CN113445122A - Method and device for improving growth efficiency and quality of SiC crystal - Google Patents
Method and device for improving growth efficiency and quality of SiC crystal Download PDFInfo
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- CN113445122A CN113445122A CN202010213648.2A CN202010213648A CN113445122A CN 113445122 A CN113445122 A CN 113445122A CN 202010213648 A CN202010213648 A CN 202010213648A CN 113445122 A CN113445122 A CN 113445122A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/36—Carbides
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Abstract
The invention discloses a method and a device for improving the growth efficiency and quality of SiC crystals, wherein the method comprises the following steps: obtaining gaseous Si through liquid Si; introducing gaseous CH4，CH4Cracking at a set temperature, then reacting with gaseous Si, pulling and rotating seed crystals in a protective gas atmosphere to realize the regulation and control of a thermal field at the growth front edge of the SiC crystal, the stability and the growth of the large-mass SiC monocrystal, and obtaining the SiC crystal ingot. The device is used for realizing the method and comprises the following steps: a crucible isolation layer and a heating unit; an isolation unit is arranged in the crucible, a first outlet is formed in the isolation unit, a first inlet connected with a first gas source is formed above the isolation unit, a second outlet connected with a gas processing unit is formed above the crucible, a seed crystal rotary lifting unit is arranged at the top of the interior of the crucible, and seed crystals are arranged below the seed crystal rotary lifting unit; and by increasing the arrangement of the laser beam, the regulation and control of the thermal field at the front of the crystal growth are provided, thereby being beneficial to the crystal diameterOptimizing growth uniformity and adjusting axial temperature gradient.
Description
Technical Field
The invention relates to the field of crystal growth in semiconductor device technology, in particular to a method and a device for improving the growth efficiency and quality of SiC crystals.
Background
Compared with silicon materials, silicon carbide (SiC) has the advantages of high critical breakdown electric field, high electron mobility and the like, is an excellent semiconductor material for manufacturing high-voltage, high-temperature and anti-radiation power semiconductor devices, and is also a third-generation semiconductor material with the best comprehensive performance, the highest commercialization degree and the most mature technology at present.
In contrast to silicon materials, SiC materials have major properties including:
(1) the critical breakdown electric field intensity is nearly 10 times of that of silicon material;
(2) the thermal conductivity is high and exceeds 3 times of that of silicon materials;
(3) the saturated electron drift velocity is high and is 2 times of that of silicon material;
(4) good radiation resistance and chemical stability.
The growth rate of SiC crystal by PVT (physical-vapor-transport) method commonly used in the industry at present is about 0.3mm/Hour, the growth rate of SiC crystal is very slow, the yield is difficult to improve, and the preparation of SiC crystal substrate material becomes the bottleneck restricting the development of SiC industry. Because the prior art takes SiC as raw material to obtain SiC crystal: obtaining gaseous SiC by heating SiC powder, crystal growth is carried out using a seed crystal, however, SiC and SiC are sublimated due to heating by SiC solid powder2、Si2C. The process of gaseous reaction substances such as Si, C and the like is slow, so that the growth process is slow and low in efficiency.
Therefore, a method for improving the growth efficiency and quality of SiC crystals is needed.
Disclosure of Invention
In view of the above-mentioned shortcomings of the prior art, the present invention at least aims to provide a method and an apparatus for improving the growth efficiency and quality of SiC crystal, aiming to improve the growth efficiency and quality of SiC crystal.
To achieve the above and other related objects, one embodiment of the present invention provides a method for improving the growth efficiency and quality of SiC crystals, comprising the steps of:
obtaining gaseous Si through liquid Si;
introducing gaseous CH4Said CH4Cracking at a set temperature, then reacting with the gaseous Si, pulling and rotating the seed crystal in a protective gas atmosphere to realize the regulation and control of a thermal field at the growth front of the SiC crystal, the stability and the growth of the large-mass SiC monocrystal, and obtaining the SiC crystal ingot.
Optionally, before the step of performing SiC crystal growth, the method further comprises the steps of:
and (5) carrying out thermal field modulation on the front edge of the crystal growth.
Optionally, the step of performing crystal growth front thermal field modulation comprises:
and modulating a thermal field of a crystal growth front by adjusting a laser beam, wherein the laser beam is positioned below the SiC crystal ingot.
Optionally, the step of obtaining gaseous Si from liquid Si comprises:
and evaporating the liquid Si to obtain gaseous Si.
Optionally, characterized in that the shielding gas comprises Ar.
To achieve the above and other related objects, an embodiment of the present invention provides an apparatus for implementing the method, including:
the crucible is provided with an isolation layer at the periphery, and a heating unit is arranged at the periphery of the isolation layer;
an isolation unit is arranged in a cavity in the crucible, the isolation unit is provided with a first outlet, a first inlet is arranged above the isolation unit, and the first inlet penetrates through the isolation layer to be connected with a first gas source;
a second outlet is arranged above the crucible and penetrates through the isolation layer to be connected with the gas processing unit;
and a seed crystal rotating and pulling unit is arranged at the top inside the crucible, and a seed crystal is arranged below the seed crystal rotating and pulling unit.
Optionally, the heating unit comprises an induction coil for heating.
Optionally, the barrier layer comprises a graphite barrier layer.
Optionally, the first gas source comprises Ar and CH gases4。
Optionally, the crucible temperature control device further comprises a laser, wherein the laser is arranged in the middle of the cavity of the crucible and used for modulating a thermal field at the front of the crystal growth so as to be beneficial to optimization of radial growth uniformity and adjustment of axial temperature gradient.
According to the technical scheme provided by the embodiment of the invention, the Si element environment with high efficiency and high purity is provided through evaporation of the Si solution, and CH is utilized4The controllable C element atmosphere is provided by the high-temperature cracking of the gas, and the temperature (the highest temperature is 2380 ℃) of the crystal growth chamber is far lower than the temperature (the highest temperature is 2800 ℃) required by the traditional PVT, so the heating cost can be further saved by utilizing the method.
The method is characterized in that a crystal growth front thermal field modulation mechanism is arranged, namely a laser is arranged below a SiC crystal ingot, the crystal ingot is integrally moved upwards in a rotating and pulling mode along with the growth of the crystal ingot, so that a thermal field emitted by the laser below the crystal ingot surrounds the crystal ingot to be grown all the time, namely, the stability of the crystal growth front thermal field is realized, the temperature of the laser can be adjusted by adjusting the laser, namely, the modulation of the crystal growth front thermal field is realized, namely, the regulation and the stability of the SiC crystal growth front thermal field and the growth of the SiC single crystal with large quality are realized, and the SiC crystal ingot with high growth efficiency and large quality is obtained.
Drawings
FIG. 1 is a schematic diagram of an apparatus for preparing SiC crystal by conventional PVT process;
FIG. 2 is a flow chart of a method for improving the growth efficiency and quality of SiC crystals according to an embodiment of the present invention;
FIG. 3 is a graph showing the distribution of laser temperature and crystal growth front surface temperature as a function of wafer size in accordance with one embodiment of the present invention;
FIG. 4 is a graph showing the temperature profile of the laser and the temperature at the center and edge of the crystal over time, in accordance with one embodiment of the present invention;
FIG. 5 is a block diagram (without a laser) of an apparatus for improving the efficiency and quality of SiC crystal growth according to one embodiment of the present invention;
FIG. 6 is a graph showing the vertical temperature profile of a crystal growth chamber during a PVT process;
FIG. 7 is a graph showing the vertical temperature profile of the crystal growth chamber according to one embodiment of the present invention;
FIG. 8 is a schematic diagram of an apparatus for improving the growth efficiency and quality of SiC crystals with a laser according to an embodiment of the present invention;
fig. 9 is a bottom view of a laser and a SiC ingot according to an embodiment of the invention.
Description of the element reference numerals
Detailed Description
The following description of the embodiments of the present invention is provided for illustrative purposes, and other advantages and effects of the present invention will become apparent to those skilled in the art from the present disclosure.
It should be understood that the terms "upper", "lower", "left", "right", "middle" and "one" used herein are for clarity of description only, and are not intended to limit the scope of the invention, and that changes or modifications in the relative relationship may be made without substantial technical changes and modifications.
As shown in fig. 1, a conventional PVT production apparatus includes: graphite crucible 01, graphite crucible 01 is equipped with graphite isolation layer 02 outward, graphite isolation layer 02 is equipped with heating coil 03 outward, heating coil 03's temperature distribution presents: a tendency to increase from top to bottom. Using powdered SiC crystal, Si gas, SiC gas, Si are obtained by heating with heating coil 032C gas, SiC2A gas. TheseThe gas may undergo the following chemical reaction:
thus, use is made of SiC in the gas2The gas reacts with the Si gas to produce SiC crystals, the top end of the graphite crucible 03 is provided with seed crystals 04, and the grown SiC crystals are arranged below the seed crystals 04.
As shown in fig. 2, an embodiment of the present invention provides a method for improving the growth efficiency and quality of SiC crystal, including the steps of:
obtaining gaseous Si through liquid Si;
introducing gaseous CH4Said CH4Cracking at a set temperature, then reacting with the gaseous Si, pulling and rotating the seed crystal in a protective gas atmosphere to facilitate the regulation and control and the stability of a thermal field at the growth front of the SiC crystal and the growth of the large-mass SiC single crystal, and growing the SiC crystal to obtain the SiC crystal ingot. The set temperature is 1000 ℃ to 1500 ℃, the methane gas can be cracked at 1000 ℃, and nearly complete cracking can be realized at 1500 ℃.
Providing an environment of Si element of high efficiency and high purity by evaporation of Si solution, using CH4The controllable C element atmosphere is provided by the high-temperature cracking of the gas, and the temperature (the highest temperature is 2380 ℃) of the crystal growth chamber is far lower than the temperature (the highest temperature is 2800 ℃) required by the traditional PVT by the method, so the heating cost can be further saved by utilizing the method; meanwhile, the seed crystal is fixed in a pulling and rotating mode so as to be beneficial to regulation and control of a thermal field at the growth front of the SiC crystal, stability and growth of the SiC single crystal with large quality.
In the technical scheme of the invention, the reaction temperature range of the crystal growth chamber is 1800-2380 ℃, wherein the temperature is gradually increased from bottom to top and then gradually decreased, and the highest point of the temperature is distributed at a distance of 20-30mm from the top end of the reaction chamber.
The temperature range required for PVT in the prior art is 2300 to 2800 degrees celsius and even higher. And the height range of the reaction chamber corresponding to the method is larger, so that the method can obtain crystals with high quality and high efficiency, and the power consumption of the method is far lower than that of the prior art.
In one embodiment, the step of obtaining gaseous Si from liquid Si comprises:
and evaporating the liquid Si to obtain gaseous Si.
The temperature requirement of the heating unit by using the liquid Si is much lower than that of the liquid Si in comparison with that of the solid Si, and the whole power consumption is favorably reduced.
In one embodiment, the shielding gas comprises Ar.
And stable crystals can be obtained by using argon for protection.
In one embodiment, the step of performing SiC crystal growth further comprises, before the step of performing SiC crystal growth, the steps of:
and (5) carrying out thermal field modulation on the front edge of the crystal growth.
The uniformity of radial growth of the crystal is provided by the leading edge thermal field modulation, and the adjustment of axial temperature gradient can be realized.
In one embodiment, the step of performing crystal growth front thermal field modulation comprises:
and modulating a thermal field of a crystal growth front by adjusting a laser beam, wherein the laser beam is positioned below the SiC crystal ingot.
The laser is arranged below the SiC crystal ingot, and the crystal ingot is integrally moved upwards in a rotating and pulling mode along with the growth of the crystal ingot, so that a thermal field emitted by laser emitted by the laser below the crystal ingot surrounds the crystal ingot to be grown all the time, namely, the stability of a thermal field at the front of crystal growth is realized, and the temperature of the laser can be adjusted by adjusting the laser, namely, the modulation of the thermal field at the front of crystal growth is realized.
As shown in fig. 3-4, the central temperature is maintained at a substantially constant level, the temperature outside the central point is periodically fluctuated with the action of the laser light, and the temperature difference between the central temperature and the edge temperature of the crystal surface is small, at the same laser temperature, by the laser beam located below the ingot. A mode of additionally arranging a laser beam is adopted to provide a regulating and controlling mechanism of a thermal field at the front edge of crystal growth so as to be beneficial to optimizing radial growth uniformity and adjusting axial temperature gradient.
As shown in fig. 5, one embodiment of the present invention provides an apparatus for improving the growth efficiency and quality of SiC crystal, for implementing the above method, including:
the crucible comprises a crucible 1, wherein an isolation layer 2 is arranged on the periphery of the crucible, and a heating unit 3 is arranged on the periphery of the isolation layer;
an isolation unit 4 is arranged in a cavity inside the crucible, the isolation unit is provided with a first outlet 5, a first inlet 6 is arranged above the isolation unit, the first inlet penetrates through the isolation layer to be connected with a first gas source, and liquid Si is stored in the crucible cavity below the isolation unit; the first outlet 5 is for the output of gaseous Si.
A second outlet 7 is arranged above the crucible, and the second outlet 7 penetrates through the isolation layer to be connected with the gas processing unit; the gas treatment unit comprises an exhaust gas treatment module and/or a gas recycling module.
And a seed crystal rotating and pulling unit is arranged at the top inside the crucible, and a seed crystal 8 is arranged below the seed crystal rotating and pulling unit. The seed crystal rotating and pulling unit is beneficial to the regulation and control and the stability of the thermal field at the growth front edge of the SiC crystal and the growth of the large-mass SiC single crystal, thereby obtaining the SiC crystal with high growth efficiency and high quality. The high quality at least comprises the meaning of high quality and large quality.
The seed crystal rotating and pulling unit can rotate and pull the seed crystal in the crystal growth process so as to obtain the crystal ingot 9 with higher growth efficiency, better quality and higher quality.
Fig. 6 and 7 show that: the traditional PVT grows SiC crystal becauseThe SiC powder is used as a raw material, so that the required temperature is high, the lowest temperature is 2300 ℃ and the highest temperature is 2800 ℃; the technical scheme of the invention provides a Si element environment with high efficiency and high purity by evaporation of Si solution, and CH is utilized4The high temperature cracking of the gas provides an adjustable C element atmosphere, and the temperature range of the crystal growth chamber by the method is as follows: the minimum temperature is 1800 ℃ and the maximum temperature is 2380 ℃, which is far lower than the temperature required by the traditional PVT, so the heating cost can be saved by using the method. Meanwhile, since the conventional PVT adopts the method of obtaining Si gas, SiC gas and Si by heating and evaporating SiC powder2C gas, SiC2Gases, reuse of SiC in gas reactions2The gas reacts with Si gas to produce SiC crystal, so the temperature in the crystal growth reaction chamber gradually rises from top to bottom, the highest temperature is positioned below the reaction chamber, and CH is adopted in the invention4The fission obtains the C atmosphere, so the temperature in the crystal growth reaction chamber of the technical scheme of the invention tends to increase and then decrease from top to bottom, and the highest temperature is positioned at the upper part in the middle of the reaction chamber.
In one embodiment, the crucible is a graphite crucible.
In one embodiment, the heating unit comprises an electric induction coil for heating.
In one embodiment, the barrier layer comprises a graphite barrier layer.
In one embodiment, the first gas source comprises Ar and CH gases4。
The first gas source comprises protective gas argon and methane, and better C atmosphere is obtained by cracking methane at high temperature, so that SiC crystal can be better obtained.
As shown in fig. 8, in one embodiment, the crucible further comprises a laser 10, the laser is disposed in the middle of the cavity of the crucible, and the laser 10 emits laser 11 to facilitate radial growth uniformity optimization and adjustment of axial temperature gradient, so as to ensure uniformity of the surface temperature of the crystal.
Fig. 9 shows a bottom view of the laser and SiC ingot. The effect after adding the laser is shown in fig. 2-3, the central temperature is maintained at a constant level basically under the same laser temperature by the laser beam positioned below the crystal ingot, the temperature outside the central point is maintained in a small range to do periodic fluctuation along with the action of the laser, and the temperature difference range of the central temperature and the edge temperature of the crystal surface is small. A mode of additionally installing laser beams is adopted to provide a regulating mechanism of a thermal field at the front edge of crystal growth so as to be beneficial to optimizing the radial growth uniformity and adjusting the axial temperature gradient, thereby improving the radial growth uniformity of the crystal.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (10)
1. A method for improving the growth efficiency and quality of SiC crystals is characterized by comprising the following steps:
obtaining gaseous Si through liquid Si;
introducing gaseous CH4Said CH4Cracking at a set temperature, then reacting with the gaseous Si, pulling and rotating the seed crystal in a protective gas atmosphere to realize the regulation and control of a thermal field at the growth front of the SiC crystal, the stability and the growth of the large-mass SiC monocrystal, and obtaining the SiC crystal ingot.
2. The method of claim 1 further comprising the step of, prior to the step of growing the SiC crystal:
and (5) carrying out thermal field modulation on the front edge of the crystal growth.
3. A method of improving the growth efficiency and quality of a SiC crystal according to claim 2, wherein the step of performing thermal field modulation of the crystal growth front comprises:
and modulating a thermal field of a crystal growth front by adjusting a laser beam, wherein the laser beam is positioned below the SiC crystal ingot.
4. A method of improving the growth efficiency and quality of SiC crystals according to claim 1, wherein the step of obtaining gaseous Si from liquid Si comprises:
and evaporating the liquid Si to obtain gaseous Si.
5. The method of claim 1 wherein the shielding gas comprises Ar.
6. An apparatus for implementing the method of any of claims 1-5, comprising:
the crucible is provided with an isolation layer at the periphery, and a heating unit is arranged at the periphery of the isolation layer;
an isolation unit is arranged in a cavity in the crucible, the isolation unit is provided with a first outlet, a first inlet is arranged above the isolation unit, and the first inlet penetrates through the isolation layer to be connected with a first gas source;
a second outlet is arranged above the crucible and penetrates through the isolation layer to be connected with the gas processing unit;
and a seed crystal rotating and pulling unit is arranged at the top inside the crucible, and a seed crystal is arranged below the seed crystal rotating and pulling unit.
7. The device for improving the growth efficiency and quality of the SiC crystal according to claim 6, wherein the heating unit comprises an induction coil for heating.
8. An apparatus for increasing the efficiency and quality of SiC crystal growth according to claim 6, wherein the isolation layer comprises a graphite isolation layer.
9. The apparatus of claim 6 wherein the first gas source comprises Ar and CH gases4。
10. The device for improving the growth efficiency and the quality of the SiC crystal according to claim 6, further comprising a laser, wherein the laser is arranged in the middle of the cavity of the crucible and is used for modulating a thermal field of a crystal growth front so as to be beneficial to optimization of radial growth uniformity and adjustment of axial temperature gradient.
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Citations (6)
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| JPH09268099A (en) * | 1996-03-29 | 1997-10-14 | Toyota Central Res & Dev Lab Inc | Production of single crystal of silicon carbide |
| US5985024A (en) * | 1997-12-11 | 1999-11-16 | Northrop Grumman Corporation | Method and apparatus for growing high purity single crystal silicon carbide |
| CN1570225A (en) * | 2003-04-24 | 2005-01-26 | 奥克麦蒂克有限公司 | Device and method for producing single crystals by vapor deposition |
| TW200506088A (en) * | 2003-04-24 | 2005-02-16 | Okmetic Oyj | Device and method for producing single crystals by vapour deposition |
| CN101426965A (en) * | 1998-10-09 | 2009-05-06 | 克里公司 | Production of bulk single crystals of silicon carbide |
| CN105543967A (en) * | 2016-02-02 | 2016-05-04 | 北京华进创威电子有限公司 | Raw material treatment method for growing 4H high-purity silicon carbide monocrystal form by stable PVT (physical vapor transport) process |
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2020
- 2020-03-24 CN CN202010213648.2A patent/CN113445122B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09268099A (en) * | 1996-03-29 | 1997-10-14 | Toyota Central Res & Dev Lab Inc | Production of single crystal of silicon carbide |
| US5985024A (en) * | 1997-12-11 | 1999-11-16 | Northrop Grumman Corporation | Method and apparatus for growing high purity single crystal silicon carbide |
| CN101426965A (en) * | 1998-10-09 | 2009-05-06 | 克里公司 | Production of bulk single crystals of silicon carbide |
| CN1570225A (en) * | 2003-04-24 | 2005-01-26 | 奥克麦蒂克有限公司 | Device and method for producing single crystals by vapor deposition |
| TW200506088A (en) * | 2003-04-24 | 2005-02-16 | Okmetic Oyj | Device and method for producing single crystals by vapour deposition |
| CN105543967A (en) * | 2016-02-02 | 2016-05-04 | 北京华进创威电子有限公司 | Raw material treatment method for growing 4H high-purity silicon carbide monocrystal form by stable PVT (physical vapor transport) process |
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