CN111088520A - Sapphire single crystal growth device and method - Google Patents

Sapphire single crystal growth device and method Download PDF

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Publication number
CN111088520A
CN111088520A CN201811358318.1A CN201811358318A CN111088520A CN 111088520 A CN111088520 A CN 111088520A CN 201811358318 A CN201811358318 A CN 201811358318A CN 111088520 A CN111088520 A CN 111088520A
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single crystal
crucible
heater
sapphire single
temperature
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CN201811358318.1A
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Inventor
李熙春
文圣皖
张桂源
金峻焕
金亨中
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Sapphire Technology Co Ltd
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Sapphire Technology Co Ltd
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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
    • C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/003—Heating or cooling of the melt or the crystallised material
    • 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
    • C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/002—Crucibles or containers for supporting the melt
    • 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
    • C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/006—Controlling or regulating
    • 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
    • C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/14—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method characterised by the seed, e.g. its crystallographic orientation
    • 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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  • 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 relates to a sapphire single crystal growth device and a growth method, wherein the sapphire single crystal growth device comprises: a refractory disposed inside the chamber and configured to insulate the inside of the chamber; a crucible arranged inside the refractory and loaded with sapphire single crystal seeds and sapphire raw materials in sequence at the bottom to realize growth of sapphire single crystal; a main heater disposed inside the refractory so as to surround the outside of the crucible, for raising the temperature of the hot zone and generating heat so as to generate a vertical temperature gradient and a horizontal temperature gradient inside the crucible; a cooling unit including a cooling plate in contact with the bottom of the crucible, for cooling the bottom of the crucible; and an auxiliary heater surrounding the cooling plate, the auxiliary heater controlling a flow rate of heat flowing out from the crucible through the cooling plate.

Description

Sapphire single crystal growth device and method
Technical Field
The present invention relates to a sapphire single crystal growth apparatus and a sapphire single crystal growth method, wherein a separate auxiliary heater surrounding a cooling plate is provided in addition to a main heater, and the flow rate of heat flowing out from a crucible to the cooling plate is controlled by controlling the auxiliary heater, so that the size of residual seeds and the crystal growth speed can be precisely and easily controlled in a seeding process.
Background
The sapphire single crystal is a single crystal of alumina (Al) in which a compound in the form of a combination of aluminum (Al) and oxygen (O) is bonded under a predetermined temperature condition2O3) A substance which solidifies in one direction in a Hexagonal system (Hexagonal system) crystal structure during solidification after melting.
Sapphire single crystal is a material having hardness after diamond, and has about 10 times higher abrasion resistance and corrosion resistance than quartz, and excellent insulating properties and permeability, and thus is widely used not only for synthetic gems and watch glasses but also in advanced material fields such as IT substrates, industrial substrates, military substrates, and LED substrates. In particular, touch screens (touch windows) as IT equipment have attracted attention as materials for military infrared detection missiles and for windows of fighters, scouts and the like.
The sapphire single crystal growth method is roughly classified into an upper Seed method (upper Seed method) in which a Seed (Seed) is placed on the upper side of a crucible and a crystal is grown downward, and a lower Seed method (lower Seed method) in which a Seed is placed on the bottom inside a crucible and a crystal is grown upward.
The top sowing method includes a Czochralski method (Czochralski), a Kyropoulos method (Kyropoulos), an edge-guided mold method (EFG), and the like.
First, the Czochralski method is to mix high-purity alumina (Al)2O3) A growth method in which seeds (Seed) are placed in an iridium crucible and melted, and then the seeds are placed in a solution and grown by spinning and pulling. Since the crystal has a long length and a diameter that can be freely adjusted, the crystal is widely used for growing a semiconductor single crystal such as silicone because of high productivity.
However, in the case of the Czochralski method, cracks are easily caused by a high temperature gradient in the culture of a crystal having a large brittleness such as a ceramic crystal, and thus the diameter of the culturable crystal is greatly limited, and moreover, the probability of occurrence of defects in the crystal such as dislocation is high.
The kyropoulos method is a growth method in which after an alumina material is melted, a seed is brought into contact with the surface of a solution and a crystal is grown by gradually lowering the temperature of the solution.
In this kyropoulos method, since movement due to rotation and pulling does not occur, there are advantages that a large ingot can be grown with a low defect density as compared with the czochralski method, but it is difficult to control the size and form of crystals, and therefore, when used as a Light Emitting Diode (LED) substrate, the yield of the substrate formed from the ingot is low.
The mold guide method is a method in which an alumina material is melted, a melt is raised through a plate-shaped capillary, seeds are brought into contact with the upper side of the melt, and then a plate-shaped ingot is grown by gradual pulling, thereby efficiently culturing a thin plate or a crystal having a complicated cross section.
However, the die-guiding method is difficult to avoid formation of many bubbles on the surface of the crystal, and therefore, it is necessary to remove about 50% of the bubbles on the surface by a method such as grinding, and therefore, the productivity is not high.
The bottom seeding Method includes a Heat Exchange Method (HEM), a Vertical Horizontal temperature Gradient cooling Method (VHGF), and the like.
The heat exchange method is a method of gradually lowering the temperature inside the chamber and growing crystals after fixing seeds at the bottom of the crucible and filling the alumina material.
This heat exchange method has advantages of low defect density and realization of large ingot growth, but the ratio of the diameter to the length of the grown crystal is limited to 1:1, and in the case of culturing a large crystal having a large cross-sectional area, the growth time of the crystal becomes excessively long, resulting in a decrease in productivity.
The vertical horizontal temperature gradient cooling method is a method in which after seeds are fixed to the bottom of a crucible and an alumina material is filled in the crucible to melt, directional solidification is performed from the direction of a heater (Heat sink) by adjusting the vertical temperature distribution and the horizontal temperature distribution in the chamber to grow crystals.
The vertical-horizontal temperature gradient cooling method has low defect density and simultaneously adds a temperature gradient to the vertical and horizontal directions to remove the limitation on the crystal shape and greatly reduce the growth time.
A conventional sapphire single crystal growth apparatus is disclosed in korean laid-open patent publication No. 10-2011-.
In patent document 1, after a crucible containing a sapphire seed crystal and a raw material is moved from a lower portion to an upper portion of a hot zone, the upward movement of the crucible is stopped when the raw material and the upper portion of the sapphire seed crystal are melted. Next, by the operation of moving the crucible downward at a slow speed, the raw material and the sapphire seed crystal are gradually crystallized by melting, and are deposited along the crystal plane of the remaining sapphire seed crystal.
However, the sapphire single crystal growth method of patent document 1 is formed by a vertical bridge method (one-direction solidification method), a sapphire seed crystal is placed in a crucible, the c-plane of the sapphire seed crystal is leveled, and the solution grows along the c-axis direction, so that the diameter of the crystal that can grow is greatly limited, and the defects in the crystal are large.
Recently, the application range of sapphire has become large, and large-caliber sapphire of 6 feet or more is required, and in order to manufacture a large-caliber sapphire ingot, a crucible and a heater having large dimensions must be used.
In addition, when a sapphire single crystal is grown by a vertical horizontal temperature gradient cooling method, imparting a vertical temperature gradient in the vertical direction and a horizontal temperature gradient in the horizontal direction is an important factor for growing a high-quality sapphire single crystal.
That is, when the temperature gradient in the vertical direction is small, bubbles in the ingot cannot float from the high liquid interface to the liquid side when the ingot grows, but solidify to cause bubble defects and the like. There is a method of removing such bubble defects by reducing the growth rate, but in this case, a cost increase occurs due to an increase in growth time, which is accompanied by a problem of an increase in crucible deformation. Also, in the cooling step, residual stress may increase and cracks may occur.
Therefore, large-caliber single crystal growth must cause a large temperature gradient and have growth stability.
Also, when sapphire single crystal growth is performed, when a seeding (seed) process is performed for high-quality single crystal growth, single crystal growth is required when loading seeds loaded at the bottom of a crucible are partially melted to obtain residual seeds of a predetermined size and a desired shape.
The quality of the single crystal is extremely sensitive to the size of the residual seed, and therefore, the size control of the residual seed is the core of a high-quality sapphire growth technique.
The bottom of the crucible, where the seeds are located, is cooled by the cooling plate, and therefore, is cooler than the rest of the crucible. Therefore, in the case of a growing apparatus using only one main heater, the maximum temperature of the main heater needs to be increased in the seeding process.
Finally, the increase in the maximum temperature of the main heater leads to an increase in production cost due to an increase in power consumption, and leads to deterioration of the heater and the refractory, thereby reducing the life. Further, the maximum temperature rise of the main heater increases the deformation of the crucible, and the graph limit decreases due to the temperature increase.
Furthermore, if the residual seed is controlled only by the main heater, the reproducibility of the size of the residual seed is reduced, and it is difficult to control the growth rate of the single crystal only by the main heater.
Korean laid-open patent publication No. 10-2011-0025716 (patent document 2) discloses a sapphire single crystal growth apparatus having a crucible for growing a single crystal from a seed crystal as a waste sapphire material melted in the furnace, in which a heating element for melting the sapphire waste material is disposed outside the crucible, a cooling means is provided at the bottom of the crucible to prevent complete melting of the seed crystal, and the heating element disposed outside the crucible is divided into a plurality of heating elements and operated independently to make the temperature of the crucible uniform in the horizontal direction.
In patent document 2, since the divided regions are heated by dividing one heating element heater and the cooling means is used only for preventing complete melting of the seed crystal, it is difficult to control the size of the residual seed with respect to the seed crystal disposed at the bottom of the crucible by only having the heating element heater, and the heating element is operated at the highest temperature, so that the above-described various problems can occur.
Documents of the prior art
Patent document
Patent document 1: korean laid-open patent publication No. 10-2011-
Patent document 2: korean laid-open patent publication No. 10-2011-
Disclosure of Invention
The present inventors have come to recognize that in the case of a sapphire single crystal growth apparatus of the bottom-seeded type, since a cooling plate is provided at the bottom of the crucible, energy (heat) of the lower portion of the crucible flows out to the lower portion through the cooling plate, and thus a method of effectively controlling the temperature of the lower portion of the crucible is required.
Accordingly, the present invention has been made keeping in mind the above problems occurring in the prior art, and an object of the present invention is to provide a sapphire single crystal growth apparatus and a sapphire single crystal growth method, in which an auxiliary heater surrounding a cooling plate is separately provided in addition to a main heater for raising the temperature of a hot zone (hot zone), and the flow rate of heat flowing out from a crucible through the cooling plate is controlled by the auxiliary heater, thereby precisely and easily controlling the size of residual seeds and the rate of crystal growth in a seeding step.
It is still another object of the present invention to provide an apparatus and a method for growing a sapphire single crystal, which can reduce power consumption by using an auxiliary heater to lower the maximum temperature of a main heater in a seeding process, reduce deterioration of the heater and a refractory to increase the life, and reduce deformation of a crucible to reduce the risk of accidents.
Another object of the present invention is to provide a sapphire single crystal growth apparatus in which, when a sapphire single crystal is grown by a vertical horizontal temperature gradient cooling method, a thickness of a zigzag resistance heater constituting a main heater is constant, and only a line width and an interval are adjusted to simultaneously impart a horizontal temperature gradient and a vertical temperature gradient to a crucible.
It is still another object of the present invention to provide a sapphire single crystal growth apparatus and a sapphire single crystal growth method, which can suppress propagation of defects into a crystal by optimizing the curvature and height of a residual seed.
In order to achieve the above object, a sapphire single crystal growth apparatus of the present invention includes: a refractory disposed inside the chamber and configured to insulate the inside of the chamber; a crucible arranged inside the refractory and loaded with sapphire single crystal seeds and sapphire raw materials in sequence at the bottom to realize growth of sapphire single crystal; a main heater disposed inside the refractory so as to surround the outside of the crucible, for raising the temperature of the hot zone and generating heat so as to generate a vertical temperature gradient and a horizontal temperature gradient inside the crucible; a cooling unit including a cooling plate in contact with the bottom of the crucible, for cooling the bottom of the crucible; and an auxiliary heater surrounding the cooling plate, the auxiliary heater controlling a flow rate of heat flowing out from the crucible through the cooling plate.
The main heater is set to a maximum temperature for the temperature rise of the molten hot zone of the loaded sapphire raw material and the seeding process of the sapphire single crystal seeds, and the auxiliary heater is maintained in a maximum power state until residual seeds of a predetermined size are obtained from the sapphire single crystal seeds.
The crucible has a bottom portion in a rectangular shape, the sapphire single crystal seed has a rectangular rod shape, an upper surface of the remaining seed has a curvature along a longitudinal direction, and a radius of curvature is set to be in a range of 200mm to 500 mm.
The height (H) of the residual seed/the height (H) of the single crystal seed satisfies H/H > 1/3.
The crucibles comprise a first crucible and a second crucible arranged inside the hot zone,
the first crucible and the second crucible each include: a bottom of rectangular form; a pair of P-surface parts connected to the front and rear surfaces of the four surfaces connected to the bottom part and inclined to open outward; and a pair of C-shaped face parts connected to two side surfaces of the four faces connected to the bottom part along a right angle direction, connected to the edge of the P-shaped face part, and having a trapezoidal shape.
The angle between the bottom and the P-face is larger than an interface angle at which a linear aging (linear) defect propagates, and when the diameter of the sapphire single crystal ingot is 6 inches or more, each of the pair of P-face includes at least one bent portion.
According to the present invention, single crystal growth is performed by only reducing the power of the auxiliary heater so that the maximum temperature of the main heater is not lowered.
The crucible includes at least one crucible or a first crucible and a second crucible disposed inside the chamber, and the main heater includes: a first P-surface heater and a second P-surface heater which are arranged in front of and behind the first crucible and the second crucible and are respectively connected with the first electrode bar and the second electrode bar; a first C-plane heater disposed on a side surface of the first crucible and electrically connected to one side edges of the first P-plane heater and the second P-plane heater through a connection member; and a second C-plane heater disposed on a side surface of the second crucible and electrically connected to the other edges of the first and second P-plane heaters through a connecting member.
The first P-side heater and the second P-side heater include: the lower part of the first path part is connected with the first electrode rod and the second electrode rod; a pair of second path portions extending in a vertical direction from the first path portions and branching to both sides; a pair of third path portions extending in a horizontal direction from respective upper ends of the pair of second path portions; and a pair of fourth path portions extending from the pair of third path portions in a lower direction, respectively, the first and second C-plane heaters including: a pair of fifth path parts connected with the first P-surface heater and the second P-surface heater and positioned at the two side edges; a pair of sixth path portions extending in the horizontal direction from respective upper ends of the pair of fifth path portions; a pair of seventh path portions extending in a downward vertical direction from respective end portions of the pair of sixth path portions; and an eighth path portion that connects lower ends of the pair of seventh path portions in the horizontal direction.
The main heater is configured such that a line width (H1) of the first path section and a line width (H3) of the eighth path section are different from a line width (H2) of the third path section and a line width (H4) of the sixth path section in order to provide a vertical temperature gradient, and the amount of heat generation is adjusted by a difference in impedance value.
The main heater increases the upper heat generation by making the line width (H2) of the third path portion and the line width (H4) of the sixth path portion smaller than the line width (H1) of the first path portion and the line width (H3) of the eighth path portion.
The main heater is configured such that a line width (L1) of the second path portion and a line width (L3) of the seventh path portion are different from a line width (L2) of the fourth path portion and a line width (L4) of the fifth path portion in order to provide a horizontal temperature gradient.
The cooling unit includes: a cooling plate for cooling the crucible by directly contacting with the lower surface of the crucible; and a water-cooled cooling unit disposed below the cooling plate for discharging heat. The cooling plate is made of Molybdenum (Molybdenum) or Molybdenum alloy material, and a first contact part contacting with the first crucible and a second contact part contacting with the second crucible can be respectively formed at the upper end of the cooling plate. The water-cooled cooling part is formed of a copper material forming a cooling water passage for circulating cooling water, and the cooling plates may be in direct contact with each other.
The auxiliary heater is composed of a front auxiliary heater and a rear auxiliary heater, the front auxiliary heater and the rear auxiliary heater are respectively arranged on the front surface and the rear surface of the cooling plate, and generate heat when power is applied, and the sapphire single crystal growth apparatus further comprises: a pair of connecting members for fixing both side end portions of the front auxiliary heater and the rear auxiliary heater; and a third electrode bar and a fourth electrode bar attached to the pair of connecting members and used for applying power. The auxiliary heater has a valve function of controlling the flow rate of heat flowing out to the lower part of the crucible through the cooling plate and the water-cooled cooling part, and the size of the residual seed of the sapphire single crystal seed mounted at the inner bottom of the crucible can be adjusted in the seeding process.
The first electrode rod and the second electrode rod are arranged on a straight line along the front-back direction of the crucible, the third electrode rod and the fourth electrode rod are arranged on a straight line along the left-right direction of the crucible, and 4 electrode rods are arranged at intervals of 90 degrees.
The invention also includes: a crucible supporting unit provided at a lower portion of the chamber to support the crucible, the crucible supporting unit including: a support plate disposed at a lower portion of the chamber; a support part which is arranged on the support plate in a height-adjustable manner and supports the lower surface of the crucible; and an inclination prevention part which is arranged on the supporting plate in a mode of adjusting the height and prevents the crucible from inclining by supporting the side surface of the crucible.
A duct for measuring the temperature using a high temperature for controlling the temperature of the main heater is formed in the chamber and the refractory, and a graphite plate for measuring the temperature at the temperature measuring position of the pyrometer is detachably attached to the inner surface of the refractory.
The tunnel allows a focal line F (focal line) of a Pyrometer (Pyrometer) to pass through a passage between the first crucible and the second crucible, and the temperature measuring graphite plate is detachably attached to an inner surface of the refractory facing the tunnel.
The sapphire single crystal growth method of another feature of the present invention utilizes a sapphire single crystal growth apparatus, the sapphire single crystal growth apparatus comprising: a crucible having a bottom in a rectangular shape; a main heater for simultaneously providing a horizontal temperature gradient and a vertical temperature gradient to the crucible; and an auxiliary heater provided so as to surround a cooling plate in contact with a bottom of the crucible, the method for growing a sapphire single crystal comprising: loading a sapphire material to be grown in the crucible, wherein a rod-shaped sapphire single crystal seed is mounted on the bottom of the crucible along the longitudinal direction; a temperature raising and seeding step of setting the main heater to a maximum temperature to simultaneously provide a horizontal direction temperature gradient and a vertical direction temperature gradient to the crucible to melt the loaded sapphire raw material until a residual seed of a predetermined size is obtained from the sapphire single crystal seed, and maintaining a maximum power state of the auxiliary heater; a single crystal growth step of growing a sapphire single crystal on the residual seed by reducing the power of an auxiliary heater so that the temperature of the main heater does not decrease; an annealing step of reducing thermal stress of the sapphire single crystal after the completion of the single crystal growth step by heating the auxiliary heater; and a cooling step of cooling the temperature of the main heater to normal temperature while maintaining the power of the auxiliary heater after the annealing step is finished.
The sapphire single crystal growth method of another feature of the present invention utilizes a sapphire single crystal growth apparatus, the sapphire single crystal growth apparatus comprising: a crucible having a bottom in a rectangular shape; a main heater for simultaneously providing a horizontal temperature gradient and a vertical temperature gradient to the crucible; and an auxiliary heater provided so as to surround a cooling plate in contact with a bottom of the crucible, the method for growing a sapphire single crystal comprising: loading a sapphire material to be grown in the crucible, wherein a rod-shaped sapphire single crystal seed is mounted on the bottom of the crucible along the longitudinal direction; a temperature raising and seeding step of setting the main heater to a maximum temperature to simultaneously provide a horizontal direction temperature gradient and a vertical direction temperature gradient to the crucible to melt the loaded sapphire raw material until a residual seed of a predetermined size is obtained from the sapphire single crystal seed, and maintaining a maximum power state of the auxiliary heater; a single crystal growth step of growing a sapphire single crystal on the residual seed by gradually reducing the maximum temperature of the main heater and the maximum power of the auxiliary heater at the same time; and a cooling step of cooling the temperature of the main heater to a normal temperature after the single crystal step is completed.
The method for growing a sapphire single crystal of the present invention further comprises an annealing step of reducing thermal stress of the sapphire single crystal after the end of the single crystal growing step by heating the auxiliary heater.
And controlling the power of the auxiliary heater to control the growth speed of the sapphire single crystal.
Further, according to an aspect of the present invention, there is provided a sapphire single crystal growth apparatus in which 2 crucibles are arranged in a hot zone, a main heater surrounds the 2 crucibles, lower portions of the 2 crucibles are connected in common to a cooling plate, and the cooling plate is controlled by an auxiliary heater surrounding the cooling plate, thereby simultaneously growing a sapphire single crystal using the 2 crucibles.
As described above, in the present invention, in addition to the main heater for raising the temperature of the raised hot zone (hot zone), the sub-heater surrounding the cooling plate is separately provided, and the flow rate of heat flowing out from the crucible through the cooling plate is controlled by the sub-heater, thereby precisely and easily controlling the size of the residual seeds and the growth rate of the crystals in the seeding process.
In the present invention, the maximum temperature of the main heater is lowered by using the auxiliary heater in the seeding step to reduce power consumption, the deterioration of the heater and the refractory is reduced to increase the life, and the deformation of the crucible is reduced to reduce the risk of accidents.
In addition, in the present invention, the reproducibility of the size of the residual seed is excellent and the residual seed can be easily controlled by using the auxiliary heater.
Further, in the present invention, when a sapphire single crystal is grown by the vertical horizontal temperature gradient cooling method, the thickness of the zigzag resistance heater constituting the main heater is constant, and only the line width and the interval are adjusted to simultaneously impart a horizontal temperature gradient and a vertical temperature gradient to the crucible.
That is, the main heater of the sapphire single crystal growth apparatus of the present invention is not required to adjust the thickness of the heater, but the line widths of the upper and lower heaters are adjusted to provide a vertical temperature gradient, and the line widths of the left and right heaters are adjusted to provide a horizontal temperature gradient, thereby making it possible to manufacture the heater very easily.
Further, the present invention provides a sapphire single crystal growth apparatus and a sapphire single crystal growth method, which can suppress propagation of defects into a crystal by optimizing the curvature and height of the residual seed, and can obtain a sapphire single crystal having excellent single crystal quality.
Drawings
Fig. 1 is a sectional view of a sapphire single crystal growth apparatus according to an embodiment of the present invention.
Fig. 2 is a diagram showing a method of measuring the temperature inside the chamber according to an embodiment of the present invention.
FIG. 3 is a perspective view of a main heater of the sapphire single crystal growth apparatus according to one embodiment of the present invention.
FIG. 4 is a top view of a P-side heater according to an embodiment of the invention.
Fig. 5 is a top view of a G-plane heater according to an embodiment of the invention.
Fig. 6 is a perspective view of an assembly in which a cooling unit and an auxiliary heater are assembled according to an embodiment of the present invention.
Fig. 7 is a side view of an assembly of a cooling unit and an auxiliary heater according to an embodiment of the present invention.
FIG. 8 is a side view showing a crucible supporting unit according to an embodiment of the present invention.
FIG. 9 is a perspective view of a crucible according to an embodiment of the present invention.
FIG. 10 is a cross-sectional view of a crucible according to an embodiment of the present invention.
Fig. 11 is a view showing ingot products and scrap portions cored in the C-axis direction when the crucible of the embodiment of the present invention is used.
Fig. 12 is a flowchart for explaining a sapphire single crystal growth method according to an embodiment of the present invention.
Fig. 13 is an enlarged cross-sectional view of the bottom portion of the crucible for explaining a method of controlling the shape of the residual seed when performing the sapphire single crystal growth according to an embodiment of the present invention.
FIG. 14 is a graph comparatively showing a single crystal growth curve based on the presence or absence of an auxiliary heater.
Fig. 15 is a graph showing comparison of the power input to the growth furnace in the seeding step with or without the auxiliary heater.
Fig. 16a and 16b are sectional photographs showing whether or not residual seeds are formed in the single crystal grown without using the auxiliary heater and with using the auxiliary heater when the same power is applied.
Detailed Description
Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings. In this process, the sizes, shapes, and the like of the constituent elements shown in the drawings are exaggerated for clarity and convenience of description. Also, terms specifically defined may be changed according to the intention or custom of a user, a referring person in consideration of the structure and action of the present invention. Definitions relating to such terms are defined throughout the present specification.
The growth of the sapphire single crystal of the present invention is explained based on the ingot growth by the Vertical horizontal temperature gradient cooling method (Vertical horizontal gradient Freezing), but other processes such as a heat exchange method by the bottom seeding method may be used.
In the vertical horizontal temperature gradient cooling method according to the present invention, a single crystal seed is fixed to the bottom of a crucible, an alumina material, which is a raw material of the sapphire single crystal, is filled in the crucible and melted, and then the crystal is grown by controlling the flow rate of heat flowing out to a cooling plate in contact with the bottom of the crucible while maintaining the vertical temperature gradient and the horizontal temperature gradient in the crucible by an auxiliary heater so as to solidify the remaining seed in the direction of the "a" axis as much as possible.
Fig. 1 is a sectional view of a sapphire single crystal growth apparatus according to an embodiment of the present invention.
Referring to fig. 1, a sapphire single crystal growth apparatus according to an embodiment of the present invention includes: a chamber 10 having an inner space; a refractory 20 disposed inside the chamber 10 and thermally insulating the inside of the chamber 10; a crucible 30 which is disposed inside the refractory 20 and into which alumina raw material is charged to grow the sapphire single crystal 60; a main heater 40 disposed inside the refractory 20 so as to surround the outside of the crucible 30, for raising the temperature of the hot zone 12 to generate heat so as to form an overall temperature gradient inside the crucible; a cooling unit 50 having a cooling plate 52 contacting a lower portion of the crucible 30 for adjusting the temperature of the crucible 30; and an auxiliary heater 82 surrounding the cooling plate 52 for controlling the flow rate of heat flowing out of the crucible 30 through the cooling plate 52.
The chamber 10 is not deformed by heat released from the refractory 20 under a high temperature condition of 2050 ℃ or lower at the melting point of the sapphire single crystal 60, and can be used in a vacuum or gas atmosphere.
Therefore, the chamber 10 uses a double chamber through which the refrigerant flows so as to cool the chamber 10 by the refrigerant cooling water, gas, or the like in order to prevent deformation by heat.
The refractory 20 functions as a heat insulator for preventing heat released from the main heater 40 from flowing out to the outside, and metals such as tungsten, molybdenum, carbon, and graphite felt, ceramics, and the like can be used as the material of the refractory 20.
The crucible 30 is formed of a metal material such as tungsten, molybdenum, iridium, or the like that does not melt under the 2050 ℃ temperature condition as the melting temperature of the alumina raw material when the sapphire single crystal 60 is grown by melting and then solidifying the alumina raw material.
The crucible 30 is vertically erected in the hot zone 12, and a sapphire single crystal seed 63 having a size allowing growth of the sapphire single crystal 60 is attached to the inner bottom of the crucible 30.
As shown in fig. 9 and 10, the crucible 30 includes: a rectangular bottom 32 on which a single crystal seed 63 is mounted; a pair of P-surface portions 34 connected to the front and rear surfaces having a long length among the four surfaces (sides) connected to the bottom portion 32, having the same length as the front and rear surfaces of the bottom portion 32, and inclined so as to open outward; and a pair of C-shaped surfaces 36 connected to both short side surfaces of the four surfaces (sides) of the bottom portion 32, and connected to the bottom portion 32 in a right angle direction, and having a width gradually increasing toward an upper side so that both side edges are connected to the edges of the P-shaped surface 34.
For example, the bottom portion 32, the P surface portion 34, and the C surface portion 36 are formed in a flat plate shape made of molybdenum (Mo), and may be joined to each other by Welding using Tungsten Inert Gas (TIG) Welding, for example.
As shown in fig. 10, each of the pair of P-surface portions 34 has a rectangular flat plate shape, and has an inclination angle θ that opens outward as the bottom portion 32 approaches the upper side direction.
The pair of C-shaped surface portions 36 are each in the form of a trapezoidal flat plate, and the width gradually increases toward the upper side.
As described above, in the overall shape of the crucible 30, the inner area of the lower portion is small, and the inner area of the upper portion is larger than that of the lower portion, so that the amount of the single crystal seeds 63 used can be minimized, and after the growth of the sapphire single crystal 60 is completed, as shown in fig. 11, coring is performed in the C-axis direction to produce ingot products 65 in the form of round rods, so that waste of remaining or discarded sapphire scraps (scrap) can be minimized.
In the case where the crucible is in a right hexahedral form, when the ingot product in the round bar form is cored along the C-plane, the scrap of the remaining portion of the sapphire ingot is large, resulting in a problem of serious waste, and on the contrary, in the crucible 30 of the present invention, as shown in fig. 11, when the ingot product 65 in the round bar form is manufactured along the C-axis, the scrap of the remaining portion Q of the sapphire ingot 60 can be minimized, and thus the waste of raw materials can be minimized.
Further, when the sapphire ingot is grown in the same time, since the ingot is grown in the same diameter and width in the case of the conventional crucible in the form of a rectangular parallelepiped or a cylindrical barrel, although it takes a long time, the area of the lower portion of the crucible 30 of the present invention is small, and the area thereof increases toward the upper side direction, so that the sapphire ingot can be grown rapidly, and productivity can be improved.
When the sapphire ingot 60 is grown in a single crystal seed, propagation of linear aging defects proceeds in the vertical direction of the solid-liquid interface in the point where the interface meets the crucible. Therefore, when a rectangular parallelepiped crucible is used, propagation of linear aging defects proceeds at an interface angle in the P-face direction where the solid-liquid interface contacts the bottom of the crucible, and when linear aging defects propagate to the outside of the sapphire ingot, there are no linear aging defects inside the crystal, or when the outside of the sapphire ingot propagates to the inside of the sapphire ingot, defects occur at corresponding positions.
In the present invention, as shown in fig. 10, the linear aging defect is prevented from propagating into the sapphire ingot by increasing the inclination angle θ formed by the bottom portion 32 and the P-face portion 34 as compared with the interface angle at which the linear aging defect propagates, and thus the linear aging defect of the sapphire ingot can be prevented.
Wherein the angle between the bottom portion 32 and the P-face portion 34 is inclined at an angle theta of 10 DEG & lttheta & lt 60 DEG, preferably 30 DEG & lttheta & lt 60 deg.
As described above, propagation of the linear aging defect proceeds from the solid-liquid interface, i.e., the point where the upper surface of the residual seed contacts the crucible, in the vertical direction of the interface, and therefore, it is preferable that the residual seed also becomes relatively small in the case of the small-diameter crucible. Therefore, in the case of a small-diameter crucible of less than 6 inches, the inclination angle θ between the bottom portion 32 and the P-face portion 34 is greater than 60 ° and less than 70 °, that is, 60 ° < θ < 70 °.
That is, the inclination angle θ between the bottom portion 32 and the P-face portion 34 needs to be larger than the interface angle at which the linear aging defect propagates, and when coring is performed along the C-axis to manufacture an ingot product in a round bar form, waste can be minimized.
The C-plane of the crucible 30 has a trapezoidal shape, and the crucible 30 has a structure suitable for manufacturing a 4-inch single crystal ingot 65, for example. However, when the diameter of the single crystal ingot is increased, the width of the upper end of the trapezoidal crucible is undesirably long.
Therefore, when a single crystal ingot product of 4 inches or more and 6 inches or less is produced, it is preferable to change the shape to a chamfered (chamfer) shape having a bent portion of 1 end to prevent the length of the upper portion of the crucible from becoming excessively long.
Further, it is preferable that when the height of the single crystal ingot is 200mm or more, that is, when an ingot of 8 inches is produced or when the thickness of the crucible is increased, the strength of Mo is lowered under a high temperature condition, and therefore, when an ingot of 8 inches or more is produced in order to prevent the crucible from being broken due to the stress concentration at the bent portion, the bent portion of 2 ends or more is introduced.
The crucible 30 is composed of the first crucible 30a and the second crucible 30b in such a manner as to increase the yield of the sapphire single crystal ingot 65, so that the sapphire single crystal growth can be simultaneously performed in both crucibles by one system.
A reflection plate 190 for reflecting heat radiated upward from the main heater 40 is provided at an upper portion of the main heater 40. That is, a reflection plate is provided on the inner surface of the upper part of the refractory, thereby preventing the heat generated in the main heater 40 from being reflected and leaking to the upper part of the chamber. Preferably, the reflection plate 190 is formed of a molybdenum material.
In order to control the temperature of the main heater 40, as shown in fig. 2, a pyrometer 150 is used to measure the temperature. The chamber 10 and the refractory 20 are formed with a duct 170 for measuring a temperature using the pyrometer 150.
The pyrometer 150 changes the measurement value according to the Emissivity (Emissivity) of the object to be measured due to its characteristics. Therefore, when the temperature of the main heater 40 of the graphite material is directly measured, the surface emissivity of the main heater 40 is changed by foreign substances (gas, adsorbed substances, dust, and the like) generated in the growth process, and thus an error occurs in the temperature measurement.
In the present embodiment, in order to reduce such temperature measurement errors, a graphite plate 160 for temperature measurement is separately installed inside the refractory 20 for measuring the temperature, and used as a temperature measurement position of the pyrometer 150.
The graphite plate 160 absorbs foreign matter less than the main heater 40, has a constant emissivity, has a quick response due to being adjacent to the main heater 40, is smaller in size than the main heater 40, is easy to replace, and can measure the temperature more precisely.
The crucible 30 is composed of a first crucible 30a and a second crucible 30b, and is disposed with a predetermined gap therebetween. Therefore, the focal line of the pyrometer 150 is caused to pass through the passage 180 between the first crucible 30a and the second crucible 30b by the port 170, the graphite plate 160 is attached to the inner surface of the refractory 40 opposite to the portion where the port 170 is formed, and the temperature is measured by the pyrometer 150.
As shown in fig. 3, the main heater 40 may be a resistance heater in a zigzag form made of a graphite material or a graphite compound.
The main heater 40 includes: a first P-side heater 42 connected to a first electrode rod 62 connected to a power supply; a second P-surface heater 44 disposed opposite to the first P-surface heater 42 and connected to the second electrode rod 64; and a first C-plane heater 46 and a second C-plane heater 48 connected to edges of the first P-plane heater 42 and the second P-plane heater 44, and disposed in a quadrangular shape and facing each other.
A first connection member 52 is provided between the first P-surface heater 42 and the first electrode rod 62, the first connection member 52 is fixed to the first P-surface heater 42 and connected to the first electrode rod 62, a second connection member 54 is provided between the second P-surface heater 44 and the second electrode rod 64, and the second connection member 54 is fixed to the second P-surface heater 44 and connected to the second electrode rod 64.
Since the first electrode rod 62 and the second electrode rod 64 connected to the external power supply are formed of a copper material, when the first P-surface heater 42 and the second P-surface heater 44 are directly connected to each other, they may be melted by the heat of the main heater 40. Therefore, the first P-surface heater 42 and the second P-surface heater 44 do not generate heat but have a high ability to receive heat, the first electrode rod 62 and the second electrode rod 64 are connected by the electrically connectable first connecting member 52 and second connecting member 54, and the first electrode rod 62 and the second electrode rod 64 are cooled by a water cooling method.
The first P-surface heater 42, the first C-surface heater 46, the second P-surface heater 44, and the second C-surface heater 48 are connected to each other at right angles by connecting members 56, and are formed in a rectangular shape as a whole.
The first P-surface heater 42 and the second P-surface heater 44 have the same shape, and the first C-surface heater 46 and the second C-surface heater 48 have the same shape.
As shown in fig. 4, the first P-surface heater 42 and the second P-surface heater 44 are in the form of flat plates having the same thickness, and include: a first path part 70, the lower part of which is connected with the first electrode bar 62 and the second electrode bar 64; a pair of second path portions 72 extending in the vertical direction at the first path portion 70 and branching to both sides; a pair of third path portions 74 extending in the horizontal direction at upper ends of the pair of second path portions 72, respectively; and a pair of fourth path portions 76 extending in the lower direction in the pair of third path portions 74.
As described above, the first P-plane heater 42 and the second P-plane heater 44 generate heat by forming the path portion in a zigzag form with the graphite material. Gaps of a predetermined interval are formed between the pair of second path portions 72 and the pair of fourth path portions 76, respectively.
As shown in fig. 3 and 5, the first C-plane heater 46 and the second C-plane heater 48 include: a pair of fifth path portions 80 connected to the first P-surface heater 42 and the second P-surface heater 44 and located at both side edges; a pair of sixth path portions 82 extending in the horizontal direction from the upper ends of the pair of fifth path portions 80; a pair of seventh path portions 84 extending in a downward vertical direction from respective end portions of the pair of sixth path portions 82; and an eighth path portion 86 that connects the lower ends of the pair of seventh path portions 84 in the horizontal direction.
The first C-plane heater 46 and the second C-plane heater 48 generate heat by forming a path in a zigzag shape with a graphite material. Gaps of a predetermined interval are formed between the pair of fifth path portions 80 and the pair of seventh path portions 84, and between the pair of seventh path portions 84, respectively.
The main heater 40 is a resistance heater made of a graphite material or a graphite compound so as to simultaneously provide temperature gradients in the vertical direction and the horizontal direction when melting the alumina raw material or cooling the molten alumina raw material, and has a flat plate shape with the same thickness.
In order to provide a vertical temperature gradient to the main heater 40, the line widths H1 and H3 of the first path portion 70 and the eighth path portion 86 are made different from the line widths H2 and H4 of the third path portion 74 and the sixth path portion 82, and the amount of heat generation is adjusted by the difference in resistance values.
That is, the line width H2 of the third path portion 74 and the line width H4 of the sixth path portion 82 are smaller than the line width H1 of the first path portion 70 and the line width H3 of the eighth path portion 86, and the upper heat generation increases, and the line width H1 of the first path portion 70 and the line width H3 of the eighth path portion 86 are increased than the line width H2 of the third path portion 74 and the line width H4 of the sixth path portion 82, and the lower heat generation increases.
In the main heater 40 of the present embodiment, in order to provide a temperature gradient so as to gradually increase the temperature in the horizontal direction with respect to the portion where the seed crystal is located, the line width H2 of the third path portion 74 and the line width H4 of the sixth path portion 82 are reduced as compared with the line width H1 of the first path portion 70 and the line width H3 of the eighth path portion 86, thereby increasing the upper heat generation.
The line widths L1 and L3 of the second and seventh path portions 72 and 84 are different from the line widths L2 and L4 of the fourth and fifth path portions 76 and 80, respectively, in order to provide the main heater 40 with a horizontal temperature gradient.
That is, heat generation at the edge of the crucible 30 increases as the line widths L2 and L4 of the fourth and fifth path portions 76 and 80 are shorter than the line widths L1 and L3 of the second and seventh path portions 72 and 84, respectively, and heat generation at the edge of the crucible decreases as the line widths L2 and L4 of the fourth and fifth path portions 76 and 80 increase than the line widths L1 and L3 of the second and seventh path portions 72 and 84, respectively.
As described above, in the present embodiment, the heater line width of the graphite material is adjusted to represent the temperature gradient in the vertical direction and the temperature gradient in the horizontal direction without adjusting the thickness of the heater, so that the heater can be manufactured very simply and a sapphire ingot of high quality can be manufactured.
As shown in fig. 6 and 7, the cooling unit 50 includes: a cooling plate 52 that is in direct contact with the lower surface of the crucible 30 to cool the crucible 30; and a water-cooled cooling unit 54 provided below the cooling plate 52 and cooling the cooling plate 52 by water cooling.
Since the cooling plate 52 is in direct contact with the crucible 30, it is made of molybdenum or a molybdenum alloy material having high strength, high ability to withstand high temperatures, and excellent heat transfer so as to prevent melting or damage by heat of the crucible 30.
The cooling plate 52 is in the form of a flat plate having a predetermined thickness, and has a first contact portion 52a contacting the first crucible 30a and a second contact portion 52b contacting the second crucible 30b formed at the upper end thereof. That is, when a pair of two crucibles is formed, the first contact portion 52a and the second contact portion 52b are formed on the upper surface of the cooling plate 52, so that the two crucibles can be cooled by one cooling plate.
The water-cooled cooling unit 54 is formed of a copper material having a cooling water passage through which cooling water circulates, and is attached to the lower portion of the cooling plate 52 to cool the cooling plate 52.
On the other hand, the cooling plate 52 includes a sub-heater portion 56, and the sub-heater portion 56 surrounds the cooling plate 52 and heats the cooling plate 52 so as to control the flow rate of heat flowing out from the lower portion of the crucible 30 through the cooling plate 52.
The sub heating part 56 includes: a pair of auxiliary heaters 82 disposed on the front and rear surfaces of the cooling plate 52, respectively, and generating heat when power is applied thereto; a pair of connection members 84 connecting both side end portions of the pair of auxiliary heaters 82 to each other; and a third electrode rod 86 and a fourth electrode rod 88 which are attached to the pair of connection members 84, respectively, and are used for applying power.
The pair of sub-heaters 82 are made of graphite material and have a zigzag pattern, and generate heat when power is applied thereto, and the heat generation temperature can be adjusted by controlling the current or power supplied to the sub-heaters 82.
The auxiliary heater 82 functions as a valve for controlling the flow rate of heat flowing out from the lower portion of the crucible 30 through the cooling plate 52 and the water-cooled cooling part 54, and adjusts the size of the residual seeds 63a of the sapphire single crystal seeds 63 mounted on the inner bottom portion of the crucible 30 during the seeding process, and the crystal growth rate of the sapphire single crystal 60 when the single crystal is grown.
The sub-heater 82 reduces the cooling time by reducing the difference in the temperature between the upper and lower sides of the single crystal ingot in the cooling step, and the temperature of the main heater 40 can be reduced by using the sub-heater 82 in the seeding step, thereby preventing damage to the heater and the refractory and reducing the overall power consumption.
The connection member 84 is formed of a material that can withstand the heat of the auxiliary heater 82 and can be connected to a power source, and the third electrode bar 86 and the fourth electrode bar 88 are copper materials and cooled by a water-cooling type.
The first electrode rod 62 and the second electrode rod 64 are arranged on a straight line along the front-back direction, the third electrode rod 86 and the fourth electrode rod 88 are arranged on a straight line along the left-right direction, and the 4 electrode rods 62, 64, 86, 88 are arranged at intervals of 90 degrees.
As shown in fig. 8, a crucible supporting unit 110 supporting the crucible 30 is provided at a lower portion of the chamber 10, and the crucible supporting unit 110 includes: a support plate 90 disposed at a lower portion of the chamber 10; a support 92 mounted to the support plate 90 in a height-adjustable manner, for supporting a lower portion of the crucible 30; and an inclination prevention portion 96 installed at an edge of the support plate 90 in a height-adjustable manner, for preventing inclination of the crucible 30 by supporting both sides of the crucible 30.
The support plate 90 is made of a graphite material having a predetermined thickness, and has a through hole formed at the center thereof, through which the cooling plate 52 in contact with the lower surface of the crucible 30 passes.
The support 92 is in the form of a bolt made of a graphite material, is screwed to the support plate 90 so as to be adjustable in height, and has a first carbonization prevention member 94 made of a tungsten material, which is in contact with the lower surface of the crucible 30 and prevents carbonization of the crucible 30, mounted on the upper surface thereof.
The anti-lean portion 96 includes: a support bar 120 combined with both side edges of the support plate 90 in a height adjustable manner, and formed of a graphite material; a head 122 mounted on the upper end of the support rod 120; the second carbonization preventing member 98 of tungsten material is attached to the head 122 and contacts the side surface of the crucible 30 to prevent carbonization of the crucible 30.
The crucible supporting unit 110 adjusts and supports the heights of the supporting portion 92 and the inclination prevention portion 96 according to the size and height of the crucible 30.
Hereinafter, a method for growing a sapphire single crystal by the sapphire single crystal growth apparatus of the present invention will be described with reference to fig. 12 to 16 b.
First, the sapphire single crystal growth apparatus of the present invention is provided with at least one crucible or a crucible 30 consisting of a first crucible 30a and a second crucible 30b inside a refractory 20, and the growth of the sapphire single crystal is controlled by a main heater 40, an auxiliary heater 56, and a cooling unit 50.
In this case, the first crucible 30a and the second crucible 30b are simultaneously in contact with the cooling plate 52, the cooling plate 52 is connected to the water-cooled cooling unit 54, and the cooling plate 52 is surrounded by the auxiliary heater 82. The auxiliary heater 82 functions as a valve for controlling the flow rate of heat flowing out from the first crucible 30a and the second crucible 30b to the lower portion of the crucible through the cooling plate 52 and the water-cooled cooling portion 54.
That is, the sub-heater 82 precisely adjusts the size of the residual seeds 63a of the sapphire single crystal seeds 63 attached to the inner bottom portions of the first crucible 30a and the second crucible 30b by controlling the flow rate of heat flowing out from the first crucible 30a and the second crucible 30b to the lower portion of the crucibles through the cooling plate 52 and the water-cooled cooling part 54 during the seeding process, and controls the growth rate of the sapphire single crystal by controlling the cooling function of the cooling plate 52.
Temperature raising and seeding step S11
In the step S11 of raising the temperature and seeding, the single crystal seed 63 is fixed to the bottom of the first crucible 30a and the second crucible 30b, and after the alumina material is loaded into the first crucible 30a and the second crucible 30b, the sapphire single crystal is grown by applying power to the main heater 40 to heat the inside of the hot zone 12 so as to form a vertical temperature gradient and a horizontal temperature gradient. In this case, the vertical temperature gradient and the horizontal temperature gradient of the main heater 40 are transferred to the first crucible 30a and the second crucible 30 b.
The single crystal seed 63 is a rod-shaped seed disposed along the bottom 32 of the first crucible 30a and the second crucible 30b, considering the point where the bottom 32 is rectangular.
At this time, the temperature of the main heater 40 is raised to a predetermined maximum temperature, for example, 2150 ℃, so that the alumina raw material loaded in the crucible is melted, and electric power is applied to the main heater 40 and simultaneously current or electric power is applied to the sub-heater 82 to reach the maximum power of the sub-heater 82, thereby starting the seeding process for the single crystal seeds 63.
The temperature of the main heater 40 and the power of the auxiliary heater 82 are maintained in the above state until the proper residual seeds 63a of the preset size are formed. For example, in the temperature raising and seeding step, the temperature of the main heater 40 is raised from the normal temperature to 2150 ℃ for 1 hour within 10 hours. In this case, the temperature rise time and the holding time are different depending on the size of the ingot being grown, and the temperature rise time is also increased as the size of the ingot is increased.
The temperature of the main heater 40 is measured by a single pyrometer 150 through a passage 180 between the first crucible 30a and the second crucible 30b from the aperture 170, thereby measuring the temperature of the temperature measuring graphite plate 160.
Hereinafter, a method of determining the length of the single crystal based on the height of the residual seed and the curvature of the residual seed according to the present invention will be described with reference to fig. 13.
When the sapphire single crystal 60 is grown, for high-quality single crystal growth, when a seeding process is performed, the single crystal growth is performed when the single crystal seeds 63 loaded on the bottom portion 32 of the crucible are partially melted to obtain residual seeds 63a of a predetermined size and a desired shape. The quality of the single crystal is very sensitive to the size of the residual seed 63a, and therefore, the size control of the residual seed 63a is very important.
Maximum radius of curvature of residual seed
The upper surface of the residual seed 63a has a curvature along the longitudinal direction, and the curvature radius R is preferably set to a range of 200mm to 500 mm. When the radius of curvature R12 is larger than 500mm, defects occur at both ends of the single crystal in the longitudinal direction, and the usable length decreases. When the curvature radius R10 is less than 200mm, the length of the residual seed 63a is too short.
Preferably, when the residual seed 63a has a radius of curvature of R14, the length of the residual seed 63a is set to 75% or more of the crucible length. With a smaller radius of curvature at both ends of the residual seed 63 a.
Minimum height of residual seed and maximum height of loaded single crystal seed
When a line along which the upper surface of the residual seed 63a extends meets the surface of the single crystal seed 63 to be loaded is denoted by H and the height of the single crystal seed 63 to be loaded is denoted by H, the height H of the residual seed 63 a/the height H of the single crystal seed 63 satisfies the following equation 1.
Mathematical formula 1
h/H＞1/3
If the H/H value is less than 1/3, the probability of propagation of defects from the interface of the residual seed 63a into the single crystal 60 increases sharply.
As the length of the crucible 30 increases, the height h of the residual seed 63a decreases by the radius of curvature R of the residual seed 63a, and thus the length of the crucible 30 is limited by the radius of curvature R and the height h of the residual seed 63 a.
The height H of the residual seed 63a cannot be greater than the height H of the single crystal seed, and therefore, in order to increase the height H of the residual seed 63a, the height H of the single crystal seed 63 needs to be increased.
However, since the seed growth performance is rapidly decreased when the height H of the single crystal seed 63 to be loaded is increased, the height H of the single crystal seed 63 is 70mm or less.
Limitation of crucible length and number of crucibles
As shown in fig. 11, when the coring processing is performed on the C axis of the sapphire single crystal 60, the length of the crucible 30 is increased by no means so as to obtain a long ingot 65, and if the above conditions are not satisfied, the single crystal quality is greatly reduced.
Therefore, it is more advantageous to simultaneously produce a plurality of sapphire single crystals 60 of an appropriate length than to produce one sapphire single crystal 60 of a long length. In view of such points, as shown in fig. 1, in the sapphire single crystal growth apparatus of the present invention, 2 first crucibles 30a and 2 second crucibles 30b are arranged in the hot zone 12, the main heater 40 surrounds the 2 crucibles, the lower portions of the 2 crucibles are connected in common to the cooling plate 52, the cooling plate 52 is controlled by the auxiliary heater 82, and sapphire single crystal growth is simultaneously performed using the 2 crucibles.
As described above, the main heater 40 controls the overall temperature of the hot zone 12, and the overall vertical temperature gradient and the overall horizontal temperature gradient in the crucible are formed based on the vertical temperature gradient and the horizontal temperature gradient of the main heater 40 itself.
The cooling water continues to circulate in a water-cooled cooling section 54 connected to a cooling plate 52 in contact with the bottom 32 of the crucible. For example, the temperature of the cooling water is maintained at about 30 ℃. The bottom 32 of the crucible in which the single crystal seed 63 is loaded maintains a temperature state below the melting point of sapphire in a manner that prevents the single crystal seed 63 from being completely melted.
In the present invention, the residual seed 63a size of the sapphire single crystal seed 63 attached to the bottom of the crucible has a predetermined size and profile by precisely controlling the flow rate of heat flowing out from the first crucible 30a and the second crucible 30b to the lower portion of the crucible through the cooling plate 52 and the water-cooled cooling part 54 by the power control of the auxiliary heater 82 during the seeding process.
Single crystal growth step S12
When alumina, which is a sapphire raw material loaded in the first crucible 30a and the second crucible 30b, is melted to form residual seeds 63a having a desired size, a single crystal growth step S12 is performed.
In the single crystal growth step S12, if the temperature of the main heater 40 and the power of the sub-heater 82 are gradually reduced at the same time, single crystal growth is performed from the residual seeds 63 a. In particular, if the power of the sub-heater 82 is gradually reduced from the highest power in the seeding step, the residual seeds 63a of the sapphire single crystal seeds 63 are not remelted, and single crystal growth is performed upward from the residual seeds 63a while maintaining the above state.
For example, the temperature of the main heater 40 is lowered to 1950 to 2050 ℃ at a cooling rate of 0.1 ℃/h until solidification is completed.
In this case, in the present invention, the single crystal growth is performed only by the power reduction of the auxiliary heater 82 without the temperature reduction of the main heater 40.
The solidification interface protrudes upward (Convex), so that, after the end of the single crystal growth, there is residual melt at the above-mentioned edge. In the present invention, as a process of completely solidifying the residual melt, the residual melt is completely solidified by rapidly lowering the temperature of the main heater 40 in a predetermined short time.
In this case, since the growth of the single crystal is completed, the auxiliary heater 82 is in a state where the power supply is terminated.
Cooling and annealing step S13
After the single crystal is completely grown, annealing for removing residual stress inside the single crystal is required as an essential process for preventing cracks (cracks) of the single crystal.
In the present invention, for example, the temperature of the main heater 40 is reduced to room temperature at a cooling rate of 0.1 to 10 ℃/min, and in this cooling step, the auxiliary heater 82 is heated during a predetermined annealing period to reduce the flow rate of heat flowing out from the first crucible 30a and the second crucible 30b to the lower portion of the crucibles through the cooling plate 52 and the water-cooled cooling unit 54. In the cooling process, the cooling rate of the main heater 40 is inversely proportional to the ingot size.
That is, the temperature of the upper portion of the single crystal 60 whose growth is completed is lowered, and the temperature of the lower portion is raised, thereby reducing the thermal stress of the single crystal 60 whose growth is completed.
After the predetermined annealing period, the temperature of the main heater 40 is cooled at a rapid cooling rate so that the cooling time of the single crystal can be reduced.
As a result, cooling to normal temperature is performed without defects such as cracks, twins (twins) that may occur during cooling.
Maximum temperature measurement of a main heater based on the presence or absence of a supplemental heater
In the case of having the auxiliary heater 82 controlling the cooling plate 52 separately from the main heater 40, as in the present invention, the height of the residual seeds 63a can be adjusted as the power of the auxiliary heater 82 is controlled. In this case, the maximum temperature of the main heater 40 for seed sowing, the ingot growth height of the time, and the input power are controlled together.
In the case of the present invention, in which the auxiliary heater 82 for controlling the cooling plate 52 independently from the main heater 40 is provided, and in the case of a general growth apparatus using only one main heater, the structure for measuring the maximum temperature of the main heater in the seeding step is shown in table 1.
TABLE 1
Auxiliary heater No (past) Is (the invention)
Highest temperature of main heater [ ° c] 2202 2080
In the case of a general growth apparatus using only one main heater, the bottom of the crucible where the seeds are located is cooled by a cooling plate, and thus, the temperature is lower than other positions of the crucible, and thus, the maximum temperature of the main heater needs to be increased in the seeding process.
However, in the case of the present invention having the sub-heater 82 in which the cooling plate 52 is controlled separately from the main heater 40, the flow rate of heat flowing out from the crucible to the lower portion of the crucible through the cooling plate 52 and the water-cooled cooling part 54 is reduced as power is supplied to the sub-heater 82 simultaneously with the driving of the main heater 40 in the seeding step, and therefore, as shown in table 1, the maximum temperature of the main heater 40 is lower than that of a general growth apparatus using only one main heater.
As a result, in the present invention, as the maximum temperature of the main heater is reduced, power consumption is reduced, deterioration of the heater and the refractory is reduced to increase the life, and deformation of the crucible is reduced to reduce the risk of accidents.
Presence or absence of auxiliary heater and single crystal growth curve
The temperature of the main heater 40 and the power reduction rate of the sub-heater 82 are adjusted for the desired growth rate of the single crystal. That is, the moving speed of the growth interface of the difference between the liquid phase and the solid phase inside the crucible decreases the power of the auxiliary heater 82 in a linear shape, and as shown in fig. 14, the height of the single crystal ingot increases at a prescribed speed with the growth time.
As shown in FIG. 14, in the present invention, as the power of the auxiliary heater 82 is controlled, the graph (dotted line) representing the height of the single crystal growth increases in a linear shape with the growth time, and the single crystal growth rate (inclination of the graph) can be constantly maintained.
In the case of having the sub-heater, as in the present invention, the single crystal growth speed (inclination of the graph) can be constantly controlled by controlling (reducing) only the power of the sub-heater 82, and in the case of using only the main heater having one temperature gradient function, the control of the remaining seed portion becomes difficult, so that it is difficult to constantly control the single crystal growth speed (inclination of the graph).
As a result, in the present invention, uniform single crystal growth is achieved within a certain growth time, and therefore, a high quality single crystal free from the occurrence of bubbles or the like is obtained.
However, in the case where the sub-heater 82 is not provided, in the case where the single crystal is grown using only one main heater, the growth rate cannot be in a linear form but in a graph (solid line) in a curved form during the growth time.
As described above, if a solid-line single crystal is grown at a nonlinear growth rate, particularly, when the inclination of the growth rate graph is large, bubbles occur.
Comparative test of input power in seeding process based on presence or absence of auxiliary heater
Fig. 15 is a graph showing comparison of electric power input in the seeding step based on the presence or absence of the sub-heater.
In the case of having both the main heater 40 and the sub-heater 82 as in the present invention, referring to the input power table (dotted line) of the seeding process and the input power table (solid line) of the general growth apparatus using only the main heater, the input power of the present invention having the sub-heater 82 is about 15 to 20% lower than that of the general growth apparatus not using the sub-heater.
Fig. 16a and 16b are photographs showing the cross-section of a single crystal grown by the use of an auxiliary heater and the cross-section of a single crystal grown by the use of an auxiliary heater when the same electric power is applied.
Referring to fig. 16a, when the same power as in the present invention is applied, the loaded tetragonal single crystal seeds are not melted but remain as they are in a general case without using the auxiliary heater. That is, in the case where the sub-heater is not provided, since the seeding is not smoothly performed in the same power, the maximum temperature of the main heater needs to be further increased in order to perform the seeding.
Referring to fig. 16b, in the case of the present invention using the auxiliary heater, a proper residual seed in a hemispherical shape is formed at the lower side of the single crystal grown due to the smoothness of the seeding.
While the present invention has been shown and described with reference to certain preferred embodiments, the present invention is not limited to the above-described embodiments, and various changes and modifications may be made by one of ordinary skill in the art to which the present invention pertains without departing from the spirit of the present invention.
Industrial applicability
The present invention is applicable to a sapphire single crystal growth apparatus and a sapphire single crystal growth method having an auxiliary heater surrounding a cooling plate separately from a main heater, and precisely and easily controlling the size of residual seeds and the rate of crystal growth in a seeding process.

Claims (22)

1. A sapphire single crystal growth apparatus is characterized in that,
the method comprises the following steps:
a refractory disposed inside the chamber and configured to insulate the inside of the chamber;
a crucible arranged inside the refractory and loaded with sapphire single crystal seeds and sapphire raw materials in sequence at the bottom to realize growth of sapphire single crystal;
a main heater disposed inside the refractory so as to surround the outside of the crucible, for raising the temperature of the hot zone and generating heat so as to generate a vertical temperature gradient and a horizontal temperature gradient inside the crucible;
a cooling unit including a cooling plate in contact with the bottom of the crucible, for cooling the bottom of the crucible; and
an auxiliary heater surrounding the cooling plate,
the auxiliary heater controls the flow rate of heat flowing from the crucible through the cooling plate.
2. The apparatus according to claim 1, wherein the main heater is set to a maximum temperature and the sub-heater is maintained in a maximum power state until a residual seed of a predetermined size is obtained from the sapphire single crystal seed, in order to heat the molten hot zone of the loaded sapphire raw material and perform a seeding process of the sapphire single crystal seed.
3. The sapphire single crystal growth apparatus of claim 2,
the crucible has a rectangular bottom, the sapphire single crystal seed has a rectangular rod shape,
the upper surface of the residual seed has a curvature along the longitudinal direction, and the curvature radius is set to be in the range of 200mm to 500 mm.
4. The sapphire single crystal growth apparatus as set forth in claim 2, wherein the height (H) of the residual seed/the height (H) of the single crystal seed satisfies H/H > 1/3.
5. The sapphire single crystal growth apparatus of claim 1,
the crucibles comprise a first crucible and a second crucible arranged inside the hot zone,
the first crucible and the second crucible each include:
a bottom of rectangular form;
a pair of P-surface parts connected to the front and rear surfaces of the four surfaces connected to the bottom part and inclined to open outward; and
and a pair of C-shaped face parts connected to the bottom part and the edge of the P-shaped face part in the right angle direction.
6. The sapphire single crystal growth apparatus of claim 5,
the angle between the base and the P-face is greater than the interface angle at which linear aging defects propagate,
when the diameter of the sapphire single crystal ingot is more than 6 inches, the pair of P-face parts respectively comprise at least one bending part.
7. The apparatus for growing a sapphire single crystal as set forth in claim 1, wherein the single crystal is grown by reducing only the power of the auxiliary heater so that the maximum temperature of the main heater is not lowered.
8. The sapphire single crystal growth apparatus of claim 1, wherein the cooling unit comprises:
a cooling plate for cooling the crucible by directly contacting with the lower surface of the crucible; and
and a water-cooled cooling part arranged at the lower part of the cooling plate and used for discharging heat.
9. The sapphire single crystal growth apparatus of claim 1,
the auxiliary heater is composed of a front auxiliary heater and a rear auxiliary heater, the front auxiliary heater and the rear auxiliary heater are respectively arranged on the front surface and the rear surface of the cooling plate, and heat is generated when power is applied,
the sapphire single crystal growth apparatus further includes:
a pair of connecting members for fixing both side end portions of the front auxiliary heater and the rear auxiliary heater; and
and a pair of electrode rods attached to the pair of connection members for applying a power source.
10. The sapphire single crystal growth apparatus of claim 1,
the crucibles comprise at least one crucible or a first crucible and a second crucible arranged inside the hot zone,
the main heater includes:
a first P-surface heater and a second P-surface heater which are arranged in front of and behind the first crucible and the second crucible and are respectively connected with the first electrode bar and the second electrode bar;
a first C-plane heater disposed on a side surface of the first crucible and electrically connected to one side edges of the first P-plane heater and the second P-plane heater through a connection member; and
and a second C-plane heater disposed on a side surface of the second crucible and electrically connected to the other edges of the first and second P-plane heaters through a connecting member.
11. The sapphire single crystal growth apparatus of claim 10,
the first P-side heater and the second P-side heater include:
the lower part of the first path part is connected with the first electrode rod and the second electrode rod;
a pair of second path portions extending in a vertical direction from the first path portions and branching to both sides;
a pair of third path portions extending in a horizontal direction from respective upper ends of the pair of second path portions; and
a pair of fourth path parts extending from the pair of third path parts in a lower direction,
the first C-plane heater and the second C-plane heater include:
a pair of fifth path parts connected with the first P-surface heater and the second P-surface heater and positioned at the two side edges;
a pair of sixth path portions extending in the horizontal direction from respective upper ends of the pair of fifth path portions;
a pair of seventh path portions extending in a downward vertical direction from respective end portions of the pair of sixth path portions; and
and an eighth path portion connecting lower ends of the pair of seventh path portions in a horizontal direction.
12. The sapphire single crystal growth apparatus of claim 11,
the main heater is configured such that a line width (H1) of the first path section and a line width (H3) of the eighth path section are different from a line width (H2) of the third path section and a line width (H4) of the sixth path section in order to provide a vertical temperature gradient,
the main heater is configured such that a line width (L1) of the second path portion and a line width (L3) of the seventh path portion are different from a line width (L2) of the fourth path portion and a line width (L4) of the fifth path portion in order to provide a horizontal temperature gradient.
13. The sapphire single crystal growth apparatus of claim 11, wherein the main heater increases the upper heat generation by making the line width (H2) of the third path portion and the line width (H4) of the sixth path portion smaller than the line width (H1) of the first path portion and the line width (H3) of the eighth path portion.
14. The sapphire single crystal growth apparatus of claim 1,
the chamber and the refractory further include:
a duct for measuring the temperature of the main heater;
a graphite plate for temperature measurement provided on an inner surface of the refractory facing the duct; and
a pyrometer, provided on an inner surface of the refractory, for measuring a temperature of the graphite plate for temperature measurement,
the temperature of the graphite plate for temperature measurement is recognized as the temperature of the main heater.
15. The sapphire single crystal growth apparatus of claim 6, wherein the angle (θ) between the bottom and the C-plane portion is in the range of 10 ° ≦ θ < 60 °, preferably 30 ° ≦ θ < 60 °.
16. The apparatus for growing a sapphire single crystal as set forth in claim 1, wherein a reflector plate reflecting heat radiated upward from the heater is disposed above the heater, and the reflector plate is attached to an inner surface of the upper refractory and is made of a molybdenum material.
17. The sapphire single crystal growth apparatus of claim 1,
also comprises a crucible supporting unit which is arranged at the lower part of the chamber and is used for supporting the crucible,
the crucible supporting unit includes:
a support plate disposed at a lower portion of the chamber;
a support part which is arranged on the support plate in a manner of adjusting the height and supports the lower surface of the crucible; and
and an inclination prevention part which is arranged on the supporting plate in a mode of adjusting the height and prevents the crucible from inclining by supporting the side surface of the crucible.
18. A sapphire single crystal growth method using a sapphire single crystal growth apparatus, the sapphire single crystal growth apparatus comprising:
a crucible having a bottom in a rectangular shape;
a main heater for simultaneously providing a horizontal temperature gradient and a vertical temperature gradient to the crucible; and
an auxiliary heater disposed to surround the cooling plate in contact with the bottom of the crucible,
the method for growing a sapphire single crystal is characterized by comprising the following steps:
loading a sapphire material to be grown in the crucible, wherein a rod-shaped sapphire single crystal seed is mounted on the bottom of the crucible along the longitudinal direction;
a temperature raising and seeding step of setting the main heater to a maximum temperature to simultaneously provide a horizontal direction temperature gradient and a vertical direction temperature gradient to the crucible to melt the loaded sapphire raw material until a residual seed of a predetermined size is obtained from the sapphire single crystal seed, and maintaining a maximum power state of the auxiliary heater;
a single crystal growth step of growing a sapphire single crystal on the residual seed by reducing the power of an auxiliary heater so that the temperature of the main heater does not decrease;
an annealing step of reducing thermal stress of the sapphire single crystal after the completion of the single crystal growth step by heating the auxiliary heater; and
and a cooling step of cooling the temperature of the main heater to a normal temperature while maintaining the power of the auxiliary heater after the annealing step is finished.
19. A sapphire single crystal growth method using a sapphire single crystal growth apparatus, the sapphire single crystal growth apparatus comprising:
a crucible having a bottom in a rectangular shape;
a main heater for simultaneously providing a horizontal temperature gradient and a vertical temperature gradient to the crucible; and
an auxiliary heater disposed to surround the cooling plate in contact with the bottom of the crucible,
the method for growing a sapphire single crystal is characterized by comprising the following steps:
loading a sapphire material to be grown in the crucible, wherein a rod-shaped sapphire single crystal seed is mounted on the bottom of the crucible along the longitudinal direction;
a temperature raising and seeding step of setting the main heater to a maximum temperature to simultaneously provide a horizontal direction temperature gradient and a vertical direction temperature gradient to the crucible to melt the loaded sapphire raw material until a residual seed of a predetermined size is obtained from the sapphire single crystal seed, and maintaining a maximum power state of the auxiliary heater;
a single crystal growth step of growing a sapphire single crystal on the residual seed by gradually reducing the maximum temperature of the main heater and the maximum power of the auxiliary heater at the same time; and
and a cooling step of cooling the temperature of the main heater to a normal temperature after the single crystal step is finished.
20. The method for growing a sapphire single crystal as claimed in claim 19, further comprising an annealing step of reducing thermal stress of the sapphire single crystal after the end of the single crystal growing step by heating the auxiliary heater.
21. The method for growing a sapphire single crystal as claimed in claim 18 or 19, wherein the sapphire single crystal growth rate is controlled by controlling the power of the auxiliary heater.
22. A sapphire single crystal growth apparatus, wherein 2 crucibles are arranged in a hot zone, a main heater surrounds the 2 crucibles, lower portions of the 2 crucibles are connected in common to a cooling plate, and the cooling plate is controlled by an auxiliary heater surrounding the cooling plate, thereby simultaneously growing a sapphire single crystal using the 2 crucibles.
CN201811358318.1A 2018-10-24 2018-11-15 Sapphire single crystal growth device and method Withdrawn CN111088520A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114737253A (en) * 2022-06-10 2022-07-12 太原彩源新材料科技有限公司 Single crystal furnace thermal field structure and method for growing large-size sapphire single crystal plate
CN114836820A (en) * 2022-04-28 2022-08-02 宁夏中欣晶圆半导体科技有限公司 Method for improving heavily phosphorus-doped low-resistance rod shaping rate
CN115029771A (en) * 2022-07-13 2022-09-09 北京铭镓半导体有限公司 Crucible adhesion preventing method for color gem crystal growth crucible by VGF method
CN115044962A (en) * 2022-07-13 2022-09-13 北京铭镓半导体有限公司 VGF method colored precious stone crystal growth crucible lid

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101580962A (en) * 2009-06-22 2009-11-18 上虞晶盛机电工程有限公司 Improved structure of heater of czochralski crystal growing furnace
CN101962800A (en) * 2010-10-09 2011-02-02 王楚雯 Device for producing single crystal ingot by directional solidification method
CN102127803A (en) * 2011-03-08 2011-07-20 中国科学院上海硅酸盐研究所 Growth method of rectangular specially-shaped sapphire crystal
KR20130035025A (en) * 2011-09-29 2013-04-08 비아이 이엠티 주식회사 Apparatus for growing sapphire single crystal and cooling supporter using thereof
CN103710741A (en) * 2012-10-05 2014-04-09 Biam株式会社 Single crystal growth device and method
CN104357906A (en) * 2014-11-21 2015-02-18 江南大学 Multi-crucible three-dimensional sapphire single crystal growing device
CN106978628A (en) * 2009-09-05 2017-07-25 科里斯科技有限公司 The method and apparatus of growing sapphire monocrystalline

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5526666B2 (en) 2009-09-08 2014-06-18 国立大学法人信州大学 Sapphire single crystal manufacturing equipment

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101580962A (en) * 2009-06-22 2009-11-18 上虞晶盛机电工程有限公司 Improved structure of heater of czochralski crystal growing furnace
CN106978628A (en) * 2009-09-05 2017-07-25 科里斯科技有限公司 The method and apparatus of growing sapphire monocrystalline
CN101962800A (en) * 2010-10-09 2011-02-02 王楚雯 Device for producing single crystal ingot by directional solidification method
CN102127803A (en) * 2011-03-08 2011-07-20 中国科学院上海硅酸盐研究所 Growth method of rectangular specially-shaped sapphire crystal
KR20130035025A (en) * 2011-09-29 2013-04-08 비아이 이엠티 주식회사 Apparatus for growing sapphire single crystal and cooling supporter using thereof
CN103710741A (en) * 2012-10-05 2014-04-09 Biam株式会社 Single crystal growth device and method
CN104357906A (en) * 2014-11-21 2015-02-18 江南大学 Multi-crucible three-dimensional sapphire single crystal growing device

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114836820A (en) * 2022-04-28 2022-08-02 宁夏中欣晶圆半导体科技有限公司 Method for improving heavily phosphorus-doped low-resistance rod shaping rate
CN114836820B (en) * 2022-04-28 2023-11-21 宁夏中欣晶圆半导体科技有限公司 Method capable of improving overall bar rate of heavily-doped phosphorus low resistance
CN114737253A (en) * 2022-06-10 2022-07-12 太原彩源新材料科技有限公司 Single crystal furnace thermal field structure and method for growing large-size sapphire single crystal plate
CN114737253B (en) * 2022-06-10 2022-11-04 太原彩源新材料科技有限公司 Single crystal furnace thermal field structure and method for growing large-size sapphire single crystal plate
CN115029771A (en) * 2022-07-13 2022-09-09 北京铭镓半导体有限公司 Crucible adhesion preventing method for color gem crystal growth crucible by VGF method
CN115044962A (en) * 2022-07-13 2022-09-13 北京铭镓半导体有限公司 VGF method colored precious stone crystal growth crucible lid

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