CN113957529A - Gallium oxide crystal growth method based on guided mode growth device - Google Patents
Gallium oxide crystal growth method based on guided mode growth device Download PDFInfo
- Publication number
- CN113957529A CN113957529A CN202111051906.2A CN202111051906A CN113957529A CN 113957529 A CN113957529 A CN 113957529A CN 202111051906 A CN202111051906 A CN 202111051906A CN 113957529 A CN113957529 A CN 113957529A
- Authority
- CN
- China
- Prior art keywords
- crystal growth
- gallium oxide
- laser
- auxiliary heater
- oxide crystal
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229910001195 gallium oxide Inorganic materials 0.000 title claims abstract description 77
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 title claims abstract description 76
- 238000002109 crystal growth method Methods 0.000 title claims abstract description 32
- 239000013078 crystal Substances 0.000 claims abstract description 116
- 238000000034 method Methods 0.000 claims abstract description 34
- 238000009413 insulation Methods 0.000 claims description 24
- 238000007789 sealing Methods 0.000 claims description 20
- 230000001678 irradiating effect Effects 0.000 claims description 2
- 230000000149 penetrating effect Effects 0.000 claims 1
- 239000007788 liquid Substances 0.000 abstract description 10
- 230000000694 effects Effects 0.000 abstract description 5
- 239000000155 melt Substances 0.000 abstract description 3
- 229910052741 iridium Inorganic materials 0.000 description 16
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 16
- 238000004321 preservation Methods 0.000 description 11
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical group O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 5
- 239000011449 brick Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 229920000742 Cotton Polymers 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000008646 thermal stress Effects 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- QZQVBEXLDFYHSR-UHFFFAOYSA-N gallium(III) oxide Inorganic materials O=[Ga]O[Ga]=O QZQVBEXLDFYHSR-UHFFFAOYSA-N 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000008642 heat stress Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000004093 laser heating Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000000825 ultraviolet detection Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Images
Classifications
-
- 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
-
- 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
- C30B15/14—Heating of the melt or the crystallised materials
- C30B15/16—Heating of the melt or the crystallised materials by irradiation or electric discharge
-
- 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
Landscapes
- 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 gallium oxide crystal growth method based on a growth device of a guided mode method, wherein the gallium oxide growth device comprises a gallium oxide crystal growth furnace and a laser auxiliary heater arranged on the side edge of the gallium oxide crystal growth furnace, and the crystal growth method comprises the following steps: in the process of crystal growth, when the mixed crystals appear on the gallium oxide crystal, the laser auxiliary heater emits laser and irradiates the mixed crystals, and the mixed crystals are removed. The invention heats and melts the mixed crystals on the gallium oxide crystal by the laser emitted by the laser auxiliary heater, has direct and quick effect and accurate and efficient positioning, and effectively solves the technical problem of mixed crystals generation caused by unpredictable and tiny disturbance at the solid-liquid interface near the die opening in the process of growing the gallium oxide crystal by a guided mode method.
Description
Technical Field
The invention relates to the technical field of gallium oxide crystal preparation, in particular to a gallium oxide crystal growth method based on a growth device adopting a guided mode method.
Background
β-Ga2O3(gallium oxide) is a direct band gap wideThe forbidden band semiconductor material has a forbidden band width of about 4.8-4.9 eV. The high-temperature high-power semiconductor laser has the advantages of large forbidden band width, high saturated electron drift speed, high thermal conductivity, high breakdown field strength, stable chemical property and the like, and has wide application prospect in the field of high-temperature, high-frequency and high-power electronic devices. In addition, the sensor can also be used for LED chips, solar blind ultraviolet detection, various sensor elements, camera elements and the like.
At present, the large-size gallium oxide crystals are prepared in batches mainly by adopting a mold guiding preparation technology. The gallium oxide crystal growing by the mold-guiding method is a process that the solid-liquid interface near the die opening is continuously changed from melt to solid, and the width of the solid-liquid interface near the die opening is subjected to the changes of equal width, narrowing, widening and equal width along with the crystal seeding, necking, shouldering and equal width growth. In the whole crystal growth process, any tiny disturbance, such as the attachment of volatile matters, tiny defects and local deformation of a die opening and local unevenness of a temperature field, at a solid-liquid interface near the die opening can cause the formation of mixed crystals, and the quality and the usable range of the grown crystals are seriously influenced.
Accordingly, the prior art is yet to be improved and developed.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a gallium oxide crystal growth method based on a growth device of a guided mode method, and aims to solve the problem of preparing beta-Ga by the conventional guided mode method2O3The problem that the mixed crystal growing on the crystal cannot be removed in the single crystal process.
The technical scheme of the invention is as follows:
a gallium oxide crystal growth method based on a growth device of a guided mode method is disclosed, wherein the gallium oxide growth device comprises a gallium oxide crystal growth furnace and a laser auxiliary heater arranged on the side edge of the gallium oxide crystal growth furnace, and the crystal growth method comprises the following steps:
in the process of crystal growth, when the mixed crystals appear on the gallium oxide crystal, the laser auxiliary heater emits laser and irradiates the mixed crystals, and the mixed crystals are removed.
The crystal growth method comprises the step of enabling the laser wavelength emitted by the laser auxiliary heater to be 800-2000 nm.
The crystal growth method is characterized in that the power of the laser auxiliary heater is 0.1-100W.
The crystal growth method is characterized in that the volume of the mixed crystal is 2mm3And irradiating the mixed crystal for 0.55s by using a laser auxiliary heater with the power of 10W and the laser wavelength of 1064 nm.
The crystal growth method comprises the steps that the gallium oxide crystal growth furnace comprises a base, a lower thermal field structure arranged on the base and an upper thermal field structure arranged on the lower thermal field structure, wherein the upper thermal field structure comprises an upper heat insulation assembly and an upper sealing layer which are concentrically arranged from inside to outside, an observation hole which is communicated with the inside and the outside and used for observing crystal growth is formed in the upper heat insulation assembly, the laser auxiliary heater is positioned on the side edge of the observation hole, and laser emitted by the laser auxiliary heater is injected into the gallium oxide crystal growth furnace through the observation hole.
The crystal growth method, wherein the crystal growth method further comprises the steps of:
and observing whether the mixed crystals exist on the crystals or not through the observation hole.
The crystal growth method is characterized in that 1-4 observation holes are formed in the heat insulation component, and a laser auxiliary heater is correspondingly arranged on the side edge of each observation hole.
The crystal growth method is characterized in that a through cavity which penetrates through the upper end face and the lower end face and is used for inserting the seed rod is arranged in the center of the upper heat insulation assembly along the axial direction.
Has the advantages that: the invention provides a gallium oxide crystal growth method based on a growth device of a guided mode method, wherein the gallium oxide growth device comprises a gallium oxide crystal growth furnace and a laser auxiliary heater arranged on the side edge of the gallium oxide crystal growth furnace, and the crystal growth method comprises the following steps: in the process of crystal growth, when the mixed crystals appear on the gallium oxide crystal, the laser auxiliary heater emits laser and irradiates the mixed crystals, and the mixed crystals are removed. The invention heats and melts the mixed crystals on the gallium oxide crystal by the laser emitted by the laser auxiliary heater, has direct and quick effect and accurate and efficient positioning, and effectively solves the technical problem of mixed crystals generation caused by unpredictable and tiny disturbance at the solid-liquid interface near the die opening in the process of growing the gallium oxide crystal by a guided mode method.
Drawings
FIG. 1 is a schematic structural diagram of a gallium oxide growth apparatus according to the present invention.
Detailed Description
The invention provides a gallium oxide crystal growth method based on a growth device of a guided mode method, and the invention is further described in detail below in order to make the purpose, technical scheme and effect of the invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
It will be understood by those skilled in the art that, unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. It will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the prior art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
In the process of growing gallium oxide crystals by the guided mode method, the gallium oxide crystals grown by the guided mode method are the process that the solid-liquid interface near the die opening is continuously changed from melt to solid, and the width of the solid-liquid interface near the die opening is subjected to the changes of equal width, narrowing, widening and equal width along with crystal seeding, necking, shouldering and equal width growth. In the whole crystal growth process, any tiny disturbance, such as the attachment of volatile matters, tiny defects and local deformation of a die opening and local unevenness of a temperature field, at a solid-liquid interface near the die opening can cause the formation of mixed crystals, and the quality and the usable range of the grown crystals are seriously influenced.
Based on the above, the invention provides a gallium oxide crystal growth method based on a growth device of a guided mode method, wherein the gallium oxide growth device comprises a gallium oxide crystal growth furnace and a laser auxiliary heater arranged on the side edge of the gallium oxide crystal growth furnace, and the crystal growth method comprises the following steps:
in the process of crystal growth, when the mixed crystals appear on the gallium oxide crystal, the laser auxiliary heater emits laser and irradiates the mixed crystals, and the mixed crystals are removed.
The invention effectively solves the technical problem that the mixed crystals are generated at the solid-liquid interface near the die opening due to unpredictable and tiny disturbance in the process of growing the gallium oxide crystals by a guide die method, thereby ensuring the smooth growth of the high-quality gallium oxide crystals.
In some embodiments, the latent heat of crystallization due to gallium oxide is 4.6 × 105J/kg, i.e. 4.6X 10 heat absorbed per 1kg of gallium oxide melted or released per 1kg of gallium oxide crystallized5J. Visible gallium oxide mixed crystal minimum volume of 2mm3Gallium oxide density 5.9g/cm3The minimum visible gallium oxide mixed crystal mass was 5.9X (2X 10)-3)≈12×10-3g＝12×10-6kg; if the mixed crystal needs to be eliminated, only 5.5J of heat is needed, and the power requirement on the laser is extremely low.
The gallium oxide single crystal has high carrier concentration and strong infrared absorption at the high temperature of the crystallization melting point, has high absorption rate to infrared laser of more than 1000nm, can be approximately considered as 100 percent, and has extremely low radiation coefficient, so the laser heating has extremely high heating efficiency. Taking a common 1064nm wavelength continuous laser with power of 10w as an example, only 0.55s of irradiation time is needed to completely melt the visible gallium oxide mixed crystal with the minimum volume, thereby achieving the purpose of eliminating the mixed crystal generated in the crystal growth process.
In some embodiments, the laser assisted heater emits a laser wavelength of 800-. The laser-assisted heater is preferably a continuous laser with a wavelength of 1064nm, or a high repetition rate quasi-continuous laser of Nd: YAG, which is the most common laser gain medium. In this embodiment, there is no blocking material between the laser light source and the target region that absorbs the laser wavelength more greatly, and the laser spot emitted by the laser auxiliary heater is adjusted to ensure that the width of the laser spot is larger than the cross-sectional area of the impurity crystal.
In some embodiments, the laser-assisted heater has a power of 0.1W to 100W. The power selection of the laser auxiliary heater is flexibly adjusted according to the size of the mixed crystal and the selected laser wavelength. The larger the size of the miscrystal, the higher the power of the laser required, in order to avoid the miscrystal affecting the quality of the gallium oxide crystal growth, usually when a visible size (e.g. 0.2 mm) is found3) And starting the laser auxiliary heater to heat and eliminate the mixed crystals, so that the power of the laser auxiliary heater is preferably 0.1-10W.
In some embodiments, since light larger than 800nm is invisible, a sub-laser for visual aiming may be collocated on the laser-assisted heater, the laser emitted by the sub-laser is visible light, and the laser emitted by the sub-laser and the laser emitted by the laser-assisted heating are in the same direction.
In some embodiments, as shown in fig. 1, the gallium oxide growth apparatus includes a gallium oxide crystal growth furnace 1 and a laser auxiliary heater 2 disposed at a side of the gallium oxide crystal growth furnace, where the gallium oxide crystal growth furnace 1 includes a base 10, a lower thermal field structure disposed on the base 10, and an upper thermal field structure disposed on the lower thermal field structure, the upper thermal field structure includes an upper thermal insulation component 20 and an upper sealing layer 30 concentrically disposed from inside to outside, and the upper thermal insulation component 20 is provided with an observation hole 21 communicating inside and outside for observing crystal growth; the center of the upper heat insulation component 20 is provided with a through cavity 22 which penetrates through the upper end face and the lower end face and is used for inserting a seed rod along the axial direction.
In this embodiment, as shown in fig. 1, the laser auxiliary heater 2 may be separately disposed at a side of the observation hole 21, and the laser emitted from the laser auxiliary heater 2 is injected into the gallium oxide crystal growth furnace 1 through the observation hole 21; of course, the laser auxiliary heater 2 may also be separately disposed at the upper end of the through cavity 22, and the laser emitted by the laser auxiliary heater 2 is emitted into the gallium oxide crystal growth furnace 1 through the through cavity 22; further, the laser auxiliary heater can be simultaneously arranged on the side of the observation hole 21 and the upper end of the through cavity 22, and the laser emitted by the laser auxiliary heater 2 can be respectively emitted into the gallium oxide crystal growth furnace 1 from different angles through the observation hole 21 and the through cavity 22.
In this embodiment, when the existence of the mixed crystal on the crystal is observed from the observation hole 21, the laser auxiliary heater arranged at the side of the observation hole 21 and/or the upper end of the through cavity 22 emits laser and irradiates on the mixed crystal, so that the mixed crystal is rapidly melted and volatilized, and the smooth growth of the high-quality gallium oxide crystal is ensured.
In some embodiments, the aperture extension direction of the observation hole 21 forms an included angle of 20-70 degrees with the through cavity 22 of the upper heat preservation assembly. In this embodiment, the aperture extending direction of the observation hole 21 and the through cavity 22 of the upper thermal insulation component form an included angle of 20-70 degrees, so that volatile matters scattered around in the through cavity 22 are not easy to enter the observation hole 21, and the adhesion of the volatile matters on the observation window extending outwards is effectively reduced.
In some specific embodiments, 1 to 4 observation holes are arranged on the upper heat preservation component, and the number of the observation windows is equal to that of the laser auxiliary heaters 2. For example, as shown in fig. 1, 2 observation holes 21 may be uniformly formed in the upper thermal insulation member, and accordingly, one laser auxiliary heater 2 is correspondingly disposed on a side of each observation hole 21. In the embodiment, the two observation holes 21 are arranged, so that the balance of the thermal field in the crystal growth furnace can be ensured, and the growth state of the crystal can be conveniently observed by workers from different angles; correspondingly, the two laser auxiliary heaters 2 are arranged, so that the heating efficiency can be improved, and the mixed crystals can be quickly eliminated.
The upper heat insulation assembly is formed by stacking at least one heat insulation layer, and the upper heat insulation assembly is stacked in a layered mode in height, so that the thermal stress at high temperature can be effectively released, and the problem of uncontrolled cracking of the upper heat insulation assembly is solved. And the heat-insulating layer is formed by splicing a plurality of sub heat-insulating layers, and the heat stress at high temperature can be further released by adopting a splicing mode, so that the uncontrolled cracking of the upper heat-insulating component is effectively avoided, the stability of a thermal field with multiple furnace growth is improved, and the large-scale production of the gallium oxide crystal with high quality and low cost is realized. The heat-insulating layer can be formed by splicing two sub heat-insulating layers or a plurality of sub heat-insulating layers. In this embodiment, the cross-sectional shape of the through cavity may be circular, square or a tapered frustum, but is not limited thereto.
In one embodiment, the heat-insulating layer is formed by splicing a plurality of sub-heat-insulating layers in a snap fastener mode, and by adopting the structure, the purpose of effectively releasing the thermal stress at high temperature can be achieved. By way of example, the heat insulation layer is formed by splicing 2-6 sub-heat insulation layers, for example, 2, 3, 4, 5 or 6 sub-heat insulation layers.
In one embodiment, as shown in fig. 1, the upper end surface of the heat insulation layer is provided with a step, the lower end surface is provided with a groove, and adjacent heat insulation layers are stacked in a manner that the step and the groove are matched. The adjacent heat-insulating layers can be firmly laminated together by adopting a mode that the steps are matched with the grooves.
That is to say, the upper end face of each heat preservation is provided with the step, and the lower terminal surface that the relative setting of upper end face was provided with the recess. Taking three heat preservation layers as an example, the step that the up end of middle heat preservation layer set up matches with the recess that the lower terminal surface of top heat preservation set up together, and the recess that the lower terminal surface of middle heat preservation layer set up matches with the step that the up end of below heat preservation set up together, reaches the stable effect of piling up of three heat preservation layers. By way of example, the insulating layer is a zirconia insulating layer, that is, the insulating layer is made of zirconia.
In some embodiments, as shown in fig. 1, the upper thermal field structure further comprises an upper seal layer 30 coaxially disposed outside the upper insulating assembly, the upper seal layer being at the same height as the upper insulating assembly. Further, the upper thermal field structure further comprises a sealing cover 40 covering the top of the upper sealing layer and the upper heat preservation component. Further, the upper sealing layer may be a quartz or glass sealing layer, and the material of the sealing cover is the same as that of the upper sealing layer. After the upper heat-insulating assembly, the upper sealing layer and the sealing cover component are combined, only a small hole is formed in the sealing cover at the top to form a gas exchange channel with the inner area, and the size of the gas exchange channel is just used for seed rods to pass through.
In this embodiment, the upper sealing layer 30 is transparent and high temperature resistant, and can form effective sealing, ensure the whole convection-free environment, and prevent the chemical equilibrium of decomposition and volatilization of gallium oxide from moving to the right, so as to effectively inhibit the decomposition and volatilization of gallium oxide, and realize the production of high-quality gallium oxide crystals, and the whole structure is simple and stable.
In one embodiment, as shown in fig. 1, the lower thermal field structure includes a lower sealing layer 50, a lower thermal insulation member 60, an iridium heating element 70 and a crucible 80, which are coaxially installed from outside to inside; wherein an iridium mold 90 is embedded in the crucible. In other words, the iridium heat-generating body 70 is coaxially disposed outside the crucible 80, the lower heat-insulating member 60 is coaxially disposed outside the iridium heat-generating body 70, and the lower sealing layer 50 is coaxially disposed outside the lower heat-insulating member 60. The material of the lower sealing layer is the same as that of the upper sealing layer.
The crucible 80 is used for loading gallium oxide raw material, and a crucible cover is covered on the crucible to prevent the gallium oxide raw material from volatilizing. The crucible is an iridium crucible, the crucible cover is an iridium crucible cover, a through hole with the same cross-sectional dimension as the iridium mold is formed in the crucible cover, and the iridium mold extends into the through hole of the crucible cover and is embedded in the center of the crucible along the axial direction. The iridium die cross-section is the same shape as the cross-section of the crystal to be grown so that the feedstock can be transported by capillary action to the top of the iridium die and spread out on top until fully covered, thereby growing the desired shape.
An iridium reflecting cover 71 is arranged at the upper end of the iridium heating element, the outer diameter of the iridium reflecting cover is the same as that of the iridium heating element, a through hole is formed in the center of the iridium reflecting cover 71, and the through hole is used for inserting a seed rod.
Wherein, lower insulation component 60 is formed by insulating brick and the bottom heated board combination of both sides. Further, the insulating brick can be a zirconia insulating brick, and the insulating board can be a zirconia insulating board.
In one embodiment, as shown in fig. 1, the lower thermal field structure further comprises: and the heat insulation material filling layer 61 is arranged between the lower sealing layer and the lower heat insulation component. Wherein, the heat preservation material can be zirconia sand or high temperature resistant cotton, such as quartz fiber cotton.
In this embodiment, the upper thermal field structure and the lower thermal field structure are butted together, the upper thermal field structure and the lower thermal field structure are separated by a partition plate, the upper thermal field structure and the lower thermal field structure are coaxially arranged at the center, and the whole structure can be a cylindrical structure. When the whole body is of a cylindrical structure, the lower sealing layer, the lower heat insulation component, the iridium heating body and the crucible with the cover are all of cylindrical structures. Of course, the present embodiment is not limited to the cylindrical structure, and other shapes and structures are also possible.
In summary, the present invention provides a gallium oxide crystal growth method based on a growth apparatus of a guided mode method, the gallium oxide growth apparatus includes a gallium oxide crystal growth furnace and a laser-assisted heater disposed at a side of the gallium oxide crystal growth furnace, the crystal growth method includes the steps of: in the process of crystal growth, when the mixed crystals appear on the gallium oxide crystal, the laser auxiliary heater emits laser and irradiates the mixed crystals, and the mixed crystals are removed. The invention heats and melts the mixed crystals on the gallium oxide crystal by the laser emitted by the laser auxiliary heater, has direct and quick effect and accurate and efficient positioning, and effectively solves the technical problem of mixed crystals generation caused by unpredictable and tiny disturbance at the solid-liquid interface near the die opening in the process of growing the gallium oxide crystal by a guided mode method.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (8)
1. A gallium oxide crystal growth method based on a growth device of a guided mode method is characterized in that the gallium oxide growth device comprises a gallium oxide crystal growth furnace and a laser auxiliary heater arranged on the side edge of the gallium oxide crystal growth furnace, and the crystal growth method comprises the following steps:
in the process of crystal growth, when the mixed crystals appear on the gallium oxide crystal, the laser auxiliary heater emits laser and irradiates the mixed crystals, and the mixed crystals are removed.
2. The crystal growth method of claim 1, wherein the laser wavelength emitted by the laser-assisted heater is 800-2000 nm.
3. The crystal growth method of claim 1, wherein the laser-assisted heater has a power of 0.1W to 100W.
4. The crystal growth method according to claim 1, wherein the volume of the hetero-crystal is 2mm3And irradiating the mixed crystal for 0.55s by using a laser auxiliary heater with the power of 10W and the laser wavelength of 1064 nm.
5. The crystal growth method of claim 1, wherein the gallium oxide crystal growth furnace comprises a base, a lower thermal field structure arranged on the base, and an upper thermal field structure arranged on the lower thermal field structure, the upper thermal field structure comprises an upper thermal insulation component and an upper sealing layer which are concentrically arranged from inside to outside, an observation hole which is communicated with the inside and the outside and used for observing crystal growth is formed in the upper thermal insulation component, the laser auxiliary heater is positioned on the side edge of the observation hole, and laser emitted by the laser auxiliary heater is emitted into the gallium oxide crystal growth furnace through the observation hole.
6. The crystal growth method of claim 5, further comprising the steps of:
and observing whether the mixed crystals exist on the crystals or not through the observation hole.
7. The crystal growth method of claim 5, wherein the heat-insulating component is provided with 1-4 observation holes, and the side of each observation hole is correspondingly provided with a laser auxiliary heater.
8. The crystal growth method of claim 5, wherein a through cavity penetrating the upper and lower end faces and into which the seed rod is inserted is provided in the center of the upper heat-insulating member in the axial direction.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111051906.2A CN113957529A (en) | 2021-09-08 | 2021-09-08 | Gallium oxide crystal growth method based on guided mode growth device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111051906.2A CN113957529A (en) | 2021-09-08 | 2021-09-08 | Gallium oxide crystal growth method based on guided mode growth device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113957529A true CN113957529A (en) | 2022-01-21 |
Family
ID=79461207
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111051906.2A Pending CN113957529A (en) | 2021-09-08 | 2021-09-08 | Gallium oxide crystal growth method based on guided mode growth device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113957529A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59121191A (en) * | 1982-12-25 | 1984-07-13 | Toshiba Corp | Apparatus for preparation of ribbon crystal of silicon |
| JP2011153054A (en) * | 2010-01-28 | 2011-08-11 | Namiki Precision Jewel Co Ltd | Method for producing gallium oxide single crystal and gallium oxide single crystal |
| CN103541008A (en) * | 2013-11-12 | 2014-01-29 | 上海硅酸盐研究所中试基地 | Growth method and growth device of large-size gallium oxide single crystal |
| CN112795986A (en) * | 2020-12-31 | 2021-05-14 | 山东大学 | Single crystal growth device capable of regulating and controlling crystallization solid-liquid interface in real time and use method |
| CN112877770A (en) * | 2021-02-02 | 2021-06-01 | 杭州富加镓业科技有限公司 | Growth device and growth method for growing gallium oxide crystal by guided mode method |
| CN113026103A (en) * | 2021-02-09 | 2021-06-25 | 杭州富加镓业科技有限公司 | Monitoring system for growing gallium oxide crystal by guided mode method and preparation method of gallium oxide crystal |
-
2021
- 2021-09-08 CN CN202111051906.2A patent/CN113957529A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59121191A (en) * | 1982-12-25 | 1984-07-13 | Toshiba Corp | Apparatus for preparation of ribbon crystal of silicon |
| JP2011153054A (en) * | 2010-01-28 | 2011-08-11 | Namiki Precision Jewel Co Ltd | Method for producing gallium oxide single crystal and gallium oxide single crystal |
| CN103541008A (en) * | 2013-11-12 | 2014-01-29 | 上海硅酸盐研究所中试基地 | Growth method and growth device of large-size gallium oxide single crystal |
| CN112795986A (en) * | 2020-12-31 | 2021-05-14 | 山东大学 | Single crystal growth device capable of regulating and controlling crystallization solid-liquid interface in real time and use method |
| CN112877770A (en) * | 2021-02-02 | 2021-06-01 | 杭州富加镓业科技有限公司 | Growth device and growth method for growing gallium oxide crystal by guided mode method |
| CN113026103A (en) * | 2021-02-09 | 2021-06-25 | 杭州富加镓业科技有限公司 | Monitoring system for growing gallium oxide crystal by guided mode method and preparation method of gallium oxide crystal |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US9021836B2 (en) | Glass welding method and glass layer fixing method | |
| KR102114985B1 (en) | Low temperature hermetic sealing via laser | |
| US9887059B2 (en) | Glass welding method | |
| JP2012134516A (en) | Manufacturing method of single crystal semiconductor wafer | |
| CN113026103B (en) | Monitoring system for growing gallium oxide crystal by guided mode method and preparation method of gallium oxide crystal | |
| KR20190004739A (en) | Quartz glass crucible, manufacturing method thereof, and manufacturing method of silicon single crystal using quartz glass crucible | |
| WO2021023253A1 (en) | Display module and cutting method therefor, and display device | |
| CN102648310A (en) | High throughput recrystallization of semiconducting materials | |
| CN114959870B (en) | Preparation method of high-temperature pressurized iron-doped zinc selenide crystal | |
| CN112877770A (en) | Growth device and growth method for growing gallium oxide crystal by guided mode method | |
| CN113957529A (en) | Gallium oxide crystal growth method based on guided mode growth device | |
| CN113957518A (en) | Gallium oxide crystal growth method based on guided mode growth device | |
| CN114086244B (en) | Method for growing gallium oxide crystal by guided mode method | |
| CN113913924A (en) | Gallium oxide single crystal growth device | |
| TW200405482A (en) | Method for fabricating semiconductor device | |
| CN216338068U (en) | Crystal growth furnace for improving volatile deposition of observation window | |
| TWI521601B (en) | Method for manufacturing polysilicon | |
| CN109280973A (en) | A kind of thermal field structure and its growing method inhibiting garnet structure scintillation crystal cracking | |
| JPS5870536A (en) | Laser annealing method | |
| KR101150848B1 (en) | Single crystal growing apparatus having cylindrical heat-reflection means | |
| WO2021079793A1 (en) | Ceramic composite and production method for ceramic composite | |
| WO2021045077A1 (en) | Ceramic composite | |
| JP2021038126A (en) | Method for manufacturing ceramic composite | |
| JP2021038346A (en) | Ceramic composite | |
| JP2021038347A (en) | Ceramic composite |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20220121 |
|
| RJ01 | Rejection of invention patent application after publication |