CN109103070A - Method based on nano graph silicon substrate preparation high quality thick film AlN - Google Patents
Method based on nano graph silicon substrate preparation high quality thick film AlN Download PDFInfo
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- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
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Abstract
The invention discloses a kind of methods based on nano graph silicon substrate preparation high quality thick film AlN, AlN material is superimposed by the stratiform that this method obtains, from bottom to top successively are as follows: nano graph silicon substrate, nano graph AlN nucleating layer, high-temperature AlN cross growth layer and high-temperature AlN longitudinal growth layer, with the air-gap of periodic arrangement in nano graph silicon substrate, nano graph AlN nucleating layer and high-temperature AlN cross growth layer, depth of the air-gap in Si substrate is 10nm~1 μm, its cross section maximum width is 50nm~1 μm, and the period is 100nm~2 μm.Compared with the method for existing growth thick film AlN, the present invention is low in cost, it can be by extensive industrial application, the defect concentration of AlN on silicon substrate is greatly reduced, the crystal quality for improving subsequent device structural material has broad application prospects in the fields such as the manufacture of the UV-LED device of vertical structure, MEMS, light emitting diode, radio-frequency filter and SAW device and high-frequency wideband communication.
Description
Technical field
The invention belongs to technical field of semiconductors, high-quality for obtaining on nano graph Si substrate more particularly to one kind
Measure the underlay producing technique and its epitaxy method of thick film AlN.
Background technique
As the group III-nitride of third generation semiconductor, including AlN, GaN and InN and its ternary and quaternary alloy, because of it
The 0.64eV of excellent optical property and electric property, the especially forbidden bandwidth of its ternary alloy three-partalloy from 6.1eV to the InN of AlN
Continuously adjustable, by the 200nm of deep ultraviolet to infrared 1.8 μm, these characteristics make corresponding band edge emission wavelength coverage area
It (has a wide range of applications in light emitting diode (LED), laser (LD) and detector in terms of PD.
In the nitride heterojunction structure material using sapphire, silicon carbide and silicon as substrate material, dimensional electron on silicon
Structural material and its device have apparent advantage in large scale, low cost and with existing Si in terms of.For example,
High quality AlN film is considered as the preferred knot for making GHz grades of surface acoustic waves (SAW), bulk acoustic wave device (BAW) on silicon substrate
Structure uses silicon that can directly utilize the existing technique of mainstream IC manufactory, equipment and underlying structure as substrate, with existing Si
Technique is mutually compatible with.AlGaN base UV-LED followed by silicon substrate is easy to the spy removed by the method for chemical attack using Si
Point goes out the vertical structure AlGaN base UV-LED of light by manufacturing the back side, greatly promotes the light extraction efficiency of AlGaN base UV-LED, this
So that AlGaN base UV-LED becomes one of the hot spot of nitride arena research in the world on silicon substrate.
In group III-nitride, aluminium nitride is due to its excellent physical characteristic and by the concern of modern study person.Nitridation
Aluminium has the physical characteristics such as high rigidity, high breakdown field strength, high heat conductance, high resistivity, is a kind of direct band of typical wide energy gap
Gap semiconductor, film can be used in the microelectronics instrument based on GaAs and InP, can also make in SiC high power high-temperature equipment
For a kind of megohmite insulant replacement of silicon dioxide.The aluminium nitride of high quality also has high sound transmission rate, lesser sound wave damage
The features such as thermal expansion coefficient similar in consumption, big piezoelectric coupling constant and Si and GaAs, especially with certain preferred orientation
AlN film have praetersonic transmission speed, excellent piezoelectric properties and high high-temp stability, be GHz grades of surface acoustic waves (SAW),
The preferred material of bulk acoustic wave device (BAW).The unique property of aluminium nitride makes it in MEMS (MEMS), light emitting diode
(LED), radio-frequency filter (RFT) and the fields such as the manufacture of surface acoustic wave (SAW) device and high-frequency wideband communication have wide
Application prospect.
And there are many problems by epitaxial growth high quality thick film AlN on Si (111) substrate.First is that Si (111) substrate with
AlN is since, containing a large amount of defect, these defects greatly limit device in the material that there are biggish lattice mismatch, extends outside
The promotion of performance, while seriously affecting the reliability of device；Second is that due to thermal mismatching, when high growth temperature AlN, is growing and dropping
AlN epitaxial layer will receive the huge tensile stress of Si substrate application during temperature, and epitaxial material is caused to generate serious warpage very
To cracking, it is difficult to meet the requirement of technique；Third is that diffusion barrier of the Al atom on surface is high, surface migration is difficult, and Al is caused to inhale
Attached atom is difficult to be incorporated to lattice in the position of minimum energy, causes to exist in AlN epitaxial layer largely through dislocation.The prior art
In for the epitaxial growth high quality thick film AlN on Si (111) substrate, improve device performance, be usually taken in the world following several
Kind method:
(1) pulsed laser deposition technique, such as [1] Yang, Hui, et al.CrystEngComm 15.36:7171-7176
(2013).The advantages of this technology, can obtain thickness uniformly and the AlN film of smooth surface on Si (111) substrate, but by
Poor, the crystal quality of strong influence follow-up function layer in the low crystal quality for leading to AlN of growth temperature, to be difficult to improve
The performance of device.
(2) reaction magnetocontrol sputtering technology, such as [2] Zhang, J.X., et al.Surface and Coatings
Technology 198.1-3:68-73(2005).This technology can prepare the single AlN film of crystal orientation, but due to growth
The limitation of temperature influences the crystal quality of follow-up function layer so that the thickness and crystal quality of AlN are all less desirable, from
And it is difficult to improve the performance of device.
(3) multilayer high/low temperature AlN technology, such as [3] Tran B T, Lin K L, Sahoo K C, et al.Electronic
Materials Letters,10(6):1063-1067(2014).Although this technology can obtain smooth surface and a wide range of
The AlN film not split, but due to the limitation of lattice mismatch and thermal mismatching, cause the thickness of AlN to be difficult to improve, so that the crystalline substance of AlN
Weight is unable to satisfy the requirement of follow-up function layer, to be difficult to improve the performance of device.
(4) pulse ammonia technology, such as [4] Fujikawa S, Hirayama H.Applied physics express, 4
(6):061002(2011).This technology can obtain thin compared with the AlN of high-crystal quality under the premise of epitaxy layer thickness is lesser
Film, but there is certain difficulty in the preparation of thick film AlN, while growth cycle is long, growth technique is complicated, has been significantly greatly increased outer
Prolong cost.
(5) AlN/AlGaN superlattices technology, such as [5] Fukushima Y, Ueda T.Japanese Journal of
Applied Physics,49(3R):032101(2010).This technology can grow the higher AlN film of crystal quality, but
Growth cycle is long, and epitaxy technique is complicated, and extension cost has been significantly greatly increased.
(6) micron figure Si substrate technology, such as [6] Tran B T, Hirayama H, Maeda N, et
al.Scientific reports,5:14734(2015).This technology can make AlN and Si serve as a contrast by Si substrate graph
Bottom interface forms periodic air-gap, and the stress of AlN film is discharged using these air-gaps and improves crystal quality, but by
It needs extremely thick AlN epitaxial layer to obtain smooth surface in the figure of micro meter periodic, to considerably increase growth cycle, increases
Extension cost is added.
Summary of the invention
It is an object of the invention to overcome the shortcomings of on existing Si grow high quality thick film AlN technology and reduce extension at
This, provide it is a kind of for obtaining the underlay producing technique and its epitaxy method of high quality thick film AlN on a si substrate, i.e., using receiving
Rice figure silicon substrate technology, to prepare high quality thick film AlN material on Si.
To achieve the goals above, technical solution is as follows:
A method of preparing thick film AlN on a si substrate, comprising the following steps:
1) one layer of aln nucleation layer is grown on a si substrate；
2) one layer of hard mask is deposited on aln nucleation layer；
3) certain thickness nano impression glue is coated on hard mask surface；
4) selection has round or polygonal hole array pattern nano-imprint stamp, by the figure on nano-imprint stamp
It is transferred on nano impression glue, wherein the aperture in hole is 50nm in the circle of the nano-imprint stamp or polygonal hole array
~1 μm, the period is 100nm~2 μm；
5) glue remaining below the depressed area with oxygen gas plasma removal nano impression glue pattern, exposes hard at depressed area
Matter mask surface；
It 6) will be in the pattern transfer to hard mask on nano impression glue by etching；
It 7) will be in the pattern transfer to aln nucleation layer on hard mask by etching；
8) the nano impression glue of surface residual is removed；
9) by etching by the pattern transfer on hard mask and aln nucleation layer to Si substrate, Si substrate etching is deep
Degree is 10nm~1 μm；
10) hard mask for removing surface residual, obtains nano graph substrate；
11) high-temperature AlN cross growth layer is grown on nano graph substrate；
12) high-temperature AlN longitudinal growth layer is grown on high-temperature AlN cross growth layer.
Thick film AlN material on the nano graph Si substrate being prepared by the above method, including successively layer from the bottom to top
Folded nano graph Si substrate, nano graph AlN nucleating layer, high-temperature AlN cross growth layer and high-temperature AlN longitudinal growth layer,
In, with the sky of periodic arrangement in nano graph Si substrate, nano graph AlN nucleating layer and high-temperature AlN cross growth layer
Air gap, depth of the air-gap in Si substrate are 10nm~1 μm, and cross section maximum width is 50nm~1 μm, and the period is
100nm~2 μm.
Further, in the above method, the thickness for the aln nucleation layer that step 1) is grown on a si substrate is preferably
10nm~2 μm.It is preferred that use metal organic chemical vapor deposition (mocvd) (MOCVD) aln nucleation layer, growth temperature be 900~
1300 DEG C, growth pressure be 10~200mbar, can also use molecular beam epitaxy (MBE), hydride gas-phase epitaxy (HVPE) with
And the methods of chemical vapor deposition (CVD) growth.
Above-mentioned steps 2) certain thickness is preferably deposited on nucleating layer with plasma enhanced chemical vapor deposition method (PECVD)
The hard mask of degree, the material of the hard mask can be silica, silicon nitride etc.；Or it is heavy using magnetron sputtering technique
Product metal mask, such as nickel, aluminium metal mask.The thickness of the hard mask is in 10nm~2 μm.
Above-mentioned steps 3) usually with sol evenning machine in the certain thickness nano impression glue of hard mask surface spin coating, nano impression
Depending on the size characteristic of the thickness of glue nano-imprint stamp used in the step 4).
Above-mentioned steps 4) described in nano-imprint stamp can according to need selection structure snd size, can be nanoscale
Round hole battle array, hexagonal hole battle array etc., aperture (maximum width of finger-hole cross section) is at 1 μm or less.
Above-mentioned steps 6) preferably use sense coupling (ICP) method by the pattern transfer on nano impression glue
Onto hard mask, until etching into aln nucleation layer surface.
Above-mentioned steps 7) preferably the pattern transfer on hard mask is arrived with sense coupling (ICP) method
On aln nucleation layer, until etching into Si substrate surface.
Above-mentioned steps 8) receiving for aln surface remnants can be removed using the corrosive liquid that the concentrated sulfuric acid and hydrogen peroxide form
Rice coining glue.
Above-mentioned steps 9) preferably use sense coupling (ICP) method.
Above-mentioned steps 10) the silicon oxide hard exposure mask of hydrofluoric acid removal substrate surface remnants can be used.
Above-mentioned steps 1) growing aluminum nitride nucleating layer, step 11) growth high-temperature AlN cross growth layer and step 12) growth
The method of high-temperature AlN longitudinal growth layer can selected from metal organic chemical vapor deposition (mocvd) (MOCVD), molecular beam epitaxy (MBE),
One of hydride gas-phase epitaxy (HVPE) and chemical vapor deposition (CVD) are a variety of.
The growth conditions of step 11) high-temperature AlN cross growth layer is preferred are as follows: temperature be 900~1300 DEG C, pressure be 10~
200mbar, V/III are 50~500, and growth thickness is 10nm~10 μm.The growth item of step 12) high-temperature AlN longitudinal growth layer
Part is preferred are as follows: temperature is 500~1300 DEG C, and pressure is 10~100mbar, and V/III is 500~1000, growth thickness 10nm
~10 μm.
The present invention substitutes traditional plain film Si substrate using unique nano graph Si substrate, can effectively overcome Si substrate
On be unable to the difficulty of extension thick film AlN, can be effective further by accurately controlling growth conditions, such as temperature, pressure, V/III
The epitaxial thickness for improving AlN, is effectively reduced the defect density in AlN epitaxial layer, increases substantially the crystal quality of AlN, improves
The crystal quality and device performance of subsequent device material.The method of the present invention obtains high quality thick film AlN, thickness on a si substrate
It can reach 4 μm or more.Refering to what is shown in Fig. 2, X-ray diffraction (XRD) plane of symmetry (002) of AlN epitaxial layer and asymmetric face (102)
The halfwidth (FWHM) of rocking curve is respectively 508arcsec and 665arcsec.
Compared with AlN material epitaxy technology on existing relatively complicated Si and micron figure Si substrate, the present invention exists
High quality thick film AlN material is grown on nano graph Si substrate, not only preparation method is simple, can be answered by extensive industrialization
With, and very high crystal quality can be obtained in certain thickness AlN material, improve the crystal matter of subsequent device material
Amount, raising device performance, and the feature easily peelable using silicon substrate, UV-LED device development of the present invention to vertical structure,
And MEMS (MEMS), light emitting diode (LED), radio-frequency filter (RFT) and surface acoustic wave (SAW) device manufacture and
The fields such as high-frequency wideband communication are of great significance, and have broad application prospects.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of high quality thick film AlN material on nano graph Si substrate of the present invention；
Fig. 2 is the flow diagram that the method for the present invention prepares nano graph Si substrate and nano graph AlN nucleating layer；
In Fig. 1 and Fig. 2: 1-Si substrate, 2-AlN nucleating layer, 3- air-gap, 4- high-temperature AlN cross growth layer, 5- high temperature
AlN longitudinal growth layer, 6- hard mask silica, 7- nano impression glue, 8- nano-imprint stamp.
Fig. 3 is X-ray diffraction (XRD) figure of AlN epitaxial layer prepared by the embodiment of the present invention 1；Wherein (a) is AlN extension
The XRD plane of symmetry (002) rocking curve of layer；It (b) is the asymmetric face XRD (102) rocking curve of AlN epitaxial layer.
Specific embodiment
With reference to the accompanying drawing, by embodiment, further the present invention will be described in detail, but does not limit in any way
The scope of the present invention.
As shown in Figure 1, on nano graph Si substrate prepared by the present invention high quality thick film AlN material structure, by down toward
On successively include: nano graph Si substrate 1, nano graph AlN nucleating layer 2, air-gap 3, high-temperature AlN cross growth layer 4 and height
Warm AlN longitudinal growth layer 5.
Embodiment 1
The preparation flow of high quality thick film AlN material is referring to fig. 2 on nano graph Si substrate, comprising the following steps:
(1) a kind of monocrystalline substrate 1 is selected, the crystal orientation of silicon can be silicon (111), silicon (100), silicon (110) etc.；
(2) the growing aluminum nitride nucleating layer 2 in monocrystalline substrate 1, growth temperature are 900-1300 DEG C, and growth pressure is
10-200mbar, growth thickness 10nm, in Fig. 2 shown in (a)；
(3) one layer of hard is deposited on aln nucleation layer 2 with plasma enhanced chemical vapor deposition method (PECVD) to cover
Film silica 6, depositing temperature are 200-400 DEG C, and growth thickness is 10nm-2 μm, in Fig. 2 shown in (b)；
(4) structure snd size for selecting nano-imprint stamp, with hexagonal hole battle array, the figure period is 1 μm, and graphic aperture is
600nm, graphics depth 500nm；
(5) according to the nano impression glue of the size characteristic spin coating specific thicknesses of nano-imprint stamp, TU7-220 is selected here
Glue is imprinted, nano impression glue 7 is spin-coated on 6 surface of hard mask silica with sol evenning machine, in Fig. 2 shown in (c)；
(6) pattern on nano-imprint stamp 8 is transferred on nano impression glue 7 with nano marking press, in Fig. 2 (d)
It is shown；
(7) the nano impression glue 7 remaining with sense coupling (ICP) removal figure depressed area lower section, such as
In Fig. 2 shown in (e), etching gas is oxygen gas plasma, etch period 5s-300s；
(8) use sense coupling (ICP) by the pattern transfer on nano impression glue 7 to hard mask dioxy
In SiClx 6, until etching into 2 surface of aln nucleation layer, in Fig. 2 shown in (f), etching gas is fluoroform, is carved
The erosion time is 10s-2000s；
(9) use sense coupling (ICP) by the pattern transfer on hard mask silica 6 to aluminium nitride
On nucleating layer 2, until etching into 1 surface of Si substrate, in Fig. 2 shown in (g), etching gas be chlorine, boron chloride and
The mixed gas of bromine gas, etch period 10s-2000s；
(10) the remaining nano impression glue 7 of the corrosive liquid removal formed with the concentrated sulfuric acid and hydrogen peroxide, (h) institute in Fig. 2
Show, the mass ratio of the concentrated sulfuric acid and hydrogen peroxide is 6:1-3:1, and corrosion temperature is 80-300 DEG C, etching time 10s-1000s；
(11) pattern on nano graph aln nucleation layer 2 is transferred to sense coupling (ICP)
On Si substrate 1, in Fig. 2 shown in (i), etching gas is the mixed gas of tetrafluoromethane and oxygen, tetrafluoromethane and oxygen
Mass flow ratio is 6:1-3:1, etch period 10s-2000s, etching depth 10nm；
(12) silica of surface residual is removed with hydrofluoric acid, etching time 10s-100s is obtained as in Fig. 2 (j)
Shown in nano graph Si substrate 1 and nano graph aln nucleation layer 2；
(13) on nano graph Si substrate 1 and nano graph AlN nucleating layer 2, high-temperature AlN cross growth layer 4 is grown, and
Air-gap 3 is formed, growth temperature is 900-1300 DEG C, and growth pressure 10-200mbar, V/III are 10~500, growth thickness
It is 1.5 μm；
(14) one layer of high-temperature AlN longitudinal growth layer, growth temperature 500- are grown on high-temperature AlN cross growth layer 4
1300 DEG C, growth pressure 10-100mbar, V/III are 500~1000, and growth thickness is 2 μm.
Fig. 3 is X-ray diffraction (XRD) figure of AlN epitaxial layer manufactured in the present embodiment, wherein (a) is AlN epitaxial layer
The XRD plane of symmetry (002) rocking curve is (b) the asymmetric face XRD (102) rocking curve of AlN epitaxial layer, it can be seen that wave
The halfwidth very little of curve illustrates that the quality of AlN thick film is fine, which is in best level in the world.
Embodiment 2
Prepare the method for high quality thick film AlN material on nano graph Si substrate referring to fig. 2, comprising the following steps:
(1) a kind of monocrystalline substrate 1 is selected, the crystal orientation of silicon can be silicon (111), silicon (100)；
(2) the growing aluminum nitride nucleating layer 2 in monocrystalline substrate 1, growth temperature are 900-1300 DEG C, and growth pressure is
10-200mbar, growth thickness 200nm；
(3) one layer of hard is deposited on aln nucleation layer 2 with plasma enhanced chemical vapor deposition method (PECVD) to cover
Film silica, depositing temperature are 200-400 DEG C, and growth thickness is 10nm-2 μm；
(4) structure snd size for selecting nano-imprint stamp, with hexagonal hole battle array, the figure period is 1.4 μm, graphic aperture
It is 1 μm, graphics depth 500nm；
(5) according to the nano impression glue of the size characteristic spin coating specific thicknesses of nano-imprint stamp, TU7-220 is selected here
Glue is imprinted, nano impression glue is spin-coated on 1 surface of Si substrate with sol evenning machine；
(6) pattern on nano-imprint stamp is transferred on nano impression glue with nano marking press；
(7) with nano impression glue remaining below sense coupling (ICP) removal figure depressed area, etching
Gas is oxygen gas plasma, etch period 5s-300s；
(8) use sense coupling (ICP) by the pattern transfer on nano impression glue to hard mask dioxy
In SiClx, until etching into 2 surface of aln nucleation layer, etching gas is fluoroform, etch period 10s-
2000s；
(9) use sense coupling (ICP) by the pattern transfer on silica to aln nucleation layer 2
On, until etching into 1 surface of Si substrate, etching gas is the mixed gas of chlorine, boron chloride and bromine gas, etch period
For 10s-2000s；
(10) the nano impression glue of the corrosive liquid removal aln surface remnants formed with the concentrated sulfuric acid and hydrogen peroxide, dense sulphur
The mass ratio of acid and hydrogen peroxide is 6:1-3:1, and corrosion temperature is 80-300 DEG C, etching time 10s-1000s；
(11) pattern on nano graph aln nucleation layer 2 is transferred to sense coupling (ICP)
On Si substrate 1, etching gas is the mixed gas of tetrafluoromethane and oxygen, and the mass flow ratio of tetrafluoromethane and oxygen is 6:1-
3:1, etch period 10s-2000s, etching depth are 10nm-5 μm；
(12) with the silica of hydrofluoric acid removal surface residual, etching time 10s-100s；
(13) on nano graph Si substrate 1 and nano graph AlN nucleating layer 2, high-temperature AlN cross growth layer 4 is grown, and
Air-gap 3 is formed, growth temperature is 900-1300 DEG C, and growth pressure 10-200mbar, V/III are 10~500, growth thickness
It is 3 μm；
(14) one layer of high-temperature AlN longitudinal growth layer, growth temperature 500- are grown on high-temperature AlN cross growth layer 4
1300 DEG C, growth pressure 10-100mbar, V/III are 500~1000, and growth thickness is 1 μm.
Embodiment described above is merely illustrative of the invention's technical idea and feature, and the description thereof is more specific and detailed,
Its object is to make those skilled in the art can understand the content of the present invention and implement it accordingly, therefore cannot be only with this
It limits the scope of protection of the present invention, but it cannot be understood as limitation of the scope of the invention.It should be pointed out that pair
For those skilled in the art, without departing from the inventive concept of the premise, several deformations can also be made and changed
Into variation made by that is, all spirit revealed according to the present invention should be included within the scope of protection of the present invention.
Claims (10)
1. the method that one kind prepares thick film AlN on a si substrate, comprising the following steps:
1) one layer of aln nucleation layer is grown on a si substrate；
2) one layer of hard mask is deposited on aln nucleation layer；
3) certain thickness nano impression glue is coated on hard mask surface；
4) selection has round or polygonal hole array pattern nano-imprint stamp, by the pattern transfer on nano-imprint stamp
Onto nano impression glue, wherein the aperture in hole is the μ of 50nm~1 in the circle of the nano-imprint stamp or polygonal hole array
M, period are 100nm~2 μm；
5) glue remaining below the depressed area with oxygen gas plasma removal nano impression glue pattern exposes hard at depressed area and covers
Film surface；
It 6) will be in the pattern transfer to hard mask on nano impression glue by etching；
It 7) will be in the pattern transfer to aln nucleation layer on hard mask by etching；
8) the nano impression glue of surface residual is removed；
9) by etching by the pattern transfer on hard mask and aln nucleation layer to Si substrate, Si substrate etching depth is
10nm~1 μm；
10) hard mask for removing surface residual, obtains nano graph substrate；
11) high-temperature AlN cross growth layer is grown on nano graph substrate；
12) high-temperature AlN longitudinal growth layer is grown on high-temperature AlN cross growth layer.
2. the method as described in claim 1, which is characterized in that the thickness for the aln nucleation layer that step 1) is grown on a si substrate
Degree is 10nm~2 μm.
3. the method as described in claim 1, which is characterized in that step 2) is with plasma enhanced chemical vapor deposition method in nitrogen
Change and deposit hard mask on aluminium nucleating layer, the material of the hard mask is silica or silicon nitride；Or it is splashed using magnetic control
Penetrate technology deposited metal hard mask；The hard mask with a thickness of 10nm~2 μm.
4. the method as described in claim 1, which is characterized in that step 6) uses sense coupling method by nanometer
It imprints in the pattern transfer to hard mask on glue, until etching into aln nucleation layer surface；Step 7) induction coupling
Method for etching plasma is closed by the pattern transfer to aln nucleation layer on hard mask, until etching into Si substrate surface
Until.
5. the method as described in claim 1, which is characterized in that the corrosive liquid that step 8) is formed using the concentrated sulfuric acid and hydrogen peroxide
Remove the nano impression glue of aln nucleation layer surface residual.
6. the method as described in claim 1, which is characterized in that step 9) is etched using sense coupling method
Si substrate.
7. the method as described in claim 1, which is characterized in that the material of the hard mask is silica, in step 10)
With the silicon oxide hard exposure mask of hydrofluoric acid removal substrate surface remnants.
8. the method as described in claim 1, which is characterized in that step 1) growing aluminum nitride nucleating layer, step 11) grow high temperature
The method of AlN cross growth layer and step 12) growth high-temperature AlN longitudinal growth layer is selected from one of following method or a variety of:
Metal organic chemical vapor deposition (mocvd), molecular beam epitaxy, hydride gas-phase epitaxy and chemical vapor deposition.
9. the method as described in claim 1, which is characterized in that the growth conditions of step 11) high-temperature AlN cross growth layer are as follows:
Temperature is 900~1300 DEG C, and pressure is 10~200mbar, and V/III is 50~500, and growth thickness is 10nm~10 μm；Step
12) growth conditions of high-temperature AlN longitudinal growth layer are as follows: temperature is 500~1300 DEG C, and pressure is 10~100mbar, and V/III is
500~1000, growth thickness is 10nm~10 μm.
10. thick film AlN material on a kind of nano graph Si substrate, including stack gradually from the bottom to top nano graph Si substrate,
Nano graph AlN nucleating layer, high-temperature AlN cross growth layer and high-temperature AlN longitudinal growth layer, wherein nano graph Si substrate,
With the air-gap of periodic arrangement in nano graph AlN nucleating layer and high-temperature AlN cross growth layer, the air-gap is in Si lining
Depth in bottom is 10nm~1 μm, and cross section maximum width is 50nm~1 μm, and the period is 100nm~2 μm.
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