KR20160049624A - growing apparatus for large diameter single crystal - Google Patents

growing apparatus for large diameter single crystal Download PDF

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KR20160049624A
KR20160049624A KR1020140146328A KR20140146328A KR20160049624A KR 20160049624 A KR20160049624 A KR 20160049624A KR 1020140146328 A KR1020140146328 A KR 1020140146328A KR 20140146328 A KR20140146328 A KR 20140146328A KR 20160049624 A KR20160049624 A KR 20160049624A
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South Korea
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crucible
guide portion
insulating material
heat insulating
single crystal
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KR1020140146328A
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Korean (ko)
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KR101629445B1 (en
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여임규
박노형
은태희
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재단법인 포항산업과학연구원
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Priority to KR1020140146328A priority Critical patent/KR101629445B1/en
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Abstract

A large-diameter single crystal growth apparatus is provided. According to the present invention, there is provided a crucible comprising: a crucible provided with an internal space for charging a single crystal raw material; a heat insulating material provided outside the crucible and surrounding the crucible; a quartz tube provided outside the heat insulating material, A seed crystal attached to the seed crystal holder; heating means provided outside the quartz tube for heating the crucible; and an induction portion formed on the inner side of the crucible for inducing sublimation to seed crystals, Is formed in a truncated conical shape having a predetermined thickness and height and passing through the upper and lower portions and increasing in diameter from the upper portion to the lower portion.

Description

[0001] The present invention relates to a large diameter single crystal growth apparatus,

The present invention relates to a large diameter single crystal growth apparatus, and more particularly, to a large diameter single crystal growth apparatus capable of growing a large diameter single crystal without intrusion of polycrystals and defects by optimizing the shape of a crucible internal guide.

In general, physical vapor transport (PVT) is widely used as a silicon carbide single crystal growth method because it has the advantage of producing silicon carbide with high yield and high quality.

As shown in Fig. 1, the physical vapor transfer method includes a heat insulating material 2 arranged to surround the crucible 1, a quartz tube 3 arranged to surround the heat insulating material 2, And a heating means 5 provided outside the crucible 3 for heating the raw material 4 charged into the crucible 1. When the single crystal inside the crucible 1 is sublimated by using the heating means 4, the sublimated raw material is adhered to the seed crystal 8 bonded to the seed crystal holder 7, whereby the single crystal 6 is grown .

In the silicon carbide growth, the crucible 1 is heated and heated at a temperature of 2000 ° C. to 2300 ° C. or higher at room temperature as a heat source material. Due to the skin effect of induction heating, the crucible thickness design plays an important role in the internal temperature distribution, since the heat transfer from the crucible to the inside is made.

Among them, guiding portion 9 is designed to be thicker than the crucible main body in order to enlarge the ingot diameter, so that a loss occurs in the heat transfer process, and the temperature of guiding portion 9 is relatively lowered. When the temperature of the induction portion 9 is low, the powder of the raw material 4 adheres to the inner peripheral surface of the guide portion 9 to form the polycrystal 10, and the polycrystal 10 grows and grows from the seed crystal 8 It can be brought into contact with the edge region of the single crystal 6. At this time, the polycrystal enters the single crystal, and the intruded polycrystal interferes with the enlargement of the diameter of the single crystal, so that there is a problem that the single crystal can not be grown in a large diameter and high quality finally.

An objective of the present invention is to provide a large diameter single crystal growth apparatus capable of growing a single crystal of a large diameter without intrusion of polycrystals and defects by optimizing the shape of the crucible internal guide.

According to an embodiment of the present invention, a crucible provided with an internal space for charging a single crystal raw material,

A heat insulating material provided outside the crucible and surrounding the crucible,

A quartz tube provided outside the heat insulating material and surrounding the crucible and the heat insulating material,

Seed seeds attached to seed holders,

Heating means provided outside the quartz tube for heating the crucible, and

And an induction portion formed on an inner upper side of the crucible for inducing sublimation to a seed crystal,

The induction unit is formed in a truncated cone shape having a predetermined thickness and height and passing through the upper and lower portions and having a larger diameter from the upper portion to the lower portion.

The outer surface of the guide portion may be inclined at a predetermined angle with the outer surface of the crucible.

A space for preventing heat conduction to the heat insulating material and confining the heat by a space convection effect may be formed outside the guide portion.

The space portion may be formed between the outer side of the guide portion and the inner side of the heat insulating material.

The space portion may be formed in an inverted triangular shape inclined downward toward the bottom of the edge of the crucible about the widthwise center portion of the crucible.

The thickness of the guide portion is determined by the following equation: D4 = D3 / (1.1 - 2.0)

D3 denotes a radial distance from the inner circumference of the upper end of the guide portion to the outer diameter of the lower end portion of the guide portion, and D4 denotes a radial distance from the outer periphery of the guide portion to the outer surface of the guide portion.

The radial distance D4 from the outer circumference of the upper end of the guide portion to the outer diameter of the lower end surface of the guide portion may be set to 15 to 22 mm.

The radial distance from the inner circumference of the upper end surface of the guide portion to the outer diameter of the lower end surface of the guide portion is determined by a relation of D3 = D2 / 2 (1.0 to 1.5)

Here, D2 indicates the inner diameter of the upper end surface of the guide portion.

The inner diameter of the upper end surface of the guide portion is determined by the following equation: D2 = D1 / (1.3-1.7)

Here, D1 indicates the outer diameter of the crucible,

The outer diameter of the crucible may be set to 150 to 250 mm.

The height D5 of the guide portion can be determined by a relationship of D4 = D5 / 1.6.

According to this embodiment, it is possible to obtain a high-quality single crystal ingot by appropriately maintaining the temperature of the induction portion. Particularly, the problem of generation of stress due to contact with the single crystal, disturbance of diameter expansion due to polycrystalline entering from the induction portion, The defect generation frequency can be remarkably reduced,

In addition, the present invention can be applied to a single crystal ingot having a diameter of 5 or 6 inches by utilizing the relational expression according to the embodiment of the present invention in the detailed configuration and the correlation.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a schematic configuration diagram of a conventional large diameter single crystal growth apparatus. FIG.
2 is a schematic diagram of a large diameter single crystal growth apparatus according to an embodiment of the present invention.
Figure 3 is a partial detail view of Figure 2;
FIG. 4 is a diagram showing the temperature distribution in the crucible by using a simulation, in which FIG. 4A shows a case according to the prior art, and FIG. 4B shows a case according to an embodiment of the present invention.
FIG. 5 is a view showing a temperature distribution on the inner circumferential surface from the lower end to the upper end of the guide portion, in which (a) is a case according to the prior art, and (b) is a case according to the embodiment of the present invention.
6 is a photograph of a 4 inch silicon carbide single crystal ingot grown according to an 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. As will be readily understood by those skilled in the art, the following embodiments may be modified in various ways within the scope and spirit of the present 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 limit 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 / And the like.

All terms including technical and scientific terms used herein have the same meaning as commonly understood by those of ordinary skill in the art to which the present 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.

2 is a schematic diagram of a large diameter single crystal growth apparatus according to an embodiment of the present invention.

Referring to FIG. 2, the apparatus for growing a large diameter single crystal according to an embodiment of the present invention includes:

A crucible 100 provided with an internal space for charging the single crystal raw material 200,

A heat insulating material 110 provided outside the crucible and surrounding the crucible 100,

A quartz tube 120 provided on the outside of the heat insulating material 110 and surrounding the crucible 100 and the heat insulating material 110,

A seed crystal 140 attached to the seed holder 130,

A heating means 150 provided outside the quartz tube 120 for heating the crucible 100,

And an induction unit 160 formed at an inner upper portion of the crucible 100 to induce sublimation of the raw material to the seed crystal 140,

The induction unit 160 may have a predetermined thickness and / or thickness to shorten the heat transfer distance due to the skin effect of induction heating of the heating unit 150 and to prevent heat loss from the outside of the crucible 10 to the inside as much as possible. And a truncated conical shape having a larger diameter from the upper part to the lower part.

The outer surface of the guide portion 160 may be inclined at a predetermined angle? With respect to the outer surface of the crucible 100.

In addition, a space 170 may be formed on the outer side of the guide part 160 to prevent heat conduction from the heat insulating material 110 and confine the heat by the convection effect by the space.

The space 170 is formed between the outer side of the induction 160 and the inner side of the heat insulating material 110 to effectively prevent heat conduction to the heat insulating material 110 and efficiently trap heat by a space- .

The space 170 may be formed in an inverted triangular shape inclined downward toward the bottom of the edge of the crucible 100 about the central portion in the width direction of the crucible 100.

The thickness t of the guiding portion 160 and the design of the space portion 170 play an important role in the temperature distribution of the crucible 100 because the heat is transferred from the outside of the crucible 100 to the inside due to the skin effect of induction heating. .

3, a radial distance D3 from the inner periphery of the upper end of the guide portion to the outer diameter of the guide portion is D3, a radial distance D4 from the outer periphery of the guide portion to the outer surface of the guide portion is D4, The angle formed by the guide portion and the outer surface of the crucible is indicated by?.

D4 = D3 / (1.1 to 2.0) where D3 = D2 / (1.1 to 2.0), which determines the thickness of the guide portion t, i.e., the lateral direction (radial direction) 2 (1.0 to 1.5), and D2 = D1 / (1.3 to 1.7).

Here, the radial distance D4 from the outer circumference of the upper end of the guide portion to the outer radius of the guide portion may be set in a range of 15 to 22 mm. At this time, the thickness of the crucible 100 may be set to 150 to 250 mm. If the radial distance D4 from the outer circumference of the upper end of the guide portion to the outer diameter of the lower end portion of the guide portion is larger than 22 mm, the thickness of the guide portion becomes thinner and deterioration at the high temperature, Also, if the radial distance D4 from the outer circumference of the upper end of the guide portion to the outer diameter of the lower end portion of the guide portion is less than 15 mm, the thickness of the guide portion 160 becomes thick, and the effect of the present invention is reduced.

The relation of the height D5 of the guide portion, that is, the vertical direction (vertical direction in Fig. 3) is D4 = D5 / 1.6. The height D5 of the guide portion varies in accordance with the radial distance D4 from the outer circumference of the upper end surface of the guide portion to the outer diameter of the guide portion lower end surface, and the guide portion angle? Also changes from the outer circumference of the guide portion to the outer radius of the guide portion, (D4).

Hereinafter, the operation of the apparatus for growing a large diameter single crystal according to one embodiment of the present invention will be described with reference to FIGS. 2 and 3. FIG.

The large diameter single crystal growth apparatus includes a crucible provided with an internal space for charging the raw material powder 200, a heat insulating material surrounding the crucible, a quartz tube, and a heating means coil provided outside the quartz tube for heating the crucible. In an embodiment of the present invention, a single crystal is grown on a seed crystal using physical vapor transport (PVT).

To this end, the raw material powder 200 is first charged into the crucible 100. The seed holder 140 having the seed crystal 140 coupled thereto is drawn into the large diameter single crystal growth apparatus and mounted on the interior of the crucible 100. The seed crystal holder 130 is made of silicon carbide.

Then, the impurities contained in the crucible 100 are removed by heating at a temperature of less than about 1000 캜 and a vacuum pressure for 2 hours to 3 hours. Thereafter, an inert gas, for example, argon (Ar) gas is injected to remove air remaining in the crucible 100 and between the crucible 100 and the heat insulating material 110. Here, the purging process using an inert gas is preferably repeated two to three times. Then, the crucible 100 is heated to a temperature of approximately 2000 ° C to 2300 ° C using the heating means 150 after raising the internal pressure of the crucible to atmospheric pressure. Here, the reason for maintaining the atmospheric pressure is to prevent the generation of undesired crystal polymorphism at the initial stage of crystal growth. That is, the raw material 200 is first raised to the growth temperature while maintaining the atmospheric pressure. Then, the raw material 200 is sublimated while growing the single crystal, while maintaining the inside of the single crystal growing apparatus at a reduced pressure of 1 torr to 20 torr to maintain the growth pressure.

In the large diameter single crystal growth apparatus according to the embodiment of the present invention, the relational expression concerning D3 and D4 that determines the thickness of the guide portion t, that is, the transverse direction (radial direction) D3 = D2 / 2 (1.0 to 1.5) and D2 = D1 / (1.3 to 1.7), and the height D5 of the guide portion, that is, the vertical direction The relation is D4 = D5 / 1.6.

Here, the radial distance D4 from the outer circumference of the upper end of the guide portion to the outer diameter of the guide portion is set in a range of 15 to 22 mm, and the thickness of the crucible 100 is set to 150 to 250 mm.

Accordingly, in order to shorten the distance of heat generated due to the skin effect of induction heating, the thickness of the guide portion can be reduced, thereby preventing heat loss from the outside to the inside as much as possible. In addition, since the void space is formed in the outer periphery of the guide portion, the heat can be prevented from being conduced to the heat insulating material, that is, heat loss can be prevented and convection due to the space of the space portion can be prevented. Can be maintained. Therefore, the temperature of the induction portion is relatively lowered, and the phenomenon that the polycrystal adheres thereto can be prevented, and the phenomenon that the adhered polycrystal enters the single crystal can be prevented.

[Experimental Example]

FIG. 4 is a view showing a temperature distribution of the entire crucible by using a simulation. FIG. 4 (a) shows a case according to the prior art, (b) shows a case according to an embodiment of the present invention, (A) is a case according to the prior art, (b) is according to an embodiment of the present invention, and Fig. 6 is a view showing the temperature distribution of the inner circumferential surface of the 4-inch silicon carbide It is a photograph of a single crystal ingot.

Since the temperature of the induction part 160 according to the embodiment of the present invention is higher than that of the prior art, polycrystalline is not attached to the inner circumferential surface of the guide part, and thus polycrystals are not infiltrated into the edge area of the single crystal ingot grown from the seed crystal have. In addition, since the roughness of the single crystal edge region is low and the facet is observed, it can be seen that the stress is low and the defect generation is low, that is, the ingot having a high crystal quality is grown.

100: Crucible 110: Insulation
120: quartz tube 130: seed holder
140: seed crystal 150: heating means
160: guide portion 170:
200: raw material

Claims (10)

A crucible provided with an internal space for charging a single crystal raw material,
A heat insulating material provided outside the crucible and surrounding the crucible,
A quartz tube provided outside the heat insulating material and surrounding the crucible and the heat insulating material,
Seed seeds attached to seed holders,
Heating means provided outside the quartz tube for heating the crucible, and
And an induction portion formed on an inner upper side of the crucible for inducing sublimation to a seed crystal,
Wherein the induction portion is formed in a truncated cone shape having a predetermined thickness and height and passing through the upper and lower portions and having a larger diameter from the upper portion to the lower portion. The method according to claim 1,
Wherein an outer side surface of the guide portion is inclined at an angle with an outer side surface of the crucible. 3. The method of claim 2,
Wherein a space is formed on the outer side of the guide to prevent heat conduction from the heat insulating material and to confine heat by a convection effect by space. The method of claim 3,
Wherein the space portion is formed between the outer side of the guide portion and the inner side of the heat insulating material. 5. The method of claim 4,
Wherein the space portion is formed in an inverted triangular shape inclined downward toward the bottom of the edge of the crucible about the widthwise center portion of the crucible. 6. The method according to any one of claims 1 to 5,
The thickness of the guide portion is determined by the following equation: D4 = D3 / (1.1 - 2.0)
D3 denotes a radial distance from the inner circumference of the upper end of the guide portion to the outer diameter of the lower end portion of the guide portion, and D4 denotes a radial distance from the outer periphery of the guide portion to the outer surface of the guide portion. The method according to claim 6,
And the radial distance (D4) from the outer circumference of the upper end of the guide portion to the outer diameter of the lower end surface of the guide portion is set to 15 to 22 mm. 8. The method of claim 7,
The radial distance from the inner circumference of the upper end surface of the guide portion to the outer diameter of the lower end surface of the guide portion is determined by a relation of D3 = D2 / 2 (1.0 to 1.5)
Here, D2 denotes the inner diameter of the upper end surface of the guide portion. 9. The method of claim 8,
The inner diameter of the upper end surface of the guide portion is determined by the following equation: D2 = D1 / (1.3-1.7)
Here, D1 indicates the outer diameter of the crucible,
Wherein an outer diameter of the crucible is set to 150 to 250 mm. 10. The method of claim 9,
Wherein the height D5 of the guide portion is determined by the following equation: D4 = D5 / 1.6.
KR1020140146328A 2014-10-27 2014-10-27 growing apparatus for large diameter single crystal KR101629445B1 (en)

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KR101908043B1 (en) * 2016-12-23 2018-10-16 주식회사 포스코 Device for growing large diameter single crystal

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101101984B1 (en) * 2008-12-12 2012-01-02 에스케이씨 주식회사 Apparatus for growing a single crystal
KR101181217B1 (en) * 2009-06-29 2012-09-07 에스케이씨 주식회사 Growing apparatus for single crystal
KR20130069192A (en) * 2011-12-16 2013-06-26 재단법인 포항산업과학연구원 Apparatus for growing of sic single crystal
KR20130083654A (en) * 2012-01-13 2013-07-23 동의대학교 산학협력단 Growing apparatus for single crystal

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101101984B1 (en) * 2008-12-12 2012-01-02 에스케이씨 주식회사 Apparatus for growing a single crystal
KR101181217B1 (en) * 2009-06-29 2012-09-07 에스케이씨 주식회사 Growing apparatus for single crystal
KR20130069192A (en) * 2011-12-16 2013-06-26 재단법인 포항산업과학연구원 Apparatus for growing of sic single crystal
KR20130083654A (en) * 2012-01-13 2013-07-23 동의대학교 산학협력단 Growing apparatus for single crystal

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