CN103820768A - Homogeneous and rapid epitaxial growth method of 4H-SiC epitaxial layer on 4H-SiC substrate - Google Patents
Homogeneous and rapid epitaxial growth method of 4H-SiC epitaxial layer on 4H-SiC substrate Download PDFInfo
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- CN103820768A CN103820768A CN201410086800.XA CN201410086800A CN103820768A CN 103820768 A CN103820768 A CN 103820768A CN 201410086800 A CN201410086800 A CN 201410086800A CN 103820768 A CN103820768 A CN 103820768A
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Abstract
The invention discloses a homogeneous and rapid epitaxial growth method of a 4H-SiC epitaxial layer on a 4H-SiC substrate. The method comprises the steps as follows: firstly, the 4H-SiC substrate is cleaned and placed in a growth chamber of vertical hot-wall low-voltage CVD (chemical vapor deposition) equipment; a reaction chamber is subjected to vacuum-pumping; pressure of the reaction chamber is set, and hydrogen stream is introduced into the reaction chamber; the reaction chamber is heated to the etching temperature, and the substrate is subjected to in-situ etching; the hydrogen stream is adjusted, the temperature of the reaction chamber is increased, growing source gas is introduced for preliminary growth when the temperature of the reaction chamber is up to the preliminary growth temperature, and the growing source gas flow is adjusted for epitaxial growth after the temperature is up to the growth temperature; after the growth ends, the growing source gas is closed, the heating is stopped, and the substrate is cooled in the hydrogen stream; and after the reaction chamber is subjected to vacuum-pumping, the substrate is continuously cooled in the hydrogen stream to the room temperature, and then argon is introduced to the growth chamber to the atmospheric pressure. According to the homogeneous and rapid epitaxial growth method of the 4H-SiC epitaxial layer on the 4H-SiC substrate, the epitaxial growth rate is increased, high-speed homogeneous epitaxial growth of 4H-SiC is realized, and a very thick high-quality 4H-SiC epitaxial layer is obtained in shorter growing time.
Description
Technical field
The invention belongs to technical field of semiconductor, what relate to is the epitaxial growth method of carbofrax material, specifically relates to the method for the quick epitaxy 4H-SiC of homogeneity epitaxial film on a kind of 4H-SiC substrate, and institute's growth material can be used for device preparation.
Background technology
Silicon carbide (SiC) is as third generation semiconductor material, having the features such as broad-band gap, high critical breakdown electric field, high heat conductance, high electronics saturation drift velocity, high physical and chemical stability, is the semiconductor material of making high temperature, high-power, high pressure resistant, anti-irradiation device.These good characteristics make it be with a wide range of applications in fields such as aerospace, high voltage power transmission, electric locomotive, electromobiles.
In the time utilizing 4H-SiC material to make device, obtain high pressure resistant (> 10kV) device, need thickness to be at least the 4H-SiC epitaxial film of 100 μ m as the drift layer of device.Utilize traditional epitaxy method to prepare thick film epitaxial material, epitaxy speed is about 6-8 μ m/h, causes the 4H-SiC epitaxial film epitaxy time will spend a few hours, and this is unfavorable for the industrial saving production time.Therefore,, in order to overcome this problem, be just necessary that epitaxy speed is risen to dozens or even hundreds of micron per hour.
In order to improve 4H-SiC epitaxy speed, growth source gas flow need to be improved.Because growth source gas can heatedly decompose in the process of ingress, growth room and arrival substrate surface, silicon source gas thermal degradation goes out Siliciumatom, and these Siliciumatoms can mutually combine.In the time that silicon source gas flow improves, its amount that decomposites Siliciumatom can increase, the degree that silicon is combined with silicon also can increase, these Siliciumatoms are combined together to form the aggregation of silicon, these aggregations for the epitaxy of 4H-SiC be do not have contributive, this has just caused exhausting of silicon source, thereby has also just limited the raising of epitaxy speed.And these aggregations can drop at substrate surface, epi-layer surface is caused severe contamination and causes surface imperfection, make epitaxial film cannot be applied to element manufacturing.
In sum, in order to obtain the high speed epitaxy speed of 4H-SiC epitaxial film, realize quick extension, need to solve the restricted problem of epitaxial process silicon aggregation for growth velocity.Use low growth pressure, large flow H
2, the processing condition such as higher growth temperature are conducive to overcome this problem, thereby improve epitaxy speed.Lower growth pressure can reduce the density of silicon composition, thereby prevents to a certain extent mutually combining of silicon and silicon.The H of large flow
2can suppress silicon hydride and decomposite Siliciumatom, thereby reduce the content of Siliciumatom in atmosphere, prevent that silicon is combined with silicon.High growth temperature can promote silicon aggregation again to decomposite the contributive activated silica composition of growing to 4H-SiC, when reducing and eliminate silicon aggregation, has improved the content of activated silica composition, thereby improves epitaxy speed.
Summary of the invention
(1) technical problem that will solve
In view of this, main purpose of the present invention has been to provide the method for the quick epitaxy 4H-SiC of homogeneity epitaxial film on a kind of 4H-SiC substrate, to solve the restricted problem of silicon aggregation for epitaxy speed, realize two-forty epitaxy, and obtain an epi-layer surface of polluting without silicon aggregation.
(2) technical scheme
For achieving the above object, the invention provides the method for the quick epitaxy 4H-SiC of homogeneity epitaxial film on a kind of 4H-SiC substrate, comprising:
Step 1: 4H-SiC substrate is cleaned and put into the growth room of vertical hot wall low pressure chemical vapor deposition equipment, and reaction chamber is vacuumized;
Step 2: reaction chamber pressure is set, and to the logical hydrogen stream of reaction chamber;
Step 3: original position etching, to etching temperature, is carried out to substrate in reacting by heating chamber;
Step 4: regulate hydrogen stream the reaction chamber temperature that raises, when reaction chamber temperature reaches pregrown temperature, pass into growth source gas and carry out pregrown, temperature reaches after growth temperature, and growth regulation source gas flow carries out epitaxy;
Step 5: after growth finishes, close growth source gas, and stop heating, cooling in hydrogen stream;
Step 6: temperature drops to 1000 ℃ when following, closes hydrogen, and reaction chamber is vacuumized;
Step 7: after reaction chamber is vacuumized, argon gas is passed into reaction chamber and carry out cooling;
Step 8: be cooled to after room temperature, reaction chamber is filled with to argon gas, make air pressure reach atmospheric pressure.
In such scheme, 4H-SiC substrate is cleaned described in step 1, adopts RCA standard cleaning technique, and the scavenging solution of use comprises sulfuric acid, hydrogen peroxide, hydrofluoric acid, ammoniacal liquor, hydrochloric acid and deionized water.
In such scheme, the silicon carbide CVD equipment described in step 1 is vertical hot wall low pressure chemical vapor deposition equipment, and it is that reaction chamber is evacuated to 10 that reaction chamber is vacuumized
-4below Torr.
In such scheme, described in step 2 reaction chamber pressure being set, is that reaction chamber pressure is set as between 10Torr~80Torr; Described to the logical hydrogen stream of reaction chamber, hydrogen flowing quantity is 1L/ minute~10L/ minute, and pressure rises to be set after pressure, keeps reaction chamber invariablenes pressure of liquid; Regulate H
2flow, between 3L/ minute~50L/ minute and base runoff, continues to pass into reaction chamber.
In such scheme, reacting by heating chamber described in step 3 is to etching temperature, substrate is carried out to original position etching, comprise: open RF radio-frequency coil induction heater, reaction chamber temperature is heated between 1350 ℃~1500 ℃ and fixed temperature, at this temperature, maintain 10 minutes~60 minutes, 4H-SiC substrate is carried out to original position etching.
In such scheme, the adjusting hydrogen stream described in step 4 reaction chamber temperature that raises, when reaction chamber temperature reaches pregrown temperature, pass into growth source gas and carry out pregrown, temperature reaches after growth temperature, and growth regulation source gas flow carries out epitaxy, comprise: after etching is complete, by H
2flow-rate adjustment is 10L/ minute~100L/ minute base runoff, and rising reaction chamber temperature, when temperature rise to 1560 ℃, passes into the C of the low discharge of certain carbon element silicon ratio
2h
4and SiH
4gas, carries out 4H-SiC pregrown; Continue reaction chamber temperature to be heated between 1600 ℃~1750 ℃ and fixed temperature; Then, by C
2h
4flow progressively rises to 8mL/ minute~300mL/ minute, SiH
4flow progressively rises to 20mL/ minute~300mL/ minute, under fixing carbon element silicon ratio, carries out epitaxy; The epitaxy time is more than 30 minutes.
In such scheme, the C of described low discharge
2h
4and SiH
4gas, C
2h
4flow is 0.4mL/ minute~5mL/ minute, SiH
4flow is 1mL/ minute~5mL/ minute.The C of the low discharge of described certain carbon element silicon ratio
2h
4and SiH
4gas, wherein carbon element silicon ratio is fixed between 0.8~2, SiH
4and H
2flow proportional be no more than 0.6%;
In such scheme, the reaction chamber that argon gas is passed into described in step 7 carries out coolingly, and argon flow amount is 0.3L/ minute~20L/ minute, and pressure when logical argon gas is cooling is 10Torr~700Torr.
(3) beneficial effect
1, the method for the quick epitaxy 4H-SiC of homogeneity epitaxial film on this 4H-SiC substrate provided by the invention, by being used low growth pressure, higher growth temperature, larger H
2flow, has avoided the formation of silicon aggregation, has realized the 4H-SiC isoepitaxial growth of two-forty, and has obtained the epi-layer surface of polluting without silicon aggregation.
2, the method for the quick epitaxy 4H-SiC of homogeneity epitaxial film on this 4H-SiC substrate provided by the invention, in shorter growth time, has obtained very thick 4H-SiC epitaxial film.
3, the method for the quick epitaxy 4H-SiC of homogeneity epitaxial film on this 4H-SiC substrate provided by the invention, the growth source gas C of use
2h
4and SiH
4non-corrosiveness, can simplify growth apparatus and improve the security of producing.
Accompanying drawing explanation
Fig. 1 is the method flow diagram of the quick epitaxy 4H-SiC of homogeneity epitaxial film on 4H-SiC substrate provided by the invention;
Fig. 2 is the process flow sheet of the quick epitaxy 4H-SiC of homogeneity epitaxial film on 4H-SiC substrate provided by the invention;
Fig. 3 is the schematic diagram according to the reaction chamber of the vertical hot wall low pressure chemical vapor deposition equipment of the use of the embodiment of the present invention.
Embodiment
For making the object, technical solutions and advantages of the present invention clearer, below in conjunction with specific embodiment, and with reference to accompanying drawing, the present invention is described in more detail.
As shown in Figure 1, Fig. 1 is the method flow diagram of the quick epitaxy 4H-SiC of homogeneity epitaxial film on 4H-SiC substrate provided by the invention, the object of the method is to solve the limiting factor that 4H-SiC isoepitaxial growth speed improves, under high growth rates, obtain high-quality 4H-SiC thick film, to be applied to high tension apparatus preparation, implementation step is:
Step 1: 4H-SiC substrate is cleaned and put into the growth room of vertical hot wall low pressure chemical vapor deposition equipment, and reaction chamber is vacuumized; Wherein, 4H-SiC substrate is cleaned, adopt RCA standard cleaning technique, the scavenging solution of use comprises sulfuric acid, hydrogen peroxide, hydrofluoric acid, ammoniacal liquor, hydrochloric acid and deionized water etc.; Silicon carbide CVD equipment is vertical hot wall low pressure chemical vapor deposition equipment; It is that reaction chamber is evacuated to 10 that reaction chamber is vacuumized
-4below Torr;
Step 2: reaction chamber pressure is set, and to the logical hydrogen stream of reaction chamber;
Reaction chamber pressure is set as between 10Torr~80Torr, H
2pass into reaction chamber, flow is 1L/ minute~10L/ minute, and pressure rises to be set after pressure, keeps reaction chamber invariablenes pressure of liquid; Regulate H
2flow, between 3L/ minute~50L/ minute and base runoff, continues to pass into reaction chamber;
Step 3: original position etching, to etching temperature, is carried out to substrate in reacting by heating chamber;
Open RF radio-frequency coil induction heater, reaction chamber temperature is heated between 1350 ℃~1500 ℃ and fixed temperature, at this temperature, maintain 10 minutes~60 minutes, 4H-SiC substrate is carried out to original position etching;
Step 4: regulate hydrogen stream the reaction chamber temperature that raises, when reaction chamber temperature reaches pregrown temperature, pass into growth source gas and carry out pregrown, temperature reaches after growth temperature, and growth regulation source gas flow carries out epitaxy;
After etching is complete, by H
2flow-rate adjustment is 10L/ minute~100L/ minute base runoff, and rising reaction chamber temperature, when temperature rise to 1560 ℃, passes into the C of the low discharge of certain carbon element silicon ratio
2h
4and SiH
4gas, carries out 4H-SiC pregrown; Continue reaction chamber temperature to be heated between 1600 ℃~1750 ℃ and fixed temperature; Then, by C
2h
4flow progressively rises to 8mL/ minute~300mL/ minute, SiH
4flow progressively rises to 20mL/ minute~300mL/ minute, under fixing carbon element silicon ratio, carries out epitaxy; The epitaxy time is more than 30 minutes;
Wherein, the C of low discharge
2h
4and SiH
4gas, C
2h
4flow is 0.4mL/ minute~5mL/ minute, SiH
4flow is 1mL/ minute~5mL/ minute; The C of the low discharge of certain carbon element silicon ratio
2h
4and SiH
4gas, wherein carbon element silicon ratio is fixed between 0.8~2, SiH
4and H
2flow proportional be no more than 0.6%;
Step 5: after growth finishes, close growth source gas, and stop heating, cooling in hydrogen stream;
After growth finishes, close C
2h
4and SiH
4gas, then closes RF radio-frequency coil induction heater; Continue to pass into H
2carry out cooling;
Step 6: temperature drops to 1000 ℃ when following, closes hydrogen, and reaction chamber is vacuumized;
Step 7: after reaction chamber is vacuumized, argon gas is passed into reaction chamber and carry out cooling; Wherein argon flow amount is 0.3L/ minute~20L/ minute, and pressure when logical argon gas is cooling is 10Torr~700Torr;
Step 8: be cooled to after room temperature, reaction chamber is filled with to argon gas, make air pressure reach atmospheric pressure.
The present invention has improved epitaxy speed, has realized the isoepitaxial growth of 4H-SiC high speed, in shorter growth time, has obtained very thick high quality 4H-SiC epitaxial film.
With reference to Fig. 2, Fig. 2 is the process flow sheet of the quick epitaxy 4H-SiC of homogeneity epitaxial film on 4H-SiC substrate provided by the invention, specifically comprises the following steps:
With reference to Fig. 2, Fig. 2 is the process flow sheet of the quick epitaxy 4H-SiC of homogeneity epitaxial film on 4H-SiC substrate provided by the invention, specifically comprises the following steps:
With reference to Fig. 2, Fig. 2 is the process flow sheet of the quick epitaxy 4H-SiC of homogeneity epitaxial film on 4H-SiC substrate provided by the invention, specifically comprises the following steps:
Above-described specific embodiment; object of the present invention, technical scheme and beneficial effect are further described; institute is understood that; the foregoing is only specific embodiments of the invention; be not limited to the present invention; within the spirit and principles in the present invention all, any modification of making, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (9)
1. a method for the quick epitaxy 4H-SiC of homogeneity epitaxial film on 4H-SiC substrate, is characterized in that, comprising:
Step 1: 4H-SiC substrate is cleaned and put into the growth room of vertical hot wall low pressure chemical vapor deposition equipment, and reaction chamber is vacuumized;
Step 2: reaction chamber pressure is set, and to the logical hydrogen stream of reaction chamber;
Step 3: original position etching, to etching temperature, is carried out to substrate in reacting by heating chamber;
Step 4: regulate hydrogen stream the reaction chamber temperature that raises, when reaction chamber temperature reaches pregrown temperature, pass into growth source gas and carry out pregrown, temperature reaches after growth temperature, and growth regulation source gas flow carries out epitaxy;
Step 5: after growth finishes, close growth source gas, and stop heating, cooling in hydrogen stream;
Step 6: temperature drops to 1000 ℃ when following, closes hydrogen, and reaction chamber is vacuumized;
Step 7: after reaction chamber is vacuumized, argon gas is passed into reaction chamber and carry out cooling;
Step 8: be cooled to after room temperature, reaction chamber is filled with to argon gas, make air pressure reach atmospheric pressure.
2. the method for the quick epitaxy 4H-SiC of homogeneity epitaxial film on 4H-SiC substrate according to claim 1, it is characterized in that, 4H-SiC substrate is cleaned described in step 1, adopt RCA standard cleaning technique, the scavenging solution of use comprises sulfuric acid, hydrogen peroxide, hydrofluoric acid, ammoniacal liquor, hydrochloric acid and deionized water.
3. the method for the quick epitaxy 4H-SiC of homogeneity epitaxial film on 4H-SiC substrate according to claim 1, it is characterized in that, silicon carbide CVD equipment described in step 1 is vertical hot wall low pressure chemical vapor deposition equipment, and it is that reaction chamber is evacuated to 10 that reaction chamber is vacuumized
-4below Torr.
4. the method for the quick epitaxy 4H-SiC of homogeneity epitaxial film on 4H-SiC substrate according to claim 1, is characterized in that, described in step 2 reaction chamber pressure is set, and is that reaction chamber pressure is set as between 10Torr~80Torr; Described to the logical hydrogen stream of reaction chamber, hydrogen flowing quantity is 1L/ minute~10L/ minute, and pressure rises to be set after pressure, keeps reaction chamber invariablenes pressure of liquid; Regulate H
2flow, between 3L/ minute~50L/ minute and base runoff, continues to pass into reaction chamber.
5. the method for the quick epitaxy 4H-SiC of homogeneity epitaxial film on 4H-SiC substrate according to claim 1, is characterized in that, original position etching, to etching temperature, is carried out to substrate in the reacting by heating chamber described in step 3, comprising:
Open RF radio-frequency coil induction heater, reaction chamber temperature is heated between 1350 ℃~1500 ℃ and fixed temperature, at this temperature, maintain 10 minutes~60 minutes, 4H-SiC substrate is carried out to original position etching.
6. the method for the quick epitaxy 4H-SiC of homogeneity epitaxial film on 4H-SiC substrate according to claim 1, it is characterized in that, adjusting hydrogen stream described in step 4 reaction chamber temperature that raises, when reaction chamber temperature reaches pregrown temperature, pass into growth source gas and carry out pregrown, temperature reaches after growth temperature, and growth regulation source gas flow carries out epitaxy, comprising:
After etching is complete, by H
2flow-rate adjustment is 10L/ minute~100L/ minute base runoff, and rising reaction chamber temperature, when temperature rise to 1560 ℃, passes into the C of the low discharge of certain carbon element silicon ratio
2h
4and SiH
4gas, carries out 4H-SiC pregrown; Continue reaction chamber temperature to be heated between 1600 ℃~1750 ℃ and fixed temperature; Then, by C
2h
4flow progressively rises to 8mL/ minute~300mL/ minute, SiH
4flow progressively rises to 20mL/ minute~300mL/ minute, under fixing carbon element silicon ratio, carries out epitaxy; The epitaxy time is more than 30 minutes.
7. the method for the quick epitaxy 4H-SiC of homogeneity epitaxial film on 4H-SiC substrate according to claim 6, is characterized in that the C of described low discharge
2h
4and SiH
4gas, C
2h
4flow is 0.4mL/ minute~5mL/ minute, SiH
4flow is 1mL/ minute~5mL/ minute.
8. the method for the quick epitaxy 4H-SiC of homogeneity epitaxial film on 4H-SiC substrate according to claim 6, is characterized in that, the C of the low discharge of described certain carbon element silicon ratio
2h
4and SiH
4gas, wherein carbon element silicon ratio is fixed between 0.8~2, SiH
4and H
2flow proportional be no more than 0.6%.
9. the method for the quick epitaxy 4H-SiC of homogeneity epitaxial film on 4H-SiC substrate according to claim 1, it is characterized in that, reaction chamber that argon gas is passed into described in step 7 carries out cooling, argon flow amount is 0.3L/ minute~20L/ minute, and pressure when logical argon gas is cooling is 10Torr~700Torr.
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Cited By (5)
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CN104131336A (en) * | 2014-07-22 | 2014-11-05 | 西安电子科技大学 | Hydrogen flow control N-type low-doped silicon carbide film epitaxial making method |
CN104514034A (en) * | 2015-01-08 | 2015-04-15 | 中国科学院半导体研究所 | High-temperature device and method for silicon carbide growth |
CN105632901A (en) * | 2016-02-02 | 2016-06-01 | 北京华进创威电子有限公司 | Method for obtaining silicon carbide substrate by dry-type etching method |
CN108439329A (en) * | 2018-03-14 | 2018-08-24 | 河南科技大学 | A kind of preparation method of micro-nano mold type groove |
CN112136203A (en) * | 2018-05-23 | 2020-12-25 | 三菱电机株式会社 | Method for manufacturing SiC epitaxial substrate |
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CN104131336A (en) * | 2014-07-22 | 2014-11-05 | 西安电子科技大学 | Hydrogen flow control N-type low-doped silicon carbide film epitaxial making method |
CN104514034A (en) * | 2015-01-08 | 2015-04-15 | 中国科学院半导体研究所 | High-temperature device and method for silicon carbide growth |
CN104514034B (en) * | 2015-01-08 | 2017-10-27 | 中国科学院半导体研究所 | High temperature service and method for growth of silicon carbide |
CN105632901A (en) * | 2016-02-02 | 2016-06-01 | 北京华进创威电子有限公司 | Method for obtaining silicon carbide substrate by dry-type etching method |
CN108439329A (en) * | 2018-03-14 | 2018-08-24 | 河南科技大学 | A kind of preparation method of micro-nano mold type groove |
CN112136203A (en) * | 2018-05-23 | 2020-12-25 | 三菱电机株式会社 | Method for manufacturing SiC epitaxial substrate |
CN112136203B (en) * | 2018-05-23 | 2024-04-09 | 三菱电机株式会社 | Method for manufacturing SiC epitaxial substrate |
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