CN110112061A - The method of molecular beam epitaxial growth process for sapphire-based AlGaN/GaN heterojunction structure - Google Patents
The method of molecular beam epitaxial growth process for sapphire-based AlGaN/GaN heterojunction structure Download PDFInfo
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
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- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
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- H01L21/02365—Forming inorganic semiconducting materials on a substrate
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- H01L21/02612—Formation types
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- H01L21/02631—Physical deposition at reduced pressure, e.g. MBE, sputtering, evaporation
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- H01L29/66462—Unipolar field-effect transistors with an active layer made of a group 13/15 material, e.g. group 13/15 velocity modulation transistor [VMT], group 13/15 negative resistance FET [NERFET] with a heterojunction interface channel or gate, e.g. HFET, HIGFET, SISFET, HJFET, HEMT
Abstract
The invention discloses a kind of methods of molecular beam epitaxial growth process for sapphire-based AlGaN/GaN heterojunction structure, use molecular beam epitaxy technique, by controlling growth parameter(s), one layer of GaN epitaxial layer of homoepitaxy on substrate, use molecular beam epitaxy technique, by controlling growth parameter(s), the extension AlN insert layer in GaN epitaxial layer;Using molecular beam epitaxy technique, by controlling growth parameter(s), one layer of Al of extension in AlN insert layerxGa(1‑x)N layers;Using molecular beam epitaxy technique, by controlling growth parameter(s), in AlxGa(1‑x)One layer of GaN cap of extension on N layer.The present invention is using molecular beam epitaxy technique in GaN epitaxial layer and AlxGa(1‑x)Different-thickness AlN insert layer is grown between N thin film layer, can optimize AlxGa(1‑x)The characteristic issues that two-dimensional electron gas low temperature transports in N/AlN/GaN hetero-junctions.
Description
Technical field
The present invention relates to a kind of method of molecular beam epitaxial growth process for sapphire-based AlGaN/GaN heterojunction structure, belong to half
Technical field of conductor materials.
Background technique
III hi-nitride semiconductor material is primarily referred to as the ternary of InN, GaN, AlN and its composition, quaternary alloy material.The
Three generations's semiconductor material, relative to first generation semiconductor material Si, Ge material system and second generation semiconductor AlGaAs material bodies
System has small big forbidden bandwidth, electronics drift saturated velocity height, dielectric constant, good heat conductivity, resistant to chemical etching etc. excellent
Property (the growth and the characterization research Xi'an [D] electronics technology of 1: Wang Danghui of document, III group-III nitride semiconductor extension layer film
University, 2012).GaN/AlGaN heterojunction structure can be in GaN and the surface AlGaN shape due to spontaneous polarization and piezoelectric polarization influence
At two-dimensional electron gas, to embody excellent carrier transport characteristic, high electron mobility transistor can be applied to, play excellent
Different switch performance and spectral characteristic.Mature Metallo-Organic Chemical Vapor compared to industrialization deposits extension GaN/
For AlGaN heterojunction structure, for molecular beam epitaxy since the slow vacuum level requirements of epitaxial growth rate are high, epitaxial growth is complicated for operation
It is only applicable to laboratory research, but the features such as MBE epitaxial growth temperature is low, growth rate is slow, so that epitaxial thickness, doping
It can accomplish accurately to control with component, it is highly beneficial especially to grow ultra-thin AlN insert layer.Ultra-thin AlN insert layer is conducive to mention
High AlGaN potential barrier and the effective conduction band band rank of GaN channel layer, deepen potential well and improve two-dimensional electron gas confinement (document 2: Lee
Really look forward or upwards relationship [j] semiconductor journal .2006.27 (6) of .AlN insert layer Yu AlGaN/GaN HEMT current collapse effect:
1055-1058).Under low temperature condition, according to momentum relaxation model (the document 3:Dziuba.Magnetic of two-dimentional degeneracy statistics
field dependent Hall data analysis of electron transport in modulation-doped
AlGaN/GaN heterostructures[J].JOURNAL OF APPLIED PHYSICS,1997,82(6):2996-
3002), hetero-junctions carrier concentration mainly has two-dimensional electron gas offer, and the mobility of carrier transport characteristic is characterized within 40K
It hardly follows temperature change and changes, mobility is mainly by acoustics scattering of wave, piezoelectricity scattering, alloy disorder scattering, interface roughness
The scattering mechanism of the characterization heterogenous junction epitaxy characteristic such as degree scattering is constituted.
In conclusion in existing domestic and foreign literature and patent, it is few to be inserted into using MBE epitaxial optimization with AlN
The process for sapphire-based Al of layerxGa(1-x)N/AlN/GaN heterojunction structure low temperature transport property Case Report.Therefore, using MBE extension
Optimize the process for sapphire-based Al with AlN insert layerxGa(1-x)N/AlN/GaN heterojunction structure low temperature transport property has important
Technological value.
Summary of the invention
The purpose of the present invention is to provide a kind of sides of molecular beam epitaxial growth process for sapphire-based AlGaN/GaN heterojunction structure
Method.
The purpose of the present invention is achieved through the following technical solutions:
A kind of method of molecular beam epitaxial growth process for sapphire-based AlGaN/GaN heterojunction structure, comprising the following steps:
1) one layer of Ti is deposited in substrate back, substrate is pre-processed;
2) molecular beam epitaxy technique is used, by controlling growth parameter(s), on substrate one layer of GaN epitaxial layer of homoepitaxy;
3) molecular beam epitaxy technique is used, by controlling growth parameter(s), the AlN of epitaxial thickness gradual change in GaN epitaxial layer
Insert layer, with a thickness of 1.19-3.57nm;
4) molecular beam epitaxy technique is used, by controlling growth parameter(s), one layer of Al of extension in AlN insert layerxGa(1-x)N
Layer;
5) molecular beam epitaxy technique is used, by controlling growth parameter(s), in AlxGa(1-x)One layer of GaN nut cap of extension on N layer
Layer;
6) the Ga ball of sample surfaces MBE (molecular beam epitaxy) epitaxial growth is removed;
7) attenuated polishing technology is used, the Ti of substrate pre-treatment growth is got rid of.
Preferably, in step 3), the growth parameter(s) of extension AlN insert layer is: growth temperature is 820-850 DEG C, the source Al beam
Flowing flow is 6 × 10-8Torr, the flow of nitrogen are 0.6-0.8sccm, and the radio-frequency power of plasma generator is 420-470W,
Growth time changes to 1min by 20s.
Preferably, GaN epitaxial layer growth parameter(s) is in step 2): growth temperature is 820-850 DEG C, and the source Ga line flow is
5.63×10-8Torr, the flow of nitrogen are 0.6-0.8sccm, and the radio-frequency power of plasma generator is 420-470W, when growth
Between be 3h, GaN epitaxial layer with a thickness of 610nm.
Preferably, in step 4), extension AlxGa(1-x)The growth parameter(s) of N thin film are as follows: growth temperature is 820-850 DEG C, Ga
Source line flow is 5.63 × 10-8The source Torr, Al line flow is 6 × 10-8Torr, the flow of nitrogen are 0.6-0.8sccm,
The radio-frequency power of plasma generator is 420-470W, growth time 7min, AlxGa(1-x)The Al component x of N thin film is
0.2421, with a thickness of 20.2nm.
Preferably, in step 5), extension GaN cap growth parameter(s) is: growth temperature is 820-850 DEG C, the source Ga line
Flow is 5.63 × 10-8Torr, the flow of nitrogen are 0.6-0.8sccm, and the radio-frequency power of plasma generator is 420-470W,
Growth time is 1min, and GaN cap is with a thickness of 6.13nm.
Preferably, in step 6), successively using acetone, alcohol and deionized water ultrasonic treatment removal Ga ball.
Preferably, in step 1) Ti with a thickness of 1.3um, the pretreatment to substrate be successively using acetone, ethyl alcohol and go from
Sub- water is cleaned by ultrasonic substrate.
Preferably, in step 7), it can guarantee the Ti for removing substrate pre-treatment using thinned machine organic semiconductor device back side 20um,
Sample is polished using polishing machine, sample is made to restore the smooth pellucidity of substrate.
Preferably, in step 8), it is coated with a layer photoresist in sample surfaces, photoetching is carried out according to exposure mask figure using litho machine
And exposure-processed is inverted, Hall test electrode 30nmTi, 150nmAl, 50nmNi and 100nmAu is deposited using PVD, uses RTA
The rapid thermal annealing for carrying out 850 DEG C, 30s, 10sccm nitrogen makes metal and sample surfaces reach Ohmic contact, in sample surfaces
6 electrodes are formed, 6 electrodes are axial symmetry, and symmetry axis includes the traverse and buttocks of sample, and contact resistance is less than between electrode
10-10Ω completes mesa-isolated using ICP technology etching GaN, and wherein ICP etching condition is 43.2sccm chlorine and 10.8sccm
Boron chloride, topping power 20W, postposition power be 60W, air pressure 10mTorr, etch period 510s pass through table top
It is 210nm that instrument, which obtains etching depth, will test electrode with silver wire by electric welding machine and is connected with package casing pin, after the completion of encapsulation
Sample be put into Montana instruments, low temperature 10K is carried out in Cryostation Hall test instrument and is surveyed to 300K Hall
Examination, and characterization sample carrier low temperature input characteristics is varied with temperature with the mobility in test data.
The present invention is changed using molecular beam epitaxy technique in process for sapphire-based AlxGa(1-x)In N/AlN/GaN heterojunction structure
The thickness of AlN insert layer optimizes the process for sapphire-based Al with AlN insert layerxGa(1-x)N/AlN/GaN heterojunction structure low temperature is defeated
The method for transporting characteristic.The present invention provides MBE extension sample surfaces Ga ball processing method and the back side because substrate pre-treatment Ti
Processing method falls the Ga ball on surface and the side of thinning back side polishing by surface acetone, alcohol and deionized water ultrasonic treatment
Method disposes Ti, and physical treatment method is simple and easy and will not additionally introduce impurity.The present invention also provides low using six electrodes
The step of warm Hall test technique is new application of the standard micro packaging technology on epitaxial wafer surface of the present invention, wherein pressing
According to axial symmetry, axial symmetry, symmetry axis includes the traverse of sample testing area and buttocks be conducive to obtain it is scientific and reasonable suddenly
The photoengraving pattern and heterogenous junction epitaxy on piece of your test data guarantee the more excellent etch thicknesses of mesa-isolated both for this hair
What bright epitaxial wafer innovation proposed.At present patent and document be seldom related to about use molecular beam epitaxy technique growth optimization have
The process for sapphire-based Al of AlN insert layerxGa(1-x)The report of N/AlN/GaN heterojunction structure low temperature transport property.
Detailed description of the invention
Fig. 1 is a kind of Al using molecular beam epitaxy technique growth with AlN insert layer of the present inventionxGa(1-x)N/
The epitaxial structure schematic diagram of AlN/GaN heterojunction structure.
Fig. 2 is the cross sectional TEM image of 1 sample of embodiment, and amplification factor is 28500 times.
Fig. 3 is the cross sectional TEM image of 1 sample of embodiment, and amplification factor is 2550000 times.
Fig. 4 is the section HRTEM image of 1 sample of embodiment.
Fig. 5 is six electrode test method Ohmic contact mask plate schematic diagram of low temperature Hall of the present invention.
Fig. 6 is six electrode test method mesa-isolated mask plate schematic diagram of low temperature Hall of the present invention.
Fig. 7 is the X-ray diffractometer ω -2 θ test result schematic diagram of 1 sample of embodiment.
Fig. 8 is 4 embodiment sample low temperature hall mobility curve synoptic diagrams of comparison, and 10K to 300K mobility is with temperature
Change curve is used to characterize carrier low temperature transport property.
Specific embodiment
It is in conjunction with the attached drawing in the embodiment of the present invention below, technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that the described embodiments are merely a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art without making creative work it is obtained it is all its
His embodiment, shall fall within the protection scope of the present invention.
Embodiment 1
Select process for sapphire-based GaN substrate, diameter is about 50.8mm, and thickness is about 430 μm, dislocation density less than 5 ×
106cm-2, surface roughness is less than 0.6nm.As shown in Figure 1, using the method for physical vapour deposition (PVD) (PVD) at the back side of substrate 1
The Titanium (Ti) of 1-1.5 μ m-thick is deposited.Then, successively substrate 1 is carried out using acetone, ethyl alcohol and deionized water ultrasonic clear
It washes.Cleaning is later dried up the surface of substrate 1 using nitrogen.By the substrate of drying be put into MBE equipment except in gas chamber, to lining
Bottom 1 carries out open surface degassing processing at least 30min and has debugged nitrogen flow.
After being determined to nitrogen flow debugging, program is designed and run, starts to grow structure of the present invention.It is first
First, isoepitaxial growth GaN epitaxial layer 2 as shown in Figure 1, underlayer temperature are 820-850 DEG C, and the power of plasma generator is
The source 420-470W, Ga baffle is kept open, and the source Ga line flow is 5.63 × 10-8The source Torr, Al baffle remains turned-off shape
State, the flow of nitrogen remain 0.6-0.8sccm, and GaN layer growth time is 3h, obtain GaN epitaxial layer by TEM image measurement
With a thickness of 610nm, as shown in Figure 2.Next AlN insert layer 3 as shown in Figure 1 is grown, the source Ga, the source Ga flapper closure are closed
The required duration is set as 5s, opens the source Al, and temperature is maintained at 820-850 DEG C, and the power of plasma generator is 420-
The source 470W, Al line flow is 6.0 × 10-8Torr, the flow of nitrogen remain 0.6-0.8sccm, and AlN layers of growth time are
20s, by TEM image measurement obtain AlN epitaxial layer with a thickness of 1.19nm, as shown in Figure 3;And pass through HRTEM image mark
AlN insert layer, about 1 atomic layer level thickness are outpoured, as shown in Figure 4.Then Al as shown in Figure 1 is grownxGa(1-x)N epitaxial layer
4, temperature is maintained at 820-580 DEG C, and the power of plasma generator is 420-470W, opens the source Ga, and the source Al is kept to open
State, the source Ga line flow are 5.63 × 10-8The source Torr, Al line flow is 6.0 × 10-8The flow of Torr, nitrogen remain
0.6-0.8sccm, AlxGa(1-x)N layers of growth time are 7min, obtain Al by TEM image measurementxGa(1-x)The thickness of N thin film
For 20.2nm, as shown in figure 4, AlxGa(1-x)Al component x is 0.2421 in N layers, finally grows GaN cap 5, temperature is maintained at
820-850 DEG C, the power of plasma generator is 420-470W, closes the source Al, and the duration needed for the flapper closure of the source Al sets
It is set to 5s, keeps the source Ga opening state, the source Ga line flow is 5.63 × 10-8Torr, GaN epitaxial layer growth time are 1min,
Obtaining GaN epitaxial layer by TEM image measurement is 6.13nm, as shown in Figure 3.
Sample is taken out after sample extension and ultrasound successively is carried out clearly to sample 1 using acetone, ethyl alcohol and deionized water
It washes to remove the Ga ball of surface attachment, the surface of sample 1 is dried up using nitrogen later, 1 use of sample of drying is subtracted by cleaning
Thin machine carries out back thinning 20um and has removed back side Ti, and the sample 1 after being thinned is processed by shot blasting the back side using polishing machine, according to
Secondary use dilute hydrochloric acid (37% concentrated hydrochloric acid mixes mixing with deionized water 1:1 in equal volume), acetone, ethyl alcohol and deionized water are to sample
1 be cleaned by ultrasonic the sample 1 after polished backside is cleaned with remove surface because be thinned and polishing treatment introduce it is inorganic
With organic pollutant and oxide layer, cleaning is later dried up the surface of sample 1 using nitrogen, then sample of the diamond pen after drying
Product middle section cuts off the test sample 1 of 1cm*1cm size, test sample 2 and test sample 3 manually respectively.Wherein test specimens
Example 1 will be by Hall test instrument test sample carrier low-temperature transport characteristic, and Al will be tested by XRD by testing sample 2xGa(1-x)N
Al component, test sample 3 will pass through TEM and measure 1 extension situation of sample, the thickness of every layer of structure as described above.Low temperature is suddenly
Your transportation characterization test is tested after needing use that will test 1 surface of sample, 6 electrode methods of vapor deposition, and the specific method is as follows: will survey
Sample example 1 carries out spin coating processing using photoresist AZ5214, then carries out light using litho machine with mask plate pattern as shown in Figure 5
Carve and invert exposure-processed, used after the completion of photoetching PVD be successively deposited on test sample 1 Hall test electrode 30nmTi,
The test sample 1 that metal has been deposited is put into acetone and stands 5min progress metal-stripping by 150nmAl, 50nmNi and 100nmAu,
Removing is sequentially placed into ethyl alcohol and deionized water later and cleans the surface standing 5min of sample 1, and cleaning uses nitrogen later
The surface drying that sample 1 will be tested moves back the sample of drying using the fast speed heat of 850 DEG C of RTA progress, 30s, 10sccm nitrogen
Fire, make metal and test 1 surface of sample reach Ohmic contact, wherein between electrode contact resistance less than 10-10Ω, after annealing
It tests sample 1 and carries out spin coating processing using photoresist AZ5214, then carried out with mask plate pattern as shown in Figure 6 using litho machine
Photoetching simultaneously inverts exposure-processed, performs etching processing using ICP after the completion of photoetching and carries out mesa-isolated, ICP etching condition is
The boron chloride of 43.2sccm chlorine and 10.8sccm, topping power 20W, postposition power are 60W, air pressure 10mTorr, are carved
The erosion time be 510s, by table top instrument obtain etching depth be 210nm, will etching complete test sample 1 respectively using acetone,
To ultrasonic clean processing is carried out to remove remained on surface photoresist, cleaning uses nitrogen by test specimens later for ethyl alcohol and deionized water
The surface of example 1 dries up, and the sample after drying is sticked in package casing, and with silver wire that test electrode and encapsulation is outer by electric welding machine
Shell pin is connected, and the test sample 1 after encapsulation is finally put into Montana instruments, Cryostation Hall test
Low temperature 10K is carried out in instrument to 300K Hall test.
Embodiment 2
Select process for sapphire-based GaN substrate, diameter is about 50.8mm, and thickness is about 430 μm, dislocation density less than 5 ×
106cm-2, surface roughness is less than 0.6nm.As shown in Figure 1, using the method for physical vapour deposition (PVD) (PVD) at the back side of substrate 1
The Titanium (Ti) of 1-1.5 μ m-thick is deposited.Then, successively substrate 1 is carried out using acetone, ethyl alcohol and deionized water ultrasonic clear
It washes.Cleaning is later dried up the surface of substrate 1 using nitrogen.By the substrate of drying be put into MBE equipment except in gas chamber, to lining
Bottom 1 carries out open surface degassing processing at least 30min and has debugged nitrogen flow.
After being determined to nitrogen flow debugging, program is designed and run, starts to grow structure of the present invention.It is first
First, isoepitaxial growth GaN epitaxial layer 2 as shown in Figure 1, underlayer temperature are 820-850 DEG C, and the power of plasma generator is
The source 420-470W, Ga baffle is kept open, and the source Ga line flow is 5.63 × 10-8The source Torr, Al baffle remains turned-off shape
State, the flow of nitrogen remain 0.6-0.8sccm, and GaN layer growth time is 3h, and the thickness of GaN epitaxial layer is inferred according to embodiment 1
Degree is 610nm.Next AlN insert layer as shown in Figure 1 is grown, the source Ga, duration needed for the flapper closure of the source Ga are closed
It is set as 5s, opens the source Al, temperature is maintained at 820-850 DEG C, and the power of plasma generator is 420-470W, the source Al Beam Current
Amount is 6.0 × 10-8Torr, the flow of nitrogen remain 0.6-0.8sccm, and AlN layers of growth time are 30s, are pushed away according to embodiment 1
Disconnected AlN epitaxial layer with a thickness of 1.785nm.Then Al as shown in Figure 1 is grownxGa(1-x)N epitaxial layer, temperature are maintained at 820-850
DEG C, the power of plasma generator is 420-470W, opens the source Ga, and keep the source Al opening state, the source Ga line flow is
5.63×10-8The source Torr, Al line flow is 6.0 × 10-8The flow of Torr, nitrogen remain 0.6-0.8sccm,
AlxGa(1-x)N layers of growth time are 7min, infer Al according to embodiment 1xGa(1-x)N thin film with a thickness of 20.2nm, and according to
Implement sample 1 and infers AlxGa(1-x)Al component x is 0.2421 in N layers, finally grows GaN cap, and temperature is maintained at 820-850
DEG C, the power of plasma generator is 420-470W, closes the source Al, and the duration needed for the flapper closure of the source Al is set as 5s,
The source Ga opening state is kept, the source Ga line flow is 5.63 × 10-8Torr, GaN epitaxial layer growth time is 1min, according to implementation
Example 1 infers that GaN epitaxial layer is 6.13nm.
Sample is taken out after sample extension and ultrasound successively is carried out clearly to sample 2 using acetone, ethyl alcohol and deionized water
It washes to remove the Ga ball of surface attachment, the surface of sample 2 is dried up using nitrogen later, 2 use of sample of drying is subtracted by cleaning
Thin machine carries out back thinning 20um and has removed back side Ti, and the sample 2 after being thinned is processed by shot blasting the back side using polishing machine, according to
Secondary use dilute hydrochloric acid (37% concentrated hydrochloric acid mixes mixing with deionized water 1:1 in equal volume), acetone, ethyl alcohol and deionized water are to sample
2 be cleaned by ultrasonic the sample 2 after polished backside is cleaned with remove surface because be thinned and polishing treatment introduce it is inorganic
With organic pollutant and oxide layer, cleaning is later dried up the surface of sample 2 using nitrogen, then sample of the diamond pen after drying
The test sample 1 of excision 1cm*1cm size will be low by Hall test instrument test sample carrier manually respectively for product middle section
Warm transportation characterization.The test of low temperature Hall transportation characterization is tested after needing use that will test 1 surface of sample, 6 electrode methods of vapor deposition,
Test sample 1 is consistent in specific method and embodiment 1.
Embodiment 3
Select process for sapphire-based GaN substrate, diameter is about 50.8mm, and thickness is about 430 μm, dislocation density less than 5 ×
106cm-2, surface roughness is less than 0.6nm.As shown in Figure 1, using the method for physical vapour deposition (PVD) (PVD) at the back side of substrate 1
The Titanium (Ti) of 1-1.5 μ m-thick is deposited.Then, successively substrate 1 is carried out using acetone, ethyl alcohol and deionized water ultrasonic clear
It washes.Cleaning is later dried up the surface of substrate 1 using nitrogen.By the substrate of drying be put into MBE equipment except in gas chamber, to lining
Bottom 1 carries out open surface degassing processing at least 30min and has debugged nitrogen flow.
After being determined to nitrogen flow debugging, program is designed and run, starts to grow structure of the present invention.It is first
First, isoepitaxial growth GaN epitaxial layer 2 as shown in Figure 1, underlayer temperature are 820-850 DEG C, and the power of plasma generator is
The source 420-470W, Ga baffle is kept open, and the source Ga line flow is 5.63 × 10-8The source Torr, Al baffle remains turned-off shape
State, the flow of nitrogen remain 0.6-0.8sccm, and GaN layer growth time is 3h, and the thickness of GaN epitaxial layer is inferred according to embodiment 1
Degree is 610nm.Next AlN insert layer as shown in Figure 1 is grown, the source Ga, duration needed for the flapper closure of the source Ga are closed
It is set as 5s, opens the source Al, temperature is maintained at 820-850 DEG C, and the power of plasma generator is 420-470W, the source Al Beam Current
Amount is 6.0 × 10-8Torr, the flow of nitrogen remain 0.6-0.8sccm, and AlN layers of growth time are 40s, are pushed away according to embodiment 1
Disconnected AlN epitaxial layer with a thickness of 2.38nm.Then Al as shown in Figure 1 is grownxGa(1-x)N epitaxial layer, temperature are maintained at 820-850
DEG C, the power of plasma generator is 420-470W, opens the source Ga, and keep the source Al opening state, the source Ga line flow is
5.63×10-8The source Torr, Al line flow is 6.0 × 10-8The flow of Torr, nitrogen remain 0.6-0.8sccm,
AlxGa(1-x)N layers of growth time are 7min, infer Al according to embodiment 1xGa(1-x)N thin film with a thickness of 20.2nm, and according to
Implement sample 1 and infers AlxGa(1-x)Al component x is 0.2421 in N layers, finally grows GaN cap, and temperature is maintained at 820-850
DEG C, the power of plasma generator is 420-470W, closes the source Al, and the duration needed for the flapper closure of the source Al is set as 5s,
The source Ga opening state is kept, the source Ga line flow is 5.63 × 10-8Torr, GaN epitaxial layer growth time is 1min, according to implementation
Example 1 infers that GaN epitaxial layer is 6.13nm.
Sample is taken out after sample extension and ultrasound successively is carried out clearly to sample 3 using acetone, ethyl alcohol and deionized water
It washes to remove the Ga ball of surface attachment, the surface of sample 3 is dried up using nitrogen later, 3 use of sample of drying is subtracted by cleaning
Thin machine carries out back thinning 20um and has removed back side Ti, and the sample 3 after being thinned is processed by shot blasting the back side using polishing machine, according to
Secondary use dilute hydrochloric acid (37% concentrated hydrochloric acid mixes mixing with deionized water 1:1 in equal volume), acetone, ethyl alcohol and deionized water are to sample
3 are cleaned to remove surface because of inorganic and organic pollutant and the oxide layer that are thinned and polishing treatment introduces, are made after cleaning
The surface of sample 3 is dried up with nitrogen, then excision 1cm*1cm is big manually respectively for sample middle section of the diamond pen after drying
Small test sample 1 will pass through Hall test instrument test sample carrier low-temperature transport characteristic.The test of low temperature Hall transportation characterization
It needs to test sample 1 one in specific method and embodiment 1 using testing after testing 1 surface of sample, 6 electrode methods of vapor deposition
It causes.
Embodiment 4
Select process for sapphire-based GaN substrate, diameter is about 50.8mm, and thickness is about 430 μm, dislocation density less than 5 ×
106cm-2, surface roughness is less than 0.6nm.As shown in Figure 1, using the method for physical vapour deposition (PVD) (PVD) at the back side of substrate 1
The Titanium (Ti) of 1-1.5 μ m-thick is deposited.Then, successively substrate 1 is carried out using acetone, ethyl alcohol and deionized water ultrasonic clear
It washes.Cleaning is later dried up the surface of substrate 1 using nitrogen.By the substrate of drying be put into MBE equipment except in gas chamber, to lining
Bottom 1 carries out open surface degassing processing at least 30min and has debugged nitrogen flow.
After being determined to nitrogen flow debugging, program is designed and run, starts to grow structure of the present invention.It is first
First, isoepitaxial growth GaN epitaxial layer 2 as shown in Figure 1, underlayer temperature are 820-850 DEG C, and the power of plasma generator is
The source 420-470W, Ga baffle is kept open, and the source Ga line flow is 5.63 × 10-8The source Torr, Al baffle remains turned-off shape
State, the flow of nitrogen remain 0.6-0.8sccm, and GaN layer growth time is 3h, and the thickness of GaN epitaxial layer is inferred according to embodiment 1
Degree is 610nm.Next AlN insert layer as shown in Figure 1 is grown, the source Ga, duration needed for the flapper closure of the source Ga are closed
It is set as 5s, opens the source Al, temperature is maintained at 820-850 DEG C, and the power of plasma generator is 420-470W, the source Al Beam Current
Amount is 6.0 × 10-8Torr, the flow of nitrogen remain 0.6-0.8sccm, and AlN layers of growth time are 60s, are pushed away according to embodiment 1
Disconnected AlN epitaxial layer with a thickness of 3.57nm.Then Al as shown in Figure 1 is grownxGa(1-x)N epitaxial layer, temperature are maintained at 820-850
DEG C, the power of plasma generator is 420-470W, opens the source Ga, and keep the source Al opening state, the source Ga line flow is
5.63×10-8The source Torr, Al line flow is 6.0 × 10-8The flow of Torr, nitrogen remain 0.6-0.8sccm,
AlxGa(1-x)N layers of growth time are 7min, infer Al according to embodiment 1xGa(1-x)N thin film with a thickness of 20.2nm, and according to
It tests sample 1 and infers AlxGa(1-x)Al component x is 0.2421 in N layers, finally grows GaN cap, and temperature is maintained at 820-850
DEG C, the power of plasma generator is 420-470W, closes the source Al, and the duration needed for the flapper closure of the source Al is set as 5s,
The source Ga opening state is kept, the source Ga line flow is 5.63 × 10-8Torr, GaN epitaxial layer growth time is 1min, according to implementation
Example 1 infers that GaN epitaxial layer is 6.13nm.
Sample is taken out after sample extension and ultrasound successively is carried out clearly to sample 3 using acetone, ethyl alcohol and deionized water
It washes to remove the Ga ball of surface attachment, the surface of sample 4 is dried up using nitrogen later, 4 use of sample of drying is subtracted by cleaning
Thin machine carries out back thinning 20um and has removed back side Ti, and the sample 4 after being thinned is processed by shot blasting the back side using polishing machine, according to
Secondary use dilute hydrochloric acid (37% concentrated hydrochloric acid mixes mixing with deionized water 1:1 in equal volume), acetone, ethyl alcohol and deionized water are to sample
4 be cleaned by ultrasonic the sample 4 after polished backside is cleaned with remove surface because be thinned and polishing treatment introduce it is inorganic
With organic pollutant and oxide layer, cleaning is later dried up the surface of sample 4 using nitrogen, then sample of the diamond pen after drying
The test sample 1 of excision 1cm*1cm size will be low by Hall test instrument test sample carrier manually respectively for product middle section
Warm transportation characterization.The test of low temperature Hall transportation characterization is tested after needing use that will test 1 surface of sample, 6 electrode methods of vapor deposition,
Test sample 1 is consistent in specific method and embodiment 1.
The sample obtained by above method is tested.As shown in fig. 7, X-ray diffractometer ω -2 θ to sample is surveyed
Test result is analyzed, AlxGa(1-x)N lattice constant a is 0.315nm, c 0.516nm, it is contemplated that forbidden band is wide in alloy material
It is 0.2421 that Al component x, which is calculated, with Vegard law in degree non-linear relation.4 groups of embodiment samples as shown in Figure 8 are from low
Warm 10K is to room temperature 300K test result it is recognised that 4 groups of embodiment sample mobilities are stablized within 40K, the section 40K to 300K
Interior 4 groups of embodiment sample mobilities are increased with temperature and are reduced, and wherein within 40K, 1 mobility of embodiment is 3836cm2/ Vs,
2 mobility of embodiment is 3696cm2/ Vs, 3 mobility of embodiment are 3241cm2/ Vs, 4 mobility of embodiment are 3039cm2/Vs;
When room temperature 300K, 1 mobility of embodiment is 850cm2/ Vs, 2 mobility of embodiment are 774cm2/ Vs, 3 mobility of embodiment are
731cm2/ Vs, 4 mobility of embodiment are 694cm2/Vs.Pass through low temperature Hall test result, it can be deduced that from low temperature 10K to normal
Warm 300K4 group embodiment sample carrier transport characteristic sequence is as follows: 3 > embodiment of embodiment 1 > embodiment, 2 > embodiment 4, with
Insert layer thickness from 1.19nm to 3.57nm, sample carrier properties decline, i.e., when AlN insert layer be 1 atomic layer level thickness
When, molecular beam epitaxy obtains AlxGa(1-x)N/AlN/GaN hetero-junctions carrier transport characteristic is best, more than 1 atomic layer level thickness
AlN insert layer can weaken AlN insert layer for AlxGa(1-x)Two-dimensional electron gas low temperature transport property is excellent in N/GaN hetero-junctions
Change.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (9)
1. a kind of method of molecular beam epitaxial growth process for sapphire-based AlGaN/GaN heterojunction structure, comprising the following steps:
1) one layer of Ti is deposited in substrate back, substrate is pre-processed;
2) molecular beam epitaxy technique is used, by controlling growth parameter(s), on substrate one layer of GaN epitaxial layer of homoepitaxy;
3) molecular beam epitaxy technique is used, by controlling growth parameter(s), one layer of AlN insert layer of extension, AlN in GaN epitaxial layer
Insert layer is with a thickness of 1.19-3.57nm;
4) molecular beam epitaxy technique is used, by controlling growth parameter(s), one layer of Al of extension in AlN insert layerxGa(1-x)N layers;
5) molecular beam epitaxy technique is used, by controlling growth parameter(s), in AlxGa(1-x)One layer of GaN cap of extension on N layer;
6) the Ga ball of sample surfaces MBE epitaxial growth is removed;
7) attenuated polishing technology is used, the Ti of substrate pre-treatment growth is got rid of.
2. the method for molecular beam epitaxial growth process for sapphire-based AlGaN/GaN heterojunction structure according to claim 1, special
Sign is:
In step 3), the growth parameter(s) of extension AlN insert layer is: growth temperature be 820-850 DEG C, the source Al line flow be 6 ×
10-8Torr, the flow of nitrogen are 0.6-0.8sccm, and the radio-frequency power of plasma generator is 420-470W, and growth time is
20s to 1min.
3. the method for molecular beam epitaxial growth process for sapphire-based AlGaN/GaN heterojunction structure according to claim 1, special
Sign is:
GaN epitaxial layer growth parameter(s) is in step 2): growth temperature is 820-850 DEG C, and the source Ga line flow is 5.63 × 10- 8Torr, the flow of nitrogen are 0.6-0.8sccm, and the radio-frequency power of plasma generator is 420-470W, and growth time is 3h,
GaN epitaxial layer with a thickness of 610nm.
4. the method for molecular beam epitaxial growth process for sapphire-based AlGaN/GaN heterojunction structure according to claim 1, special
Sign is:
In step 4), extension AlxGa(1-x)The growth parameter(s) of N thin film are as follows: growth temperature is 820-850 DEG C, and the source Ga line flow is
5.63×10-8The source Torr, Al line flow is 6 × 10-8Torr, the flow of nitrogen are 0.6-0.8sccm, plasma generator
Radio-frequency power be 420-470W, growth time 7min, AlxGa(1-x)The Al component x of N thin film is 0.2421, with a thickness of
20.2nm。
5. the method for molecular beam epitaxial growth process for sapphire-based AlGaN/GaN heterojunction structure according to claim 1, special
Sign is
In step 5), extension GaN cap growth parameter(s) is: growth temperature be 820-850 DEG C, the source Ga line flow be 5.63 ×
10-8Torr, the flow of nitrogen are 0.6-0.8sccm, and the radio-frequency power of plasma generator is 420-470W, and growth time is
1min, GaN cap are with a thickness of 6.13nm.
6. the method for molecular beam epitaxial growth process for sapphire-based AlGaN/GaN heterojunction structure according to claim 1, special
Sign is:
In step 6), successively using acetone, alcohol and deionized water ultrasonic treatment removal Ga ball.
7. the method for molecular beam epitaxial growth process for sapphire-based AlGaN/GaN heterojunction structure according to claim 1, special
Sign is:
Ti is in step 1) with a thickness of 1.3um, the pretreatment to substrate be successively using acetone, ethyl alcohol and deionized water to substrate into
Row ultrasonic cleaning.
8. the method for molecular beam epitaxial growth process for sapphire-based AlGaN/GaN heterojunction structure according to claim 7, special
Sign is:
In step 7), using thinned machine organic semiconductor device back side 20um, sample is polished using polishing machine, so that sample is restored substrate smooth
Pellucidity.
9. molecular beam epitaxial growth process for sapphire-based AlGaN/GaN heterojunction structure according to claim 1 to 8
Method, it is characterised in that:
Further include step 8): being coated with a layer photoresist in sample surfaces, photoetching is carried out according to exposure mask figure using litho machine and is inverted
Exposure-processed, is deposited Hall test electrode 30nmTi, 150nmAl, 50nmNi and 100nmAu using PVD, carries out 850 using RTA
DEG C, the rapid thermal annealing of 30s, 10sccm nitrogen, so that metal and sample surfaces is reached Ohmic contact, form 6 in sample surfaces
Electrode, 6 electrodes are axial symmetry, and symmetry axis includes the traverse and buttocks of sample, and contact resistance is less than 10 between electrode-10Ω,
Mesa-isolated is completed using ICP technology etching GaN, wherein ICP etching condition is the trichlorine of 43.2sccm chlorine and 10.8sccm
Change boron, topping power 20W, postposition power is 60W, and air pressure 10mTorr, etch period 510s are obtained by table top instrument
Etching depth is 210nm, will test electrode with silver wire by electric welding machine and is connected with package casing pin, the sample after the completion of encapsulating
It puts and carries out low temperature 10K in Hall test instrument to 300K Hall test, and vary with temperature characterization with the mobility in test data
Sample carrier low temperature input characteristics.
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