KR101639627B1 - Sapphire single crystal growing apparatus and method using of cruciable supporter - Google Patents

Sapphire single crystal growing apparatus and method using of cruciable supporter Download PDF

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KR101639627B1
KR101639627B1 KR1020150126285A KR20150126285A KR101639627B1 KR 101639627 B1 KR101639627 B1 KR 101639627B1 KR 1020150126285 A KR1020150126285 A KR 1020150126285A KR 20150126285 A KR20150126285 A KR 20150126285A KR 101639627 B1 KR101639627 B1 KR 101639627B1
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crucible
single crystal
support
sapphire single
sapphire
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Korean (ko)
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윤영권
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에스엠엔티 주식회사
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02518—Deposited layers
    • H01L21/02587—Structure
    • H01L21/0259—Microstructure
    • H01L21/02598—Microstructure monocrystalline
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02612—Formation types
    • H01L21/02617—Deposition types
    • H01L21/02636—Selective deposition, e.g. simultaneous growth of mono- and non-monocrystalline semiconductor materials
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/22—Diffusion of impurity materials, e.g. doping materials, electrode materials, into or out of a semiconductor body, or between semiconductor regions; Interactions between two or more impurities; Redistribution of impurities
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/324—Thermal treatment for modifying the properties of semiconductor bodies, e.g. annealing, sintering

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Abstract

The present invention relates to a sapphire single crystal growth apparatus using a crucible support and a sapphire single crystal growth chamber using the same. At least one crucible located inside the furnace, wherein the sapphire raw material is melted and a single crystal is grown from the seed crystal; A heating element disposed outside the crucible and heating the crucible; And a crucible supporter provided on the bottom and sides of the crucible.
It is an object of the present invention to simultaneously grow a large sapphire single crystal from a plurality of crucibles and to prevent deformation of the crucible during crystal growth and to improve yield and to arrange a plurality of crucibles in a growth furnace to simultaneously grow multiple sapphire single crystals A sapphire single crystal growth apparatus and a growth method using the same, which economically and efficiently increase the productivity.

Description

TECHNICAL FIELD The present invention relates to a sapphire single crystal growth apparatus using a crucible support, and a sapphire single crystal growth method using the same. BACKGROUND ART < RTI ID = 0.0 >

The present invention relates to a sapphire single crystal growth apparatus and a growth method thereof, and more particularly, to a sapphire single crystal growth apparatus and a method for growing the same by a supporting means of a crucible so that a quadrangular crucible can maintain its shape during a crystal growth time, And a sapphire single crystal growth method using the same. BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a sapphire single crystal growth apparatus using a crucible support.

GaN semiconductors have been used to fabricate blue or white LEDs which have been recently invented. In principle, GaN monocrystalline wafers should be used as substrates for growing GaN semiconductors by CVD. However, it is difficult to grow GaN monocrystals, so GaN monocrystal growth methods that can be practically used have not been developed.

On the other hand, Nakamura of Japan made blue LED by growing GaN single crystal on sapphire wafer, and succeeded in practical use of blue LED. In recent 20 years, many crystal growth scholars have tried to grow GaN monocrystals, but economical growth methods have not been developed. Therefore, it is natural that sapphire (Al 2 O 3 ) monocrystalline wafers should be used to manufacture blue or white LEDs, and the demand is increasing.

Recently, there has been a move to use sapphire as a cover glass material of a smart phone by using the excellent hardness and light transmittance of sapphire. If applied to smart phones, sapphire demand will surge and technology development for mass production and cost reduction should follow.

The sapphire single crystal can be grown by a number of growth methods such as Bernoulli's method, hydrothermal method, chalcoglossus method, heat exchange method, keyropulosic method, EFG method and the like. The heat exchange method and the key pull-down method can be used. In order to cope with the increase in demand in the conventional sapphire growth method, it is essential to increase the crystal size in the productivity improvement method aiming at mass production. However, in order to grow a large crystal, it is inevitable to extend the crystal growth time and the cooling time, It is not possible to improve the productivity as expected and it is faced with the difficulty of developing a high technology to secure the quality of the crystal.

In order to overcome the above problems and improve productivity, it is indispensable to increase the utilization factor of the material by making the shape of the crystal square, and to simultaneously grow a plurality of single crystals.

In Korean Patent No. 10-1229984, in order to grow a single crystal having a long length in the horizontal direction in a vertical direction and to produce a large single crystal in a short time, a heating element arranged outside the crucible is arranged in a plurality of divided states The present invention provides a sapphire single crystal growing apparatus which is operated independently and provides a method of uniformizing the temperature in the horizontal direction inside the growth furnace.

Also, in Korean Patent No. 10-1196445, when a plurality of crucibles are placed in a single thermosensitive body, it is possible to prevent the heat from being radiated directly from the heat-generating body of the crucible, thereby ensuring temperature uniformity in the longitudinal direction, Since the temperature difference generated in the crucible is divided into the crucible having a smaller temperature difference, it is possible to grow a plurality of single crystals of relatively good quality by preventing the temperature difference in the crucible from being generated.

Crucibles used for single crystal growth of high temperature molten oxides such as sapphire use high melting point metals such as Ir, Mo and W which do not react with alumina at the crystal growth temperature. However, in order to grow the sapphire single crystal, a high temperature of 2000 DEG C or more is required, and even if the high melting point metal is used, the strength is lowered at a high temperature of 2000 DEG C or more, so that the sapphire single crystal can easily be deformed. Therefore, in most crystal growth methods industrially producing sapphire single crystals such as the keyless pull method, the chalcogallery method and the heat exchange method, it is natural to use a circular crucible. By using a circular crucible, even a comparatively thin thickness, Which can best withstand the deformation of

It is difficult to make the shape of the crucible circular and it is most economical and feasible to arrange the rectangular crucibles in a row if many crucibles are placed inside the growth furnace to improve the productivity. There is a problem that it is very difficult to avoid the crucible from being deformed.

Korean Registered Patent No. 10-1196445 (Registration date: October 25, 2012) Korean Patent Publication No. 10-2011-0025716 (Published Date: March 11, 2011)

The sapphire single crystal growth apparatus using the crucible support according to the present invention and the sapphire single crystal growth method have the following problems.

First, the present invention is to provide a sapphire single crystal growing apparatus and method for growing large-sized sapphire single crystals simultaneously from a plurality of crucibles and preventing deformation of the crucible during crystal growth.

Second, the present invention aims to provide an economical and efficient sapphire single crystal growth apparatus which improves the yield and dramatically increases productivity by arranging a plurality of crucibles in a growth furnace and simultaneously growing a plurality of sapphire single crystals, and a growth method using the same.

The present invention has been made in view of the above problems, and it is an object of the present invention to provide an apparatus and method for controlling the same.

A first aspect of the present invention for solving the above-mentioned problems is a furnace comprising: a furnace; At least one crucible located inside the furnace, wherein the sapphire raw material is melted and a single crystal is grown from the seed crystal; A heating element disposed outside the crucible and heating the crucible; And a crucible support provided on the bottom and sides of the crucible.

The crucible may further include a cooling unit connected to the seed crystal located at the bottom of the crucible and extending to the bottom of the crucible bottom. The seed crystal is connected to the melt contained in the crucible, It is preferable to further include a pulling rod disposed at an upper portion of the crucible to grow crystals in a downward direction from the upper surface of the post-melt.

Preferably, the crucible and the crucible support have a quadrangular cross section and are spaced apart from each other. The crucible support includes: a bottom support disposed outside the crucible bottom; And four side supports provided outside the side surface of the crucible, wherein the bottom support and the side supports are assembled and disassembled.

Preferably, the crucible support is made of a material selected from the group consisting of tungsten, molybdenum, tantalum and alloys thereof, ceramics or graphite, and a reinforcing plate or a spacer member is provided between the crucible and the crucible support, Minimizing the area and inhibiting the reaction.

In addition, it is preferable that the reinforcing plate or the spacer member is made of a material selected from the group consisting of tungsten, molybdenum, tantalum and alloys thereof, and the spacer member has a plurality of spacing pins uniformly spaced from the crucible, And a pin-shaped member disposed at an interval.

The pin-shaped member is preferably made of a material selected from the group consisting of tungsten, molybdenum, tantalum and alloys thereof. The reinforcing plate provided between the bottom of the crucible and the crucible support includes a plurality of plate- And a plurality of spacers disposed between the bottom of the crucible and the crucible support and spaced apart from the bottom of the crucible support by a plurality of spaced apart spaced apart spacers .

It is preferable that the spacing pins are formed by forming grooves in the bottom of the crucible supporter and inserting the grooves into the grooves, and the multiple support plate is made of a material selected from the group consisting of tungsten, molybdenum, tantalum and alloys thereof , And a structure in which different materials are alternately stacked.

A second aspect of the present invention is to provide a sapphire single crystal growth apparatus that uses the above-described sapphire single crystal growth apparatus to shield radiant heat directly from a heating element and to block foreign substances penetrating into the crucible, melt the raw material of the sapphire, And growing the sapphire single crystal on the sapphire substrate.

The sapphire single crystal growth apparatus using the crucible support according to the present invention and the sapphire single crystal growth method using the same have the following effects.

First, the present invention can use a quadrangular crucible having a thin thickness, which is very vulnerable to deformation at a high-temperature sapphire single crystal growth temperature, thereby enabling a plurality of crucibles to be arranged and grown simultaneously in the growth furnace. And provides a growth method using the same.

Second, since the thickness of crucible can be reduced, the present invention can reduce the production cost of a single crystal of sapphire by reducing the cost of a crucible used as a disposable consumable, which greatly affects the cost, and a growth method using the same to provide.

Third, the present invention can be applied to a circular crucible, and provides an economical and efficient sapphire single crystal growing apparatus and a growth method using the same, wherein the economic effect is doubled as the size of a crucible and the size of a single crystal to be grown grow.

The effects of the present invention are not limited to those mentioned above, and other effects not mentioned can be clearly understood by those skilled in the art from the following description.

1 is a plan view showing a configuration of a sapphire single crystal growing apparatus according to an embodiment of the present invention.
FIG. 2 is a diagram illustrating a configuration of a sapphire single crystal growth apparatus having multiple support plates according to another embodiment of the present invention. FIG.
3 is a diagram illustrating a configuration of a sapphire single crystal growth apparatus having multiple support plates and spacing fins according to another embodiment of the present invention.
4 is a diagram illustrating a configuration of a sapphire single crystal growing apparatus according to a key pull-down method as another embodiment of the present invention.

Hereinafter, embodiments of the present invention will be described with reference to the accompanying drawings so that those skilled in the art can easily carry out the present invention. It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the spirit or scope of the invention. Wherever possible, the same or similar parts are denoted using the same reference numerals in the drawings.

The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The singular forms as used herein include plural forms as long as the phrases do not expressly express the opposite meaning thereto.

Means that a particular feature, region, integer, step, operation, element and / or component is specified and that other specific features, regions, integers, steps, operations, elements, components, and / It does not exclude the existence or addition of a group.

All terms including technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Predefined terms are further interpreted as having a meaning consistent with the relevant technical literature and the present disclosure, and are not to be construed as ideal or very formal meanings unless defined otherwise.

Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the drawings.

FIG. 1 is a plan view showing a structure of a sapphire single crystal growing apparatus according to an embodiment of the present invention. FIG. 2 is a view showing another example of a sapphire single crystal growing apparatus having a multiple support plate 535 according to another embodiment of the present invention. 3 is a diagram illustrating a configuration of a sapphire single crystal growth apparatus having multiple support plates 535 and spacing fins 570 according to another embodiment of the present invention. As another embodiment, there is shown an example of a structure of a sapphire single crystal growing apparatus by the key pull-down method.

Figs. 2 to 4 illustrate the structures of the crucible 200 and the crucible supporter 400, which illustrate examples 1 to 3, and show a part of the structure of a sapphire single crystal growing apparatus.

1, a sapphire single crystal growth apparatus according to an embodiment of the present invention includes a furnace 100; At least one crucible (200) located inside the furnace (100), in which the raw material of the sapphire is melted and a single crystal is grown from the seed crystal; A heating element 300 disposed outside the crucible 200 and heating the crucible 200; And a crucible supporter 400 installed on the bottom and side surfaces of the crucible 200.

As shown in FIG. 1, in the embodiment of the present invention, one or more quadrangular crucibles 200 are used. The crucibles 200 are held at a high temperature for a long period of time and maintained at a high temperature. The present invention also provides a device for growing a plurality of sapphire single crystals having excellent quality and a growth method using the device by providing a crucible supporting means for cutting off foreign matter penetrating into the sapphire substrate.

In one embodiment of the present invention, a sapphire single crystal growth apparatus in which one or a plurality of rectangular crucibles 200 are disposed is manufactured, and a crucible supporter 400 using high purity graphite or tungsten, It was confirmed that the shape of the crucible 200 could be maintained until the growth was completed and the sapphire single crystals of good quality could be grown.

In the embodiment of the present invention shown in Fig. 2, the furnace 100 is heated from the surroundings so that the internal temperature is raised above the melting temperature of the raw material of the crystal; At least one crucible (200) located inside the furnace (100) and maintaining the melt while the raw material is melted and the single crystal is grown; A plurality of heat generating elements 300 divided into a plurality of parts arranged outside the crucible 200 and heating the crucible 200; And a crucible support 400 installed outside and on the bottom of the crucible 200. The crucible 200 supports the crucible 200 and shields the crucible 200 and the crucible support 200 from external foreign substances, And a reinforcing plate 500 installed on the bottom and side surfaces of the crucible.

The sapphire single crystal growth apparatus according to an embodiment of the present invention may include a temperature control system including a temperature sensor, a temperature controller, and a power control device for providing electric power for obtaining a desired temperature from the heating element 300 (Not shown)

2 and 3, the seed crystals are placed on the bottom of the crucible 200 and placed on the bottom of the crucible 200 to grow crystals from the bottom of the crucible 200 As shown in the embodiment of FIG. 4, the seed crystal is brought into contact with the surface of the melt contained in the crucible 200, and then the upper surface of the melt An embodiment of a sapphire single crystal growth apparatus including a pulling rod 700 disposed on the crucible 200 to grow crystals in a downward direction is possible.

In the embodiment of the present invention, as shown in Fig. 1, four crucibles 200 may be arranged in a row in the furnace 100, but four or more crucibles 200 (four to twenty ) Crucibles 200 may be arranged in a line. Further, the cooling means 600 may be disposed for each crucible 200, and can be individually controlled independently, or can be integrally controlled.

A crucible 200 used in a sapphire single crystal growth apparatus according to an embodiment of the present invention is a crucible 200 for melting a raw material and containing a melt while maintaining its shape at a high temperature for a long time, Can be used. In addition, the crucible 200 may be made of a material selected from the group consisting of tungsten, molybdenum, tantalum, and alloys thereof. That is, tungsten, molybdenum, or an alloy thereof is used as a material of the crucible 200 for commercial sapphire single crystal growth. In addition, it is also possible to use a metal or an alloy made of at least one of high melting point metal as a material.

Here, the high melting point metal of 2000 ° C or higher refers to a metal having a high melting point, and tungsten (3,400 ° C), rhenium (3,147 ° C), tantalum (2,850 ° C), molybdenum (2,620 ° C), hafnium Belongs.

It is well known that metal materials are easily deformed due to their low strength at high temperatures, and even tungsten and molybdenum can easily be deformed with a small force at a high temperature of 2000 ° C or more. In order to prevent deformation of the crucible 200, a method of making the shape of the crucible 200 into a vertical cylindrical shape is preferable. Therefore, the crucible 200 for the majority of single crystal growth as well as sapphire is generally designed in a cylindrical shape .

Therefore, as shown in FIG. 1, when a hexagonal crucible 200 having a rectangular cross section is applied so that a plurality of crucibles 200 can be efficiently disposed on the furnace 100 and a single crystal can be grown in a large amount, It is not an easy task. For example, molybdenum crucible 200 containing 7 kg of melt was not able to be used due to severe deformation even when the thickness was set to 10 mm in order to grow a 120 × 120 × 120 mm cubic sapphire single crystal.

Of course, by welding a reinforcing material to the outside of the crucible 200, it is possible to maintain a certain degree of shape, but if the size of the crucible 200 is increased and the weight of the melt to be accommodated is increased to several tens of kilograms, It is obvious that it will not be a supporting method.

Therefore, in order to support the hexagonal crucible 200 for growing a sapphire single crystal having a large rectangular shape, a crucible 200 having a high-temperature strength is formed on the outside of the crucible 200 And a crucible support 400 of a crucible.

In addition, a ceramic material or graphite having a high melting point may be used as the material of the crucible support 400 applied to the embodiment of the present invention. However, since a refractory metal such as tungsten or a high purity isotropic graphite is used as the heating element 300 for growing sapphire single crystal, a sapphire single crystal growth furnace or a furnace 100 has a vacuum or an inert atmosphere Therefore, materials that easily volatilize in the above atmosphere can not be used.

The high purity graphite does not have a large strength as compared with the metal at room temperature, but has a feature of increasing the strength at a high temperature, which is suitable for the use of the crucible support 400 applied to the embodiment of the present invention. However, since graphite can react with tungsten or molybdenum used as crucible 200 at a high temperature to form a compound, there is a problem that means for suppressing the reaction must be followed.

In the sapphire growth furnace in which the graphite is used as the heating element 300 and the heat insulating material, volatilization of molybdenum and graphite used as materials of the crucible 200 at a high temperature is generated and tends to react with each other. Therefore, in order to suppress the reaction between the crucible 200 and the graphite (graphite), an inert gas is injected to lower the degree of vacuum, thereby suppressing the reaction with the crucible 200 due to the volatilization of the graphite. Therefore, in order to use the graphite crucible support 400 to support the molybdenum crucible 200, it is necessary to effectively suppress the reaction between the crucible 200 and the volatile carbon.

Therefore, in the embodiment of the present invention, the following apparatus and method are provided as means for suppressing the reaction of the molybdenum crucible 200 and the crucible support 400 made of graphite.

As shown in FIG. 2, a refractory metal reinforcing plate 500 is installed between the molybdenum crucible 200 and the graphite crucible support 400. For example, by using the reinforcing plate 500 made of tungsten, the crucible 200 and the graphite crucible support 400 are prevented from directly contacting and reacting with each other.

When the crucible 200 and the crucible supporter 400 are in direct contact with each other without using the above method, the crucible 200 reacts with the crucible 200 support 400 to melt the crucible 200, However, since the tungsten reinforcing plate 500 is inserted between the crucible 200 and the crucible support 400 as described above, melting of the crucible 200 is prevented and the sapphire single crystal can be efficiently grown .

2, in the embodiment of the present invention, a multi-support plate 535 structure in which different refractory metal reinforcing plates 500 are stacked between the molybdenum crucible 200 and the graphite crucible support 400 is stacked I suggest. For example, a triple high melting point plate composed of tungsten, molybdenum, and tungsten plate is inserted between the crucible 200 and the graphite crucible support 400 so that the carbon component from the graphite crucible support 400 is crystallized in the crucible 200 As shown in FIG.

In the case of using the triple high melting point reinforcing plate 500, not only the physical penetration of the carbon component is delayed but also the reaction proceeds in one direction due to the difference in chemical potential between the plates There is an effect of suppressing it.

3, in the embodiment of the present invention, the crucible supporter 400 is composed of a bottom support body provided outside the bottom of the crucible 200 and four side support members provided outside the crucible 200 side surface A plurality of support plates 535 having a plurality of plate-shaped supports laminated between the bottom support and the crucible 200 and a plurality of support plates 535 spaced apart from each other such that the bottoms of the multiple support plates 535 and the crucible support 400 are spaced apart (Not shown).

That is, a structure is proposed in which a groove is formed in the bottom of the graphite crucible support body 400 and a separating pin 570 made of tungsten is formed to support the crucible 200. In this case, since the load is concentrated on the tungsten spacing pin 570 by the weight of the crucible 200, the thickness, number, or position of the spacing pin 570 required can be adjusted according to the thickness of the crucible 200 and the weight of the raw material . However, it is also important that the location where the crucible 200 and the spacing pin 570 contact with each other is different from other places, so that the placement of the crucible 200 so as to exclude the bad influence on the quality due to the temperature difference as much as possible .

3, in the embodiment of the present invention, in order to suppress the reaction between the crucible 200 made of molybdenum and the crucible support 400 made of graphite, a reinforcing plate 500 made of tungsten And the spacer 550 made of molybdenum is installed on the upper surface of the crucible support 400 to effectively prevent the carbon component of the crucible supporter 400 from penetrating into the molybdenum crucible 200, A sapphire single crystal growing apparatus and a growth method capable of growing a sapphire single crystal having a square shape with excellent quality are provided.

Unlike the case of using the crucible supporter 400 made of graphite, when the ceramic material is used as the material of the crucible supporter 400, the molybdenum crucible 200 is not reacted with the molybdenum crucible 200, 200 and the crucible support 400, sapphire monocrystalline growth can be performed without using any means. Ceramic materials that can serve as effective crucible supports 400 include partially stabilized zirconia, calcia, magnesia, boron nitride, Fully of partially stabilized zirconia (Calcia, Magnesia, Boron Nitride, Boron Carbide) And a high-melting-point ceramic material.

[ Example ]

Hereinafter, the present invention will be described in more detail with reference to Examples. It is to be understood by those skilled in the art that these embodiments are only for illustrating the present invention and that the scope of the present invention is not construed as being limited by these embodiments.

In particular, the specific structure and structure of other sapphire single crystal growing apparatuses are omitted because they are similar to those in known prior arts, and a specific embodiment of the present invention having the above structure will be described below.

Example  One: Temperature gradient Solidification  Single Crystal Growth Device Using Sapphire

The specifications of the sapphire single crystal growth apparatus and the materials used are shown in Table 1 below.

division Detail Crystal growth method On tool hungry speech Crucible material Mo (molybdenum) Crucible size and number 120W × 250H × 150LX1t (unit mm) 1 piece Crucible support material High purity isotropic graphite Seed determination 30W x 30H x 140L (unit mm) Cooling means Cooling plate, Mo 30W × 100HX80L (Unit mm) Cooling system Water-cooled Heating element High purity isotropic graphite 8t temperature Senser Pyrometer Temperature control method PID control

In Example 1, as shown in Table 1 and FIG. 2, a rectangular crucible 200 and a graphite crucible support 400 are disposed at the center of growth, and a heating element 300 And a temperature control system for supplying power to the heating element 300. The sapphire monocrystal growth apparatus was used to grow a sapphire single crystal.

First, 8.5 kg of high purity alumina as a raw material of sapphire was filled in the crucible 200, and then the temperature was raised from room temperature to 2110 캜 for 15 hours and maintained for 2 hours. The crystal growth was performed by slowly cooling the temperature of the heating element 300 to 1920 占 폚 at a rate of 0.2 to 5 占 폚 / hr. Thereafter, it was slowly cooled to room temperature for 40 hours.

2, the graphite crucible supporter 400 used to support the crucible 200 and cut off radiant heat directly from the external heating element 300 is formed to have a larger size than the crucible 200, And the four sides of the side wall portion are separately manufactured and assembled so that the assembling and disassembling process can proceed easily. A plurality of supporting plates 535 made of tungsten, molybdenum and tungsten in the order of tungsten, molybdenum and tungsten are used between the crucible supporter 400 and the bottom of the crucible 200 to form a carbon component from the crucible supporter 400 of the graphite crucible The crucible support 400 of the tungsten reinforcing plate 500 is used between the sidewall of the crucible supporter 400 and the sidewall of the crucible 200.

The thickness of the plate used as the reinforcing plate 500 was 0.2 to 0.5 mm, respectively. If it is thicker than this, the effect on cost is increased.

The operation time for the crystal growth was about 10 days or longer from the temperature elevation to the cooling. During the period, the crucible 200 was exposed to a high temperature of 2000 ° C or more for more than 6 days. After the growth, No deformation occurred.

As shown in Table 1, the thickness of the molybdenum crucible 200 used was 1 mm, and when the crucible support 400 was not used, the deformation of the crucible 200 was so severe that normal crystal growth could not be performed , It is possible to effectively maintain the shape of the crucible 200 without causing deformation by using the crucible supporter 400 as in the present embodiment.

The grown sapphire single crystals had no defects such as bubbles or cracks, and they were processed by a wafer and etched in a KOH solution at 300 ° C to measure EPD (Etch Pit Density) And an average of about 150 pieces / cm 2 . This is remarkably superior to conventional wafers (500-1000 / cm 2 on average) by conventional techniques, and it is expected that the crystal growth rate can be increased to improve the productivity.

Example  2: Temperature gradient Solidification  And a sapphire single crystal growth apparatus for simultaneously growing a plurality of crystals

division Detail Crystal growth method On tool hungry speech Crucible material Mo (molybdenum) Crucible size and number 240W × 280H × 240LX1t (unit: mm) 4 pieces Crucible support material High purity isotropic graphite Seed determination 30W x 30H x 220L (unit mm) Cooling means Cooling plate, Mo 30W × 100H × 150L (unit: mm) 4 pieces Cooling system Water-cooled Heating element High purity isotropic graphite 8t: Split into 6 pieces temperature Senser Pyrometer Temperature control method PID control

In Example 2, as shown in [Table 2] and FIG. 3, a sapphire single crystal growth apparatus using the same tool-hulling method as in Example 1 was used to grow a larger and larger number of sapphire single crystals in the crucible 200 So that the crystal can be grown simultaneously in four crucibles (200). The six heating elements 300 are disposed on the side of the crucible 200 and controlled by independent power control devices so that the individual crucibles 200 can have a uniform temperature.

The crucible supporter 400 made of graphite material was manufactured by assembling four bottom and side plates in the same manner as in Example 1, so that installation and disassembly work could be easily performed. The bottom of the crucible supporter 400 was made of a multi- The separating plate and the tungsten spacing fins 570 are used to prevent the bottom of the crucible 200 and the graphite crucible support 400 from coming into direct contact with each other and the side surfaces of the reinforcing plate 500 made of tungsten plate and the plate made of molybdenum The crucible support body 400 and the crucible 200 are prevented from being in direct contact with each other by using the spacer 550.

The crucible support 400 of the bottom portion is formed by grooving to insert a tungsten spacing pin 570 so that about 60 tungsten spacing pins 570 per crucible 200 support the crucible 200 In order to avoid direct contact of the tungsten pin to the bottom surface of the crucible 200, a tungsten, molybdenum, and tungsten ternary reinforcing plate 500 is disposed between the tungsten spacing pin 570 and the crucible 200 in this order. The multiple support plates 535 were inserted.

The joining of the crucible supporters 400 having four faces was performed by combining the carbon fibers and the graphite composite (CC composite) by screwing them, and they were suitable for the use of the embodiments of the present invention.

Each of the molybdenum crucibles 200 made of molybdenum plate 1 mm in thickness was filled with a total of 140 kg of seed crystal and 35 kg of the sapphire raw material and the temperature was raised from room temperature to 2110 캜 for 20 hours and maintained for 5 hours. The crystal growth was carried out by slowly cooling the temperature of the heating body 300 to 1920 ° C at a rate of 0.2-5 ° C / hr. After the annealing, the crystal was cooled to room temperature for 80 hours. As the size of the single crystal increased, the time required in the melting step, the crystal growth step by slow cooling, and the cooling time increased, respectively, and it took 12 to 15 days in total to vary depending on the crystal growth rate.

The crucible 200 having been cooled completely did not undergo large deformation but deformation of the bottom portion of the crucible 200 was observed at a maximum of about 1 mm at the portion where the separation pin 570 was supported and the portion where the separation pin 570 was not.

It is expected that the above-described degree of deformation will be caused by the deformation of the crucible 200 and the tungsten spacing provided on the bottom of the crucible support 400 It is expected that the number of pins 570 can be improved sufficiently. The grown sapphire single crystal had no defects such as bubbles and cracks and the dislocation density of crystals was also excellent as about 150 pieces / cm 2 on average. In the sapphire single crystal grown from four different crucibles 200, No significant quality deviation was observed.

Example  3: Kylopoulos method  A sapphire single crystal growth apparatus using a square crucible

division Detail Crystal growth method Kylopoulos method Crucible material Mo (molybdenum) Size and number of crucibles 240W × 280H × 240LX1t (unit: mm) 1 piece Crucible support material High purity isotropic graphite Heating element High purity isotropic graphite 8t temperature Senser Pyrometer Temperature control method Power control

In Example 3, as shown in [Table 3] and Fig. 4, one crucible 200 as in Example 2 was used, and the seed crystal was suspended on the pulling rod 700 above the crucible 200 to melt the seed crystal Sapphire single crystal is grown using a sapphire single crystal growing apparatus by a pull-rous method in which a sapphire single crystal is grown in the crucible 200 by contacting the surface of the melt stored in the crucible 200 and gradually lowering the power .

The crucible 200 used for the crystal growth was the same as the crucible 200 used in Example 2. Since only one crucible 200 was used, a newly prepared crucible support 400 was used. A tungsten spacing pin 570 and a multiple support plate 535 composed of a tungsten and molybdenum triple plate were used between the crucible supporter 400 and the crucible 200 in the same manner as in Example 2, The crucible 200 was not deformed until it was completed.

The dislocation density of the crystals grown by the above method was as high as about 300-500 / cm 2 on average, and the bubbles were also similar to those of the sapphire single crystals grown by conventional pull-rous method. The shape of the crystal shows a rectangular shape with rounded corners, thus achieving the original purpose of obtaining a rectangular single crystal.

While the present invention has been particularly shown and described with reference to specific embodiments thereof, those skilled in the art will appreciate that such specific embodiments are merely preferred embodiments and that the scope of the present invention is not limited thereto will be. Accordingly, the actual scope of the present invention will be defined by the appended claims and their equivalents.

100: Furnace 200: Crucible
300: Heating element 350: Thermostat
400: crucible support 500: reinforcement plate
535: multiple support plate 550: spacer
570: Spacer pin 600: Cooling means
700: Pooling rod

Claims (15)

A furnace;
At least one crucible located inside the furnace, wherein the sapphire raw material is melted and a single crystal is grown from the seed crystal;
A heating element disposed outside the crucible and heating the crucible; And
And a crucible support disposed on the bottom and side surfaces of the crucible,
Wherein a reinforcing plate or a spacer member is provided between the crucible and the crucible support to minimize a contact area and inhibit a reaction for forming a compound by contact, wherein the reinforcing plate is a multiple support plate in which a plurality of plate- A sapphire single crystal growth device. The method according to claim 1,
Further comprising cooling means connected to the seed crystals located at the bottom of the crucible and extending below the bottom of the crucible. The method according to claim 1,
Further comprising a pulling rod disposed on the upper portion of the crucible to connect the seed crystal with the melt contained in the crucible and to grow the crystal in a downward direction from the upper surface of the melt, Growth device. The method according to claim 1,
Wherein the crucible and the crucible support are hexahedrons having a rectangular cross section and are spaced apart from each other. The method according to claim 1,
The crucible-
A bottom support disposed outside the crucible bottom; And
And four side supports provided outside the crucible side surface,
Wherein the bottom support and the side support are assembled and disassembled. The method according to claim 1,
The crucible-
Tungsten, molybdenum, tantalum, an alloy thereof, ceramics, or graphite. delete The method according to claim 1,
The reinforcing plate member or the spacer member may be formed,
Tungsten, molybdenum, tantalum, and an alloy thereof. The method according to claim 1,
Wherein the spacer member comprises:
And a pin-shaped member having a plurality of spacing pins arranged at even intervals so as to separate the crucible and the crucible support from each other. Claim 9
The pin-
Tungsten, molybdenum, tantalum, and an alloy thereof. delete The method according to claim 1,
And a spacer member provided between the bottom of the crucible and the crucible support,
And a plurality of spaced fins spaced from each other at a uniform interval to separate the bottom of the crucible support from the multi-support plate. The method of claim 12,
The spacing pin
Wherein a groove is formed in a bottom portion of the crucible supporter and inserted into the groove. The method according to claim 1,
The multi-
Tungsten, molybdenum, tantalum, and alloys thereof, and a structure in which different materials are alternately stacked. A method of manufacturing a sapphire single crystal according to any one of claims 1 to 3, wherein the sapphire single crystal growth apparatus is used to block radiant heat directly from a heating element and to block foreign substances penetrating into the crucible, Wherein the sapphire single crystal is grown on the sapphire substrate.
KR1020150126285A 2015-09-07 2015-09-07 Sapphire single crystal growing apparatus and method using of cruciable supporter KR101639627B1 (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101886188B1 (en) * 2017-02-27 2018-08-07 주식회사 사파이어테크놀로지 Growing sapphire single crystal
CN109898136A (en) * 2019-04-03 2019-06-18 贝民贤 Multiple Sapphire Crystal Growth device and growing method

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20110025716A (en) 2009-09-05 2011-03-11 주식회사 크리스텍 Method and apparatus for growing sapphire single crystal
KR101196445B1 (en) 2012-05-03 2012-11-01 주식회사 크리스텍 Apparatus for Growing Sapphire Crystal and Method for Growing Sapphire Crystal Using the Same
KR20140039031A (en) * 2011-06-06 2014-03-31 지티에이티 코포레이션 Heater assembly for crystal growth apparatus
JP2015048296A (en) * 2013-09-04 2015-03-16 株式会社福田結晶技術研究所 Growth unit and growth method of single crystal

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20110025716A (en) 2009-09-05 2011-03-11 주식회사 크리스텍 Method and apparatus for growing sapphire single crystal
KR20140039031A (en) * 2011-06-06 2014-03-31 지티에이티 코포레이션 Heater assembly for crystal growth apparatus
KR101196445B1 (en) 2012-05-03 2012-11-01 주식회사 크리스텍 Apparatus for Growing Sapphire Crystal and Method for Growing Sapphire Crystal Using the Same
JP2015048296A (en) * 2013-09-04 2015-03-16 株式会社福田結晶技術研究所 Growth unit and growth method of single crystal

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101886188B1 (en) * 2017-02-27 2018-08-07 주식회사 사파이어테크놀로지 Growing sapphire single crystal
CN109898136A (en) * 2019-04-03 2019-06-18 贝民贤 Multiple Sapphire Crystal Growth device and growing method

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