CN105714380A - Silicon carbide epitaxial growth device and method - Google Patents
Silicon carbide epitaxial growth device and method Download PDFInfo
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- CN105714380A CN105714380A CN201610263330.9A CN201610263330A CN105714380A CN 105714380 A CN105714380 A CN 105714380A CN 201610263330 A CN201610263330 A CN 201610263330A CN 105714380 A CN105714380 A CN 105714380A
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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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- 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
- C30B25/02—Epitaxial-layer growth
- C30B25/14—Feed and outlet means for the gases; Modifying the flow of the reactive gases
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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
- C30B25/02—Epitaxial-layer growth
- C30B25/18—Epitaxial-layer growth characterised by the substrate
- C30B25/186—Epitaxial-layer growth characterised by the substrate being specially pre-treated by, e.g. chemical or physical means
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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
- C30B25/02—Epitaxial-layer growth
- C30B25/18—Epitaxial-layer growth characterised by the substrate
- C30B25/20—Epitaxial-layer growth characterised by the substrate the substrate being of the same materials as the epitaxial layer
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Abstract
The invention discloses a silicon carbide epitaxial growth device, comprising a cylinder body and a heating coil, wherein an inner cavity of the cylinder body is a reaction cavity; one end of the cylinder body is provided with a gas inlet, and the other end of the cylinder body is provided with a gas outlet; the side wall of the cylinder body sequentially comprises a quartz wall, a graphite soft felt layer and a graphite supporting layer from outside to inside; a substrate base is arranged on the graphite supporting layer; and a gas supply passage and an air-floatation gas supply passage, which are connected with an external gas source, are arranged in the graphite soft felt layer, wherein the gas outlet end of the air-floatation gas supply passage is arranged on the substrate base, a silicon carbide substrate is air-floated on the substrate base, and the gas outlet end of the gas supply passage is positioned above the silicon carbide substrate. According to the silicon carbide epitaxial growth device disclosed by the invention, a gas supply pipe is drawn in from the top of the reaction cavity, gas enters the reaction cavity from top to bottom to mix with gas at the inlet of the reaction cavity so as to form a silicon carbide epitaxial film on the silicon carbide substrate through reaction, and then the silicon carbide epitaxial film flows out of the reaction cavity, so that the purpose of quickly growing silicon carbide epitaxial wafers with uniform heights is achieved. The invention also discloses a silicon carbide epitaxial growth method using the device.
Description
Technical field
The present invention relates to technical field of semiconductor material preparation, particularly a kind of Device for epitaxial growth of silicon carbide, and use the silicon carbide epitaxial growth method of this device.
Background technology
Carborundum (SiC) is the third generation semi-conducting material grown up after first generation Semiconducting Silicon Materials, germanium and the second carrying semiconductor material GaAs, indium phosphide, the broad stopband of carbofrax material is 2~3 times of silicon and GaAs so that semiconductor device (more than 500 DEG C) can work and have the ability launching blue light at relatively high temperatures;High breakdown electric field is intended to a high order of magnitude than silicon and GaAs, determines the high pressure of semiconductor device, high-power performance;High saturated electron drift velocity and low-k determine the high frequency of device, high speed operation performance;Thermal conductivity is 3.3 times of silicon, 10 times of GaAs, it is meant that its good heat conductivity, it is possible to be greatly improved the integrated level of circuit, reduces cooling heat radiation system, thus greatly reducing the volume of complete machine.It can thus be anticipated that in the near future, constantly perfect along with carbofrax material and device technology, it is within sight to substitute that part Si field is carbonized silicon.There is due to carborundum the features such as broad-band gap, high critical breakdown strength, high thermal conductivity, the high saturated elegant speed of electronics, be particularly suitable for high-power, high-voltage power electronic device, become the study hotspot of current power electronic applications.
The main method growing SiC epitaxial material at present is chemical vapor transport method (CVD).The method can grow high-purity, large-sized SiC epitaxial wafer, and can efficiently reduce the various defects in SiC epitaxial material.Obtain high-quality epitaxial crystal and must accurately control multiple crystal growth parameters, as: depositing temperature, chamber pressure, chamber vacuum, each reacting gas dividing potential drop (proportioning) etc..
Chemical vapour deposition (CVD) principle: chemical vapor deposition growth carborundum (SiC) crystal closed reactor, external heat makes reative cell keep required reaction temperature, reacting gas SiH4By H2Or Ar carrier band, with C2H4Mixing, then pass into reactor together, decomposing under reacting gas high temperature and generate carborundum attachment substrate material surface, and constantly grow along material surface, reaction generation residual gas waste treatment device processes and emits.
It mainly includes following reaction: 2SiH4+C2H4=2SiC+6H2。
The epitaxy layer thickness that high-tension silicon carbide power electronic device needs reaches tens microns and arrives microns up to a hundred, the about 100um of epitaxial thickness that the device of general voltage 10kV needs, and silicon carbide epitaxial growth speed ripe at present only has about 5~7um/h, if growing the thick silicon carbide epitaxy material of 100um under such growth rate, need 14-20 hour, obviously manufacturing cost it is greatly increased, and the prolongation along with epitaxial growth cycle, more pollutant can be deposited in reactor wall, and then pollution epitaxial wafer, so to grow high-quality, thick silicon carbide epitaxial wafer must improve the growth rate of extension.
The silicon aggregation that the slow possible cause of growth rate is that the resolution ratio of reaction source gas is low and is easily formed in reacting gas, how to improve growth rate namely develop into the resolution ratio improving reaction source or suppress the generation of silicon aggregation, in prior art, by introducing Cl compound in reaction gas flow, utilize the corrasion of Cl element to suppress the formation of silicon aggregation, growth rate is improved with this, but the introducing of Cl compound, increase the equipment such as extra gas pipeline, and the tail gas environmental pollution containing Cl element is very big.
Additionally, growth course can exist " exhausting " phenomenon, refer to when reacting gas is parallel to substrate flow, above air-flow, concentration is bigger, the lower section concentration of air-flow is less, then substrate surface near air-flow position above epitaxial layer can thicker and can be thinner at the epitaxial layer at position near wind underside.
Epitaxial thickness needed for high voltage device is more thick, and the thickness offset caused by " exhausting " phenomenon is more serious, thus realize quick epitaxially grown while, also need solve non-uniformity problem.
Summary of the invention
For the defect existed in prior art, the invention provides the Device for epitaxial growth of silicon carbide of a kind of improvement;Present invention also offers a kind of silicon carbide epitaxial growth method using said apparatus.
To achieve these goals, technical scheme is as follows:
A kind of Device for epitaxial growth of silicon carbide, this device includes a horizontally disposed cylinder and is arranged on the heating coil outside this cylinder, the inner chamber of cylinder is reaction chamber, one end of this cylinder is provided with air inlet, the other end is provided with air vent, cylinder lateral wall is certainly extremely interior outward is quartz wall according to this, graphite soft felt layer and graphite supporting layer, described graphite supporting layer is provided with substrate pedestal, described graphite soft felt layer is provided with the air supply passage being connected with external air source and air supporting air supply channel, wherein, the outlet side of described air supporting air supply channel is arranged on described substrate pedestal, silicon carbide substrates air supporting is on substrate pedestal, the outlet side of described air supply passage is positioned at the top of silicon carbide substrates.
Further, the wall of described air supply passage and described air supporting air supply channel is made up of graphite, and the internal diameter of the two is 0.3~0.7cm.
Further, the inner surface of described graphite supporting layer, the inwall of described air supply passage and the inwall of air supporting air supply channel are coated with coating;Described coating is carborundum or ramet coating, and thickness is 50~70um.
Further, the inlet end of described air supply passage and described air supporting air supply channel is provided with gas flowmeter.
Further, the middle part of described silicon carbide substrates is corresponding to the outlet side of described air supporting air supply channel, and this outlet side is concordant with the upper surface of substrate pedestal;Giving vent to anger of described air supply passage is rectified in the middle part of this silicon carbide substrates, and its this outlet side is from silicon carbide substrates upper surface 4~11cm.
Further, the internal diameter of described cylinder is 15~32cm, and described quartz wall thickness is 5~10mm, and described graphite supporting layer thickness is 1.5~2.5cm, and described reaction chamber is cuboid, and described substrate pedestal is made up of graphite.
A kind of silicon carbide epitaxial growth method using said apparatus, the method comprises the steps:
A. charging: under normal pressure, substrate pedestal in the reactor chamber puts silicon carbide substrates;
B. heat temperature raising:, to described reaction chamber evacuation, backward reaction chamber in be filled with hydrogen to 2000~50000 handkerchiefs, and reaction chamber is heated to 900 DEG C~1600 DEG C;
C. in-situ etch: pass into hydrogen and/or hydrogen chloride in reaction chamber, and described silicon carbide substrates is carried out in-situ etch by carbon-source gas, brushes 5~10 minutes with hydrogen after 5~15 minutes;
D. growth is precipitated: reaction chamber heating is carried out silicon carbide epitaxial growth as reacting gas source to passing into silicon source, carbon source and adulterant after 1600~1700 DEG C.
Further, described carbon source is CH4、C2H4And C3H8In one or more combination in any.
Further, described silicon source is SiH4。
Further, described adulterant is trimethyl aluminium or nitrogen.
The present invention is by reaction chamber blowdown pipe introduced above, pass through blowdown pipe, air-flow enters reaction chamber from top to bottom and mixes with the air-flow of reaction chamber entrance, silicon carbide epitaxial film is formed on silicon carbide substrates through reaction, flow out reaction chamber again, reach the purpose of the silicon carbide epitaxial wafer of fast-growth high uniformity.At reaction chamber air supporting pipe introduced below, make wafer levitation by air supporting pipe air inlet, improve the thickness of epitaxial wafer and doping content is uneven and property.
Accompanying drawing explanation
Fig. 1 is the structural representation of Device for epitaxial growth of silicon carbide.
Detailed description of the invention
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is elaborated.
A kind of Device for epitaxial growth of silicon carbide of the present invention as shown in Figure 1, including cylinder 11 and heating coil 1, cylinder 11 is cylindrical, its inner hollow forms reaction chamber 9, the internal diameter of cylinder 11 is 15~32cm, one end of cylinder 11 is provided with air inlet 8, the other end is provided with air vent 5, it is respectively arranged with air intake installation and air-out apparatus near air inlet 8 and steam vent 5, cylinder 11 sidewall is certainly extremely interior outward is quartz wall 2 according to this, graphite soft felt layer 3 and graphite supporting layer 4, quartz wall 2 thickness is 4mm, graphite supporting layer 4 thickness is 1.5cm, graphite supporting layer 4 inwall is coated with coating, coating is carborundum, thickness is 70um, graphite supporting layer 4 is provided with substrate pedestal 6, graphite soft felt layer 10 is provided with the air supply passage 10 and air supporting air supply channel 7 that are connected with external air source, wherein, the outlet side of air supporting air supply channel 7 is arranged on substrate pedestal 6, silicon carbide substrates air supporting is on substrate pedestal 6, the outlet side of air supply passage 10 is positioned at the top of silicon carbide substrates.The middle part of silicon carbide substrates is corresponding to the outlet side of air supporting air supply channel 7, and this outlet side is concordant with the upper surface of substrate pedestal 6;Giving vent to anger of air supply passage 10 is rectified in the middle part of this silicon carbide substrates, and its this outlet side is from silicon carbide substrates upper surface 4~11cm.The wall of air supply passage 10 and air supporting air supply channel 7 is made up of graphite, is coated with coating in the inner side of wall, and this coating is carborundum or ramet coating, and thickness is 50~70um, and the internal diameter of air supply passage 10 and air supporting air supply channel 7 is 0.3~0.7cm.Inlet end at air supply passage 10 and air supporting air supply channel 7 is provided with gas flowmeter.
It is of course also possible to reaction chamber 9 is processed into cuboid.
Silicon carbide epitaxial growth method step is as follows:
A. charging: put into, in reaction chamber 9 after cleaning, the silicon carbide substrates cleaned through ultrasonic cleaning apparatus under normal pressure, and to pass into flotation gas hydrogen flowing quantity be 20sccm.
B. heat temperature raising: after reaction chamber 9 is adopted mechanical pump series connection diffusion pump evacuation, be filled with hydrogen in the reaction chamber 9 of vacuum to 2000 handkerchiefs, be warming up to 900 DEG C;Keep 5 minutes;
C. in-situ etch: pass into hydrogen and CH to reaction chamber 94Silicon carbide substrates is carried out in-situ etch and brushes 5 minutes with hydrogen after 10 minutes by gas;H2Flow is 10SLM;
D. growth is precipitated: heated after 1650 DEG C by reaction chamber 9 and pass into the gas SiH drying through gas purification apparatus, filtering, purify4(flow is 20SCCM), C2H4(flow is 10SCCM) and adulterant trimethyl aluminium (0.004SCCM) carry out epitaxial growth, gaseous state product H2Departing from from substrate material surface and remove, constantly pass into reacting gas, SiC film material constantly grows, and grows into target thickness and namely cuts off reaction source and power supply begins to cool down.
Growth thickness is the silicon carbide epitaxial wafer of 15um, and growth rate reaches 27um/h, and the time used is about 33 minutes.
Selecting 10 points in epitaxial wafer correspondence airflow direction position, measure corresponding one-tenth-value thickness 1/10, uniformity is 0.94%.
Above-mentioned example is only intended to the present invention is described, embodiments of the present invention are not limited to these examples, and the various detailed description of the invention of inventive concept that what those skilled in the art were made meet are all within protection scope of the present invention.
Claims (10)
1. a Device for epitaxial growth of silicon carbide, it is characterized in that, this device includes a horizontally disposed cylinder and is arranged on the heating coil outside this cylinder, the inner chamber of cylinder is reaction chamber, one end of this cylinder is provided with air inlet, the other end is provided with air vent, cylinder lateral wall is certainly extremely interior outward is quartz wall according to this, graphite soft felt layer and graphite supporting layer, described graphite supporting layer is provided with substrate pedestal, described graphite soft felt layer is provided with the air supply passage being connected with external air source and air supporting air supply channel, wherein, the outlet side of described air supporting air supply channel is arranged on described substrate pedestal, silicon carbide substrates air supporting is on substrate pedestal, the outlet side of described air supply passage is positioned at the top of silicon carbide substrates.
2. device as claimed in claim 1, it is characterised in that the wall of described air supply passage and described air supporting air supply channel is made up of graphite, and the internal diameter of the two is 0.3~0.7cm.
3. device as claimed in claim 2, it is characterised in that be coated with coating on the inner surface of described graphite supporting layer, the inwall of described air supply passage and the inwall of air supporting air supply channel;Described coating is carborundum or ramet coating, and thickness is 50~70um.
4. device as claimed in claim 1, it is characterised in that the inlet end of described air supply passage and described air supporting air supply channel is provided with gas flowmeter.
5. device as claimed in claim 1, it is characterised in that the middle part of described silicon carbide substrates is corresponding to the outlet side of described air supporting air supply channel, and this outlet side is concordant with the upper surface of substrate pedestal;Giving vent to anger of described air supply passage is rectified in the middle part of this silicon carbide substrates, and its this outlet side is from silicon carbide substrates upper surface 4~11cm.
6. device as claimed in claim 1, it is characterised in that the internal diameter of described cylinder is 15~32cm, and described quartz wall thickness is 5~10mm, and described graphite supporting layer thickness is 1.5~2.5cm, and described reaction chamber is cuboid, and described substrate pedestal is made up of graphite.
7. the silicon carbide epitaxial growth method using device described in the claims 1, it is characterised in that the method comprises the steps:
A. charging: under normal pressure, substrate pedestal in the reactor chamber puts silicon carbide substrates;
B. heat temperature raising:, to described reaction chamber evacuation, backward reaction chamber in be filled with hydrogen to 2000~50000 handkerchiefs, and reaction chamber is heated to 900 DEG C~1600 DEG C;
C. in-situ etch: pass into hydrogen and/or hydrogen chloride in reaction chamber, and described silicon carbide substrates is carried out in-situ etch by carbon-source gas, brushes 5~10 minutes with hydrogen after 5~15 minutes;
D. growth is precipitated: reaction chamber heating is carried out silicon carbide epitaxial growth as reacting gas source to passing into silicon source, carbon source and adulterant after 1600~1700 DEG C.
8. method as claimed in claim 7, it is characterised in that described carbon source is CH4、C2H4And C3H8In one or more combination in any.
9. method as claimed in claim 7, it is characterised in that described silicon source is SiH4。
10. method as claimed in claim 7, it is characterised in that described adulterant is trimethyl aluminium or nitrogen.
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Cited By (6)
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CN111020693A (en) * | 2019-12-27 | 2020-04-17 | 季华实验室 | Air inlet device of silicon carbide epitaxial growth equipment |
CN113945728A (en) * | 2021-10-18 | 2022-01-18 | 复旦大学 | Epitaxial reactor tray base rotational speed detection device and epitaxial reactor |
CN114507900A (en) * | 2022-03-04 | 2022-05-17 | 季华实验室 | Reaction cavity inner surface protection device, epitaxial reaction monitoring device and method |
CN114892147A (en) * | 2022-07-13 | 2022-08-12 | 芯三代半导体科技(苏州)有限公司 | Method for repairing graphite component of silicon carbide deposition equipment |
CN115613139A (en) * | 2022-12-01 | 2023-01-17 | 浙江晶越半导体有限公司 | Chemical vapor deposition reactor and method for epitaxially growing silicon carbide film |
CN116230597A (en) * | 2023-05-09 | 2023-06-06 | 内蒙古晶环电子材料有限公司 | Hydrogen etching tool and method for silicon carbide wafer |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN111020693A (en) * | 2019-12-27 | 2020-04-17 | 季华实验室 | Air inlet device of silicon carbide epitaxial growth equipment |
CN113945728A (en) * | 2021-10-18 | 2022-01-18 | 复旦大学 | Epitaxial reactor tray base rotational speed detection device and epitaxial reactor |
CN114507900A (en) * | 2022-03-04 | 2022-05-17 | 季华实验室 | Reaction cavity inner surface protection device, epitaxial reaction monitoring device and method |
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CN116230597A (en) * | 2023-05-09 | 2023-06-06 | 内蒙古晶环电子材料有限公司 | Hydrogen etching tool and method for silicon carbide wafer |
CN116230597B (en) * | 2023-05-09 | 2023-09-08 | 内蒙古晶环电子材料有限公司 | Hydrogen etching tool and method for silicon carbide wafer |
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