CN102359956B - Raman characterization method of corrosion stress of alpha surface GaN epitaxial layer film - Google Patents
Raman characterization method of corrosion stress of alpha surface GaN epitaxial layer film Download PDFInfo
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Abstract
The invention discloses a Raman characterization method of corrosion stress of an alpha surface GaN epitaxial layer film. The Raman characterization method comprises the following steps of 1, cleaning the surface of an alpha surface GaN epitaxial layer film, 2, carrying out a Raman scattering test on the alpha surface GaN epitaxial layer film to obtain a frequency shift value of an uncorroded E2 phonon mode, 3, carrying out a KOH solution corrosion test and decontamination treatment on the alpha surface GaN epitaxial layer film, and carrying out a Raman scattering test on the corroded alpha surface GaN epitaxial layer film to obtain a frequency shift value of a corroded E2 phonon mode, and 4, according to an offset delta E2 which is the difference of the frequency shift value of the corroded E2 phonon mode of the alpha surface GaN epitaxial layer film and the frequency shift value of the uncorroded E2 phonon mode of the alpha surface GaN epitaxial layer film, calculating corrosion stress of the alpha surface GaN epitaxial layer film by a formula of sigma xx=delta E2/k, wherein k is a constant. Through adopting two Raman scattering tests on an alpha surface GaN epitaxial layer film before and after the corrosion, the Raman characterization method eliminates the influence from a substrate on alpha surface GaN epitaxial layer film stress, wherein when a conventional Raman characterization method is adopted, the influence exists. Through the Raman characterization method, calculated corrosion stress of an alpha surface GaN epitaxial layer film has a small error. Therefore, the Raman characterization method can be utilized for characterization of corrosion stress of alpha surface GaN epitaxial layer films having different structures.
Description
Technical field
The invention belongs to microelectronics technology, relate to corrosion and the characterizing method of semiconductor material, specifically a kind of Raman characterization method of thin film corrosive stress.
Background technology
The Micrometer-Nanometer Processing Technology based on silicon materials take integrated circuit as sign has brought up modern information society.It is generally acknowledged, the manufacturing limit of silicon materials is 10nm live widths.Be subjected to the restriction of physical principle, just unlikely produce stable performance, high frequency, high speed and powerful photoelectric device that integrated level is higher less than 10nm.Therefore, current technical progress on silicon materials will seem more and more difficult, and people place hope on third generation semiconductor material, i.e. the electronic behavior of III-V group-III nitride and alloy material thereof.That cause at first that people pay close attention to is the GaN of wurtzite structure, and it has high electron mobility, and high thermal conductivity and good current capacity etc. are well suited for and make power device, photoelectric device, HEMT, LED and LD.But owing to being difficult to produce large-sized monocrystalline, make people can only use MOCVD, on the substrate of some stable performances, these substrates generally have the methods such as MBE and ELOG with the GaN film growth, sapphire, SiC, ZnO, LiAlO
2Deng.People wish that it can replace silicon, provide the current information era development desired high speed, and high frequency and powerful demand overcome the more and more less dimension limit effect that runs into of present electron device.
The GaN of wurtzite structure is a kind of of close-packed hexagonal structure, the characteristics of this structure, make in the nitride material of wurtzite structure and exist very large spontaneous polarization effect and piezoelectric polarization effect, these effects are useful to power device, it can in the situation that the heterojunction boundary place that makes different materials of need not adulterating forms highdensity 2DEG, make device with high electron mobility become possibility.In addition, according to the quantum well devices that the GaN of wurtzite structure makes, its light emitting region has comprised the frequency range of blue light, makes the general lighting pattern that subversive change occur.Particularly at the r face, namely
The nonpolar a face of the Grown on Sapphire Substrates of face
Material can be eliminated the red shift of wavelength that occurs because of quantum confinement Stark effect.But the dislocation desity in nonpolar a face GaN is very high, for example, adopts the material of mocvd method growth, and line dislocation density has reached 3 * 10
10/ cm
2, and the density of stacking fault has reached 3.5 * 10
5/ cm
2
The reason that causes a face GaN material to have highdensity dislocation like this and defective mainly contains two: the one, lack the backing material that is complementary with the GaN lattice parameter; The 2nd, the lattice mismatch between backing material and epitaxial loayer film and thermal mismatching and the stress that causes.Fig. 1 is the Lattice Matching schematic diagram of a face GaN epitaxial loayer film and r surface sapphire substrate, as can be seen from Figure 1, the a face GaN epitaxial loayer film of growing on the r surface sapphire substrate, the lattice mismatch that causes due to the size of lattice parameter separately, the dislocation that tends to form and larger stress, thereby affect the crystalline quality of a face GaN epitaxial loayer film, and then have influence on the luminescent properties of material.
Although people generally use horizontal outgrowth (ELOG) method can reduce greatly dislocation and the defective of GaN film now, but the stress that causes because of lattice mismatch and thermal mismatching is to produce the main cause that the GaN membraneous material has highdensity dislocation like this and defective, it is the key factor of GaN epitaxial loayer crystalline quality, emission wavelength and the luminescence efficiency of GaN based quantum well have directly been affected, therefore, the sign for the epitaxial loayer membrane stress just seems particularly important.
Although GaN membraneous material, heterojunction and quantum well devices thereof all have the stronger stronger resistance to corrosions such as antiacid alkali resistant, theoretical according to elastic stress, the size of stress can accelerated corrosion speed, reduce reliability and the service life of materials and devices, the corrosion stress that discharges therefrom can compare acquisition by the frequency displacement with the front Raman scattering of corrosion.The method of measuring at present membrane stress is a lot, mainly contain the Raman method, x-ray diffraction method, double crystal diffraction method and laser interferance method etc., these methods all need by the counting lattice parameter, with the lattice parameter of body material, namely theoretical lattice parameter compares, and calculates the strain parameter of epitaxial loayer film, then theoretical according to elastic strain, obtain the stress state of epitaxial loayer film, means are comparatively complicated, and the error that produces therefrom is also larger; And conventional Raman characterizes the method for stress, because single just utilizes the skew at Raman phonon peak, can't eliminate the skew at the phonon peak that brings out because of backing material, and extension layer film stress is produced larger error.
Summary of the invention
The object of the invention is to avoid above-mentioned the deficiencies in the prior art, a kind of Raman characterization method of a face GaN epitaxial loayer thin film corrosive stress is proposed, by the relative size to Raman scattering peak frequency displacement before and after thin film corrosive, eliminate because of and backing material between the skew at the stress phonon peak that brings out, the sign of realization to extension layer film corrosion stress.
Key problem in technology of the present invention is to utilize corrosion membraneous material to be produced the characteristics of stress, i.e. corrosion stress is poor by twice frequency displacement in conjunction with the difference at Raman phonon peak, twice of corrosion front and back, has eliminated the impact of backing material on the peak frequency displacement of extension layer film phonon.Implementation step comprises as follows:
1) a face GaN epitaxial loayer film being carried out cleaning surfaces processes;
2) the Raman scattering test before the Argon ion laser that is at room temperature 514.5nm with wavelength with a face GaN epitaxial loayer film after cleaning corrodes is measured its a face GaN epitaxial loayer film before corrosion and is existed
Under polarization mode, phonon vibration pattern E
2Frequency shift value E
2, pre
3) be 10%～20% pure KOH solution of analysis with mass concentration, a face GaN epitaxial loayer film is carried out corrosion treatment;
4) a face GaN epitaxial loayer film after corrosion is carried out Raman scattering, a face GaN epitaxial loayer film of measuring after corroding exists
Under polarization mode, phonon vibration pattern E
2Frequency shift value E
2, post
5) exist according to a face GaN epitaxial loayer film before and after corrosion
Under polarization mode, phonon vibration pattern E
2Frequency displacement position offset Δ E
2=E
2, post-E
2, pre, the stress of calculating a face GaN epitaxial loayer film: σ
xx=Δ E
2/ k, wherein k is constant.
Describedly a face GaN epitaxial loayer film is carried out cleaning surfaces processing, is that a face GaN epitaxial loayer film is placed on vacuum tightness 5.0 * 10
-3In the CVD furnace chamber of mbar; Pass at ambient temperature the nitrogen that flow is 60～100 liter/mins of clocks, remove cut and the surface attachments of film surface.
Described a face GaN epitaxial loayer film is carried out corrosion treatment, carries out as follows:
3a) a face GaN epitaxial loayer film being put into mass concentration is that 10%～20% pure KOH solution of analysis soaked 1～3 minute;
3b) take out a face GaN epitaxial loayer film, float with hydrochloric acid is little, remove the KOH solution and the corrosion product that condense on a face GaN epitaxial loayer film;
3c) carry out ultrasonic processing with acetone, alcohol and deionized water respectively, remove the pollutant on surface, cleaned 1～3 minute with plasma water;
3d) under the room temperature condition, do with the nitrogen punching that flow is 60～100 liter/mins of clocks, kept the attachment that is produced to remove corrosion 1～5 minute.
The present invention is owing to having adopted twice Raman scattering before and after a face GaN epitaxial loayer thin film corrosive, thereby eliminated thermal stress between backing material and film to the impact of the skew at a face GaN phonon peak, avoided the derivation of equation and mathematical computations comparatively complicated in general characterizing method; Simultaneously because the present invention utilizes the nonpolar phonon vibration pattern E that uses in conventional Raman characterization method
2Peak offset Δ E
2=E
2, post-E
2, pre, the corrosion stress of a face GaN epitaxial loayer film is characterized, formula is simple, be easy to realize, and error is less.
Description of drawings
Fig. 1 is the Lattice Matching schematic diagram of existing three kinds of a face GaN epitaxial loayer films and r surface sapphire substrate;
Fig. 2 is a face GaN epitaxial loayer film schematic diagram of existing different structure;
Fig. 3 is process flow diagram of the present invention.
Embodiment
The present invention carries out the stress of a face GaN epitaxial loayer film to characterize on three a face GaN epitaxial loayer films shown in Figure 2.This Fig. 2 (a) is the structure of superlattice type a face GaN epitaxial loayer film, be 25nm low temperature AI N cushion by a layer thickness of first growing on the r surface sapphire substrate, continued growth a layer thickness again is 1020 ℃ of AlN cushions of high temperature of 100nm, then continued growth a layer thickness is the AlN/AlGaN superlattice layer of 200nm, and a layer thickness of growing at last is that a face GaN cap rock of 1500nm forms; Fig. 2 (b) is the structure of enhancement mode a face GaN epitaxial loayer film, be 25nm low temperature AI N cushion by a layer thickness of first growing on the r surface sapphire substrate, continued growth a layer thickness again is 1020 ℃ of AlN cushions of high temperature of 100nm, and a layer thickness of growing at last is that a face GaN cap rock of 1500nm forms; Fig. 2 (c) is the structure of plain edition a face GaN epitaxial loayer film, is 25nm low temperature AI N cushion by a layer thickness of first growing on the r surface sapphire substrate, and a layer thickness of growing at last is that a face GaN cap rock of 1500nm forms.
With reference to Fig. 3, the present invention provides following three embodiment to the Raman characterization method of a face GaN epitaxial loayer thin film corrosive stress shown in Figure 2.
Embodiment 1: the Raman that the superlattice type a face GaN sample shown in Fig. 2 (a) is carried out corrosion stress characterizes.
Step 1 is carried out cleaning surfaces to superlattice type a face GaN epitaxial loayer film and is processed.
Superlattice type a face GaN sample is placed on vacuum tightness 5.0 * 10
-3In the CVD furnace chamber of mbar, and pass into the nitrogen that flow is 60 liter/mins of clocks, at ambient temperature, remove sample surfaces cut and surface attachments.
Step 2 will have been removed the superlattice type a face GaN epitaxial loayer film sample of surface contaminant, and the Argon ion laser that is at room temperature 514.5nm with wavelength carries out the Raman scattering test.
Superlattice type a face GaN epitaxial loayer film sample is placed on the Raman scattering test board, and characteristics nonpolar according to a face GaN thin-film material are made as the polarization mode of Raman scattering instrument
For a face GaN film, in the phonon vibration pattern that may occur under this polarization mode, phonon vibration pattern E
2Horizontal optics ripple be commonly used to characterize the non-polar nature of a face GaN, be designated as E
2Due to E
2Phonon vibration pattern intensity is large, is offset little and halfwidth is narrower, can clearly characterize the stress state of nonpolar a face GaN epitaxial loayer film.Therefore the Argon ion laser that is at room temperature 514.5nm with wavelength carries out the Raman scattering test to the superlattice type a face GaN epitaxial loayer film sample of having removed surface contaminant, to obtain
Polarization mode under E
2The phonon frequency shift value.The Raman scattering test result shows, superlattice type a face GaN epitaxial loayer film exists
Polarization mode under, E
2The frequency shift value E of scattering peak
2, preBe 571.200cm
-1, higher than the standard value 568.00cm of a face GaN body material that provides in various kinds of document
-1, result shows, superlattice type a face GaN epitaxial loayer film has been subject to coming from the compressive stress of cushion and backing material.
Step 3 is carried out corrosion treatment to superlattice type a face GaN epitaxial loayer film.
Taking off superlattice type a face GaN epitaxial loayer film sample from the Raman scattering test board, is 10% analytically pure KOH solution with massfraction, superlattice type a face GaN epitaxial loayer film sample is put into this etchant solution soaked 1 minute; Subsequently, etching-stop; Take out superlattice type a face GaN epitaxial loayer film, float with hydrochloric acid is little, remove the KOH solution that condenses on superlattice type a face GaN epitaxial loayer film; Then carry out ultrasonic processing with acetone, alcohol and deionized water respectively, remove the pollutant on surface, and cleaned 1 minute with plasma water; At ambient temperature, do with the nitrogen punching that flow is 60 liter/mins of clocks, kept the attachment that is produced to remove corrosion 1 minute.
Step 4 is carried out the Raman scattering test to the superlattice type a face GaN epitaxial loayer film sample after corrosion.
Superlattice type a face GaN epitaxial loayer film sample after corrosion is placed on the Raman scattering test board again, the Argon ion laser that is at room temperature 514.5nm with wavelength carries out the Raman scattering test to the superlattice type a face GaN epitaxial loayer film sample of having removed surface contaminant after corroding, and the film sample after corrosion exists
E under polarization mode
2Phonon frequency shift value E
2, postBe 570.745cm
-1Can find, corrosion makes the stress between Sapphire Substrate and epitaxial loayer film obtain release, shows as in the Raman scattering test
E under polarization mode
2The skew of phonon frequency shift value.
Step 5, the corrosion stress of calculating superlattice type a face GaN epitaxial loayer film sample.
Obtain release because corrosion makes the stress between Sapphire Substrate and superlattice type a face GaN epitaxial loayer film, shown as E in the Raman scattering test
2 The skew of the phonon frequency shift value under polarization mode is therefore by E before and after relatively corroding
2The skew of phonon peak frequency shift value can realize the sign to superlattice type a face GaN epitaxial loayer membrane stress.
(5.1) E before and after Calculation of corrosion
2The offset Δ E of phonon peak frequency shift value
2
Raman scattering result after corrosion shows,
Polarization mode under, phonon vibration pattern E
2Frequency shift value E
2, postBe 570.745cm
-1, and E before corrosion
2Frequency shift value E
2, preBe 571.200cm
-1, as can be known at corrosion front and back E
2There is offset Δ E in phonon peak frequency shift value
2, this offset Δ E
2For:
ΔE
2＝E
2，post-E
2，pre＝0.455cm
-1
(5.2) according to E before and after corrosion
2The offset Δ E of phonon peak frequency shift value
2Calculate the corrosion stress of superlattice type a face GaN epitaxial loayer film:
σ
xx＝ΔE
2/k
Wherein k is constant, for the biaxial stress system between a face GaN thin-film material and Sapphire Substrate, and k=2.43cm
-1/ GPa.
The corrosion stress size that obtains superlattice type a face GaN epitaxial loayer film according to this formula is 0.1872GPa.
Embodiment 2: the Raman that the enhancement mode a face GaN sample shown in Fig. 2 (b) is carried out corrosion stress characterizes.
Step 1 is carried out cleaning surfaces to enhancement mode a face GaN epitaxial loayer film and is processed.
1.1) enhancement mode a face GaN sample is placed on vacuum tightness 5.0 * 10
-3In the CVD furnace chamber of mbar; 1.2) pass into the nitrogen that flow is 80 liter/mins of clocks in the CVD furnace chamber, at ambient temperature, remove cut and the surface attachments on film sample surface.
Step 2 will have been removed the enhancement mode a face GaN epitaxial loayer film sample of surface contaminant, and the Argon ion laser that is at room temperature 514.5nm with wavelength carries out the Raman scattering test.
Enhancement mode a face GaN epitaxial loayer film sample is placed on the Raman scattering test board, and the Argon ion laser that is at room temperature 514.5nm with wavelength carries out the Raman scattering test to the enhancement mode a face GaN epitaxial loayer film sample of having removed surface contaminant.The Raman scattering test result shows, enhancement mode a face GaN epitaxial loayer film exists
Polarization mode under, E
2The frequency shift value E of scattering peak
2, preBe 568.615cm
-1, a little more than the standard value 568.00cm of a face GaN body material that provides in various kinds of document
-1, result shows, enhancement mode a face GaN epitaxial loayer film has been subject to coming from the compressive stress of cushion and backing material.
Step 3 is carried out corrosion treatment to enhancement mode a face GaN epitaxial loayer film.
3.1) take off enhancement mode a face GaN epitaxial loayer film sample from the Raman scattering test board, be 15% analytically pure KOH solution with massfraction, enhancement mode a face GaN epitaxial loayer film sample is put into this etchant solution soaked 2 minutes, etching-stop;
3.2) take out enhancement mode a face GaN epitaxial loayer film, float with hydrochloric acid is little, remove the KOH solution that condenses on enhancement mode a face GaN epitaxial loayer film;
3.3) respectively with acetone, alcohol and deionized water to through step 3.2) enhancement mode a face GaN epitaxial loayer film after processing carries out ultrasonic processing, remove the pollutant on surface, and cleaned 2 minutes with plasma water;
3.4) at ambient temperature, the nitrogen that is 80 liter/mins of clocks with flow rushes the enhancement mode a face GaN epitaxial loayer film of doing after cleaning, and keeps the attachment that is produced to remove corrosion 3 minutes.
Step 4 is carried out the Raman scattering test to the enhancement mode a face GaN epitaxial loayer film sample after corrosion.
Enhancement mode a face GaN epitaxial loayer film sample after corrosion is placed on the Raman scattering test board again, the Argon ion laser that is at room temperature 514.5nm with wavelength carries out the Raman scattering test to the enhancement mode a face GaN epitaxial loayer film sample of having removed surface contaminant after corroding, and the film sample after corrosion exists
E under polarization mode
2Phonon frequency shift value E
2, postBe 568.085cm
-1Can find, corrosion makes the stress between Sapphire Substrate and epitaxial loayer film obtain release, shows as in the Raman scattering test
E under polarization mode
2The skew of phonon frequency shift value.
Step 5, the corrosion stress of calculating enhancement mode a face GaN epitaxial loayer film sample.
Obtain release because corrosion makes the stress between Sapphire Substrate and enhancement mode a face GaN epitaxial loayer film, shown as E in the Raman scattering test
2 
The skew of the phonon frequency shift value under polarization mode is therefore by E before and after relatively corroding
2The skew of phonon peak frequency shift value can realize the sign to enhancement mode a face GaN epitaxial loayer membrane stress.
(5.1) E before and after Calculation of corrosion
2The offset Δ E of phonon peak frequency shift value
2
Raman scattering result after corrosion shows,
Polarization mode under, phonon vibration pattern E
2Frequency shift value E
2, postBe 568.085cm
-1, and E before corrosion
2Frequency shift value E
2, preBe 568.615cm
-1, as can be known at corrosion front and back E
2There is offset Δ E in phonon peak frequency shift value
2, this offset Δ E
2For:
ΔE
2＝E
2，post-E
2，pre＝0.530cm
-1
(5.2) according to E before and after corrosion
2The offset Δ E of phonon peak frequency shift value
2Calculate the corrosion stress of enhancement mode a face GaN epitaxial loayer film:
σ
xx＝ΔE
2/k
Wherein k is constant, for the biaxial stress system between enhancement mode a face GaN thin-film material and Sapphire Substrate, and k=2.43cm
-1/ GPa.
Be 0.2181GPa according to the be enhanced corrosion stress size of type a face GaN epitaxial loayer film of this formula.
Embodiment 3: the Raman that the plain edition a face GaN sample shown in Fig. 2 (c) is carried out corrosion stress characterizes.
Steps A is carried out cleaning surfaces to plain edition a face GaN epitaxial loayer film and is processed.
Plain edition a face GaN sample is placed on vacuum tightness 5.0 * 10
-3In the CVD furnace chamber of mbar, and pass into the nitrogen that flow is 100 liter/mins of clocks, at ambient temperature, remove sample surfaces cut and surface attachments.
Step B will remove the plain edition a face GaN epitaxial loayer film sample of surface contaminant, and the Argon ion laser that is at room temperature 514.5nm with wavelength carries out the Raman scattering test.
Plain edition a face GaN epitaxial loayer film sample is placed on the Raman scattering test board, and the Argon ion laser that is at room temperature 514.5nm with wavelength carries out the Raman scattering test to the plain edition a face GaN epitaxial loayer film sample of having removed surface contaminant.The Raman scattering test result shows, plain edition a face GaN epitaxial loayer film exists
Polarization mode under, E
2The frequency shift value E of scattering peak
2, preBe 569.500cm
-1, higher than the standard value 568.00cm of a face GaN body material that provides in various kinds of document
-1, result shows, plain edition a face GaN epitaxial loayer film has been subject to coming from the compressive stress of cushion and backing material.
Step C carries out corrosion treatment to plain edition a face GaN epitaxial loayer film.
Taking off plain edition a face GaN epitaxial loayer film sample from the Raman scattering test board, is 20% analytically pure KOH solution with massfraction, plain edition a face GaN epitaxial loayer film sample is put into this etchant solution soaked 3 minutes; Subsequently, etching-stop; Take out plain edition a face GaN epitaxial loayer film, float with hydrochloric acid is little, remove the KOH solution that condenses on plain edition a face GaN epitaxial loayer film; Then carry out ultrasonic processing with acetone, alcohol and deionized water respectively, remove the pollutant on surface, and cleaned 3 minutes with plasma water; At ambient temperature, do with the nitrogen punching that flow is 100 liter/mins of clocks, kept the attachment that is produced to remove corrosion 5 minutes.
Step D carries out the Raman scattering test to the plain edition a face GaN epitaxial loayer film sample after corrosion.
Plain edition a face GaN epitaxial loayer film sample after corrosion is placed on the Raman scattering test board again, the Argon ion laser that is at room temperature 514.5nm with wavelength carries out the Raman scattering test to the plain edition a face GaN epitaxial loayer film sample of having removed surface contaminant after corroding, and the film sample after corrosion exists
E under polarization mode
2Phonon frequency shift value E
2, postBe 568.149cm
-1Can find, corrosion makes the stress between Sapphire Substrate and epitaxial loayer film obtain release, shows as in the Raman scattering test
E under polarization mode
2The skew of phonon frequency shift value.
Step e, the corrosion stress of calculating plain edition a face GaN epitaxial loayer film sample.
Obtain release because corrosion makes the stress between Sapphire Substrate and plain edition a face GaN epitaxial loayer film, shown as E in the Raman scattering test
2 
The skew of the phonon frequency shift value under polarization mode is therefore by E before and after relatively corroding
2The skew of phonon peak frequency shift value can realize the sign to plain edition a face GaN epitaxial loayer membrane stress.
(E1) E before and after Calculation of corrosion
2The offset Δ E of phonon peak frequency shift value
2
Raman scattering result after corrosion shows,
Polarization mode under, phonon vibration pattern E
2Frequency shift value E
2, postBe 568.149cm
-1, and E before corrosion
2Frequency shift value E
2, preBe 569.500cm
-1, as can be known at corrosion front and back E
2There is offset Δ E in phonon peak frequency shift value
2, this offset Δ E
2For:
ΔE
2＝E
2，post-E
2，pre＝1.351cm
-1
(E2) according to E before and after corrosion
2The offset Δ E of phonon peak frequency shift value
2Calculate the corrosion stress of plain edition a face GaN epitaxial loayer film:
σ
xx＝ΔE
2/k
Wherein k is constant, for the biaxial stress system between plain edition a face GaN thin-film material and Sapphire Substrate, and k=2.43cm
-1/ GPa.
The corrosion stress size that obtains plain edition a face GaN epitaxial loayer film according to this formula is 0.5560GPa.
Be only below several concrete example example of the present invention, do not consist of any limitation of the invention.Can find out from three above results, the present invention is practicality and ubiquity having certain aspect the corrosion stress sign of different structure a face GaN epitaxial loayer film.
Claims (3)
1. the Raman characterization method of an a face GaN epitaxial loayer thin film corrosive stress comprises following process:
1) a face GaN epitaxial loayer film being carried out cleaning surfaces processes;
2) the Raman scattering test before the Argon ion laser that is at room temperature 514.5nm with wavelength with a face GaN epitaxial loayer film after cleaning corrodes is measured its a face GaN epitaxial loayer film before corrosion and is existed
Under polarization mode, phonon vibration pattern E
2Frequency shift value E
2, pre
3) be 10%～20% pure KOH solution of analysis with mass concentration, a face GaN epitaxial loayer film is carried out corrosion treatment;
4) a face GaN epitaxial loayer film after corrosion is carried out Raman scattering, a face GaN epitaxial loayer film of measuring after corroding exists
Under polarization mode, phonon vibration pattern E
2Frequency shift value E
2, post
5) exist according to a face GaN epitaxial loayer film before and after corrosion
Under polarization mode, phonon vibration pattern E
2Frequency displacement position offset Δ E
2=E
2, post-E
2, pre, the corrosion stress of calculating a face GaN epitaxial loayer film: σ
xx=Δ E
2/ k, wherein k is constant.
2. the Raman characterization method of a face GaN epitaxial loayer thin film corrosive stress according to claim 1, wherein step 1) is described carries out cleaning surfaces to a face GaN epitaxial loayer film and processes, and is that a face GaN epitaxial loayer film is placed on vacuum tightness 5.0 * 10
-3In the CVD furnace chamber of mbar; Pass at ambient temperature the nitrogen that flow is 60～100 liter/mins of clocks, remove cut and the surface attachments of film surface.
3. the Raman characterization method of a face GaN epitaxial loayer thin film corrosive stress according to claim 1, step 3) wherein, carry out as follows:
3a) a face GaN epitaxial loayer film being put into mass concentration is that 10%～20% pure KOH solution of analysis soaked 1～3 minute;
3b) take out a face GaN epitaxial loayer film, float with hydrochloric acid is little, remove the KOH solution and the corrosion product that condense on a face GaN epitaxial loayer film;
3c) carry out ultrasonic processing with acetone, alcohol and deionized water respectively, remove the pollutant on surface, cleaned 1～3 minute with plasma water;
3d) under the room temperature condition, do with the nitrogen punching that flow is 60～100 liter/mins of clocks, kept the attachment that is produced to remove corrosion 1～5 minute.
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