.Along with the increase of the market demand, the sapphire product size utilizing EFG technique to grow is continuously increased, as Chinese patent CN201010147683.5 relates to the manufacturing technology of sapphire crystal, the growing method of a kind of large-size flaky sapphire crystals；And utilize guided mode general laws disposably to grow branched sapphire product, as Chinese patent CN201310371528.5 relates to a kind of branched shaping sapphire crystallization device.
On the one hand, traditional EFG method or Ky method, select material density less than crystalline density, its reason is that raw material is contained within pore, for putting into the impurity of raw material in crucible, raw material melt the bubble of parcel be dependent on waiting for a long time being expected to thermally equilibrated during run its course, the energy not only wasted adds cost and effect is undesirable, and crystals is often coated with the optical defect such as bubble and impurity.
On the other hand, no matter EFG large-size sapphire grows or EFG multi-disc sapphire growth, disposable inventory significantly limit crystalline size or amount of crystals, it is necessary to takes constantly to put into new raw material in technical process, and newly put into melting sources time introduce bubble and impurity.
Therefore, research and development one can effectively remove bubble in raw material, at utmost guarantees raw material cleaning in crucible, and improves bubble in the removing sapphire crystal melt material of crystal end 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 can effectively remove bubble in raw material,
At utmost guarantee raw material cleaning in crucible, and improve air bubble apparatus in the removing sapphire crystal melt material of crystal end product quality, also provide for a kind of utilizing this removing device to remove the method for bubble in sapphire crystal melt material.
For solving above-mentioned technical problem, the technical scheme is that air bubble apparatus in a kind of removing sapphire crystal melt material, its innovative point is: described device includes a crucible, mould, crucible cover, bubble trap and high frequency pumping device；
Described crucible cover is located at the top of crucible, and keeps the gap of 1mm-200mm with crucible；The rotation axes of symmetry of described crucible cover overlaps with the rotation axes of symmetry of crucible, and also has one on the crucible cover of described side and add material through hole；Described mould is arranged on the center of crucible cover, and its lower end is positioned at crucible, and the axis of symmetry of described mould is additionally provided with a capillary channel；Described bubble trap is arranged on the lowermost end of crucible interior, and described high frequency pumping device is arranged on crucible bottom center, and high frequency pumping device is connected through crucible with bubble trap；
Described device also includes that a support component, described support component are located at crucible bottom, and is fixed on removing the device of bubble in sapphire crystal melt material in crystal growing furnace by this support component.
Further, if the network structure that described bubble trap is woven by dried layer refractory metal silk is constituted, and if dried layer network structure from top to bottom, mesh is sequentially reduced；Refractory metal silk dendritic support net structure it is additionally provided with between described each lamina reticularis.
Further, the minimum dimension of described mesh is 0.5mm-5mm, and described dendritic angle is 30 °-120 °.
Further, described refractory metal is molybdenum, tungsten, tungsten-molybdenum alloy or tungsten-rhenium alloy.
A kind of by the sweep-out method of air bubble apparatus in above-mentioned removing sapphire crystal melt material, its innovative point is: described sweep-out method comprises the steps:
(1) when the melt off-capacity of storage is with continued growth sapphire crystal in molybdenum crucible, make mould separate with the liquation in crucible together with crucible cover, and reduce heter temperature value to less than 2000 DEG C；(2) the high purity aluminium oxide raw material that will clean up, by adding during material through hole puts in crucible on crucible cover；(3) controlling crystal growing furnace and be warming up to 2000-2100 DEG C, aluminum feedstock to be oxidized is fused into melt in bubble trap；(4) starting high frequency pumping incoming dither in bubble trap, remove the microbubble of release in melting process of raw material, persistently charging is so that obtaining sufficient melt in crucible；(5) make contacting dies melt material, and implement long crystalline substance operation, repeat S1 to S4 until crystal product meets the requirements.
Further, described step (4) is including at least 3 regulations parameters, i.e. power, frequency and waveform；Described power is generally at 1W/cm2-1KW/ cm2, described frequency is generally at 1KHz-10MHz, and described waveform is usually sinusoidal wave or square wave.
It is an advantage of the current invention that:
(1) method of bubble in the removing sapphire crystal melt material of the present invention, utilizes dither to the bubble formation resonance effect on bubble trap, forces the bubble disengagement on bubble trap fast and effectively, and float to above melt liquid level；Meanwhile, frequency vibration reduces the waiting time eliminating bubble, saves material power, can effectively remove bubble in raw material, and the gas content of melt in reduction crucible at utmost guarantees raw material cleaning in crucible, and then improves crystal end product quality；And the inventive method uses alumina raw material, it is allowed to its density is relatively low, makes cellular alumina raw material not increase in guarantee and has reached use requirement in crystal on the premise of bubble, reduces Feedstock treating cost；
(2) bubble trap removed in sapphire crystal melt material in air bubble apparatus of the present invention, if it is to be made up of the network structure of dried layer refractory metal silk braiding, can effectively increase the contact area of alumina raw material and thermal source, improve melting efficiency, prevent raw material collision metal device or cause smelt splashes, and quickly collect the gas in melt, reduce the nucleation energy barrier surface potential barrier of bubble, reduce gas and form the risk of bubble at crystals.
Accompanying drawing explanation
The present invention is further detailed explanation with detailed description of the invention below in conjunction with the accompanying drawings.
Fig. 1 is that the present invention removes the structural representation of air bubble apparatus in sapphire crystal melt material.
Fig. 2 is the three-layer network shape structure schematic top plan view that the present invention removes bubble trap in air bubble apparatus in sapphire crystal melt material.
Fig. 3 is three-layer network shape structure schematic top plan view and the weaving dendroid tungsten-rhenium wire support enlarged diagram that the present invention removes bubble trap in air bubble apparatus in sapphire crystal melt material.
Detailed description of the invention
The following examples can make professional and technical personnel that the present invention is more fully understood, but the most therefore limits the present invention among described scope of embodiments.
Embodiment
The present embodiment removes air bubble apparatus in sapphire crystal melt material, as it is shown in figure 1, this device includes a cylindrical molybdenum crucible 3, the disk that is arranged at cylindrical molybdenum crucible 3 fills molybdenum crucible lid 2, and keeps the gap of 1mm-200mm with crucible；And disk dress molybdenum crucible lid 2 rotation axes of symmetry overlaps with the rotation axes of symmetry of cylindrical molybdenum crucible 3, it is additionally provided with one in the left side of disk dress molybdenum crucible lid 2 and adds material through hole；And it being provided with a molybdenum mould 1 in the center of disk dress molybdenum crucible lid 2, this molybdenum mould 1 lower end is positioned at cylindrical molybdenum crucible 3, and the axis of symmetry of molybdenum mould 1 is additionally provided with a capillary channel.
Lowermost end at cylindrical molybdenum crucible 3 inner chamber is additionally provided with bubble trap 7, as shown in Figure 2, bubble trap 7 is three-layer network shape structure, tungsten-rhenium alloy weaving filaments form, and three-layer network shape structure is from top to bottom, mesh is sequentially reduced, bottom mesh is 2mm, as it is shown on figure 3, there is dendroid tungsten-rhenium wire weaving structure to support between stratum reticulare, tungsten-rhenium wire braiding stagger angle is 30 °, and supporting construction guarantees the gap having more than 2cm between stratum reticulare simultaneously.
After sapphire ball material falls on bubble trap 7, owing to alumina balls material has the kinetic energy that necessarily falls, and the multiple structure that the tungsten-rhenium wire of bubble trap 7 supports coordinates loose structure simultaneously, its eyelet is sequentially reduced from top to bottom, on the one hand can effectively guarantee that ball material falls in bubble trap 7 smoothly, on the other hand can effectively prevent ball material directly through bubble trap 7, prevent ball material from falling directly into crucible, ball material falls into and effectively converts the elastic potential energy that ball material kinetic energy is bubble trap 7 on bubble trap 7, prevent ball material from falling to colliding crucible or cause smelt splashes.
As it is shown in figure 1, be additionally provided with a high frequency pumping device in cylindrical molybdenum crucible 3 bottom center, 6, and this high frequency pumping device 6 is connected through cylindrical molybdenum crucible 3 with bubble trap 7；In this removing sapphire crystal melt material, air bubble apparatus also includes a support component 5, and this support component 5 is located at cylindrical molybdenum crucible 3 bottom, and is fixed on removing the device of bubble in sapphire crystal melt material in crystal growing furnace by this support component 5.
Air bubble apparatus in the removing sapphire crystal melt material of the present embodiment, utilizes dither to the bubble formation resonance effect on bubble trap, forces the bubble disengagement on bubble trap fast and effectively, and float to above melt liquid level；Can effectively remove bubble in raw material, the gas content of melt in reduction crucible, at utmost guarantee raw material cleaning in crucible, and then improve crystal end product quality.
After ball material melted by heat, gas contained by ball material pore is dissolved in alumina melt, when melt flows through bubble trap 7, owing to 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 jeep of bubble, and R is the size of bubble, and σ is the surface tension of alumina melt, PoIt is the pressure of bubble present position, PvBeing the saturated vapor pressure of alumina melt, Euler integral of the second kind is shape function, and θ is the infiltration angle of alumina melt and tungsten-rhenium wire, and α is the angle that bubble trap 7 dendroid tungsten-rhenium wire is staggeredly placed.The value of infiltration angle θ is at 10 ° to 50 °, and when α is 30 ° to 120 °, trying to achieve shape function Γ has minimum, branch alternate angle α to be optimal corner.
If melt is without bubble trap 7, then shape function Γ takes 1, oversaturated gaseous solute cannot separate out, but in crystal growing process, when being risen to the top of mould by die end along with melt, at capillary channel or the die surface bubble of mould, and enter into crystals with crystallization process, become the mass defect in crystal.
If melt flows through bubble trap 7, and adjust its dendroid tungsten-rhenium wire angle of cut α to optimal corner, shape function Γ can be made close to 0, then the bubble Gibbs free energy in aluminium oxide liquation significantly reduces, at catcher dendroid staggered place fast nucleation, after nucleation, around bubble, solute concentration reduction forces neighbouring gaseous solute to flow to nucleation district, it is achieved the most effectively bubble is collected.
Bubble adhesion after collection is after the nucleation of tungsten-rhenium wire staggered place, gas and minute bubbles are constantly close to nucleation district, at nucleation, bubble size is slowly increased, and its buoyancy was often not enough to leave tungsten-rhenium wire staggered place and float to liquation liquid level until being discharged in ambiance in the considerably long waiting time.In order to the bubble after making collection leaves tungsten-rhenium wire, the nucleation core of supersaturated gas is provided for the raw material of follow-up addition, needs the resonance caused by high frequency pumping by bubble disengagement.
The vibration of the most any frequency all can be excited bubble to resonate by bubble absorption.Resonant frequency is affected by except factors such as the density of added raw material and internal porosity sizes, additionally depends on the size of bubble.Free energy Δ G determines into the size of nuclei air bubble, and high frequency pumping starts the difference on opportunity simultaneously, all have impact on the size of bubble.The resonant frequency ω determined by parameters such as bubble size Rr, 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, ωrBeing resonant frequency, ρ is sapphire fusant density, and γ is isobaric and the ratio of constant volume specific heat appearance.The size of R is generally between tens microns to hundreds of micron, then is estimated by sapphire parameters, and resonant frequency is generally at 100KHz to 1MHz.
Now utilizing the higher-order of oscillation excitation nucleation district bubble of certain frequency, bubble border absorbs excitation energy, and interface energy increases so that absorption affinity is not enough to keep bubble to rest on original tungsten-rhenium wire reports to the leadship after accomplishing a task place, and final bubble is to floating to liquid level.Expand because ambient pressure constantly reduces during bubble floating, rupture to melt liquid level and release all kinds of gaseous impurities contained by ball material, and gas contained by melt in crucible, as CO, Ar equal size then declines to a great extent.
The present embodiment high frequency waves excitation acoustic pressure take 3 subharmonic optimize formula [4]:
PA = Psin(ωt) + P1sin(ωt + φ1) +P2sin(ωt + φ2)
[4]
Wherein, PABeing high frequency pumping acoustic pressure, ω is multiplied by 2 π equal to higher frequency, and P, P1 and P2 are harmonic pressure respectively, φ1And φ2It it is the phase contrast of harmonic wave.
Although having formula [3] and formula [4], it is clear and definite that technological parameter seems comparison, as long as applying larger sound pressure with resonant frequency to bubble, forcing bubble quickly to absorb energy and expanding and collapse.But in practical situation, the every constant coefficient of the sapphire such as coefficient of viscosity, vapour pressure is all relevant with practicable process temperature with surface tension, so operating process is numerous and diverse.
The present embodiment passes through 1 group of parameters optimization group, and 3 contrast groups, and different with differential, design parameter is as follows:
| Parameter name | High frequency power | Excitation acoustic pressure (PA) | Frequency (ω/2 π) | Phase contrast (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, do not start high frequency pumping；Contrast groups 2, excitation acoustic pressure is slightly larger than frequency (0.04MHz) close to pressure at bubble, frequency selective reaonance frequency；Contrast groups 3, excitation acoustic pressure is close to pressure 2 times at bubble, and frequency is close to resonant frequency 0.5 times；Optimization group, excitation acoustic pressure is close to pressure 2 times at bubble, and frequency is close to resonant frequency 0.5 times, and selecting its phase contrast of 3 subharmonic is π/4 and π/6 respectively.
The present embodiment removes the method for bubble in sapphire melt, and according to above-mentioned experimental design thinking, it specifically comprises the following steps that
Step S1: when melt 4 off-capacity of storage is with continued growth sapphire crystal in molybdenum crucible 3, make molybdenum mould 1 separate with molybdenum crucible 3 together with molybdenum crucible lid 2 and (if melt solidification shrinkage touches mould, draw mould, molybdenum die deformation is made even to tilt), and reduce heter temperature value to less than 2000 DEG C；
Step S2: the high purity aluminium oxide ball material that will clean up, in putting in crucible；
Step S3: controlling crystal growing furnace and be warming up to 2000-2100 DEG C, aluminum ball material to be oxidized melts in bubble trap 7；
Step S4 and the S5 of contrast groups 1 are as follows:
Step S4: according to embodiment mentality of designing contrast groups 1, does not start high frequency pumping 6, and persistently charging is so that obtaining sufficient melt material in crucible, waits and reaches thermal balance in 2 hours；
Step S5: make mould again contact melt 4, and implement long crystalline substance operation.
Step S4 and the S5 of contrast groups 2 are as follows:
Step S4: according to embodiment mentality of designing contrast groups 2, starts high frequency pumping 6, power 5w/cm2, pressure 0.12MPa, frequency 0.05MHz, without harmonic wave, persistently charging is so that obtaining sufficient melt material in crucible；
Step S5: make contacting dies melt material, and implement long crystalline substance operation.
Step S4 and the S5 of contrast groups 3 are as follows:
Step S4: according to embodiment mentality of designing contrast groups 3, starts high frequency pumping 6, power 5w/cm2, pressure 0.25MPa, frequency 0.02MHz, without harmonic wave, persistently charging is so that obtaining sufficient melt material in crucible；
Step S5: make contacting dies melt material, and implement long crystalline substance operation.
Step S4 and the S5 of optimization group are as follows:
Step S4: according to embodiment mentality of designing optimization group, starts high frequency pumping 6, power 5w/cm2, pressure 0.25MPa, frequency 0.02MHz, harmonic phase difference is not π/4 and π/6, and persistently charging is so that obtaining sufficient melt material in crucible；
Step S5: make contacting dies melt material, and implement long crystalline substance operation, until long crystalline substance terminates.
In the present embodiment gained colourless transparent crystal, contrast groups 1-3 gained crystal is respectively present bubble in various degree, and wherein contrast groups 2 bubble is the most maximum, and contrast groups 1 is better than contrast groups 2 close to contrast groups 3, and optimization group gained crystal mass is best, there is not the macroscopic bubble being more than 50 microns.
The ultimate principle of the present invention and principal character and advantages of the present invention have more than been shown and described.Skilled person will appreciate that of the industry; the present invention is not restricted to the described embodiments; the principle that the present invention is simply described described in above-described embodiment and description; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements both fall within scope of the claimed invention.Claimed scope is defined by appending claims and equivalent thereof.
Claims (6)
1. remove air bubble apparatus in sapphire crystal melt material for one kind, it is characterised in that: described device includes a crucible, mould, crucible cover, bubble trap and high frequency pumping device；
Described crucible cover is located at the top of crucible, and keeps the gap of 1mm-200mm with crucible；The rotation axes of symmetry of described crucible cover overlaps with the rotation axes of symmetry of crucible, and also has one on the crucible cover of described side and add material through hole；Described mould is arranged on the center of crucible cover, and its lower end is positioned at crucible, and the axis of symmetry of described mould is additionally provided with a capillary channel；Described bubble trap is arranged on the lowermost end of crucible interior, and described high frequency pumping device is arranged on crucible bottom center, and high frequency pumping device is connected through crucible with bubble trap；
Described device also includes that a support component, described support component are located at crucible bottom, and is fixed on removing the device of bubble in sapphire crystal melt material in crystal growing furnace by this support component.
Air bubble apparatus in removing sapphire crystal melt material the most according to claim 1, it is characterised in that: if the network structure that described bubble trap is woven by dried layer refractory metal silk is constituted, and if dried layer network structure from top to bottom, mesh is sequentially reduced；Refractory metal silk dendritic support net structure it is additionally provided with between described each lamina reticularis.
Air bubble apparatus in removing sapphire crystal melt material the most according to claim 2, it is characterised in that: the minimum dimension of described mesh is 0.5mm-5mm, and described dendritic angle is 30 °-120 °.
Air bubble apparatus in removing sapphire crystal melt material the most according to claim 2, it is characterised in that: described refractory metal is molybdenum, tungsten, tungsten-molybdenum alloy or tungsten-rhenium alloy.
5. one kind with removing the sweep-out method of air bubble apparatus in sapphire crystal melt material described in claim 1, it is characterised in that: described sweep-out method comprises the steps:
When the melt off-capacity of storage is with continued growth sapphire crystal in molybdenum crucible, makes mould separate with the liquation in crucible together with crucible cover, and reduce heter temperature value to less than 2000 DEG C；
The high purity aluminium oxide raw material that will clean up, by adding during material through hole puts in crucible on crucible cover；
Controlling crystal growing furnace and be warming up to 2000-2100 DEG C, aluminum feedstock to be oxidized is fused into melt in bubble trap；
Starting high frequency pumping incoming dither in bubble trap, remove the microbubble of release in melting process of raw material, persistently charging is so that obtaining sufficient melt in crucible；
Make contacting dies melt material, and implement long crystalline substance operation, repeat S1 to S4 until crystal product meets the requirements.
The sweep-out method of air bubble apparatus in removing sapphire crystal melt material the most according to claim 5, it is characterised in that: described step (4) is including at least 3 regulations parameters, i.e. power, frequency and waveform；Described power is generally at 1W/cm2-1KW/
cm2, described frequency is generally at 1KHz-10MHz, and described waveform is usually sinusoidal wave or square wave.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106637397A (en) * | 2016-12-30 | 2017-05-10 | 江西赛维Ldk太阳能高科技有限公司 | Polycrystalline silicon ingot, preparation method of polycrystalline silicon ingot and polycrystalline silicon ingot furnace |
| 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 |
| AT16098U1 (en) * | 2017-05-03 | 2019-01-15 | Plansee Se | Glass melting component |
| 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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