CN104018217A - 4H-SiC homoepitaxial growth method - Google Patents
4H-SiC homoepitaxial growth method Download PDFInfo
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- CN104018217A CN104018217A CN201410260580.8A CN201410260580A CN104018217A CN 104018217 A CN104018217 A CN 104018217A CN 201410260580 A CN201410260580 A CN 201410260580A CN 104018217 A CN104018217 A CN 104018217A
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- silicon carbide
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Abstract
The invention relates to a homoepitaxial method on a 4H-SiC substrate, which comprises the following steps: putting a silicon carbide substrate in a reaction chamber of silicon carbide CVD (chemical vapor deposition) equipment, and vacuumizing the reaction chamber; introducing H2, and carrying out in-situ etching for 10 minutes; lowering the pressure of the reaction chamber is 40 mbars, keeping the temperature and pressure constant, introducing 42 mL/minute SiH4 and 14 mL/minute C3H8, and carrying out epitaxial growth for 2 hours to obtain a substrate slice with a silicon carbide epitaxial layer; and when the temperature drops to 700 DEG C, vacuumizing the reaction chamber, charging Ar, and naturally cooling the substrate slice to room temperature in the argon environment. The 4H-SiC homoepitaxial growth method greatly enhances the growth rate of the epitaxial layer, greatly saves the production cost, and reduces the waste of resources.
Description
Technical field
The present invention relates to field of manufacturing semiconductor devices, relate in particular to a kind of low pressure 4H-SiC isoepitaxial growth method.
Background technology
Silicon carbide (SiC) has the advantages such as broad-band gap, high critical breakdown strength, high heat conductance, high saturated electron drift velocity and high bonding energy, being the starting material of making the semiconducter device such as high temperature, high pressure, high frequency, high-power, anti-irradiation, is also the main raw of making micro-electromechanical system (MEMS) under " extreme electronics device " and extreme condition; In addition, SiC is a kind of good light-emitting semiconducting material, is not only suitable for making opto-electronic semiconductor module, also can utilize the characteristic of its broad-band gap and low current to make ultraviolet sensitivity device.Because SiC material has these superior characteristics, it is all had a wide range of applications in fields such as chemical industry, Aerospace Engineering, automobile industry, mineral processing and exploitation, nuclear power engineerings.
Chemical vapor deposition (CVD) is one of common method of growth SiC iso-epitaxy at present.Utilizing in CVD method growth SiC epitaxial film process, SiH
4and C
3h
8as growth source gas, H
2as carrier gas.The SiC power electronic devices of preparation work under high pressure needs thick SiC epitaxial film, and for the preparation of thick film SiC epitaxial film, adopts the growth time that common process (5 μ m/h) need to be very long, greatly increased preparation cost.
Raising source gas SiH
4and C
3h
8more than flow can be brought up to 10 μ m/h by the growth velocity of SiC extension, but be the nucleation of component of the same race in gas phase by increasing source gas flow with the subject matter that method was run into that obtains high growth rates, the appearance that Si drips.If air-flow can not drip Si to transport out vitellarium timely, will cause growth velocity to reach capacity, Si drip also can deposition substrate on, cause the degeneration of epitaxial surface pattern and the reduction of quality of materials, this all can make a big impact to follow-up device manufacture and device performance.
Summary of the invention
The object of the invention is to the defect for above-mentioned prior art, a kind of 4H-SiC isoepitaxial growth method is provided, to solve the lower problem of SiC outer layer growth speed under common process condition, overcome the larger problem of SiC epi-layer surface defect concentration under the gas flow condition of high source simultaneously.
For achieving the above object, the invention provides a kind of iso-epitaxy method on 4H-SiC substrate, said method comprising the steps of:
Step S1, is placed into silicon carbide substrates in the reaction chamber of silicon carbide CVD equipment, and reaction chamber is evacuated;
Step S2, passes into hydrogen H to reaction chamber
2until reaction chamber air pressure arrives 100mbar, keep reaction chamber air pressure constant, then by H
2flow increases to 64L/min gradually, continues to ventilate to reaction chamber;
Step S3, raises to 1400 DEG C reaction chamber temperature gradually, carries out the original position etching of 10 minutes;
Step S4, is increased to 1580 DEG C-1620 DEG C by temperature, and reaction chamber pressure is reduced to 40mbar, keeps temperature and invariablenes pressure of liquid, opens SiH
4and C
3h
8switch, pass into the SiH of 42mL/min
4c with 14mL/min
3h
8, carry out the epitaxy of 2 hours, obtain the long substrate slice that has silicon carbide epitaxial layers;
Step S5, after stopping growing, continues to pass into H in reaction chamber
2, substrate slice is lowered the temperature in hydrogen stream;
Step S6, when temperature is reduced to 700 DEG C, then is evacuated reaction chamber, and is filled with Ar, makes substrate slice naturally cool to room temperature under ar gas environment.
Further, in described step S1, silicon carbide substrates is specially 4 ° of drift angle silicon carbide substrates.
Further, in described step S1, reaction chamber is pumped into air pressure lower than 1 × 10
-7the vacuum of mbar.
Further, described step S3 specifically comprises: open radio-frequency coil induction heater RF, increase gradually the power of this well heater, reaction chamber temperature is raise gradually to 1400 DEG C, carry out the original position etching of 10 minutes.
Further, in described step S4, reaction chamber pressure is 40mbar.
Further, described step S5 specifically comprises: after the epitaxy time reaches 2 hours of setting, close C
3h
8and SiH
4switch, stop growing; Then the H that leads to reaction chamber is set
2flow is 20L/min, and keeping reaction chamber air pressure is 100mbar, makes the long substrate cooling 25min in hydrogen stream that has silicon carbide epitaxial layers; Again reaction chamber air pressure is elevated to 700mbar, in hydrogen stream, continues cooling.
Further, described step S6 specifically comprises: when reaction chamber temperature is reduced to after 700 DEG C, close the H that leads to reaction chamber
2switch; Reaction chamber is vacuumized, until air pressure is lower than 1 × 10
-7mbar, then open Ar switch, pass into reaction chamber the Ar that flow is 12L/min, make length have the substrate of silicon carbide epitaxial layers under ar gas environment, to continue cooling 30min; Slowly improve reaction chamber air pressure to normal pressure, make substrate naturally cool to room temperature, take out silicon carbide epitaxy sheet.
4H-SiC isoepitaxial growth method of the present invention grows silicon carbide epitaxial layers in 4 ° of drift angle silicon carbide substrates, with respect to common iso-epitaxy on the substrate that has drift angle used, significantly improve the growth velocity of epitaxial film, save to a great extent production cost, reduced the waste of resource.Adopt low-pressure growth technique, overcome the gas-phase nucleation problem of component of the same race under the gas flow condition of high source, obtain smooth surface, ladder gathering groups and triangle defect is less, the measured 4H-SiC homogeneity epitaxial layer of crystalline, can be used for the device manufacture of SiC.
Brief description of the drawings
Fig. 1 is the schema of the iso-epitaxy method on 4H-SiC substrate of the present invention.
Embodiment
Below by drawings and Examples, technical scheme of the present invention is described in further detail.
Fig. 1 is the schema of the iso-epitaxy method on 4H-SiC substrate of the present invention, and as shown in the figure, present method specifically comprises the following steps:
Step 101, is placed into silicon carbide substrates in the reaction chamber of silicon carbide CVD equipment, and reaction chamber is evacuated;
Step 102, passes into hydrogen H to reaction chamber
2until reaction chamber air pressure arrives 100mbar, keep reaction chamber air pressure constant, then by H
2flow increases to 64L/min gradually, continues to ventilate to reaction chamber;
Step 103, raises to 1400 DEG C reaction chamber temperature gradually, carries out the original position etching of 10 minutes;
Step 104, is increased to 1580 DEG C-1620 DEG C by temperature, and reaction chamber pressure is reduced to 40mbar, keeps temperature and invariablenes pressure of liquid, opens SiH
4and C
3h
8switch, pass into the SiH of 42mL/min
4c with 14mL/min
3h
8, carry out the epitaxy of 2 hours, obtain the long substrate slice that has silicon carbide epitaxial layers;
Step 105, after stopping growing, continues to pass into H in reaction chamber
2, substrate slice is lowered the temperature in hydrogen stream;
Step 106, when temperature is reduced to 700 DEG C, then is evacuated reaction chamber, and is filled with Ar, makes substrate slice naturally cool to room temperature under ar gas environment.
Embodiment 1
Step 1, is placed into silicon carbide substrates in the reaction chamber of silicon carbide CVD equipment.
Concrete, choose the 4H-SiC substrate of 4 ° of drift angles, after cleaning, be placed in the reaction chamber of silicon carbide CVD equipment; Reaction chamber is vacuumized, until reaction chamber air pressure is lower than 1 × 10
-7mbar.
Step 2, reacting by heating chamber in hydrogen stream.
Concrete, open the H that leads to reaction chamber
2switch, controls its flow and increases to gradually 64L/min; Open the gas of vacuum pump abstraction reaction chamber, keep reaction chamber air pressure at 100mbar; Tune up gradually the power of RF heating source, reaction chamber temperature is slowly raise.
Step 3, carries out original position etching to substrate.
Concrete, when reaction chamber temperature reaches after 1400 DEG C, keep the constant original position etching of carrying out 10 minutes of reaction chamber temperature.
Step 4, arranges growth conditions, starts growing silicon carbide epitaxial film.
Concrete, after reaction chamber temperature reaches 1580 DEG C, reaction chamber pressure is reduced to 40mbar, keep reaction chamber temperature and invariablenes pressure of liquid; Open C
3h
8and SiH
4switch, pass into the SiH of 42mL/min
4c with 14mL/min
3h
8, growing silicon carbide epitaxial film.
Step 5, cooling substrate in hydrogen stream.
Concrete, after the epitaxy time reaches 2 hours of setting, close C
3h
8and SiH
4switch, stop growing; The H of reaction chamber is led in setting
2flow is 20L/min, and keeping reaction chamber air pressure is 100mbar, makes the long substrate cooling 25min in hydrogen stream that has silicon carbide epitaxial layers; Reaction chamber air pressure is elevated to 700mbar, in hydrogen stream, continues cooling.
Step 6, cooling substrate in argon gas.
Concrete, when reaction chamber temperature is reduced to after 700 DEG C, close the H that leads to reaction chamber
2switch; Reaction chamber is vacuumized, until air pressure is lower than 1 × 10
-7mbar; Open argon gas switch, pass into reaction chamber the Ar that flow is 12L/min, make length have the substrate of silicon carbide epitaxial layers under ar gas environment, to continue cooling 30min; Slowly improve reaction chamber air pressure to normal pressure, make substrate naturally cool to room temperature, take out silicon carbide epitaxy sheet.
Embodiment 2
Step 1, chooses the 4H-SiC substrate of 4 ° of drift angles, is placed in the reaction chamber of silicon carbide CVD equipment; Reaction chamber is vacuumized, until reaction chamber air pressure is lower than 1 × 10
-7mbar.
Step 2, opens the H that leads to reaction chamber
2switch, controls hydrogen flowing quantity and increases to gradually 64L/min, opens the gas of vacuum pump abstraction reaction chamber simultaneously, keeps reaction chamber air pressure at 100mbar; Tune up gradually the power of RF heating source, reaction chamber temperature is slowly raise, after reaction chamber temperature arrives 1400 DEG C, carry out the original position etching of 10min.
Step 3, when reaction chamber temperature reaches after 1600 DEG C, is reduced to 40mbar by pressure, keeps reaction chamber temperature and invariablenes pressure of liquid, opens C
3h
8and SiH
4switch, add the C that inbound traffics are 14mL/min
3h
8, the flow SiH that is 42mL/min
4, growing silicon carbide epitaxial film.
Step 5, after the epitaxy time reaches 2 hours of setting, closes C
3h
8and SiH
4switch, stop growing; Then the H that leads to reaction chamber is set
2flow is 20L/min, and keeping reaction chamber air pressure is 100mbar, makes the long substrate cooling 25min in hydrogen stream that has silicon carbide epitaxial layers; Again reaction chamber air pressure is elevated to 700mbar, in hydrogen stream, continues cooling.
Step 6, when reaction chamber temperature is reduced to after 700 DEG C, closes the H that leads to reaction chamber
2switch; Reaction chamber is vacuumized, until air pressure is lower than 1 × 10
-7mbar, then open Ar switch, pass into reaction chamber the Ar that flow is 12L/min, make length have the substrate of silicon carbide epitaxial layers under ar gas environment, to continue cooling 30min; Slowly improve reaction chamber air pressure to normal pressure, make substrate naturally cool to room temperature, take out silicon carbide epitaxy sheet.
Embodiment 3
Step 1, is placed into silicon carbide substrates in the reaction chamber of silicon carbide CVD equipment.
Concrete, choose the 4H-SiC substrate of 4 ° of drift angles, after cleaning, be placed in the reaction chamber of silicon carbide CVD equipment; Reaction chamber is vacuumized, until reaction chamber air pressure is lower than 1 × 10
-7mbar.
Step 2, reacting by heating chamber in hydrogen stream.
Concrete, open the H that leads to reaction chamber
2switch, controls its flow and increases to gradually 64L/min; Open the gas of vacuum pump abstraction reaction chamber, keep reaction chamber air pressure at 100mbar; Tune up gradually the power of RF heating source, reaction chamber temperature is slowly raise.
Step 3, carries out original position etching to substrate.
Concrete, when reaction chamber temperature reaches after 1400 DEG C, keep the constant original position etching of carrying out 10 minutes of reaction chamber temperature.
The 4th step, arranges growth conditions, starts growing silicon carbide epitaxial film.
Concrete, when reaction chamber temperature reaches after 1620 DEG C, pressure is reduced to 40mbar, keep reaction chamber temperature and invariablenes pressure of liquid; Open C
3h
8and SiH
4switch, in hydrogen stream, add the C that inbound traffics are 14mL/min simultaneously
3h
8, the flow SiH that is 42mL/min
4, growing silicon carbide epitaxial film.
The 5th step, cooling substrate in hydrogen stream.
Concrete, after the epitaxy time reaches 2 hours of setting, close C
3h
8and SiH
4switch, stop growing; The H of reaction chamber is led in setting
2flow is 20L/min, and keeping reaction chamber air pressure is 100mbar, makes the long substrate cooling 25min in hydrogen stream that has silicon carbide epitaxial layers; Reaction chamber air pressure is elevated to 700mbar, in hydrogen stream, continues cooling.
The 6th step, cooling substrate in argon gas.
Concrete, when reaction chamber temperature is reduced to after 700 DEG C, close the H that leads to reaction chamber
2switch; (6.2) reaction chamber is vacuumized, until air pressure is lower than 1 × 10
-7mbar; Open Ar switch, pass into reaction chamber the Ar that flow is 12L/min, make length have the substrate of silicon carbide epitaxial layers under ar gas environment, to continue cooling 30min; Slowly improve reaction chamber air pressure to normal pressure, make substrate naturally cool to room temperature, take out silicon carbide epitaxy sheet.
Embodiment 4
Step 1, is placed into silicon carbide substrates in the reaction chamber of silicon carbide CVD equipment.
Concrete, choose the 4H-SiC substrate of 4 ° of drift angles, after cleaning, be placed in the reaction chamber of silicon carbide CVD equipment; Reaction chamber is vacuumized, until reaction chamber air pressure is lower than 1 × 10
-7mbar.
Step 2, reacting by heating chamber in hydrogen stream.
Concrete, open the H that leads to reaction chamber
2switch, controls its flow and increases to gradually 64L/min; Open the gas of vacuum pump abstraction reaction chamber, keep reaction chamber air pressure at 100mbar; Tune up gradually the power of RF heating source, reaction chamber temperature is slowly raise.
Step 3, carries out original position etching to substrate.
Concrete, when reaction chamber temperature reaches after 1400 DEG C, keep the constant original position etching of carrying out 10 minutes of reaction chamber temperature.
The 4th step, arranges growth conditions, starts growing silicon carbide epitaxial film.
Concrete, after etching finishes, rise in 1580 DEG C of processes by 1400 DEG C at reaction chamber temperature, growth pressure is reduced to 40mbar by 100mbar, keep afterwards reaction chamber temperature and invariablenes pressure of liquid; Open C
3h
8and SiH
4switch, in hydrogen stream, add the C that inbound traffics are 14mL/min simultaneously
3h
8, the flow SiH that is 42mL/min
4, growing silicon carbide epitaxial film.
The 5th step, cooling substrate in hydrogen stream.
Concrete, after the epitaxy time reaches 2 hours of setting, close C
3h
8and SiH
4switch, stop growing; The H of reaction chamber is led in setting
2flow is 20L/min, and keeping reaction chamber air pressure is 100mbar, makes the long substrate cooling 25min in hydrogen stream that has silicon carbide epitaxial layers; Reaction chamber air pressure is elevated to 700mbar, in hydrogen stream, continues cooling.
The 6th step, cooling substrate in argon gas.
Concrete, when reaction chamber temperature is reduced to after 700 DEG C, close the H that leads to reaction chamber
2switch; Reaction chamber is vacuumized, until air pressure is lower than 1 × 10
-7mbar; Open Ar switch, pass into reaction chamber the Ar that flow is 12L/min, make length have the substrate of silicon carbide epitaxial layers under ar gas environment, to continue cooling 30min; Slowly improve reaction chamber air pressure to normal pressure, make substrate naturally cool to room temperature, take out silicon carbide epitaxy sheet.
4H-SiC isoepitaxial growth method of the present invention grows silicon carbide epitaxial layers in 4 ° of drift angle silicon carbide substrates, with respect to common iso-epitaxy on the substrate that has drift angle used, significantly improve the growth velocity of epitaxial film, save to a great extent production cost, reduced the waste of resource.Adopt low-pressure growth technique, overcome the gas-phase nucleation problem of component of the same race under the gas flow condition of high source, obtain smooth surface, ladder gathering groups and triangle defect is less, the measured 4H-SiC homogeneity epitaxial layer of crystalline, can be used for the device manufacture of SiC.
Above-described embodiment; object of the present invention, technical scheme and beneficial effect are further described; institute is understood that; the foregoing is only the specific embodiment of the present invention; the protection domain being not intended to limit the present invention; within the spirit and principles in the present invention all, any amendment of making, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (7)
1. the iso-epitaxy method on 4H-SiC substrate, is characterized in that, said method comprising the steps of:
Step S1, is placed into silicon carbide substrates in the reaction chamber of silicon carbide CVD equipment, and reaction chamber is evacuated;
Step S2, passes into hydrogen H to reaction chamber
2until reaction chamber air pressure arrives 100mbar, keep reaction chamber air pressure constant, then by H
2flow increases to 64L/min gradually, continues to ventilate to reaction chamber;
Step S3, raises to 1400 DEG C reaction chamber temperature gradually, carries out the original position etching of 10 minutes;
Step S4, is increased to 1580 DEG C-1620 DEG C by temperature, and reaction chamber pressure is reduced to 40mbar, keeps temperature and invariablenes pressure of liquid, opens SiH
4and C
3h
8switch, pass into the SiH of 42mL/min
4c with 14mL/min
3h
8, carry out the epitaxy of 2 hours, obtain the long substrate slice that has silicon carbide epitaxial layers;
Step S5, after stopping growing, continues to pass into H in reaction chamber
2, substrate slice is lowered the temperature in hydrogen stream;
Step S6, when temperature is reduced to 700 DEG C, then is evacuated reaction chamber, and is filled with Ar, makes substrate slice naturally cool to room temperature under ar gas environment.
2. method according to claim 1, is characterized in that, in described step S1, silicon carbide substrates is specially 4 ° of drift angle silicon carbide substrates.
3. method according to claim 1, is characterized in that, in described step S1, reaction chamber is pumped into air pressure lower than 1 × 10
-7the vacuum of mbar.
4. method according to claim 1, is characterized in that, described step S3 specifically comprises: open radio-frequency coil induction heater RF, increase gradually the power of this well heater, reaction chamber temperature is raise gradually to 1400 DEG C, carry out the original position etching of 10 minutes.
5. method according to claim 1, is characterized in that, in described step S4, reaction chamber pressure is 40mbar.
6. method according to claim 1, is characterized in that, described step S5 specifically comprises: after the epitaxy time reaches 2 hours of setting, close C
3h
8and SiH
4switch, stop growing; Then the H that leads to reaction chamber is set
2flow is 20L/min, and keeping reaction chamber air pressure is 100mbar, makes the long substrate cooling 25min in hydrogen stream that has silicon carbide epitaxial layers; Again reaction chamber air pressure is elevated to 700mbar, in hydrogen stream, continues cooling.
7. method according to claim 1, is characterized in that, described step S6 specifically comprises: when reaction chamber temperature is reduced to after 700 DEG C, close the H that leads to reaction chamber
2switch; Reaction chamber is vacuumized, until air pressure is lower than 1 × 10
-7mbar, then open Ar switch, pass into reaction chamber the Ar that flow is 12L/min, make length have the substrate of silicon carbide epitaxial layers under ar gas environment, to continue cooling 30min; Slowly improve reaction chamber air pressure to normal pressure, make substrate naturally cool to room temperature, take out silicon carbide epitaxy sheet.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110117814A (en) * | 2018-02-05 | 2019-08-13 | 西安电子科技大学 | The preparation method of silicon carbide epitaxy with low-density C vacancy defect |
| CN110117816A (en) * | 2018-02-05 | 2019-08-13 | 西安电子科技大学 | The method that low pressure prepares carborundum films extension |
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Application publication date: 20140903 |