CN104131336A - Hydrogen flow control N-type low-doped silicon carbide film epitaxial making method - Google Patents

Hydrogen flow control N-type low-doped silicon carbide film epitaxial making method Download PDF

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Publication number
CN104131336A
CN104131336A CN201410350046.6A CN201410350046A CN104131336A CN 104131336 A CN104131336 A CN 104131336A CN 201410350046 A CN201410350046 A CN 201410350046A CN 104131336 A CN104131336 A CN 104131336A
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reaction chamber
silicon carbide
temperature
pass
purity
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CN201410350046.6A
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王悦湖
胡继超
张艺蒙
宋庆文
张玉明
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Xidian University
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Xidian University
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Abstract

The invention relates to a hydrogen flow control N-type low-doped silicon carbide film epitaxial making method. The making method comprises the following steps: 1, placing a silicon carbide substrate in a reaction chamber of a silicon carbide CVD apparatus, and vacuumizing the reaction chamber; 2, introducing H2 to the reaction chamber until the pressure in the reaction chamber reaches 100mbar, maintaining the pressure in the reaction chamber unchanged, gradually increasing the H2 flow to 60L/min, and continuously introducing H2 to the reaction chamber; 3, starting a high frequency coil induction heater RF, gradually increasing the power of the heater, and carrying out in situ etching when the temperature of the reaction chamber gradually rises to 1400DEG C; and 4, maintaining the temperature and the pressure unchanged when the temperature of the reaction chamber reaches 1580-1600DEG C, introducing C3H8 and SiH4 to the reaction chamber, introducing highly pure N2 to the reaction chamber as an N-type doping source, stopping the introduction of SiH4, C3H8 and highly pure N2 to the reaction chamber and maintaining for 1min after a first-layer N-type doping layer grows, reducing the H2 flow from 60L/min to 40L/min, and continuously introducing SiH4, C3H8 and the highly pure N2 to the reaction chamber to grow a second-layer N-type doping layer.

Description

The low-doped carborundum films epitaxial preparation method of a kind of control hydrogen flowing quantity N-type
Technical field
The invention belongs to semiconductor device processing technology field, relate in particular to a kind of existing carbofrax material MOCVD growth technique that utilizes, prepare the method for the low-doped silicon carbide epitaxial layers of N-type gradient.
Background technology
Silicon carbide has broad-band gap, high thermal conductivity, high disruptive strength, high electronics saturation drift velocity, high advantages such as hardness, also has very strong chemical stability.The physics that these are good and electric property make silicon carbide have a lot of advantages in application.The wide silicon carbide intrinsic carrier that makes in forbidden band at high temperature still can keep lower concentration, thereby can be operated at very high temperature.High breaking down field strength makes silicon carbide can bear high strength of electric field, and this makes the silicon carbide can be for making high pressure, high-power semiconducter device.High heat conductance makes silicon carbide have good thermal diffusivity, contribute to improve the power density of device and integrated level, the attached cooling infrastructure of minimizing, thereby the volume and weight that makes system reduces widely, efficiency improves widely, and this is for the electron device very advantageous in development space field.The saturated electrons travelling speed of silicon carbide is very high, and this characteristic also makes it can be for radio frequency or microwave device, thereby improves device working speed.
The carrier concentration of carbofrax material is the basic electricity parameter of materials and devices.This parameter realizes by material doped control.Therefore, the doping of silicon carbide epitaxy material is one of critical process in device preparation.Yet because the bonding strength of silicon carbide is high, the doping in device making technics can not adopt diffusion technique, can only utilize extension controlled doping and high temperature ion implantation doping.The membership of high temperature implantation causes a large amount of lattice damages, forms a large amount of lattice imperfections, even if annealing is also difficult to eliminate completely, had a strong impact on the performance of device, and ion implantation efficiency is very low, thereby is not suitable for doing big area doping.Meanwhile, when the semiconducter device of some multilayered structures of preparation, need the gradient of the longitudinal doping content of epitaxial film controlled.Only have by reasonable adjustment growth parameter(s), grow the epitaxial film that doping reaches pre-provisioning request, just can produce the satisfactory device of performance, thereby the control of the grade doping of silicon carbide epitaxial layers is a very large difficult point during current device is manufactured.
Summary of the invention
The object of the invention is to the deficiency for above-mentioned prior art, the preparation method of the low-doped silicon carbide epitaxial layers of a kind of N-type gradient is provided, utilize the CVD equipment of silicon carbide, prepare the controlled silicon carbide epitaxial layers of longitudinal doping content gradient, met the requirement of the low-doped epitaxial film of preparation gradient.
For achieving the above object, preparation method of the present invention comprises the following steps.
(1) silicon carbide substrates is placed in the reaction chamber of silicon carbide CVD equipment, reaction chamber is evacuated;
(2) to reaction chamber, pass into H 2until reaction chamber air pressure arrives 100mbar, keep reaction chamber air pressure constant, then by H 2flow increases to 60L/min gradually, continues to ventilate to reaction chamber;
(3) open radio-frequency coil induction heater RF, increase gradually the power of this well heater, when reaction chamber temperature gradually to 1400 ℃ that raise carried out original position etching;
(4) when reaction chamber temperature reaches 1580 ℃-1600 ℃, keep temperature and invariablenes pressure of liquid, to reaction chamber, pass into C 3h 8and SiH 4; By high-purity N 2as N-type doped source, pass in reaction chamber.After the growth of the first layer N-type doped layer finishes, stop passing into SiH to reaction chamber 4, C 3h 8and high-purity N 2and keep 1min, therebetween by H 2flow is reduced to 40L/min by 60L/min.Continue afterwards to pass into SiH to reaction chamber 4, C 3h 8and high-purity N 2growth second layer N-type doped layer.
(5) after reaching the epitaxy time of 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, is then slowly filled with argon gas, make substrate slice naturally cool to room temperature under ar gas environment.
Compared with prior art, tool has the following advantages in the present invention:
1. the present invention adopts high-purity N 2as doped source, the aluminium nuclear power mixing is effectively replaced C atom in carbofrax material, forms substitutional impurity, with respect to ion implantation technology, and the low-doped carbofrax material lattice perfection of preparation, defect is few, is conducive to improve device performance.
2. the present invention adopts the CVD epitaxial device of silicon carbide, carbonization substrate at silicon carbide substrates or existing epitaxial film carries out extension, by growth parameter(s), control longitudinal doping content, the N-type epitaxial film of the different low doping concentrations of can growing continuously, simplifies the preparation technology of device.
Accompanying drawing explanation
By describing in more detail exemplary embodiment of the present invention with reference to accompanying drawing, above and other aspect of the present invention and advantage will become and more be readily clear of, in the accompanying drawings:
Fig. 1 is the process flow sheet of technical solution of the present invention.
Embodiment
Hereinafter, now with reference to accompanying drawing, the present invention is described more fully, various embodiment shown in the drawings.Yet the present invention can implement in many different forms, and should not be interpreted as being confined to embodiment set forth herein.On the contrary, it will be thorough with completely providing these embodiment to make the disclosure, and scope of the present invention is conveyed to those skilled in the art fully.
Referring to accompanying drawing 1, technical scheme of the present invention is described in further detail, below provide two kinds of embodiment.
Embodiment 1
Step 1, is 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 4 °, is 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 60L/min;
(2.2) open the gas of vacuum pump abstraction reaction chamber, keep reaction chamber air pressure at 100mbar;
(2.3) tune up gradually heating source power, reaction chamber temperature is slowly raise.
Step 3, carries out original position etching to substrate.
(3.1), when reaction chamber temperature reaches after 1400 ℃, 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.
(4.1), when reaction chamber temperature reaches at 1580 ℃, keep reaction chamber temperature and invariablenes pressure of liquid;
(4.2) open C 3h 8, SiH 4and high-purity N 2switch, in reaction chamber, pass into the C that flow is 7mL/min 3h 8, the flow SiH that is 21mL/min 4with the flow high-purity N that is 100mL/min 2, starting growing silicon carbide epitaxial film N1, growth time is 20min.Close afterwards C 3h 8, SiH 4and high-purity N 2switch 1min, therebetween by H 2flow is reduced to 40L/min.Open C 3h 8, SiH 4and high-purity N 2switch, in reaction chamber, pass into the C that flow is 7mL/min 3h 8, the flow SiH that is 21mL/min 4with the flow high-purity N that is 100mL/min 2, starting growing silicon carbide epitaxial film N2, growth time is 20min.
Step 5, cooling substrate in hydrogen stream.
(5.1) after epitaxial film N2 growth finishes, close C 3h 8, SiH 4and high-purity N 2switch, stop growing;
(5.2) hydrogen flowing quantity lead to reaction chamber being set 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;
(5.3) reaction chamber air pressure is elevated to 700mbar, in hydrogen stream, continues cooling.
Step 6, cooling substrate in argon gas.
(6.1) when reaction chamber temperature is reduced to after 700 ℃, close the hydrogen switch that leads to reaction chamber;
(6.2) reaction chamber is vacuumized, until air pressure is lower than 1 * 10 -7mbar;
(6.3) open argon gas switch, to reaction chamber, pass into the argon gas that flow is 12L/min, make length have the substrate of silicon carbide epitaxial layers under ar gas environment, to continue cooling 30min;
(6.4) 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, is 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 °, is 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 60L/min;
(2.2) open the gas of vacuum pump abstraction reaction chamber, keep reaction chamber air pressure at 100mbar;
(2.3) tune up gradually heating source power, reaction chamber temperature is slowly raise.
Step 3, carries out original position etching to substrate.
(3.1) when reaction chamber temperature reaches after 1400 ℃, in reaction chamber, pass into the C that flow is 7mlL/min 3h 8, 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.
(4.1), when reaction chamber temperature reaches at 1580 ℃, keep reaction chamber temperature and invariablenes pressure of liquid;
(4.2) open SiH 4and high-purity N 2switch, in reaction chamber, pass into the C that flow is 7mL/min 3h 8, the flow SiH that is 21mL/min 4with the flow high-purity N that is 100mL/min 2, starting growing silicon carbide epitaxial film N1, growth time is 20min.Close afterwards C 3h 8, SiH 4and high-purity N 2switch 1min, therebetween by H 2flow is reduced to 40L/min.Open C 3h 8, SiH 4and high-purity N 2switch, in reaction chamber, pass into the C that flow is 7mL/min 3h 8, the flow SiH that is 21mL/min 4with the flow high-purity N that is 100mL/min 2, starting growing silicon carbide epitaxial film N2, growth time is 20min.
Step 5, cooling substrate in hydrogen stream.
(5.1) after epitaxial film N2 growth finishes, close C 3h 8, SiH 4and high-purity N 2switch, stop growing;
(5.2) hydrogen flowing quantity lead to reaction chamber being set 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;
(5.3) reaction chamber air pressure is elevated to 700mbar, in hydrogen stream, continues cooling.
Step 6, cooling substrate in argon gas.
(6.1) when reaction chamber temperature is reduced to after 700 ℃, close the hydrogen switch that leads to reaction chamber;
(6.2) reaction chamber is vacuumized, until air pressure is lower than 1 * 10 -7mbar;
(6.3) open argon gas switch, to reaction chamber, pass into the argon gas that flow is 12L/min, make length have the substrate of silicon carbide epitaxial layers under ar gas environment, to continue cooling 30min;
(6.4) slowly improve reaction chamber air pressure to normal pressure, make substrate naturally cool to room temperature, take out silicon carbide epitaxy sheet.
The foregoing is only embodiments of the invention, be not limited to the present invention.The present invention can have various suitable changes and variation.All any modifications of doing within the spirit and principles in the present invention, be equal to replacement, improvement etc., within protection scope of the present invention all should be included in.

Claims (1)

1. control the low-doped carborundum films epitaxial preparation method of hydrogen flowing quantity N-type, it is characterized in that:
Described preparation method comprises the following steps:
(1) silicon carbide substrates is placed in the reaction chamber of silicon carbide CVD equipment, reaction chamber is evacuated;
(2) to reaction chamber, pass into H 2until reaction chamber air pressure arrives 100mbar, keep reaction chamber air pressure constant, then by H 2flow increases to 60L/min gradually, continues to ventilate to reaction chamber;
(3) open radio-frequency coil induction heater RF, increase gradually the power of this well heater, when reaction chamber temperature gradually to 1400 ℃ that raise carried out original position etching;
(4) when reaction chamber temperature reaches 1580 ℃-1600 ℃, keep temperature and invariablenes pressure of liquid, to reaction chamber, pass into C 3h 8and SiH 4; By high-purity N 2as N-type doped source, pass in reaction chamber; After the growth of the first layer N-type doped layer finishes, stop passing into SiH to reaction chamber 4, C 3h 8and high-purity N 2and keep 1min, therebetween by H 2flow is reduced to 40L/min by 60L/min; Continue afterwards to pass into SiH to reaction chamber 4, C 3h 8and high-purity N 2growth second layer N-type doped layer;
(5) after reaching the epitaxy time of 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, is then slowly filled with argon gas, make substrate slice naturally cool to room temperature under ar gas environment.
CN201410350046.6A 2014-07-22 2014-07-22 Hydrogen flow control N-type low-doped silicon carbide film epitaxial making method Pending CN104131336A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS62214614A (en) * 1986-03-17 1987-09-21 Fujitsu Ltd Reduced pressure cvd device
CN102592976A (en) * 2012-03-22 2012-07-18 西安电子科技大学 P-type heavily-doped silicon carbide film extension preparation method
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
CN103422164A (en) * 2013-08-13 2013-12-04 西安电子科技大学 Method for controlling N-type 4H-SiC homogenous epitaxial doping
CN103820768A (en) * 2014-03-11 2014-05-28 中国科学院半导体研究所 Homogeneous and rapid epitaxial growth method of 4H-SiC epitaxial layer on 4H-SiC substrate

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS62214614A (en) * 1986-03-17 1987-09-21 Fujitsu Ltd Reduced pressure cvd device
CN102592976A (en) * 2012-03-22 2012-07-18 西安电子科技大学 P-type heavily-doped silicon carbide film extension preparation method
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
CN103422164A (en) * 2013-08-13 2013-12-04 西安电子科技大学 Method for controlling N-type 4H-SiC homogenous epitaxial doping
CN103820768A (en) * 2014-03-11 2014-05-28 中国科学院半导体研究所 Homogeneous and rapid epitaxial growth method of 4H-SiC epitaxial layer on 4H-SiC substrate

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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: 20141105