CN108155090A - A kind of high quality AlN epitaxial films and its preparation method and application - Google Patents
A kind of high quality AlN epitaxial films and its preparation method and application Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000758 substrate Substances 0.000 claims abstract description 55
- 238000000034 method Methods 0.000 claims abstract description 35
- 239000010980 sapphire Substances 0.000 claims abstract description 29
- 229910052594 sapphire Inorganic materials 0.000 claims abstract description 27
- 238000000137 annealing Methods 0.000 claims abstract description 24
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- 208000012868 Overgrowth Diseases 0.000 claims abstract description 11
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- 229910052681 coesite Inorganic materials 0.000 claims description 9
- 229910052906 cristobalite Inorganic materials 0.000 claims description 9
- 238000000407 epitaxy Methods 0.000 claims description 9
- 229910052682 stishovite Inorganic materials 0.000 claims description 9
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- 238000012986 modification Methods 0.000 description 2
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02367—Substrates
- H01L21/02428—Structure
- H01L21/0243—Surface structure
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02538—Group 13/15 materials
- H01L21/0254—Nitrides
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
- H01L21/02617—Deposition types
- H01L21/0262—Reduction or decomposition of gaseous compounds, e.g. CVD
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- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02656—Special treatments
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- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/0256—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
- H01L31/0264—Inorganic materials
- H01L31/0304—Inorganic materials including, apart from doping materials or other impurities, only AIIIBV compounds
- H01L31/03044—Inorganic materials including, apart from doping materials or other impurities, only AIIIBV compounds comprising a nitride compounds, e.g. GaN
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- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
- H01L31/184—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof the active layers comprising only AIIIBV compounds, e.g. GaAs, InP
- H01L31/1852—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof the active layers comprising only AIIIBV compounds, e.g. GaAs, InP comprising a growth substrate not being an AIIIBV compound
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- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
- H01L31/184—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof the active layers comprising only AIIIBV compounds, e.g. GaAs, InP
- H01L31/1856—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof the active layers comprising only AIIIBV compounds, e.g. GaAs, InP comprising nitride compounds, e.g. GaN
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- H01L33/005—Processes
- H01L33/0062—Processes for devices with an active region comprising only III-V compounds
- H01L33/0066—Processes for devices with an active region comprising only III-V compounds with a substrate not being a III-V compound
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- H01L33/02—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
- H01L33/26—Materials of the light emitting region
- H01L33/30—Materials of the light emitting region containing only elements of group III and group V of the periodic system
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- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The present invention relates to a kind of AlN epitaxial films and its preparation method and application.The present invention combines two core links of graphical sapphire substrate or AlN templates and high annealing, the approach of residual stress is effectively reduced by epitaxial lateral overgrowth process and high annealing, the very low AlN epitaxial films of flawless, atomically flating, dislocation density are obtained, to realizing that AlGaN base deep ultraviolet high-performance shines and sensitive detection parts and industry application are of great significance.
Description
Technical field
The present invention relates to a kind of flawless, atom level surfacing, the AlN epitaxial films of low-dislocation-density and its preparation sides
Method and application belong to III nitride semiconductor preparing technical field.
Background technology
High Al contents AlGaN and its low-dimensional quantum structure photoelectric functional material are to prepare solid-state deep ultraviolet (DUV) phototube
The irreplaceable material system of part in the field of environment protection such as sterilizing, water and air purification and the transmission of large capacity information and is deposited
Storage etc. message areas have extensive use, be current III- group-III nitride semiconductors most have development potentiality field and industry it
One." Minamata pact " is participated in since the Chinese government is S signed, the production and trade that the year two thousand twenty will start to forbid mercurous product in the world
Easily, therefore, the development of high-performance AlGaN bases solid-state DUV-LED light sources just becomes more urgent task.
Since the AlN substrates of business are expensive in the world at present, size is small, and it is difficult to obtain, c surface sapphire substrates
Upper hetero-epitaxy AlN films are current mainstream technology routes.However, as lattice mismatch and thermal mismatching, cause outside this AlN
Prolong often have in film it is very high through dislocation density (109-1010cm-2).Through dislocation, generally to extend to device active for these
In area, the performance of device is seriously affected.By taking DUV light emitting diodes (LED) as an example, a large amount of dislocations extended in Quantum Well can pole
The promotion of big limitation luminous efficiency.Thus breakthrough prepares the effective of the AlN epitaxial films of low-dislocation-density on a sapphire substrate
Method has particularly important meaning.
The common technology path for preparing AlN epitaxial films is mainly the following in the world at present:One be utilized in it is flat
By adjusting low temperature nucleation and the method for the technological parameter of high temperature epitaxy in whole Sapphire Substrate;Second is that using pulse III group
The method of source metal or group V source;Third, using the method for multilayer alternating growth, such as hypo-hyperthermia alternating growth;Fourth, figure serves as a contrast
The method at bottom etc..It is difficult often simultaneously although these methods can promote the crystal quality of AlN epitaxial films to a certain extent
Ensure that height obtains that complete flawless, atomic level are smooth, and the AlN epitaxial films of low-dislocation-density repeatablely.
Also having in the prior art can prepare that complete flawless, atomic level are smooth, and the AlN epitaxial films of low-dislocation-density
Method, but often there are process window it is narrow, it is repeatable difference the shortcomings that.Although in addition, using physical vapor transport (PVT)
Prepare class homoepitaxy scheme prepared by AlN substrates or PVT combinations hydride gas-phase epitaxy (HVPE) and can preferably realize with
Upper target, but it is excessive there are cost, AlN is small-sized and the defects of can not realizing large-scale industrial production.
Invention content
(1) technical problems to be solved
The technical problem to be solved by the present invention is to how inexpensive, industrialization, high repeatabilities to realize complete flawless, original
The smooth AlN epitaxial films with low-dislocation-density of sub- rank.
(2) technical solution
In order to solve the above-mentioned technical problem, the present invention has on graphical substrate by epitaxial lateral overgrowth process and high annealing
Effect reduces residual stress, so as to obtain the very low AlN epitaxial films of flawless, atomically flating, dislocation density.
The present invention is realized using following scheme.
A kind of preparation method of AlN epitaxial films, including:AlN preliminary growths, high temperature are carried out successively on concave substrate surface
Annealing, AlN laterally overgrowns continue epitaxial growth to target thickness after completing polymerization process, obtain AlN epitaxial films.
The concave substrate is selected from concave surface Sapphire Substrate or concave surface AlN/ sapphire composite shutterings.
The period of the concave substrate is controlled at 0.5-3 microns, and preferably 0.9-2 microns, further preferably 1-1.6 is micro-
Rice;Mesa width is 300-400nm.Pattern transfer technology cooperation dry etching method can be used in the concave substrate or wet method is rotten
Erosion method is prepared;The pattern transfer technology is selected from ultraviolet photolithographic or nano impression;The dry etching method is selected from electricity consumption
Feel coupled plasma (ICP), reactive ion etching method.
Preferably, heretofore described concave substrate comprises the following steps:
S101, first in concave substrate surface spin coating photoresist or nano impression glue;Spin coating photoresist or nano impression glue
Thickness be 200-400nm.
If concave substrate is concave surface Sapphire Substrate, first certain thickness mask layer must be deposited on concave substrate surface
(such as SiO2), then in the top spin coating photoresist of mask layer or nano impression glue;Wherein, the deposition method such as PECVD (etc.
Gas ions enhance chemical vapor deposition) etc..Mask layer thickness is 200-300nm.
S102, using standard nano impression or photoetching process by the pattern transfer on impression block or photolithography plate to nanometer pressure
It prints on glue or photoresist;
S103, will be in the substrate obtained by pattern transfer to S102 using dry etching or wet etching method;
S104, the remaining mask layer of removal, obtain graphical substrate;
S105, substrate is thoroughly cleaned, is dried after removing impurity, obtain concave substrate.
The temperature of the AlN preliminary growths is 1100-1500 DEG C, and growth pressure is low as possible, such as 50-100mbar, is gone back simultaneously
It needs that the molar flow ratio for adjusting ammonia and metal organic source is configured according to MOCVD.The thickness of the AlN preliminary growths usually comes
Say that, to reach preferable tensile stress releasing effect, the thickness is preferred with 200-400nm less than polymerization thickness.If with indigo plant
Jewel substrate is substrate, then need to before AlN preliminary growths first growing AIN nucleating layer under cryogenic, the AlN nucleating layers
Thickness is 10-70nm, and growth temperature is 920-960 DEG C.
The process conditions of the high annealing are:1400-1800 DEG C of temperature, preferably 1650-1750 DEG C;Atmosphere is nitrogen.
The temperature of the AlN epitaxial lateral overgrowths aggregation growth is 1100-1500 DEG C, the AlN epitaxial lateral overgrowths aggregation growth side
Method is selected from metal-organic chemical vapor deposition equipment (MOCVD), hydride gas-phase epitaxy (HVPE), molecular beam epitaxy (MBE) etc..
The present invention also provides the AlN epitaxial films that above-mentioned preparation method obtains.
The present invention also provides above-mentioned AlN epitaxial films in the development of the photoelectric devices such as deep-UV light-emitting, detection, production field
Application.
(3) advantageous effect
The present invention organically combines nano graph substrate with high-temperature annealing process, targetedly solves respectively high
Two big critical issues in quality AlN preparations, first, reducing dislocation density;Second is that eliminate the crackle easily generated.The former passes through
Utilize the multi-panel growth competition mechanism of self-assembling formation in concave graphics Sapphire Substrate or concave surface AlN/sapphire templates
Epitaxial lateral overgrowth effectively reduces the position of AlN epitaxial films up to polymerization process control after carrying out the growth of starting stage AlN and annealing
It is wrong;The latter effectively reduces the very big tensile stress accumulated in AlN preliminary growths using high annealing, avoid AlN because
Tensile stress accumulation cracks, and so as to obtain, surfacing, dislocation density be low, high quality AlN extensions of flawless
Film.AlN method for manufacturing thin film provided by the invention has the characteristics that efficient, reproducible, is suitble to widely popularize.
Description of the drawings
The flow chart of Fig. 1, AlN epitaxial films preparation method of the present invention.
Fig. 2, concave graphics array schematic diagram of the present invention.
Fig. 3, graph substrate AlN template epitaxial lateral overgrowths of the present invention the Physical Mechanism of polymerization process Dislocations reduction show
It is intended to.Wherein:AlN Dislocations density is mainly determined that process A is that lattice mismatch causes on table top by three dynamic process A-C
Dislocation by c faces image force traction upwardly extend;Process B is position caused by unpolymerized preceding hole area (void) scope of freedom image force
Wrong bending effect causes dislocation to reduce;Process C is that the excessive crystal orientation difference in the zone of convergency causes dislocation to increase.
Specific embodiment
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..
Fig. 1 illustrates patterned substrate and the high annealing method provided in this embodiment of being used in combination and realizes flawless, low
The core thinking of dislocation density AlN film preparations, main there are three important steps:First, prepare concave graphics Sapphire Substrate
Or concave graphics AlN/sapphire templates;Second is that AlN preliminary growth mistakes are effectively reduced using high-temperature atmosphere method for annealing
The tensile residual stresses accumulated in journey;Third, by the polymerization process of AlN epitaxial lateral overgrowths, effectively reduce in AlN films and run through position
It is wrong.
Specifically include following steps (illustrating by taking Sapphire Substrate as an example):
Step S1:Prepare concave graphics substrate.It is as follows, preferred concave graphics array is as shown in Figure 2
Hexagonal Close-packed array is preferred.
The first step uses PECVD (plasma enhanced chemical vapor deposition) first in 2 inches of c- surface sapphire substrates
Deposit the SiO of 200-300nm thickness2As hard mask, nano impression glue in spin coating again later, thickness 200-400nm.
Figure 2 on 2 inches of impression blocks is transferred on polymer by second step using nano marking press, then will polymerization
Figure on object is impressed on coining glue.
Third walks, and uses ICP to imprint glue as mask by pattern transfer to SiO2On.
4th step, further with SiO2It, will be in pattern transfer to Sapphire Substrate as mask dry etching sapphire.
5th step, with HF acid solutions by SiO remaining on sapphire2Removal, obtains nano-patterned sapphire substrate, and
Thoroughly dried after cleaning substrate.
Step S2:The low-temperature epitaxy AlN nucleating layers on ready graphical sapphire substrate, thickness 10-70nm are raw
Long temperature is 920-960 DEG C;Then at 1100-1500 DEG C of progress AlN preliminary growth, the thickness of AlN preliminary growths is less than polymerization thickness
Degree, to reach best tensile stress releasing effect, which is needed to optimize, be generally preferred with 200-400nm, and AlN is preliminary
Growth pressure is low as possible, such as 50-100mbar, need to use the ammonia of optimization and the molar flow ratio (V/III of metal organic source
Than), it is specific to need that adjustment is configured according to MOCVD.
Step S3:The high temperature anneal is carried out to gained AlN films, the temperature range of annealing is 1400-1800 DEG C, preferably
1650-1750 DEG C, atmosphere is preferably nitrogen, and the time of annealing needs to be optimized according to used temperature, to remove completely
The tensile strain accumulated in AlN is preferred so that compressive strain state is presented in the AlN after annealing.
Step S4:Further AlN laterally overgrowns complete polymerization process on the AlN films for having moved back fire.High temperature epitaxy
Growing AIN layer temperature is 1100-1500 DEG C, and growth pressure is low as possible, such as 50-100mbar, need to use the molar flow ratio of optimization
V/III。
Step S5:Continue the certain thickness AlN of high temperature epitaxy, reach target thickness to get.
The present invention S1-S4 steps are coordinated for the first time, the wherein tight fit of step S1, S2 and S4, by the figure period,
Appropriately selected and being precisely controlled to the polymerization process in growth course of mesa width can be effectively eliminated on growth table top
Through dislocation, specific control mechanism is as shown in Figure 3.Pass through suitable substrate figure and matched epitaxial growth conditions, AlN
Epitaxial lateral overgrowth in, dislocation can effectively be bent, and then completely eliminate life by the effect of the image force of the crystal face of hole (void)
Dislocation on long table top.Further, since the orientation difference of adjacent table top crystal grain can also generate greatly in AlN in AlN polymerization processes
Dislocation (process C) is measured, low crystal orientation difference is realized by technical arrangement plan, so as to reduce dislocation density.
Another key point of the present invention is the cooperation of S2 and S3 steps, due to the tensile strain in AlN mainly in the course of the polymerization process
Accelerated accumulation, thus need that the growth thickness of step S2 high temperatures AlN is in optimized selection so that it is carried out in S3 steps effective
Annealing can effectively reduce the tensile strain accumulated in AlN polymerization processes.
In short, low-dislocation-density, flawless target have been respectively adopted and have been directed to necessary to realizing high quality AlN epitaxial films
Property epitaxial lateral overgrowth polymerization process control and high-temperature atmosphere annealing means, pass through optimize two kinds of means linking, realization
Best matching, so as to reach the preparation purpose of high quality AlN epitaxial films.
In conclusion one kind provided by the invention is based on that patterned substrate epitaxial lateral overgrowth and high-temperature atmosphere annealing is used in combination
Process, by matching both processing methods, so as to reach completely eliminate crackle, realize low-dislocation-density high quality
The preparation of AlN epitaxial films.
Embodiment 1 (by taking prepared by Sapphire Substrate as an example)
S1:Concave graphics Sapphire Substrate is prepared, the specific steps are:
1) using the SiO of PECVD deposition 200nm thickness first in 2 inches of c- surface sapphire substrates2, spin coating again later
Upper TU7-220 glue, thickness 300nm.
2) using nano marking pressTo it be 1.2 microns in the period, Circularhole diameter is the impression block of 800nm
On pattern transfer polymer on (mesa dimensions 400nm), then by the figure on polymer in the pushing of uv-exposure condition
It prints on coining glue.
3) use ICP to imprint glue as mask by pattern transfer to SiO2On.
4) with SiO2As mask H2SO4And H3PO4Mixed solution corrodes sapphire under 270 DEG C of temperature conditions, will scheme
Shape is transferred in Sapphire Substrate.
5) with HF acid solutions by SiO remaining on sapphire2Removal obtains nano-patterned sapphire substrate, and thoroughly
It is dried after cleaning substrate.
S2:Graphic sapphire lining is put into MOCVD device (3 × 2 " Aixtron CCS FP-MOCVD) reative cell
Bottom is passed through H2, it is warming up at 930 DEG C, stablizes 50 seconds, is passed through trimethyl aluminium (TMAl) and ammonia and keeps its V/III molar ratio
For the AlN nucleating layers of 5000 growth 15nm thickness, then proceed to be passed through ammonia, turn off TMAl;
It then heats at 1250 DEG C, stablizes 50 seconds, holding chamber pressure is 50mbar, is passed through TMAl and ammonia simultaneously
It is 450 to keep its V/III molar ratio, and 1250 DEG C of growing AIN 300nm of high temperature turn off TMAl and stop growing, cooling.
S3:AlN samples are put into the graphite support of high-temperature annealing furnace, holding furnace atmosphere is N2, pressure is an air
Pressure is to slowly warm up to 1750 DEG C with 4 DEG C per minute of speed, and keeps 1750 DEG C of 1 hours of annealing, cooling.
S4:It will be dried after the AlN of annealing cleanings, be put into MOCVD reative cells, then heat to 1250 DEG C
Under, stablize 50 seconds, holding chamber pressure is 50mbar, and it is 400 to be passed through TMAl and ammonia and keep its V/III molar ratio, high
1250 DEG C of epitaxial growth AlN of temperature complete the complete polymerization process of each adjacent crystal column on table top.
S5:Keep 1250 DEG C of high temperature constant, holding chamber pressure is 50mbar, adjusts the V/ of ammonia and TMAl flows
III molar ratios are 200, continue to be passed through ammonia and TMAl, continue high temperature epitaxy growing AIN, until its thickness reaches 5 microns.
Embodiment 2 (for being grown in concave graphics AlN templates)
S1:Concave surface AlN template substrates are prepared, the specific steps are:
1) AlN templates are prepared using MOCVD device (3 × 2 " Aixtron CCS FP-MOCVD), thickness is 1 micron.
SU8 glue in AlN templates, thickness 600nm.
2) using nano marking pressTo it be 1 micron in the period, Circularhole diameter is the impression block (platform of 650nm
Face size is 350nm) on pattern transfer polymer on, then the figure on polymer is impressed under the conditions of uv-exposure
It imprints on glue.
3) ICP is used to be transferred in AlN templates as mask pattern to imprint glue, 300 nanometers of hole depth.
4) SU8 glue remaining in AlN templates is removed with acetone, obtains nano patterning AlN templates and thoroughly cleaning lining
It is dried behind bottom.
S2:The nano patterning AlN templates prepared are placed on and are passed through H in MOCVD reative cells2, it is warming up to 1250
DEG C, stablize 50 seconds, holding chamber pressure is 50mbar, is passed through trimethyl aluminium (TMAl) and ammonia epitaxial growth AlN, high temperature
1250 DEG C of growing AIN 200nm, turn off TMAl and stop growing, cooling.
S3:AlN is put into the graphite support of high-temperature annealing furnace, holding furnace atmosphere is N2, pressure is an atmospheric pressure, with
4 DEG C per minute of speed is to slowly warm up to 1750 DEG C, and keeps 1650 DEG C of 1.5 hours of annealing, cooling.
S4:It will be dried after AlN film cleanings by annealing, be then placed in MOCVD reative cells, be warming up to high temperature
1250 DEG C, holding chamber pressure is 50mbar, and the V/III molar ratios for adjusting ammonia and TMAl flows are 500, continue high temperature
1250 DEG C of epitaxial growth AlN complete the complete polymerization process of each adjacent crystal column on table top.
S5:Keep 1250 DEG C of high temperature constant, holding chamber pressure is 50mbar, adjusts the V/ of ammonia and TMAl flows
III molar ratios are 200, continue to be passed through ammonia and TMAl, continue high temperature epitaxy growing AIN, until its thickness reaches 5 microns.
Compliance test result
Embodiment 1,2 gained AlN epitaxial films of embodiment are tested by detection method commonly used in the art:
(1) light microscope detects, embodiment 1,2 gained AlN epitaxial film flawlesses;
(2) atomic force microscope detects, and embodiment 1,2 gained AlN epitaxial films have atomically flating surface;
(3) X-ray diffractometer or transmission electron microscope detection, embodiment 1,2 gained AlN epitaxial films have low dislocation
Density.
Although above the present invention is described in detail with a general description of the specific embodiments,
On the basis of the present invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Cause
This, these modifications or improvements, belong to the scope of protection of present invention without departing from theon the basis of the spirit of the present invention.
Claims (10)
1. a kind of preparation method of AlN epitaxial films, which is characterized in that including:It is preliminary that AlN is carried out successively on concave substrate surface
Growth, high annealing, AlN laterally overgrowns continue epitaxial growth to target thickness after completing polymerization process, obtain outside AlN
Prolong film.
2. the preparation method of AlN epitaxial films according to claim 1, which is characterized in that the concave substrate is selected from recessed
Surface sapphire substrate or concave surface AlN/ sapphire composite shutterings.
3. the preparation method of AlN epitaxial films according to claim 1 or 2, which is characterized in that the week of the concave substrate
Phase is controlled at 0.5-3 microns, preferably 0.9-2 microns, further preferably 1-1.6 microns;Mesa width is 300-400nm.
4. according to the preparation method of any AlN epitaxial films of claim 1-3, which is characterized in that the concave substrate
It comprises the following steps:
S101, first in concave substrate surface spin coating photoresist or nano impression glue;The thickness of spin coating photoresist or nano impression glue
It spends for 200-400nm;
S102, using standard nano impression or photoetching process by the pattern transfer on impression block or photolithography plate to nano impression glue
Or on photoresist;
S103, will be in the substrate obtained by pattern transfer to S102 using dry etching or wet etching method;
S104, the remaining mask layer of removal, obtain graphical substrate;
S105, substrate is thoroughly cleaned, is dried after removing impurity, obtain concave substrate.
5. according to the preparation method of any AlN epitaxial films of claim 1-4, which is characterized in that the AlN is tentatively raw
Long temperature is 1100-1500 DEG C.
6. according to the preparation method of any AlN epitaxial films of claim 1-5, which is characterized in that if being served as a contrast with sapphire
Bottom is substrate, then need to before the AlN preliminary growths first growing AIN nucleating layer under cryogenic;The thickness of the AlN nucleating layers
It spends for 10-70nm, growth temperature is 920-960 DEG C.
7. according to the preparation method of any AlN epitaxial films of claim 1-6, which is characterized in that the high annealing
Process conditions be:1400-1800 DEG C of temperature, preferably 1650-1750 DEG C.
8. according to the preparation method of any AlN epitaxial films of claim 1-7, which is characterized in that the AlN is laterally outer
The temperature for prolonging aggregation growth is 1100-1500 DEG C;The AlN epitaxial lateral overgrowths aggregation growth method is selected from metal organic-matter chemical gas
Mutually deposition, hydride gas-phase epitaxy or molecular beam epitaxy.
9. the AlN epitaxial films that any preparation methods of claim 1-8 obtain.
10. AlN epitaxial films that any the methods of claim 1-8 obtain are ground in deep-UV light-emitting, detection photoelectric device
Application in system, production field.
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