CN106544643A - A kind of preparation method of nitride film - Google Patents
A kind of preparation method of nitride film Download PDFInfo
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- CN106544643A CN106544643A CN201611114438.8A CN201611114438A CN106544643A CN 106544643 A CN106544643 A CN 106544643A CN 201611114438 A CN201611114438 A CN 201611114438A CN 106544643 A CN106544643 A CN 106544643A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/301—AIII BV compounds, where A is Al, Ga, In or Tl and B is N, P, As, Sb or Bi
- C23C16/303—Nitrides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0209—Pretreatment of the material to be coated by heating
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
Abstract
The invention discloses a kind of preparation method of nitride film, comprises the following steps：During nitride isoepitaxial growth, V clan source gas is continuously and uninterruptedly passed through in reative cell, and periodically modulates the size for being passed through III clan source gas flow in reative cell.The present invention is strengthened the lateral transfer ability of III clan source atom, reduces surface defect, improved crystalline quality, improve the flatness on surface by periodically III clan source air-flow size of modulation.The inventive method economy, simple, the nitride film material property of acquisition is good, is to realize nitride epitaxial thin film high-quality, the effective solution of low cost growth.
Description
Technical field
The invention belongs to technical field of semiconductors, more particularly to a kind of preparation method of nitride film.
Background technology
Group III-nitride (includes gallium nitride, aluminium nitride, aluminium gallium nitride alloy, indium nitride, InGaN, indium nitride gallium aluminium etc.),
Its energy gap can be adjusted between 0.7eV-6.28eV, cover whole mid-infrared, visible ray and ultraviolet band.In optoelectronic applications
The aspects such as aspect, such as white light-emitting diodess (LED), blue laser (LD), ultraviolet detector obtain important application and development.
In addition, as gallium nitride (GaN) material of one of third generation quasiconductor representative, with direct band gap, high saturated electrons drift speed
Degree, high breakdown electric field and high heat conductance, while with very high heat stability and chemical stability, can be used to make high temperature, height
Frequently, HIGH-POWERED MICROWAVES device, such as HEMT (HEMT), heterojunction bipolar transistor (HBT) etc..
However, due to GaN homo-substrates prepare it is more difficult, current GaN base semi-conducting material mainly sapphire,
On the substrates such as SiC, Si, hetero-epitaxy is carried out.There is lattice mismatch and thermal mismatching with GaN in foreign substrate, cause GaN epitaxial layer
In have higher dislocation density (108～1010cm-2), so as to constrain the further raising of device performance.In recent years, with
The development of GaN substrate technology of preparing, many units have been obtained for Free-standing GaN substrate, many major companies of the world and research aircraft
Structure puts into huge man power and material in the technical elements of homoepitaxy GaN device and is studied.It is contemplated that, GaN substrate
Application in semiconductor microelectronics field will be more extensive.Different with heterogeneous epitaxial technology, GaN substrate homoepitaxy is not
Affected by substrate lattice mismatch, be not usually required to carry out the growth of low temperature nucleation layer；But due to by substrate surface adsorbing contaminant
Affect with cut, damage etc. is polished, after GaN substrate homoepitaxy, surface forms the micro structure of a large amount of Pyramids, causes table
Face rises and falls, and forms gully type surface, causes material surface Quality Down, affects performance (the Phys.Status Solidi of device
A 213,(2016)p1236–1240；J.Cryst.Growth 371,(2013)p7–10).Therefore, the homoepitaxy of GaN substrate
Need to develop new technique, new technology to improve epi-layer surface pattern in technology, reduce surface undulation, obtain surfacing light
Nitride film.
The content of the invention
Goal of the invention：The technical problem to be solved in the present invention is：A kind of process is simple is provided, can effectively be reduced surface and be lacked
Fall into, improve crystalline quality, improve surface smoothness, the method for preparing high-quality nitride film.
Technical scheme：Adopt the technical scheme that to solve the above-mentioned technical problem present invention：A kind of system of nitride film
Preparation Method, comprises the steps：
(1) a kind of substrate is selected, is transferred in nitride film growing system；
(2) substrate surface heat treatment stages：Reative cell to step (1) growing system is passed through V clan source gas and load
Gas, the temperature of reative cell are promoted to the growth temperature of nitride film, carry out heat treatment to the surface of step (1) substrate；
(3) the epitaxial deposition stage：V clan source gas, carrier gas and III clan source are passed through simultaneously in step (1) reative cell,
Carry out epitaxial growth；
(4) the surface modification stage：Continue to be passed through V clan source gas and carrier gas in step (1) reative cell, stop logical
Enter III clan source, carry out surface decomposition；
(5) the alternating growth stage：Step (3) and (4) are alternately repeated, nitride film is obtained.
In step (1), gallium nitride substrate of the substrate for c faces, m faces or a faces；The growing system is metallorganics
Vapour deposition or hydride gas-phase epitaxy system.
In step (2), the carrier gas is hydrogen or hydrogen nitrogen mixed gas, V clan source gas gas in the reative cell
In the cumulative volume of body, shared volume ratio is not less than 5%, and preferred V clan source gas accounts for the 5～30% of the totality of gas.
In step (2)～(5), the temperature of the reative cell is 850～1100 DEG C, the pressure of the reative cell is 50～
500torr, the V clan source gas are ammonia.
In step (3) and (4), III clan source is selected from trimethyl gallium, diethyl gallium, trimethyl indium, trimethyl aluminium or chlorine
Change one or more in gallium.
The time of heat treatment described in step (2) is 30～600s.
In step (3), the mol ratio of the V clan source gas and III clan source is 1000～5000：1, it is described epitaxially grown
Time is 1～30s, and the epitaxially grown deposit thickness is 1～30nm.
In step (4), the carrier gas is hydrogen, and in the reative cell, the mol ratio of H2 and NH3 is 5～20, the surface
The time of decomposition is 1～30s.
In step (5), the alternately repeated number of times is 120～3600 times.
Preferably, in step (1)～(5), all using H2For carrier gas, using H2Corrosivity to nitride, are conducive to obtaining
Obtain more smooth nitride surface.
As substantial amounts of foreign atom is easily adsorbed on GaN substrate surface, impurity on substrate surface adsorption layer is formed, affect homogeneity
Epitaxial nucleation grows, therefore needs to carry out Surface heat-treatent to substrate before growing, to reduce surface adsorption impurity to epitaxial growth
Impact.Simultaneously in order to prevent GaN substrate too fast in heat treatment stages decomposition rate, cause surface to form metal Ga drops, cause
The problem of surface blackening, needs a certain proportion of V clan source gas is passed through in reative cell in temperature-rise period, to slow down GaN substrate
Decomposition.So, ratio of the V clan source gas of substrate surface heat treatment stages in mixed gas should be not less than 5%, heat treatment
Temperature should be higher than that the heat decomposition temperature of GaN substrate, and preferred heat treatment temperature is 950～1100 DEG C, heat treatment time 30～
600s。
Epitaxial deposition phase deposition thickness should not be too thick, as growth pattern is affected by Surface binding energy, during growth
Between oversize, thickness it is too thick, easily form the defects such as larger contoured surface gully, cut, therefore step in surface dislocation, injury region
(3), in, the mol ratio of the V clan source gas and III clan source is 1000～5000：1, the epitaxially grown time be 1～
30s, the epitaxially grown deposit thickness are 1～30nm.
In the surface modification stage, now GaN epitaxial layer is in H2/NH3There is slow decomposition, Ga-N, In- in mixed gas atmosphere
N, Al-N chemical bond produces fracture, and N atoms leave epi-layer surface, the remaining III race atom (Ga, In, Al) in surface by desorption
Generation lateral transfer, the atom of surface raised areas are gathered in low areas by lateral transfer, and epi-layer surface becomes more
It is smooth.H in the stage2/NH3The ratio of mixed gas is particularly significant：When ratio is low, nitride decomposition rate is slow, is unfavorable for III race
The surface migration of atom；When ratio is high, nitride decomposition rate is fast, a large amount of III race atom aggregations in surface, forms molten drop, gold
Category drop is formed such that the surface topography of subsequent epitaxial layer is deteriorated, and is unfavorable for the epitaxial growth of material.Therefore, reative cell H2/
NH3Mixed proportion is preferably mol ratio 5～20, and the time that surface is decomposed is 1～30s.
During the alternating growth stage, epitaxial deposition and surface modification alternately, can increase epitaxy layer thickness, improve crystal
Quality, can reduce surface undulation again, reduce surface roughness.In order to obtain high-quality nitride film, alternate cycle is preferred
120～3600 times, the growth thickness for obtaining nitride film is 0.2～4 μm.
The present invention need not be by outside substrate surface treatment technology, such as reactive ion etching, corona treatment etc.
Technology, carries out situ heat treatment by epitaxial device system to substrate surface, and the present invention is without using other equipment, economical simple
Just, the foreign ion of surface adsorption can be effectively removed, clean, smooth growing surface is obtained.The present invention passes through epitaxial deposition
Stage and surface modification stages period alternately, can strengthen the transfer ability of surface atom, reduce surface gully, cut
Etc. defect, the defect concentration of epitaxial film can be effectively reduced, improve thin film surface planeness, obtain high-quality nitride film
Material.
Beneficial effect：.The inventive method economy, simple, the nitride film material property of acquisition is good, is real
Existing nitride epitaxial thin film high-quality, the effective solution of low cost growth.
Description of the drawings
The process flow diagram of Fig. 1 present invention；
Surface defect pattern optical microscope image common after Fig. 2 GaN substrate homoepitaxies；
The nitride film surface pattern optical microscope image that Fig. 3 the inventive method is obtained.
Specific embodiment
According to following embodiments, the present invention may be better understood.However, as it will be easily appreciated by one skilled in the art that real
Apply the content described by example and be merely to illustrate the present invention, and should not also without limitation on sheet described in detail in claims
Invention.
Referring to the accompanying drawing of the present invention, detailed is depicted embodiments of the invention.
Embodiment 1：
1) a piece of c faces self-support gallium nitride substrate is selected, it is ultrasonic 5 minutes respectively using acetone, ethanol and deionized water, most
Afterwards will be its moisture purging clean with high pure nitrogen；
2) gallium nitride substrate after cleaning is transferred in MOCVD systems, front-(0001) faces upwards, chamber pressure
For 100torr, reative cell is NH3/H2Mixed atmosphere (ratio 5% of the ammonia in mixed gas), reaction chamber temperature is risen to
1050 DEG C, heat treatment time 300s；
3) pressure, temperature-resistant is kept, while V clan source (ammonia) and III clan source (trimethyl gallium) are passed through, with V/III ratios
For 3000, in H2Grow 1 second under the conditions of carrier gas；
4) keep pressure, temperature, ammonia constant, stopping is passed through reaction source trimethyl gallium, the process duration 1 second；
5) be periodically alternately repeated 3), 4) step, alternate cycle is 3600 times, epitaxial growth high-quality gallium nitride film,
2 μm of thickness.
6) growth terminates, and thin-film material is taken out in cooling.
Embodiment 2：
1) a piece of a faces self-support gallium nitride substrate is selected, it is ultrasonic 5 minutes respectively using acetone, ethanol and deionized water, most
Afterwards will be its moisture purging clean with high pure nitrogen；
2) gallium nitride substrate after cleaning is transferred in MOCVD systems, a is faced upwards, chamber pressure is 500torr,
Reative cell is NH3/H2Reaction chamber temperature is risen to 850 DEG C by mixed atmosphere (ratio 10% of the ammonia in mixed gas), at heat
Reason time 600s；
3) pressure, temperature-resistant is kept, while V clan source (ammonia) and III clan source (diethyl gallium, trimethyl indium) are passed through,
With V/III ratios as 5000, in hydrogen and nitrogen gas gaseous mixture (1：1) grow 10 seconds under the conditions of carrier gas；
4) keep pressure, temperature, ammonia constant, stopping is passed through III clan source diethyl gallium, trimethyl indium, when the process continues
Between 10 seconds；
5) be periodically alternately repeated 3), 4) step, alternate cycle is 150 times, and epitaxial growth high-quality InGaN film is thick
0.2 μm of degree.
6) growth terminates, and thin-film material is taken out in cooling.
Embodiment 3：
1) a piece of m faces self-support gallium nitride substrate is selected, it is ultrasonic 5 minutes respectively using acetone, ethanol and deionized water, most
Afterwards will be its moisture purging clean with high pure nitrogen；
2) gallium nitride substrate after cleaning is transferred in MOCVD systems, m is faced upwards, chamber pressure is 50torr, instead
Room is answered to be NH3/H2Reaction chamber temperature is risen to 1100 DEG C, heat treatment by mixed atmosphere (ratio 30% of the ammonia in mixed gas)
Time 30；
3) pressure, temperature-resistant is kept, while V clan source (ammonia) and III clan source (trimethyl gallium, trimethyl aluminium) are passed through,
With V/III ratios as 1000, grow 30 seconds under the conditions of hydrogen carrier gas；
4) keep pressure, temperature, ammonia constant, stopping is passed through reaction source trimethyl gallium, trimethyl aluminium, when the process continues
Between 30 seconds；
5) be periodically alternately repeated 3), 4) step, alternate cycle is 120 times, and epitaxial growth high-quality gallium aluminium nitrogen film is thick
1 μm of degree.
6) growth terminates, and thin-film material is taken out in cooling.
Embodiment 4：
1) a piece of c surface gallium nitrides substrate is selected, it is ultrasonic 5 minutes respectively using acetone, ethanol and deionized water, finally with height
Pure nitrogen gas will be its moisture purging clean；
2) gallium nitride substrate after cleaning is transferred in HVPE systems, front-(0001) faces upwards, and chamber pressure is
300torr, reative cell are NH3/H2Mixed atmosphere (ratio 10% of the ammonia in mixed gas), reaction chamber temperature is risen to
1050 DEG C, heat treatment time 450s；
3) pressure, temperature-resistant is kept, while being passed through V clan source (ammonia) and III clan source (gallium chloride), with V/III ratios is
2000, in H2Grow 2 seconds under the conditions of carrier gas；
4) keep pressure, temperature, ammonia constant, stopping is passed through III clan source, the process duration 2 seconds；
5) be periodically alternately repeated 3), 4) step, alternate cycle is 1800 times, epitaxial growth high-quality GaN thin film, thickness
4μm。
6) growth terminates, and thin-film material is taken out in cooling.
Test analysis are carried out to the nitride film surface using this inventive method extension.
Fig. 2 is the common under an optical microscope surface defect pattern of nitride film of homoepitaxy, can be with from figure
It was observed that intensive Pyramid micro structure, forms gully type surface, causes film surface big rise and fall.
And adopting the nitride film surface light that the method is obtained smooth, gully type surface relief structure disappears, such as Fig. 3
It is shown.It can be seen that, this method can be effectively improved the surface topography of homoepitaxy nitride film, be to realize that nitride homoepitaxy is thin
Film high-quality, the effective scheme of low cost growth.
Claims (9)
1. a kind of preparation method of nitride film, it is characterised in that comprise the steps：
(1) a kind of substrate is selected, is transferred in nitride film growing system；
(2) substrate surface heat treatment stages：Reative cell to step (1) growing system is passed through V clan source gas and carrier gas,
The temperature of reative cell is promoted to the growth temperature of nitride film, carries out heat treatment to the surface of step (1) substrate；
(3) the epitaxial deposition stage：V clan source gas, carrier gas and III clan source are passed through simultaneously in step (1) reative cell, carry out
Epitaxial growth；
(4) the surface modification stage：Continue to be passed through V clan source gas and carrier gas in step (1) reative cell, stopping is passed through III
Clan source, carries out surface decomposition；
(5) the alternating growth stage：Step (3) and (4) are alternately repeated, nitride film is obtained.
2. the preparation method of nitride film according to claim 1, it is characterised in that in step (1), the substrate is
The gallium nitride substrate in c faces, m faces or a faces；The growing system is metal organic vapor phase epitaxy or hydride gas-phase epitaxy system
System.
3. according to claim 1, the preparation method of nitride film, it is characterised in that in step (2), the carrier gas
For hydrogen or hydrogen nitrogen mixed gas, shared in the cumulative volume of the gas volume ratio in the reative cell of the V clan source gas is not
Less than 5%.
4. the preparation method of nitride film according to claim 1, it is characterised in that in step (2)～(5), described
The temperature of reative cell is 850～1100 DEG C, and the pressure of the reative cell is 50～500torr, and the V clan source gas is ammonia.
5. the preparation method of nitride film according to claim 1, it is characterised in that in step (3) and (4), described
One or more in trimethyl gallium, diethyl gallium, trimethyl indium, trimethyl aluminium or gallium chloride of III clan source.
6. the preparation method of nitride film according to claim 1, it is characterised in that heat treatment described in step (2)
Time be 30～600s.
7. the preparation method of nitride film according to claim 1, it is characterised in that in step (3), V clan source
The mol ratio of gas and III clan source is 1000～5000：1, the epitaxially grown time is 1～30s, described epitaxially grown
Deposit thickness is 1～30nm.
8. the preparation method of nitride film according to claim 1, it is characterised in that in step (4), the carrier gas is
Hydrogen, H in the reative cell2And NH3Mol ratio be 5～20, the time that the surface is decomposed is 1～30s.Will according to right
Seek the preparation method of the nitride film described in 1, it is characterised in that in step (5), the alternately repeated number of times be 120～
3600 times.
9. the preparation method of nitride film according to claim 1, it is characterised in that in step (5), the nitride
The growth thickness of thin film is 0.2～4 μm.
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Cited By (6)
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| CN107180747A (en) * | 2017-06-26 | 2017-09-19 | 镓特半导体科技（上海）有限公司 | Semiconductor structure, self-standing gan layer and preparation method thereof |
| CN107195535A (en) * | 2017-06-26 | 2017-09-22 | 镓特半导体科技（上海）有限公司 | Semiconductor structure, self-standing gan layer and preparation method thereof |
| CN109385621A (en) * | 2018-11-26 | 2019-02-26 | 合肥彩虹蓝光科技有限公司 | A kind of clean method of the reaction cavity of metal-organic chemical vapor deposition equipment |
| CN110556454A (en) * | 2018-06-01 | 2019-12-10 | 上海新微技术研发中心有限公司 | Nitride epitaxial structure grown on silicon-based substrate and growth method thereof |
| CN113451451A (en) * | 2020-08-20 | 2021-09-28 | 重庆康佳光电技术研究院有限公司 | LED epitaxial layer, growth method of current expansion layer of LED epitaxial layer and LED chip |
| CN113493927A (en) * | 2021-05-07 | 2021-10-12 | 中山大学 | Method for preparing InGaN epitaxial layer |
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| CN107180747A (en) * | 2017-06-26 | 2017-09-19 | 镓特半导体科技（上海）有限公司 | Semiconductor structure, self-standing gan layer and preparation method thereof |
| CN107195535A (en) * | 2017-06-26 | 2017-09-22 | 镓特半导体科技（上海）有限公司 | Semiconductor structure, self-standing gan layer and preparation method thereof |
| CN107195535B (en) * | 2017-06-26 | 2019-12-31 | 镓特半导体科技（上海）有限公司 | Semiconductor structure, self-supporting gallium nitride layer and preparation method thereof |
| CN107180747B (en) * | 2017-06-26 | 2020-01-07 | 镓特半导体科技（上海）有限公司 | Semiconductor structure, self-supporting gallium nitride layer and preparation method thereof |
| CN110556454A (en) * | 2018-06-01 | 2019-12-10 | 上海新微技术研发中心有限公司 | Nitride epitaxial structure grown on silicon-based substrate and growth method thereof |
| CN110556454B (en) * | 2018-06-01 | 2021-08-03 | 上海新微技术研发中心有限公司 | Nitride epitaxial structure grown on silicon-based substrate and growth method thereof |
| CN109385621A (en) * | 2018-11-26 | 2019-02-26 | 合肥彩虹蓝光科技有限公司 | A kind of clean method of the reaction cavity of metal-organic chemical vapor deposition equipment |
| CN113451451A (en) * | 2020-08-20 | 2021-09-28 | 重庆康佳光电技术研究院有限公司 | LED epitaxial layer, growth method of current expansion layer of LED epitaxial layer and LED chip |
| CN113451451B (en) * | 2020-08-20 | 2022-09-13 | 重庆康佳光电技术研究院有限公司 | LED epitaxial layer, growth method of current expansion layer of LED epitaxial layer and LED chip |
| CN113493927A (en) * | 2021-05-07 | 2021-10-12 | 中山大学 | Method for preparing InGaN epitaxial layer |
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