CN103422164A - Method for controlling N-type 4H-SiC homogenous epitaxial doping - Google Patents
Method for controlling N-type 4H-SiC homogenous epitaxial doping Download PDFInfo
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- CN103422164A CN103422164A CN2013103557493A CN201310355749A CN103422164A CN 103422164 A CN103422164 A CN 103422164A CN 2013103557493 A CN2013103557493 A CN 2013103557493A CN 201310355749 A CN201310355749 A CN 201310355749A CN 103422164 A CN103422164 A CN 103422164A
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Abstract
The invention discloses a method for controlling N-type 4H-SiC homogenous epitaxial doping. The method includes steps of placing silicon carbide substrates into a reaction chamber; heating the reaction chamber in hydrogen stream; adding C<3>H<8> into the hydrogen stream after the temperature of the reaction chamber reaches 1400 DEG C; performing in-situ etching on the substrates for 10-30 minutes after the temperature of the reaction chamber reaches 1580 DEG C; keeping the temperature of the reaction chamber at the temperature of 1580 DEG C, keeping the pressure of the reaction chamber within the range of 300mbar-700mbar, adding SiH<4> at a flow rate of 15-24mL/min, C<3>H<8> at a flow rate of 5-10mL/min and N<2> at a flow rate of 2L/min into the hydrogen stream at a rate of 80L/min and growing epitaxial layers; cooling the silicon carbide substrates in the hydrogen stream after the epitaxial layers complete growing; filling argon into the reaction chamber until the pressure of the reaction chamber reaches the normal pressure. The method has the advantages that only the pressure of the reaction chamber is changed, operation is simple and convenient, and the manufactured silicon carbide epitaxial layers are doped uniformly, have smooth surfaces and can be used for manufacturing silicon carbide devices.
Description
Technical field
The invention belongs to technical field of semiconductor, especially relate to a kind of N-type 4H-SiC iso-epitaxy doping control method, the epitaxial film grown can be used for the device manufacture of SiC.
Background technology
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, not only is suitable for making opto-electronic semiconductor module, also can utilize the characteristic of its broad-band gap and low current to make the ultraviolet sensitivity device.Because the 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.
In recent years, relevant carbofrax material related process progress is very fast, and the single-crystal silicon carbide substrate slice of 4 inches has been realized commercialization, and the aspects such as the extension of carbofrax material, oxidation, doping, etching, semiconductor alloy contact are all progressively ripe.
Silicon carbide has high chemistry and physical stability, makes its high temperature single crystal growing and chemical and mechanical treatment all very difficult.Therefore, the carbofrax material that is applied at present to manufacture device is all the epitaxial thin film material by the film preparing technology growth.Because the bonding strength of silicon carbide is high, the desired temperature of diffusion of contaminants is greater than 1800 ℃, substantially exceed the condition of normal component technique, so the doping in device making technics can not adopt diffusion technique, can only utilize extension controlled doping and high temperature ion implantation doping.
Employing high temperature is ion implantation, injects the ion pair lattice damage very large, causes a large amount of lattice imperfections, even annealing also is difficult to eliminate fully, has had a strong impact on the performance of device, and ion implantation efficiency is very low simultaneously, thereby is not suitable for doing the big area doping.In the MOCVD of silicon carbide epitaxy technique, usually adopt SiH
4And C
3H
8As reactant, N
2As the N-type doped source, hydrogen, as carrier gas, needs to control ratio, the reaction conditions of each reactant, just can reach high quality, the growth of two-forty, and reach needed doped level.Only have by reasonable adjustment growth parameter(s), grow defect few, doping reaches the epitaxial film of pre-provisioning request, just can produce the satisfactory device of performance, thereby the doping of silicon carbide epitaxial layers control is a very large difficult point during current device is manufactured.
Summary of the invention
Technical problem to be solved by this invention is: for the deficiency of above-mentioned prior art, a kind of N-type 4H-SiC iso-epitaxy doping control method is proposed, by controlling the air pressure of reaction chamber, prepare the epitaxial film of different levels of doping, solved the N-type 4H-SiC iso-epitaxy uppity technical barrier that adulterates.
For solving the problems of the technologies described above, technical scheme of the present invention is: a kind of N-type 4H-SiC iso-epitaxy doping control method comprises the steps:
(1) silicon carbide substrates is placed in the reaction chamber of silicon carbide CVD equipment, reaction chamber is evacuated;
(2) pass into H to reaction chamber
2Until reaction chamber air pressure arrives 300mbar～700mbar, in hydrogen stream, use heating source heated substrate gradually, make its temperature slowly increase, after temperature surpasses 1400 ℃, add the C that inbound traffics are 5～10mL/min in hydrogen stream
3H
8
(3) after reaction chamber temperature reaches 1550-1600 ℃ ℃, keep homo(io)thermism, continue to keep the C added in reaction chamber air pressure and hydrogen stream
3H
8Flow is constant, adopts H
2And C
3H
8Mixed gas carries out the original position etching of 10～30min to substrate;
(4) keep reaction chamber air pressure and homo(io)thermism, add the SiH that inbound traffics are 15～24mL/min in hydrogen stream
4, the C that flow is 5～10mL/min
3H
8With the flow N that is 1.8-2L/min
2, and pass into reaction chamber; Growth N-type epitaxial film;
(5) after the epitaxy time that reaches setting, stop growing, at reaction chamber, continue to pass into hydrogen, substrate slice is lowered the temperature in hydrogen stream;
(6) after temperature is reduced to below 700 ℃, again reaction chamber is evacuated, then slowly is filled with argon gas, make substrate slice naturally cool to room temperature under ar gas environment.
Preferably, the SiH in described step (4)
4And C
3H
8Flow ratio be controlled at 1.
Preferably, the flow that passes into Ar in described step (6) is 12L/min.
Adopted technique scheme, beneficial effect of the present invention is:
1. the present invention adopts the CVD epitaxial device of silicon carbide, at the carbonization substrate of silicon carbide substrates or existing epitaxial film, carries out extension, by growth parameter(s) controlled doping concentration, the preparation technology of device is simplified.
2. the present invention adopts nitrogen as doped source, and the nitrogen-atoms mixed can effectively be replaced Siliciumatom in carbofrax material, forms substitutional impurity, and with respect to ion implantation technology, the doped silicon carbide material lattice of preparation is complete, and defect is few, is conducive to improve device performance.
3. the present invention, with respect to existing silicon carbide epitaxy processing condition, only changes the air pressure of reaction chamber, and the flow that does not change doped source just can be controlled the doping content of epitaxial film, and the epitaxial film of preparing meets the requirement of device.
The accompanying drawing explanation
Fig. 1 is the silicon carbide CVD equipment structure chart that the present invention uses;
Fig. 2 is process flow sheet of the present invention.
Embodiment
Below in conjunction with drawings and Examples, the present invention is further described.
As shown in Figure 1, the silicon carbide CVD equipment that the present invention uses, mainly be comprised of main body growing system, RF induction heating source, exhaust treatment system, circulating water system, the steady origin system of voltage and interface operation system.
As shown in Figure 2, the present invention provides following three kinds of embodiment.
Embodiment 1
Step 1, be placed into silicon carbide substrates in the reaction chamber of silicon carbide CVD equipment.
(1.1) choose deflection
The 4H silicon carbide substrates that crystal orientation is 8 °, be placed in the reaction chamber of silicon carbide CVD equipment;
(1.2) reaction chamber is vacuumized, until reaction chamber air pressure is lower than 1 * 10
-7Mbar.
Step 2, reacting by heating chamber in hydrogen stream.
(2.1) open the hydrogen switch that leads to reaction chamber, control hydrogen flowing quantity and increase to gradually 80L/min;
(2.2) open the gas of vacuum pump abstraction reaction chamber, keep reaction chamber air pressure at 300mbar;
(2.3) tune up gradually heating source power, reaction chamber temperature is slowly raise, after temperature surpasses 1400 ℃, add the C that inbound traffics are 5mL/min in hydrogen stream
3H
8.
Step 3, carry out the original position etching to substrate.
(3.1) reach after 1550 ℃ when reaction chamber temperature, keep reaction chamber temperature constant;
(3.2) continue to pass into to reaction chamber the hydrogen that flow is 80L/min, and add the C that inbound traffics are 5mL/min in hydrogen stream
3H
8, at H
2And C
3H
8Situ etched substrate 10min.
Step 4, arrange growth conditions, starts the growing silicon carbide epitaxial film.
(4.1) controlling reaction chamber air pressure is 300mbar, and keeping temperature is 1550 ℃;
(4.2) open C
3H
8And SiH
4Switch, pass into the SiH of 15mL/min
4, the C of 5mL/min
3H
8N with 1.8L/min
2, the growing silicon carbide epitaxial film.
Step 5, cooling substrate in hydrogen stream.
(5.1) after the epitaxy time reaches the time of setting, close C
3H
8, SiH
4And N
2Switch, stop growing;
(5.2) H that leads to reaction chamber is set
2Flow is 20L/min, makes long substrate cooling 25min in hydrogen stream that silicon carbide epitaxial layers is arranged;
(5.3) reaction chamber air pressure is elevated to 700mbar, continues cooling in hydrogen stream.
Step 6, cooling substrate in argon gas.
(6.1) be reduced to after 700 ℃ when reaction chamber temperature, close the H that leads to reaction chamber
2Switch;
(6.2) reaction chamber is vacuumized, until air pressure is lower than 1 * 10
-7Mbar;
(6.3) open the argon gas switch, to reaction chamber, pass into the Ar that flow is 12L/min, make length have the substrate of silicon carbide epitaxial layers to continue cooling 30min under ar gas environment;
(6.4) slowly improve reaction chamber air pressure to normal pressure, make substrate naturally cool to room temperature, take out the silicon carbide epitaxy sheet.
Embodiment 2
Step 1, choose deflection
The 4H silicon carbide substrates that crystal orientation is 8 °, 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, open the H that leads to reaction chamber
2Switch, control hydrogen flowing quantity and increase to gradually 80L/min, opens the gas of vacuum pump abstraction reaction chamber simultaneously, keeps reaction chamber air pressure at 500mbar; Tune up gradually the power of RF heating source, reaction chamber temperature is slowly raise, after reaction chamber temperature arrives 1400 ℃, add the C that inbound traffics are 7mL/min in hydrogen stream
3H
8.
Step 3, when reaction chamber temperature reaches after 1580 ℃, keep reaction chamber temperature constant, keeps reaction chamber to pass into the H that flow is 80L/min
2With the flow C that is 7mL/min
3H
8, adopt H
2With C
3H
8Mixed gas original position etched substrate 20min.
Step 4, be 500mbar at reaction chamber air pressure, and temperature is under 1580 ℃, opens C
3H
8And SiH
4Switch, add the C that inbound traffics are 7mL/min
3H
8, the flow SiH that is 21mL/min
4, and the flow N that is 1.9L/min
2, the growing silicon carbide epitaxial film.
Step 5, after the epitaxy time reaches the time of setting, close C
3H
8, SiH
4And N
2Switch, stop growing; Then the H that leads to reaction chamber is set
2Flow is 20L/min, makes long substrate cooling 25min in hydrogen stream that silicon carbide epitaxial layers is arranged; Again reaction chamber air pressure is elevated to 700mbar, continues cooling in hydrogen stream.
Step 6, when reaction chamber temperature is reduced to after 700 ℃, close the H that leads to reaction chamber
2Switch; Reaction chamber is vacuumized, until air pressure is lower than 1 * 10
-7Mbar, then open the Ar switch, pass into to reaction chamber the Ar that flow is 12L/min, make length have the substrate of silicon carbide epitaxial layers to continue cooling 30min under ar gas environment; Slowly improve reaction chamber air pressure to normal pressure, make substrate naturally cool to room temperature, take out the silicon carbide epitaxy sheet.
Embodiment 3
The first step, choose deflection
The 4H silicon carbide substrates that crystal orientation is 8 °, 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.
Second step, open the H that leads to reaction chamber
2Switch, control hydrogen flowing quantity and increase to gradually 80L/min, opens the gas of vacuum pump abstraction reaction chamber simultaneously, keeps reaction chamber air pressure at 700mbar; Tune up gradually the power of RF heating source, reaction chamber temperature is slowly raise, after reaction chamber temperature arrives 1400 ℃, add the C that inbound traffics are 10mL/min in hydrogen stream
3H
8
The 3rd step, carry out the original position etching to substrate.
(3.1) reach after 1600 ℃ when reaction chamber temperature, keep reaction chamber temperature constant;
(3.2) continue to pass into to reaction chamber the H that flow is 80L/min
2With the flow C that is 10mL/min
3H
8, adopt H
2With C
3H
8Mixed gas original position etched substrate 10min.
The 4th step, arrange growth conditions, starts the growing silicon carbide epitaxial film.
(4.1) keeping reaction chamber air pressure is 700mbar, and temperature is 1600 ℃;
(4.2) open C
3H
8And SiH
4Switch, add the C that inbound traffics are 10mL/min in hydrogen stream simultaneously
3H
8, the flow SiH that is 24mL/min
4N with 2L/min
2, the growing silicon carbide epitaxial film.
The 5th step, cooling substrate in hydrogen stream.
(5.1) after the epitaxy time reaches 2 hours of setting, close C
3H
8And SiH
4Switch, stop growing;
(5.2) H that leads to reaction chamber is set
2Flow is 20L/min, makes long substrate cooling 25min in hydrogen stream that silicon carbide epitaxial layers is arranged;
(5.3) reaction chamber air pressure is elevated to 700mbar, continues cooling in hydrogen stream.
The 6th step, cooling substrate in argon gas.
(6.1) be reduced to after 700 ℃ when reaction chamber temperature, close the H that leads to reaction chamber
2Switch;
(6.2) reaction chamber is vacuumized, until air pressure is lower than 1 * 10
-7Mbar;
(6.3) open the Ar switch, to reaction chamber, pass into the Ar that flow is 12L/min, make length have the substrate of silicon carbide epitaxial layers to continue cooling 30min under ar gas environment;
(6.4) slowly improve reaction chamber air pressure to normal pressure, make substrate naturally cool to room temperature, take out the silicon carbide epitaxy sheet.
The present invention is not limited to above-mentioned concrete embodiment, and those of ordinary skill in the art is from above-mentioned design, and without performing creative labour, all conversion of having done, within all dropping on protection scope of the present invention.
Claims (3)
1. a N-type 4H-SiC iso-epitaxy doping control method, is characterized in that, comprises the steps:
(1) silicon carbide substrates is placed in the reaction chamber of silicon carbide CVD equipment, reaction chamber is evacuated;
(2) pass into H to reaction chamber
2Until reaction chamber air pressure arrives 300mbar～700mbar, in hydrogen stream, use heating source heated substrate gradually, make its temperature slowly increase, after temperature surpasses 1400 ℃, add the C that inbound traffics are 5～10mL/min in hydrogen stream
3H
8
(3) after reaction chamber temperature reaches 1550-1600 ℃, keep homo(io)thermism, continue to keep the C added in reaction chamber air pressure and hydrogen stream
3H
8Flow is constant, adopts H
2And C
3H
8Mixed gas carries out the original position etching of 10～30min to substrate;
(4) keep reaction chamber air pressure and homo(io)thermism, add the SiH that inbound traffics are 15～24mL/min in hydrogen stream
4, the C that flow is 5～10mL/min
3H
8With the flow N that is 1.8-2L/min
2, and pass into reaction chamber; Growth N-type epitaxial film;
(5) after the epitaxy time that reaches setting, stop growing, at reaction chamber, continue to pass into hydrogen, substrate slice is lowered the temperature in hydrogen stream;
(6) after temperature is reduced to below 700 ℃, again reaction chamber is evacuated, then slowly is filled with argon gas, make substrate slice naturally cool to room temperature under ar gas environment.
2. N-type 4H-SiC iso-epitaxy doping control method according to claim 1, is characterized in that the SiH in described step (4)
4And C
3H
8Flow ratio be controlled at 1.
3. N-type 4H-SiC iso-epitaxy doping control method according to claim 1, is characterized in that, the flow that passes into Ar in described step (6) is 12L/min.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104018216A (en) * | 2014-06-12 | 2014-09-03 | 西安电子科技大学 | 4H-SiC homoepitaxial growth system |
| 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 |
| CN104233461A (en) * | 2014-07-22 | 2014-12-24 | 西安电子科技大学 | Method for preparing N-type heavily-doped silicon carbide thin film epitaxy by controlling hydrogen flow |
| CN104233465A (en) * | 2014-07-22 | 2014-12-24 | 西安电子科技大学 | Preparation method for controlling epitaxial growth of heavily doped pressure N-type silicon carbide film |
| 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 |
| CN109576784A (en) * | 2017-09-29 | 2019-04-05 | 上海新昇半导体科技有限公司 | A kind of preparation method and device of SiC epitaxial layer |
| RU2691772C1 (en) * | 2018-03-06 | 2019-06-18 | Публичное Акционерное Общество "Электровыпрямитель" | Method for growth of epitaxial structure of monocrystalline silicon carbide with low density of epitaxial defects |
| CN112684832A (en) * | 2019-10-17 | 2021-04-20 | 中国石油化工股份有限公司 | Method and equipment for overcoming temperature reaction lag of silicon carbide annular carrier |
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| CN102610500A (en) * | 2012-03-22 | 2012-07-25 | 西安电子科技大学 | Method for preparing N-type heavily-doping silicon carbide film epitaxy |
| CN102859654A (en) * | 2010-05-10 | 2013-01-02 | 三菱电机株式会社 | Silicon carbide epitaxial wafer and process for production thereof, silicon carbide bulk substrate for epitaxial growth purposes and process for production thereof, and heat treatment apparatus |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104018216A (en) * | 2014-06-12 | 2014-09-03 | 西安电子科技大学 | 4H-SiC homoepitaxial growth system |
| 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 |
| CN104233461A (en) * | 2014-07-22 | 2014-12-24 | 西安电子科技大学 | Method for preparing N-type heavily-doped silicon carbide thin film epitaxy by controlling hydrogen flow |
| CN104233465A (en) * | 2014-07-22 | 2014-12-24 | 西安电子科技大学 | Preparation method for controlling epitaxial growth of heavily doped pressure N-type silicon carbide film |
| 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 |
| CN105632901B (en) * | 2016-02-02 | 2018-05-25 | 北京世纪金光半导体有限公司 | A kind of method that silicon carbide substrates are obtained using dry etching method |
| CN109576784A (en) * | 2017-09-29 | 2019-04-05 | 上海新昇半导体科技有限公司 | A kind of preparation method and device of SiC epitaxial layer |
| RU2691772C1 (en) * | 2018-03-06 | 2019-06-18 | Публичное Акционерное Общество "Электровыпрямитель" | Method for growth of epitaxial structure of monocrystalline silicon carbide with low density of epitaxial defects |
| CN112684832A (en) * | 2019-10-17 | 2021-04-20 | 中国石油化工股份有限公司 | Method and equipment for overcoming temperature reaction lag of silicon carbide annular carrier |
| CN112684832B (en) * | 2019-10-17 | 2022-01-28 | 中国石油化工股份有限公司 | Method and equipment for overcoming temperature reaction lag of silicon carbide annular carrier |
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Application publication date: 20131204 |