KR101227051B1 - Single crystal method and single crystal rawmaterial - Google Patents

Single crystal method and single crystal rawmaterial Download PDF

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KR101227051B1
KR101227051B1 KR1020100028363A KR20100028363A KR101227051B1 KR 101227051 B1 KR101227051 B1 KR 101227051B1 KR 1020100028363 A KR1020100028363 A KR 1020100028363A KR 20100028363 A KR20100028363 A KR 20100028363A KR 101227051 B1 KR101227051 B1 KR 101227051B1
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single crystal
raw material
powder
crucible
growth
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KR20110108896A (en
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신병철
이원재
여임규
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동의대학교 산학협력단
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Abstract

The single crystal growth method according to the present invention has a density of 0.5 g / m 3 to 1 g / m 3 and is characterized by growing a single crystal using a raw material in which Si powder is mixed with SiC powder.
Therefore, according to the present invention, a semi insulating single crystal can be easily manufactured. That is, a semi insulating single crystal having a carrier concentration of 1 × 10 16 or less and high transmittance can be produced. In the case of such semi-insulating single crystal, the resistance is large, and the circuit or the wiring can be prevented from being energized in the highly integrated circuit or the nano-width wiring.

Description

Single crystal method and single crystal raw material

The present invention relates to a single crystal growth method and a single crystal raw material, and relates to a single crystal growth method and a single crystal raw material for growing a semi insulating single crystal.

As Si used as a representative semiconductor device material shows physical limitations, broadband semiconductor materials such as SiC, GaN, AlN, and ZnO are in the spotlight as next-generation semiconductor device materials. Here, SiC has excellent thermal stability and excellent oxidation resistance compared to GaN, AlN, and ZnO. In addition, SiC has an excellent thermal conductivity of about 4.6 W / cm ℃, and has the advantage that can be produced as a large-diameter substrate of 2 inches or more in diameter, has been spotlighted compared to substrates such as GaN, AlN and ZnO.

On the other hand, in order to solve the problem that the circuit becomes highly integrated and the width of the wiring is reduced to nano size, the current between the circuits is applied, a semi-insulating single crystal is used as the substrate. Here, semi-insulating single crystal refers to a single crystal having a carrier concentration of 1 × 10 16 or less. In the case of general SiC single crystal substrates, which are not semi-insulated, the conductivity is strong, so that current between circuits is energized.

In addition, conventionally, SiC single crystals were produced using SiC powders of yellow-green color. However, when manufacturing a single crystal substrate using the SiC powder as described above, there is a disadvantage that the transmittance is low. In addition, the carrier concentration of the single crystal can be inferred through the transmittance. The lower the transmittance, the higher the carrier concentration, making it difficult to produce a semi-insulating single crystal. In order to solve this problem, conventionally, vanadium (Vanadium) powder is mixed with SiC powder, and a semi-insulating single crystal is manufactured using this as a raw material. However, the difference between the sublimation temperature of vanadium (Vanadium) and the sublimation temperature of SiC is large, there is a problem that the vanadium is not uniformly doped in the single crystal. As such, if vanadium is unevenly doped in a single crystal, charge mobility is reduced, resulting in a problem of deterioration of product characteristics.

One technical problem of the present invention is to provide a single crystal growth method and a single crystal raw material for growing a semi insulating single crystal.

One technical problem of the present invention is to provide a growth method and a single crystal raw material for growing a semi insulating single crystal having high resistance and low carrier concentration.

Single crystal growth method according to the present invention is a density of 0.5g / m 3 to about 1g / m 3 or preparing a SiC powder, the density of the SiC powder, a mixture of Si powder of 0.5g / m 3 to about 1g / m 3 Preparing a raw material and growing a single crystal using the raw material in which Si powder is mixed with the SiC powder.

A raw material in which Si powder is mixed with 1 wt% to 5 wt% is used for the SiC powder.

The seed crystal holder in a growth method of growing a single crystal by subliming the raw material using a growth apparatus including a crucible into which the raw material is charged, a seed crystal holder to which seed crystals are attached, and a heating means for heating the crucible. Attaching the seed crystal to the seed crystal, introducing the seed crystal holder with the seed crystal into the growth apparatus, charging the raw material into a crucible disposed inside the growth apparatus, and heating the crucible using the heating means. And subliming the raw material charged into the crucible to grow single crystals in seed crystals.

The raw material is white.

6H-SiC single crystals are grown using the raw materials.

Single crystal material according to the invention is prepared by mixing a density of .5g / m 3 to about 1g / m 3 of Si powder, a density of 0.5g / m 3 to about 1g / m 3 to the SiC powder, a single crystal Si-containing over- To grow.

The transmittance of the single crystal is 55% to 64% at 400 nm to 800 nm.

The resistance of the single crystal is 1 × 10 5 Ωcm or more.

The carrier concentration of the single crystal is set to 1 × 10 16 / cm 3 or less.

As described above, the embodiments of the present invention have a density of 0.5g / m 3 to 1g / m 3 of the raw material and facilitate semi-insulating single crystals by using a raw material in which Si powder is mixed with SiC powder. Can be made. That is, a semi insulating single crystal having a carrier concentration of 1 × 10 16 / cm 3 or less and high transmittance can be produced. In the case of such semi-insulating single crystal, the resistance is large, and the circuit or the wiring can be prevented from being energized in the highly integrated circuit or the nano-width wiring.

1 is a cross-sectional view showing a growth apparatus according to an embodiment of the present invention
Figure 2a is a photograph showing a raw material according to an embodiment of the present invention, Figure 2b is a photograph showing a raw material according to a comparative example of the embodiment
3 is an XPS graph of a raw material according to an embodiment of the present invention.
4A is an XRD graph of single crystals in an embodiment of the present invention, and FIG. 4B is an XRD graph of single crystals according to a comparative example.
5A is a photograph showing a single crystal according to an embodiment, and FIG. 5B is a photograph showing a single crystal according to a comparative example.
6 is a graph showing transmittances of single crystals according to Examples and single crystals according to Comparative Examples
7 is a graph showing a Raman spectrum of a single crystal according to an embodiment of the present invention and a single crystal according to a comparative example

Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings. However, the present invention is not limited to the embodiments disclosed below, but may be implemented in various forms, and only the embodiments are intended to complete the disclosure of the present invention and to those skilled in the art. It is provided for complete information.

1 is a cross-sectional view showing a growth apparatus according to an embodiment of the present invention.

Referring to FIG. 1, the growth apparatus includes a crucible 100 having an internal space in which raw materials are charged, a seed crystal holder 300 to which the seed crystal 200 is attached, an insulating material 400 surrounding the crucible 100, and The quartz tube 500 and the quartz tube 500 are provided outside the heating means 600 for heating the crucible 100. In addition, it may further include a control device (not shown) for operating the heating means 600 independently.

The crucible 100 is preferably made of a material having a melting point higher than the sublimation temperature of the raw material. For example, a material made of graphite or having a melting point above the sublimation temperature of the raw material may be applied onto the graphite material. Here, the material to be applied on the graphite material is preferably used a material that is chemically inert to silicon and hydrogen at the temperature at which the raw material is sublimed to grow single crystal. For example, metal nitrides may be used as the metal carbide, and in particular, carbides formed of carbon with Ta, Hf, Nb, Zr, W, V and a mixture of at least two of them, and Ta, Hf, Nb, Zr, W , Ni, and a mixture of V and at least two or more of them and nitrogen.

Figure 2a is a photograph showing a raw material according to an embodiment of the present invention, Figure 2b is a photograph showing a raw material according to a comparative example of the embodiment. 3 is an XPS graph of a raw material according to an embodiment of the present invention.

In the crucible 100, a raw material that is a raw material for growing single crystals is charged. In the embodiment, a material in which SiC powder and Si powder are mixed is used as a raw material. In this case, the SiC powder and the Si powder according to the embodiment have a density of 0.5 g / m 3 to 1 g / m 3 , and in addition to the SiC, Si powder is included in 1wt% to 5w%. In this case, adding 1 wt% to 5 w% of Si powder to the SiC powder is for growing a single crystal in a semi-insulating state. In addition, the raw material according to the comparative example has a density of 1 g / m 3 to 3 g / m 3 and uses SiC powder not containing Si powder. 2A and 2B, the raw material according to the embodiment is white, and the raw material according to the comparative example is yellow-green. This different color of the raw material is related to the oxygen saturation by the density of the raw material. In other words, the high density of the raw material means that the particles are agglomerated, and when the particles are agglomerated, the porosity is very small, and thus the probability of impurity intrusion and bonding is small every week. However, the raw material according to the embodiment is 0.5g / m 3 to 1g / m 3 has a lower density than the raw material according to the comparative example. Thus, the raw material according to the embodiment has a plurality of pores compared to the raw material according to the comparative example. Thus, as shown in FIG. 3, as shown in the XPS graph of the raw material according to the embodiment, Si or C is combined with oxygen, indicating that oxygen is contained in the raw material. As such, when the oxygen saturation increases, the color of the raw material becomes white as shown in FIG. 2A. However, when the density of the raw material is 1g / m 3 to 3g / m 3 as in the comparative example, the particles are agglomerated so very little pore. As a result, as described above, the probability of oxygen invading and binding is very low, and thus the oxygen saturation is low, so that the color is yellow-green as shown in FIG. 2B. Therefore, in the embodiment, the density of the raw material is 0.5 g / m 3 to 1 g / m 3 . The single crystal grown with white raw material has higher transmittance than the single crystal grown with raw material that is not grown. For example, when the density of the raw material is less than 0.5g / m 3 , a larger amount of impurities may bind than SiC, which is a basic material of the raw material. In addition, when the density of the raw material is more than 1g / m 3 There are few pores can not produce a raw material with high oxygen saturation. Thus, transparent single crystals cannot be produced. A description of the transmittance of the single crystal according to the color of the raw material will be described below.

In addition, as described above, in order to grow a semi-insulating single crystal, the Si powder is included in an amount of 1 wt% to 5 wt%. Here, the single crystal in semi-insulating state has a carrier concentration of 1 × 10 16 / cm 3 It means the following single crystal. For example, if the Si powder is added below 1 wt%, semi-insulating single crystals cannot be grown. On the other hand, when the Si powder is added in excess of 5wt%, Si is excessively added so that Si is sublimed at low temperature during single crystal growth, causing defects, that is, polymorphism or polycrystal. In this embodiment, the SiC powder is used as a raw material in which 1wt% to 5wt% of Si powder is added.

The seed crystal holder 300 is a means for supporting the seed crystal 200, and is manufactured using high density graphite. The seed crystal holder 300 to which the seed crystal 200 is attached is mounted on the upper part of the crucible 100 to form a single crystal on the seed crystal 200.

The heat insulating material 400 and the quartz tube 500 are provided outside the crucible 100 to maintain the temperature of the crucible 100 at a crystal growth temperature. At this time, since the crystal growth temperature of the raw material is very high, it is preferable to use the graphite felt fabricated into a tubular cylindrical shape having a predetermined thickness by compressing the graphite fibers as the heat insulating material 400. In addition, the heat insulating material 400 may be formed of a plurality of layers to surround the crucible 100.

The heating means 600 is provided outside the quartz tube 500, and for example, a high frequency induction coil may be used. The crucible 100 is heated by flowing a high frequency current through the high frequency induction coil, and the raw material is heated to a desired temperature.

Hereinafter, a single crystal growth method according to an embodiment of the present invention will be described with reference to FIG. 1.

In an embodiment, 6H-SiC single crystals are grown on seed crystals 200 using a physical vapor transport (PVT) method. To this end, first, the seed crystal 200 made of SiC is prepared, and the seed crystal 200 is attached to the seed crystal holder 300 using an adhesive. At this time, it is preferable to attach to the seed crystal holder 300 such that the m-plane (1-100) or the a-plane (11-20) of the seed crystal 200 becomes a growth surface. Of course, the present invention is not limited thereto and may be attached to the seed crystal holder 300 such that the other surface of the seed crystal 200 becomes a growth surface.

Subsequently, the seed crystal holder 300 to which the seed crystal 200 is attached is introduced into the growth apparatus and mounted on the upper part of the crucible 100. At this time, it is preferable that the growth surface of the seed crystal 200 attached to the seed crystal holder 300 is disposed above the inside of the crucible 100. In an embodiment, the m-surface 1-100 or the a-surface 11-20 is disposed correspondingly to the inner upper side of the crucible 100. Then, the raw material according to the mixed embodiment of the SiC powder and Si powder is charged into the crucible 100. In the embodiment, the SiC powder uses a raw material in which 1 wt% to 5 wt% of Si powder is added. In this case, the density of the raw material is preferably 0.5g / m 3 to 0.5g / m 3 . Subsequently, it is heated for 2 to 3 hours at a temperature of 1300 ℃ to 1500 ℃ and vacuum pressure to remove impurities contained in the crucible 100. Thereafter, an inert gas, for example, argon (Ar) gas is injected to remove air remaining inside the crucible 100 and between the crucible 100 and the heat insulating material 400. Subsequently, after raising the pressure to atmospheric pressure, the crucible 100 is heated to a temperature of 2000 ° C to 2300 ° C using the heating means 600. Here, the reason for maintaining the atmospheric pressure is to prevent the occurrence of unwanted crystal polymorphism at the beginning of crystal growth. That is, first, the atmospheric pressure is maintained and the raw material is heated to the growth temperature. Subsequently, the single crystal is grown by subliming the raw material while maintaining the growth pressure by reducing the inside of the growth apparatus to 20 mbar to 60 mbar. At this time, the grown single crystal is 6H-SiC.

As described above, when single crystals are grown by using a raw material in which Si is excessively formed in SiC, the single crystals according to the embodiment have higher transmittance, lower carrier concentration, and higher resistance than conventional single crystals. In this case, as described above, the single crystal according to the embodiment exhibits semi insulating properties having a carrier concentration of 1 × 10 16 / cm 3 or less. In addition, the single crystal according to the embodiment has a high resistance of 1 × 10 5 dBm or more.

In the following, the characteristics of the single crystal prepared using the raw material according to the comparative example and the single crystal manufactured using the raw material according to the embodiment are compared with reference to 4a to 7b. In this case, the single crystal according to the embodiment has a density of 1 g / m 3 to 3 g / m 3 , and is grown using SiC powder using a raw material having 1 wt% to 5 w% of Si powder. In addition, the single crystal according to the comparative example has a density of 1 g / m 3 to 3 g / m 3 , and was grown using SiC powder as a raw material. In Comparative Example, nitrogen (N 2 ) is mixed and doped during single crystal growth.

4A is an XRD graph of a single crystal in an embodiment of the present invention, and FIG. 4B is an XRD graph of a single crystal according to a comparative example. Referring to FIG. 4A, in the case of the first single crystal grown using the raw material according to the embodiment, a peak of Si appears between 27 ° and 30 °, and a peak of αC Si between 34 ° and 78 ° appears. This is because single crystals were grown using a raw material in which Si powder was added to SiC powder. For this reason, as shown in FIG. 4A, a single crystal containing SiC and Si can be produced. Meanwhile, referring to FIG. 2B, in the case of the second single crystal grown using the raw material according to the comparative example, the SiC peak of the a phase appears at 34 ° to 76 °. However, the peak of Si does not appear. This is because, in the comparative example, the raw material including only SiC powder was used instead of the raw material including Si powder as in the example.

5A is a photograph showing a single crystal according to an embodiment, and FIG. 5B is a photograph showing a single crystal according to a comparative example. 6 is a graph showing transmittances of single crystals according to Examples and single crystals according to Comparative Examples.

First, referring to FIGS. 5A and 5B, the single crystal according to the comparative example has a higher transmittance than the single crystal according to the embodiment. That is, as shown in Figure 6, the transmittance of the single crystal according to the embodiment at a wavelength of 430nm to 800nm is 60% to 65%, the transmittance of the single crystal according to the comparative example is 50% to 59%. That is, the transmittance of the single crystal according to the embodiment is higher than that of the single crystal according to the comparative example. This density than the comparative example the case of the embodiment, because hayeotgi using raw materials of low 0.5g / m 3 to about 1g / m 3. That is, a large number of pores are generated between the particles of the raw material having a low density, and oxygen penetrates into the pores of the raw material, resulting in a single crystal raw material having high oxygen saturation. Due to such high oxygen saturation, the single crystal according to the embodiment has a higher transmittance than the single crystal raw material according to the comparative example. In the graph of the transmittance of the single crystal according to the comparative example, a sudden change in the transmittance was observed at 570 nm to 700 nm. That is, as the wavelength increases from 570 nm to 630 nm, the transmittance rapidly decreases from 58% to 50%, and as the wavelength increases from 630 nm to 700 nm, the transmittance rapidly increases from 50% to 57%. Such rapid change in transmittance means that nitrogen (N 2 ) is incorporated into the single crystal during single crystal growth according to a comparative example. When nitrogen (N 2 ) is mixed, there is a problem that the transmittance of the single crystal is lowered. Therefore, the transmittance according to the embodiment in which nitrogen (N 2 ) is not mixed during the single crystal growth is higher than that of the single crystal according to the comparative example. The transmittance data can be inferred that the carrier concentration of the single crystal according to the embodiment is lower than the carrier concentration of the single crystal according to the comparative example. On the other hand, in the transmittance graph of the single crystal according to the embodiment, there is no sudden change in the transmittance. Through this, it can be seen that nitrogen is not mixed during single crystal growth according to the embodiment.

FIG. 7 is a graph illustrating a Raman spectrum of a single crystal according to an embodiment of the present invention and a single crystal according to a comparative example.

Referring to the Raman spectrum shown in FIG. 7, two peaks appear in the wavelength range of 50 nm to 800 nm, and one peak appears in the wavelength range of 950 nm to 975 nm. In this case, each of the two peaks within the wavelength of 750 nm to 800 nm is a peak in which the lattice of the single crystal vibrates in a direction perpendicular to the electromagnetic wave, and a peak in the wavelength of 950 nm to 975 nm is the peak at which the lattice of the single crystal vibrates horizontally in the electromagnetic wave. The position of these three peaks means that the single crystal according to the embodiment and the single crystal according to the comparative example are 6H-SiC single crystals. In addition, the electrical properties can be known from the intensity of the Raman spectrum. The lower the carrier concentration, the higher the intensity and the sharper the shape of the peak. On the contrary, the higher the carrier concentration, the lower the intensity and the morphology of the peak is gentle. In addition, when the carrier concentration is 1 × 10 16 / cm 3 or less, it is referred to as semiintrinsic single crystal. Referring to FIG. 7, the carrier concentration of the single crystal according to the embodiment is 5 × 10 16 / cm 3 , and the carrier concentration of the single crystal according to the comparative example is 5.6 × 10 18 / cm 3 . Thus, the single crystal to which 1wt% to 5wt% of Si is added has the characteristics of a semicrystalline single crystal, that is, the single crystal according to the comparative example does not have the characteristics of the semicrystalline single crystal. In addition, the single crystal according to the embodiment has a high resistance of 1 × 10 5 Ωcm or more, but the single crystal according to the comparative example has a low resistance of 0.1 Ωcm or less. Therefore, the single crystal according to the embodiment can be easily used in an integrated circuit and an electric device requiring a nano-sized wiring. However, when the single crystal according to the comparative example is applied to an integrated circuit or an electric element requiring a nano-width wiring, there is a problem that the circuit or wiring may be energized. The single crystal wafer according to the embodiment is more transparent than the single crystal wafer according to the comparative example. And the single crystal according to the comparative example is green.

Such a semi-insulated single crystal wafer can be used as a substrate of an electronic device, for example, MEFEST, which requires highly integrated circuits and nano-sized wiring.

100: crucible 200: seed crystal
300: seed crystal holder 400: insulation

Claims (9)

Preparing a SiC powder having a density of 0.5 g / m 3 to 1 g / m 3 ;
The method comprising: preparing an Si powder to the SiC powder has a density 0.5g / m 3 to about 1g / m 3;
Preparing a raw material by mixing the SiC powder so that Si powder is more than 3wt% and 5wt% or less;
Charging the raw material into a crucible in a growth apparatus;
Heating at a vacuum pressure to remove impurities contained in the crucible into which the raw material is charged;
Raising the pressure to atmospheric pressure; And
The crucible was heated up to the growth temperature of the raw material, and the inside of the growth apparatus was decompressed to sublimate the raw material to grow single crystals. The transmittance was 55% to 64% at 400 nm to 800 nm, and the resistance was 1 × 10 5 kcm. The single crystal growth method of growing a single crystal having a carrier concentration of 1 × 10 16 / cm 3 or less as described above. delete The method according to claim 1,
In a growth method of growing a single crystal by subliming the raw material by using a growth apparatus including a crucible into which the raw material is charged, a seed crystal holder to which seed crystals are attached, and heating means for heating the crucible.
Attaching seed crystals to the seed crystal holder; And
Introducing the seed crystal holder, to which the seed crystal is attached, into a growth device;
Single crystal listing method comprising a. The method according to claim 1 or 3,
The raw material is white single crystal growth method. The method of claim 4,
The single crystal growth method of growing a 6H-SiC single crystal using the raw material. delete delete delete delete
KR1020100028363A 2010-03-30 2010-03-30 Single crystal method and single crystal rawmaterial KR101227051B1 (en)

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KR101480491B1 (en) * 2012-12-28 2015-01-12 주식회사 포스코 Method for manufacturing sintered bulk of raw materials, and growing nethod for single crystal using sintered bulk
KR102237931B1 (en) * 2014-01-23 2021-04-08 엘지이노텍 주식회사 Preparing method of silicon carbide powder
KR102402639B1 (en) 2017-11-24 2022-05-26 삼성전자주식회사 Electronic device and method for communicating thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6048398A (en) 1995-10-04 2000-04-11 Abb Research Ltd. Device for epitaxially growing objects
KR20070015447A (en) * 2004-06-17 2007-02-02 신닛뽄세이테쯔 카부시키카이샤 Silicon carbide single crystal and single crystal wafer
KR20070036654A (en) * 2005-09-29 2007-04-03 네오세미테크 주식회사 Growing method of semi-conducting sic single crystal with low resitivity

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6048398A (en) 1995-10-04 2000-04-11 Abb Research Ltd. Device for epitaxially growing objects
KR20070015447A (en) * 2004-06-17 2007-02-02 신닛뽄세이테쯔 카부시키카이샤 Silicon carbide single crystal and single crystal wafer
KR20070036654A (en) * 2005-09-29 2007-04-03 네오세미테크 주식회사 Growing method of semi-conducting sic single crystal with low resitivity

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