CN102359956A - 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 PDF

Info

Publication number
CN102359956A
CN102359956A CN2011102935240A CN201110293524A CN102359956A CN 102359956 A CN102359956 A CN 102359956A CN 2011102935240 A CN2011102935240 A CN 2011102935240A CN 201110293524 A CN201110293524 A CN 201110293524A CN 102359956 A CN102359956 A CN 102359956A
Authority
CN
China
Prior art keywords
gan epitaxial
epitaxial loayer
face gan
film
corrosion
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN2011102935240A
Other languages
Chinese (zh)
Other versions
CN102359956B (en
Inventor
郝跃
王党会
许晟瑞
张进城
张金凤
毕志伟
毛维
马晓华
赵胜雷
薛晓咏
艾姗
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Yunnan Hui Hui Electronic Technology Co Ltd
Original Assignee
Xidian University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Xidian University filed Critical Xidian University
Priority to CN 201110293524 priority Critical patent/CN102359956B/en
Publication of CN102359956A publication Critical patent/CN102359956A/en
Application granted granted Critical
Publication of CN102359956B publication Critical patent/CN102359956B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

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

The Raman characterizing method of a face GaN epitaxial loayer thin film corrosive stress
Technical field
The invention belongs to microelectronics technology, relate to the corrosion and the characterizing method of semiconductor material, specifically a kind of Raman characterizing method of thin film corrosive stress.
Background technology
With the integrated circuit is that the Micrometer-Nanometer Processing Technology based on silicon materials that indicates has brought up modern information society.It is generally acknowledged that the manufacturing limit of silicon materials is 10nm live widths.Receive 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 the silicon materials more and more difficult that will seem, 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 be difficult to produce large-sized monocrystalline, make people can only use MOCVD, on the substrate of some stable performances, these substrates generally have methods such as MBE and ELOG with the GaN film growth, sapphire, SiC, ZnO, LiAlO 2Deng.People hope 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 littler 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 and exist very large spontaneous polarization effect and piezoelectric polarization effect in the nitride material of wurtzite structure; These effects are useful to power device, and it can make the heterojunction boundary place of different materials form highdensity 2DEG under situation about need not mix, and makes device with high electron mobility become possibility.In addition, according to the quantum well devices that the GaN of wurtzite structure processes, its light emitting region has comprised the frequency range of blue light, makes the general lighting pattern that subversive change take place.Particularly at the r face; Nonpolar a face
Figure BDA0000094839060000012
material of promptly growing on the Sapphire Substrate of
Figure BDA0000094839060000011
face can be eliminated the red shift of wavelength that takes place because of quantum limit Stark effect.But the dislocation desity among the 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, lattice mismatch between backing material and the epitaxial loayer film and thermal mismatching and the stress that causes.Fig. 1 is the lattice matched synoptic 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 on the r surface sapphire substrate, growing is owing to the lattice mismatch that the size of lattice parameter separately causes, dislocation that tends to form and bigger stress; Thereby influence the crystalline quality of a face GaN epitaxial loayer film, and then have influence on the luminescent properties of material.
Though people generally use horizontal outgrowth (ELOG) method can reduce the dislocation and the defective of GaN film greatly now; But the stress that is caused 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; Directly influenced the emission wavelength and the luminescence efficiency of GaN based quantum well, therefore, just seemed particularly important for the sign of epitaxial loayer membrane stress.
Though GaN membraneous material; Heterojunction and quantum well devices thereof all have stronger stronger resistance to corrosions such as antiacid alkali resistant; Theoretical according to elastic stress; The size of stress can accelerated corrosion speed, reduces the reliability and the service life of material and device, and the corrosion stress that discharges therefrom can compare acquisition through the frequency displacement with the preceding Raman scattering of corrosion.The method of MEASUREMENTS OF THIN stress is a lot of at present, mainly contains the Raman method, x-ray diffraction method; Double crystal diffraction method and laser interferance method etc., these methods all need be through calculating lattice parameter, with the lattice parameter of body material; Promptly theoretical lattice parameter compares, and calculates the strain parameter of epitaxial loayer film, and is theoretical according to elastic strain then; Obtain the stress state of epitaxial loayer film, means are comparatively complicated, and the error that produces therefrom is also bigger; And conventional Raman characterizes the method for stress, owing to be the skew that single utilizes 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 bigger error.
Summary of the invention
The objective of the invention is to avoid the deficiency of above-mentioned prior art; A kind of Raman characterizing method of a face GaN epitaxial loayer thin film corrosive stress is proposed; Through relative size to Raman scattering peak frequency displacement before and after the thin film corrosive; Eliminate because of and backing material between the skew at the phonon peak that brings out of stress, realize sign to extension layer film corrosion stress.
Key problem in technology of the present invention is to utilize the characteristics of corrosion to membraneous material generation stress, and promptly corrosion stress is poor through twice frequency displacement in conjunction with the difference at twice Raman phonon peak before and after the corrosion, has eliminated the influence of backing material to 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 handles;
2) at room temperature use wavelength to corrode preceding Raman scattering test a face GaN epitaxial loayer film after the clean, measure its a face GaN epitaxial loayer film before corrosion and exist as the Argon ion laser of 514.5nm
Figure BDA0000094839060000021
Under the polarization mode, phonon vibration pattern E 2Frequency shift value E 2, pre
3) using mass concentration is the pure KOH solution of 10%~20% analysis, and a face GaN epitaxial loayer film is carried out corrosion treatment;
4) a face GaN epitaxial loayer film after the corrosion is carried out Raman scattering, a face GaN epitaxial loayer film of measuring after corroding exists Under the 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 the corrosion
Figure BDA0000094839060000032
Under the 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 a constant.
Describedly a face GaN epitaxial loayer film is carried out cleaning surfaces handling, is that a face GaN epitaxial loayer film is placed on vacuum tightness 5.0 * 10 -3In the CVD furnace chamber of mbar; Feed flow at ambient temperature and be 60~100 liters/minute nitrogen, remove the 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 the pure KOH solution of 10%~20% analysis soaked 1~3 minute;
3b) take out a face GaN epitaxial loayer film, float, remove the KOH solution and the corrosion product that condense on a face GaN epitaxial loayer film with hydrochloric acid is little;
3c) carry out sonicated 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, using flow is that 60~100 liters/minute nitrogen dashes and does, and keeps 1~5 minute, corrodes the attachment that is produced to remove.
The present invention is owing to adopted twice Raman scattering before and after a face GaN epitaxial loayer thin film corrosive; Thereby eliminated thermal stress between backing material and the film to the influence of the skew at a face GaN phonon peak, avoided the derivation of equation and mathematical computations comparatively complicated in the general characterizing method; Simultaneously because the present invention utilizes the nonpolar phonon vibration pattern E that uses in the conventional Raman characterization method 2Peak offset 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 matched synoptic 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 synoptic diagram of existing different structure;
Fig. 3 is a 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; Through one deck thickness of on the r surface sapphire substrate, growing earlier is 25nm low temperature AI N cushion; Continued growth one layer thickness is 1020 ℃ of AlN cushions of high temperature of 100nm again; Continued growth one layer thickness is the AlN/AlGaN superlattice layer of 200nm then, and the 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; Through one deck thickness of on the r surface sapphire substrate, growing earlier is 25nm low temperature AI N cushion; Continued growth one layer thickness is 1020 ℃ of AlN cushions of high temperature of 100nm again, and the 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 through one deck thickness of on the r surface sapphire substrate, growing earlier, and the 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 characterizing 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 handled.
Superlattice type a face GaN sample is placed on vacuum tightness 5.0 * 10 -3In the CVD furnace chamber of mbar, and to feed flow be 60 liters/minute nitrogen, at ambient temperature, removes sample surfaces cut and surface attachments.
Step 2 with the superlattice type a face GaN epitaxial loayer film sample of having removed surface contaminant, at room temperature uses wavelength to carry out the Raman scattering test as the Argon ion laser of 514.5nm.
Superlattice type a face GaN epitaxial loayer film sample is placed on the Raman scattering test board,, the polarization mode of Raman scattering appearance is made as according to the nonpolar characteristics of a face GaN thin-film material
Figure BDA0000094839060000041
As far as a face GaN film, in the phonon vibration pattern that under this polarization mode, possibly occur, phonon vibration pattern E 2Horizontal optics ripple be commonly used to characterize the non-polar nature of a face GaN, be designated as E 2Because E 2The phonon vibration mode intensity is big, squints little and halfwidth is narrower, can clearly characterize the stress state of nonpolar a face GaN epitaxial loayer film.Therefore at room temperature use wavelength the superlattice type a face GaN epitaxial loayer film sample of having removed surface contaminant to be carried out the Raman scattering test, to obtain as the Argon ion laser of 514.5nm Polarization mode under E 2The phonon frequency shift value.The Raman scattering test result shows that 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, be higher than the standard value 568.00cm of a face GaN body material that provides in the various kinds of document -1, the result shows that superlattice type a face GaN epitaxial loayer film has received the compressive stress that comes from cushion and backing material.
Step 3 is carried out corrosion treatment to superlattice type a face GaN epitaxial loayer film.
Take off superlattice type a face GaN epitaxial loayer film sample from the Raman scattering test board, using massfraction is 10% analytically pure KOH solution, superlattice type a face GaN epitaxial loayer film sample is put into this etchant solution soaked 1 minute; Subsequently, corrosion stops; Take out superlattice type a face GaN epitaxial loayer film, float, remove the KOH solution that condenses on the superlattice type a face GaN epitaxial loayer film with hydrochloric acid is little; Then carry out sonicated with acetone, alcohol and deionized water respectively, remove the pollutant on surface, and cleaned 1 minute with plasma water; At ambient temperature, using flow is that 60 liters/minute nitrogen dashes and does, and keeps 1 minute, corrodes the attachment that is produced to remove.
Step 4 is carried out the Raman scattering test to the superlattice type a face GaN epitaxial loayer film sample after the corrosion.
Superlattice type a face GaN epitaxial loayer film sample after the corrosion is placed on the Raman scattering test board once more; At room temperature use wavelength as the Argon ion laser of 514.5nm the superlattice type a face GaN epitaxial loayer film sample of having removed surface contaminant after corroding to be carried out the Raman scattering test, the film sample after the corrosion exists
Figure BDA0000094839060000051
E under the polarization mode 2Phonon frequency shift value E 2, postBe 570.745cm -1Can find that corrosion makes the stress between Sapphire Substrate and the epitaxial loayer film obtain release, in the Raman scattering test, show as
Figure BDA0000094839060000052
E under the 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.
Because corrosion makes the stress between Sapphire Substrate and the superlattice type a face GaN epitaxial loayer film obtain release, show as E in the Raman scattering test 2
Figure BDA0000094839060000053
The skew of the phonon frequency shift value under the polarization mode is therefore through 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) calculate corrosion front and back E 2The offset E of phonon peak frequency shift value 2
Raman scattering result after the corrosion shows,
Figure BDA0000094839060000054
Polarization mode under, phonon vibration pattern E 2Frequency shift value E 2, postBe 570.745cm -1, and E before the corrosion 2Frequency shift value E 2, preBe 571.200cm -1, can know E before and after corrosion 2There is offset E in phonon peak frequency shift value 2, this offset E 2For:
ΔE 2=E 2,post-E 2,pre=0.455cm -1
(5.2) according to E before and after the corrosion 2The offset 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 a constant, for the biaxial stress system between a face GaN thin-film material and the 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 handled.
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) the feeding flow is 80 liters/minute a nitrogen in the CVD furnace chamber, at ambient temperature, removes the cut and the surface attachments on film sample surface.
Step 2 with the enhancement mode a face GaN epitaxial loayer film sample of having removed surface contaminant, at room temperature uses wavelength to carry out the Raman scattering test as the Argon ion laser of 514.5nm.
Enhancement mode a face GaN epitaxial loayer film sample is placed on the Raman scattering test board, at room temperature uses wavelength the enhancement mode a face GaN epitaxial loayer film sample of having removed surface contaminant to be carried out the Raman scattering test as the Argon ion laser of 514.5nm.The Raman scattering test result shows that enhancement mode a face GaN epitaxial loayer film exists
Figure BDA0000094839060000061
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 the various kinds of document -1, the result shows that enhancement mode a face GaN epitaxial loayer film has received the compressive stress that comes from 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, using massfraction is 15% analytically pure KOH solution, enhancement mode a face GaN epitaxial loayer film sample is put into this etchant solution soaked 2 minutes, corrosion stops;
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 the 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 handling carries out sonicated, remove the pollutant on surface, and cleaned 2 minutes with plasma water;
3.4) at ambient temperature, the use flow is that 80 liters/minute nitrogen dashes the enhancement mode a face GaN epitaxial loayer film of doing after cleaning, and keeps 3 minutes, corrodes the attachment that is produced to remove.
Step 4 is carried out the Raman scattering test to the enhancement mode a face GaN epitaxial loayer film sample after the corrosion.
Enhancement mode a face GaN epitaxial loayer film sample after the corrosion is placed on the Raman scattering test board once more; At room temperature use wavelength as the Argon ion laser of 514.5nm the enhancement mode a face GaN epitaxial loayer film sample of having removed surface contaminant after corroding to be carried out the Raman scattering test, the film sample after the corrosion exists E under the polarization mode 2Phonon frequency shift value E 2, postBe 568.085cm -1Can find that corrosion makes the stress between Sapphire Substrate and the epitaxial loayer film obtain release, in the Raman scattering test, show as
Figure BDA0000094839060000071
E under the 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.
Because corrosion makes the stress between Sapphire Substrate and the enhancement mode a face GaN epitaxial loayer film obtain release, show as E in the Raman scattering test 2
Figure BDA0000094839060000072
The skew of the phonon frequency shift value under the polarization mode is therefore through 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) calculate corrosion front and back E 2The offset E of phonon peak frequency shift value 2
Raman scattering result after the corrosion shows,
Figure BDA0000094839060000073
Polarization mode under, phonon vibration pattern E 2Frequency shift value E 2, postBe 568.085cm -1, and E before the corrosion 2Frequency shift value E 2, preBe 568.615cm -1, can know E before and after corrosion 2There is offset E in phonon peak frequency shift value 2, this offset E 2For:
ΔE 2=E 2,post-E 2,pre=0.530cm -1
(5.2) according to E before and after the corrosion 2The offset 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 a constant, for the biaxial stress system between enhancement mode a face GaN thin-film material and the 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 handled.
Plain edition a face GaN sample is placed on vacuum tightness 5.0 * 10 -3In the CVD furnace chamber of mbar, and to feed flow be 100 liters/minute nitrogen, at ambient temperature, removes sample surfaces cut and surface attachments.
Step B with the plain edition a face GaN epitaxial loayer film sample of having removed surface contaminant, at room temperature uses wavelength to carry out the Raman scattering test as the Argon ion laser of 514.5nm.
Plain edition a face GaN epitaxial loayer film sample is placed on the Raman scattering test board, at room temperature uses wavelength the plain edition a face GaN epitaxial loayer film sample of having removed surface contaminant to be carried out the Raman scattering test as the Argon ion laser of 514.5nm.The Raman scattering test result shows that 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, be higher than the standard value 568.00cm of a face GaN body material that provides in the various kinds of document -1, the result shows that plain edition a face GaN epitaxial loayer film has received the compressive stress that comes from cushion and backing material.
Step C carries out corrosion treatment to plain edition a face GaN epitaxial loayer film.
Take off plain edition a face GaN epitaxial loayer film sample from the Raman scattering test board, using massfraction is 20% analytically pure KOH solution, plain edition a face GaN epitaxial loayer film sample is put into this etchant solution soaked 3 minutes; Subsequently, corrosion stops; Take out plain edition a face GaN epitaxial loayer film, float, remove the KOH solution that condenses on the plain edition a face GaN epitaxial loayer film with hydrochloric acid is little; Then carry out sonicated with acetone, alcohol and deionized water respectively, remove the pollutant on surface, and cleaned 3 minutes with plasma water; At ambient temperature, using flow is that 100 liters/minute nitrogen dashes and does, and keeps 5 minutes, corrodes the attachment that is produced to remove.
Step D carries out the Raman scattering test to the plain edition a face GaN epitaxial loayer film sample after the corrosion.
Plain edition a face GaN epitaxial loayer film sample after the corrosion is placed on the Raman scattering test board once more; At room temperature use wavelength as the Argon ion laser of 514.5nm the plain edition a face GaN epitaxial loayer film sample of having removed surface contaminant after corroding to be carried out the Raman scattering test, the film sample after the corrosion exists E under the polarization mode 2Phonon frequency shift value E 2, postBe 568.149cm -1Can find that corrosion makes the stress between Sapphire Substrate and the epitaxial loayer film obtain release, in the Raman scattering test, show as
Figure BDA0000094839060000083
E under the 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.
Because corrosion makes the stress between Sapphire Substrate and the plain edition a face GaN epitaxial loayer film obtain release, show as E in the Raman scattering test 2
Figure BDA0000094839060000084
The skew of the phonon frequency shift value under the polarization mode is therefore through 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) calculate corrosion front and back E 2The offset E of phonon peak frequency shift value 2
Raman scattering result after the corrosion shows,
Figure BDA0000094839060000085
Polarization mode under, phonon vibration pattern E 2Frequency shift value E 2, postBe 568.149cm -1, and E before the corrosion 2Frequency shift value E 2, preBe 569.500cm -1, can know E before and after corrosion 2There is offset E in phonon peak frequency shift value 2, this offset E 2For:
ΔE 2=E 2,post-E 2,pre=1.351cm -1
(E2) according to E before and after the corrosion 2The offset 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 a constant, for the biaxial stress system between plain edition a face GaN thin-film material and the 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.
Below only be several concrete example instance of the present invention, do not constitute any restriction of the present invention.Can find out that from three above results the present invention is practicality and ubiquity aspect the corrosion stress sign of different structure a face GaN epitaxial loayer film, having certain.

Claims (3)

1. the Raman characterizing 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 handles;
2) at room temperature use wavelength to corrode preceding Raman scattering test a face GaN epitaxial loayer film after the clean, measure its a face GaN epitaxial loayer film before corrosion and exist as the Argon ion laser of 514.5nm
Figure FDA0000094839050000011
Under the polarization mode, phonon vibration pattern E 2Frequency shift value E 2, pre
3) using mass concentration is the pure KOH solution of 10%~20% analysis, and a face GaN epitaxial loayer film is carried out corrosion treatment;
4) a face GaN epitaxial loayer film after the corrosion is carried out Raman scattering, a face GaN epitaxial loayer film of measuring after corroding exists
Figure FDA0000094839050000012
Under the 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 the corrosion
Figure FDA0000094839050000013
Under the 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 a constant.
2. the Raman characterizing method of a face GaN epitaxial loayer thin film corrosive stress according to claim 1, wherein step is with 1) describedly a face GaN epitaxial loayer film is carried out cleaning surfaces handle, be that a face GaN epitaxial loayer film is placed on vacuum tightness 5.0 * 10 -3In the CVD furnace chamber of mbar; Feed flow at ambient temperature and be 60~100 liters/minute nitrogen, remove the cut and the surface attachments of film surface.
3. the Raman characterizing method of a face GaN epitaxial loayer thin film corrosive stress according to claim 1, wherein step is with 3), carry out as follows:
3a) a face GaN epitaxial loayer film being put into mass concentration is that the pure KOH solution of 10%~20% analysis soaked 1~3 minute;
3b) take out a face GaN epitaxial loayer film, float, remove the KOH solution and the corrosion product that condense on a face GaN epitaxial loayer film with hydrochloric acid is little;
3c) carry out sonicated 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, using flow is that 60~100 liters/minute nitrogen dashes and does, and keeps 1~5 minute, corrodes the attachment that is produced to remove.
CN 201110293524 2011-10-02 2011-10-02 Raman characterization method of corrosion stress of alpha surface GaN epitaxial layer film Active CN102359956B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 201110293524 CN102359956B (en) 2011-10-02 2011-10-02 Raman characterization method of corrosion stress of alpha surface GaN epitaxial layer film

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 201110293524 CN102359956B (en) 2011-10-02 2011-10-02 Raman characterization method of corrosion stress of alpha surface GaN epitaxial layer film

Publications (2)

Publication Number Publication Date
CN102359956A true CN102359956A (en) 2012-02-22
CN102359956B CN102359956B (en) 2013-06-12

Family

ID=45585317

Family Applications (1)

Application Number Title Priority Date Filing Date
CN 201110293524 Active CN102359956B (en) 2011-10-02 2011-10-02 Raman characterization method of corrosion stress of alpha surface GaN epitaxial layer film

Country Status (1)

Country Link
CN (1) CN102359956B (en)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104900767A (en) * 2015-04-07 2015-09-09 圆融光电科技股份有限公司 Light-emitting diode P-type doped layer growth method
CN105745366A (en) * 2013-11-07 2016-07-06 日本碍子株式会社 GaN template substrate and device substrate
CN106707044A (en) * 2015-11-16 2017-05-24 中国科学院苏州纳米技术与纳米仿生研究所 Method for testing piezoelectric effect based on ultraviolet Raman spectrum
CN108398415A (en) * 2017-02-06 2018-08-14 中国科学院苏州纳米技术与纳米仿生研究所 The method and system of wurtzite structure single crystal orientation are tested using Raman spectrometer
CN110333221A (en) * 2019-07-15 2019-10-15 天津大学 { 110 } crystal face plane stress component measurement method and system
CN111948235A (en) * 2020-08-07 2020-11-17 广西大学 Method for measuring semipolar plane III group nitride film defect density and application thereof
WO2024075328A1 (en) * 2022-10-06 2024-04-11 日本碍子株式会社 Group iii element nitride semiconductor substrate

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101471402A (en) * 2007-12-27 2009-07-01 深圳市方大国科光电技术有限公司 Method for preparing graphical substrate of GaN-based LED by silicon 001 crystal face
CN101510504A (en) * 2009-03-13 2009-08-19 苏州纳晶光电有限公司 Transversal epitaxial growth method for nano area of semiconductor film

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101471402A (en) * 2007-12-27 2009-07-01 深圳市方大国科光电技术有限公司 Method for preparing graphical substrate of GaN-based LED by silicon 001 crystal face
CN101510504A (en) * 2009-03-13 2009-08-19 苏州纳晶光电有限公司 Transversal epitaxial growth method for nano area of semiconductor film

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
冯倩 等: "SiC衬底上异质外延GaN薄膜XPS谱和PL谱研究", 《光子学报》 *
许晟瑞 等: "金属有机物化学气相沉积生长的a(11?0)面GaN三角坑缺陷的消除研究", 《物理学报》 *

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105745366A (en) * 2013-11-07 2016-07-06 日本碍子株式会社 GaN template substrate and device substrate
CN104900767A (en) * 2015-04-07 2015-09-09 圆融光电科技股份有限公司 Light-emitting diode P-type doped layer growth method
CN104900767B (en) * 2015-04-07 2017-10-20 圆融光电科技股份有限公司 LED P-type doped layer growing method
CN106707044A (en) * 2015-11-16 2017-05-24 中国科学院苏州纳米技术与纳米仿生研究所 Method for testing piezoelectric effect based on ultraviolet Raman spectrum
CN106707044B (en) * 2015-11-16 2019-05-17 中国科学院苏州纳米技术与纳米仿生研究所 A method of the test piezoelectric effect based on uv raman spectroscopy
CN108398415A (en) * 2017-02-06 2018-08-14 中国科学院苏州纳米技术与纳米仿生研究所 The method and system of wurtzite structure single crystal orientation are tested using Raman spectrometer
CN108398415B (en) * 2017-02-06 2021-05-14 中国科学院苏州纳米技术与纳米仿生研究所 Method and system for testing wurtzite structure single crystal orientation by applying Raman spectrometer
CN110333221A (en) * 2019-07-15 2019-10-15 天津大学 { 110 } crystal face plane stress component measurement method and system
CN111948235A (en) * 2020-08-07 2020-11-17 广西大学 Method for measuring semipolar plane III group nitride film defect density and application thereof
WO2024075328A1 (en) * 2022-10-06 2024-04-11 日本碍子株式会社 Group iii element nitride semiconductor substrate

Also Published As

Publication number Publication date
CN102359956B (en) 2013-06-12

Similar Documents

Publication Publication Date Title
CN102359956B (en) Raman characterization method of corrosion stress of alpha surface GaN epitaxial layer film
US8853828B2 (en) Epitaxial substrate for semiconductor device, method for manufacturing epitaxial substrate for semiconductor device, and semiconductor device
Guo et al. Comparative study of etching high crystalline quality AlN and GaN
Han et al. Control and elimination of cracking of AlGaN using low-temperature AlGaN interlayers
EP2313543B1 (en) Growth of planar and semi-polar {1 1-2 2} gallium nitride with hydride vapor phase epitaxy (hvpe)
Park et al. Efficient stress-relaxation in InGaN/GaN light-emitting diodes using carbon nanotubes
Kim et al. Highly efficient InGaN/GaN blue LED on 8-inch Si (111) substrate
Wang et al. Residual thermal strain in thick GaN epifilms revealed by cross-sectional Raman scattering and cathodoluminescence spectra
Kurin et al. CHVPE growth of AlGaN‐based UV LEDs
Cho et al. Growth and separation of high quality GaN epilayer from sapphire substrate by lateral epitaxial overgrowth and wet chemical etching
Lee et al. A novel growth method of freestanding GaN using in situ removal of Si substrate in hydride vapor phase epitaxy
Stepanov et al. Influence of Poisson's ratio uncertainty on calculations of the bowing parameter for strained InGaN layers
US20100297790A1 (en) Method for producing semiconductor devices
Kurin et al. UV LEDs for high-current operation
JP2004119423A (en) Gallium nitride crystal substrate, its producing process, gallium nitride based semiconductor device, and light emitting diode
Xu et al. Stress and morphology of a nonpolar a-plane GaN layer on r-plane sapphire substrate
JP2005097045A (en) Method for manufacturing group iii nitride wafer
JP5381581B2 (en) Gallium nitride substrate
Lee et al. Epitaxial growth of crack-free GaN on patterned Si (111) substrate
Ravikiran et al. Effect of stress mitigating layers on the structural properties of GaN grown by ammonia molecular beam epitaxy on 100 mm Si (111)
KR100793443B1 (en) Substrate structure for semiconductor device based on nitride and method of manufacturing the same
Zhang et al. The Formation and Characterization of GaN Hexagonal Pyramids
Dikme MOVPE and characterization of GaN-based structures on alternative substrates
Chemekova et al. Aluminum nitride substrates for ultraviolet light-emitting diode structures
Kim et al. Highly efficient InGaN/GaN blue LED grown on Si (111) substrate

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
C41 Transfer of patent application or patent right or utility model
TR01 Transfer of patent right

Effective date of registration: 20161208

Address after: 650221 Yunnan city of Kunming province Dabanqiao Street office office building No. 7 room 7-114

Patentee after: Yunnan Hui Hui Electronic Technology Co., Ltd.

Address before: Xi'an City, Shaanxi province Taibai Road 710071 No. 2

Patentee before: Xidian University