CN101201330A - Nondestructive detecting method for strain silicon heterojunction in insulator - Google Patents
Nondestructive detecting method for strain silicon heterojunction in insulatorDownload PDFInfo
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Abstract
Description
Technical field
The invention belongs to a kind of analytical approach of strain silicon heterojunction in insulator, especially the lossless detection method of Si/SiGe/Si-SOI heterojunction.
Background technology
Strained silicon can improve the mobility in electronics and hole, promises to be the n type and the p type channel material of high-performance metal-oxide-semiconductor field (MOSFETs).As substrate, can obtain strain silicon channel n type and p type MOSFETs that electronics and hole mobility are improved with the SiGe epitaxial loayer of relaxation on the insulator.This technology integrated silicon-on-insulator (Silicon-On-Insulator, SOI) and the advantage of SiGe technology.The deformation relaxation process of SiGe epitaxial loayer normally realize by introducing on the interface between SiGe epitaxial loayer and its substrate by misfit dislocation (Misfit Dislocation).The deformation relaxation degree of the total length decision SiGe epitaxial loayer of misfit dislocation, the two ends of misfit dislocation terminate in the surface of SiGe epitaxial loayer with the form of threading dislocation (ThreadingDislocation).These threading dislocations may penetrate the epitaxial loayer of subsequent growth, enter the device function district, reduce carrier mobility, increase leakage current and cause the field effect transistor variations in threshold voltage.
Si with surface smoothing and deformation relaxation1-xGexAlloy-layer can obtain the strain Si layer that carrier mobility increases thereon as " empty substrate ", meets the Si of above-mentioned condition1-xGex" empty substrate " both can obtain on the Si substrate, also can obtain on SOI.Developed the technology of being prepared as follows in order on SOI, to obtain relaxation SiGe layer: wafer bonding (Wafer Bonding), smart peeling (Smart Cut), oxonium ion injects isolates (Separation by Implantation of Oxygen), and SOI is gone up low Ge content Si1-xGexLayer carries out oxidation, and deposits Si on SOI1-xGex(Post-DepositionAnnealing of Si anneals behind the layer1-xGexFilms Deposited on SOI).Can see that above-mentioned technological process has generally adopted high annealing.For SOI, high annealing can make its insulation course present glutinousness, thereby guarantees that misfit strain is from Si1-xGexAlloy-layer transmits to the SOI top layer Si, realizes Si1-xGexDeformation relaxation under the alloy-layer low-dislocation-density.Yet high annealing causes dislocation to generate the degradation phenomena relevant with other easily, such as Ge segregation, surface roughening etc., so the reduction annealing temperature is useful for the acquisition of high-quality SiGe layer.Employing BSG (Boron-Silicate-Glass) such as Huang have obtained high-quality deformation relaxation SiGe layer and have reduced annealing temperature as the insulated substrate layer.
Be directed to that the analytical approach of dislocation mainly contains in the semiconductor epitaxial layers: optical microscopy, transmission electron microscopy, atomic force microscopy, Raman spectroscopy and synchrotron radiation topography etc.Optical microscopy will carry out surface corrosion to sample, carries out optical imagery then, can obtain the distributed intelligence of sample surfaces threading dislocation; Transmission electron microscopy needs earlier analyzed specimen preparation to be become film sample, observes in transmission electron microscope then.Adopting optical microscopy analysis and transmission electron microscopy is destructive to the analysis of sample.When preparation is used for the sample of tem study, very easily artificially introduce defective, and because observed sample is very thin, dislocation shifts out specimen surface probably in the observation process, cause observations can not reflect the truth of defective in sample.Atomic force microscope and Raman spectrum are Dynamic Non-Destruction Measurement, yet, generally can only obtain the structural information on sample surfaces or top layer, can't determine the space distribution situation of dislocation.Synchrotron radiation twin crystal topography is as a kind of Dynamic Non-Destruction Measurement of high spatial resolution, can obtain the space distribution information of defective in epitaxial loayer and the substrate simultaneously, but, adopt synchrotron radiation twin crystal topography to fail to obtain the space distribution information of defective in strain silicon heterojunction in insulator epitaxial loayer and the substrate at present, this is because for adopt the strain silicon heterojunction that distinct methods obtained on SOI, merging appears in a plurality of Si layer diffraction peak in the twin crystal rocking curve by the asymmetrical diffraction acquisition, make and to judge the corresponding relation of Si layer diffraction peak and each Si layer, therefore, after needing to adopt a kind of method that the corresponding relation of Si layer diffraction peak and each Si layer is distinguished, analyze strain Si layer and other Si layer structure with synchrotron radiation twin crystal topography again.
Summary of the invention
The object of the present invention is to provide a kind of lossless detection method of strain silicon heterojunction in insulator, by method step provided by the invention, can be from synchrotron radiation twin crystal topography, determine the corresponding relation of each diffraction structure of strain silicon heterojunction in insulator and diffraction peak, acquisition simultaneously comprises the synchrotron radiation twin crystal pattern picture of each diffraction structure of strained silicon layer.
For achieving the above object, the present invention takes following design proposal:
1, according to the crystallography architectural feature of the strain silicon heterojunction that will detect, by how much layouts that experimentize of X ray twin crystal asymmetrical diffraction;
2, utilize synchrotron radiation monochromatic light that sample is carried out asymmetrical diffraction and obtain the twin crystal rocking curve, obtain the diffraction peak of strain silicon heterojunction;
3, be a Rotate 180 ° with sample with surface normal, obtain the twin crystal rocking curve once more;
4, the twin crystal rocking curve of Rotate 180 ° front and back is relatively judged the corresponding relation of each diffraction peak and diffraction structure;
5, adjust the incident angle of incident ray, present asymmetry or discrete peak occurs so that Si layer diffraction closes the peak;
6, be fixed into the incident angle of ray, at the synchrotron radiation pattern picture of the corresponding diffraction structure of each diffraction peak photographs.
Advantage of the present invention is: experimental arrangement is simple, quick, need not destroy space distribution situation and relevant crystallography information that sample can obtain dislocation in the strain silicon heterojunction.
Description of drawings
Fig. 1: the synoptic diagram of Si/SiGe/Si-SOI heterojunction synchrotron radiation twin crystal topography experimental arrangement.
Synchrotron radiation (004) diffraction twin crystal rocking curve before the rotation of Fig. 2 a:Si/SiGe/Si-SOI heterojunction sample,
Synchrotron radiation (004) diffraction twin crystal rocking curve behind Fig. 2 b:Si/SiGe/Si-SOI heterojunction sample Rotate 180 °.
The synchrotron radiation twin crystal pattern picture of Fig. 3 a:Si/SiGe/Si-SOI heterojunction SOI body Si substrate,
Near interface synchrotron radiation twin crystal pattern picture on Fig. 3 b:Si/SiGe/Si-SOI heterojunction SiGe layer,
Near interface synchrotron radiation twin crystal pattern picture under Fig. 3 c:Si/SiGe/Si-SOI heterojunction SiGe layer,
The synchrotron radiation twin crystal pattern picture of Fig. 3 d:Si/SiGe/Si-SOI heterojunction strain Si layer,
The synchrotron radiation double crystal diffraction pattern picture of Si layer below Fig. 3 e:Si/SiGe/Si-SOI heterojunction SiGe layer.
Fig. 4: Si/SiGe/Si-SOI heterojunction Si floor height is differentiated threeX-ray diffraction 2 θ-ω scanning curves.
The high resolution transmission electron microscopy two-dimensional crystal lattice picture of Fig. 5 a:Si/SiGe/Si-SOI heterojunction strain Si layer,
The high resolution transmission electron microscopy two-dimensional crystal lattice picture of Si layer below Fig. 5 b:Si/SiGe/Si-SOI heterojunction SiGe layer.
Among Fig. 3 a, S is a SOI body Si substrate surface cut, and g is the projection of incident wave vector on diffraction surfaces.Among Fig. 3 d, TD is a threading dislocation.The position that mutually perpendicular straight line indication dislocation exists among Fig. 5 b.
Embodiment
Embodiment 1 (the strain silicon heterojunction Si/SiGe/Si-SOI that on bonding back of the body erosion SOI (BESOI) substrate, obtains):
1 summary
Utilize high vacuum chemical gas deposition (UHVCVD) epitaxial growth Si/SiGe/Si heterojunction on bonding back of the body erosion SOI (BESOI) substrate, and it is carried out SiGe layer and the strain Si layer that in-situ low-temperature thermal treatment obtains the part relaxation.Utilization the present invention has obtained comprising the synchrotron radiation twin crystal pattern picture of the Si/SiGe/Si-SOI heterojunction of strain Si layer.High-resolution X-ray diffraction (HRTXD) and high-resolution transmission electron microscopy (HREM) experimental verification the result that obtains of the utility model.
2 experiments
Sample adopts BESOI as backing material, and top layer is Si (001).Utilize UHVCVD continuous epitaxial growth Si/SiGe/Si on this substrate.Before carrying out epitaxial growth, at first BESOI is placed the H of boiling2SO4: H2O2Carry out 15 minutes chemical cleaning in=4: 1 solution, rinsing 10 minutes in deionized water then.Before sample put into the dress specimen chamber, in 10%HF solution, soak and removed surface film oxide in 30 seconds.When the epitaxial growth system vacuum reaches 10-5During Pa, sample is pushed the growth room.The growth room is vacuumized by the turbomolecular pump of 1000l/s, and substrate vacuum tightness can reach 5x10-7Pa, growth room's pressure is lower than 0.13Pa in the epitaxial process.After vacuum reaches substrate vacuum tightness, sample is rapidly heated to 750-800 ℃ carries out surperficial high temperature deoxidation, be incubated and reduce to growth temperature after 5 minutes, be 600 ℃ for Si, SiGe is 550 ℃.Epitaxially grown gas source adopts SiH4With by H2Dilution is 15% GeH4, flow velocity is respectively 10sccm and 2sccm during growth.The heterojunction that finally obtains is followed successively by Si cap layer, SiGe layer, Si cushion and BESOI from top to bottom.After epitaxial growth is finished, sample is carried out 750 ℃ of in-situ low-temperature thermal treatments of 30 minutes.
Carry out at the pattern station of synchrotron radiation twin crystal looks physiognomy on the 4WIA line of Beijing Synchrotron Radiation laboratory (BSRL).First crystal of double crystal diffraction be (+n ,-Si (111) crystal n) arranged is selected (004) diffraction imaging, experimental arrangement is as shown in Figure 1.Energy storage ring operating voltage 2.2GeV, line scope 50-100mA.Synchrotron radiation twin crystal pattern picture record adopts the high-resolution Fuji Photo film, takes the single face backwashing manner for improving the image sharpness film development.High-resolution three axialite X-ray diffractions are measured and are carried out on Philips X ' pert X-ray diffractometer, through the CuK of four crystal Ge (220) monochromatorsα 1(
) ray is as radiation source, angular resolution is installed triple reflection Ge (220) analyzing crystal (accept the angle and be about 12 second of arcs) less than 12 second of arcs before the detector.Operating voltage 40kV, working current 40mA.Variation of ambient temperature is less than 1 ℃.Microscopic observation is carried out on JEOL-2010 type high-resolution electron microscope, and operating voltage is 200kV.
3 experimental results
Select the incident direction of synchrotron radiation incoming beam and make it satisfy (004) crystal face Bragg diffraction conditions.With the sample surfaces normal is axle, draws 004 rocking curve respectively in Rotate 180 ° front and back, shown in Fig. 2 a and Fig. 2 b.Horizontal ordinate is the angle ω of incident ray and sample surfaces, and ordinate is represented the diffracted intensity counting.Synchrotron radiation twin crystal pattern picture is taken at halfwidth A, the B-C at 1,2 and 3 peaks, D-E place in Fig. 2 a, shown in Fig. 3 a, Fig. 3 b, Fig. 3 c, Fig. 3 d, Fig. 3 e.At these positions of rocking curve, because the gradient of curve is very steep, so have small strain or lattice constant poor in crystal, the variation of intensity counting is obvious, and is therefore sensitive unusually to the detection of crystal defect.
Often have misorientation between epitaxial loayer and the substrate in the epitaxially grown single or multiple lift heterojunction, the high-resolution characteristic of three axialite X-ray diffractions can make a distinction the structural information of misorientation in the crystal structure and interplanar distance.This paper takes following operation that sample is carried out 2 θ-ω scanning: at first, sample is carried out the twin crystal rocking curve measure, obtain the diffraction peak of this heterojunction substructure; Then, the ω angle is fixed on certain peak position, utilizes three axialites to carry out 2 θ scanning.Utilize three axialite X-ray diffractions according to above-mentioned steps Si layer (004) crystal face to be done 2 θ-ω scanning curve, the gained result as shown in Figure 4.Occur on the interface of deformation relaxation in the SiGe layer or/and introduce dislocation in the Si substrate through being everlasting between SiGe layer and the Si substrate, in order to observe the distribution situation of dislocation in the Si/SiGe/Si-SOI strain silicon heterojunction, employing is looked closely method the xsect of Si/SiGe/Si-SOI strain silicon heterojunction is carried out the imaging of high-resolution electron microscopic, shown in Fig. 5 a and Fig. 5 b.
4 discuss
(1) in Fig. 2 a, Fig. 2 b, by the intensity of diffraction peak counting and peak shape as can be known, 1 peak is the diffraction peak of BESOI body Si substrate.The position of sample Rotate 180 ° front and back diffraction peak is closed and is: the angular separation at 1 and 3 peaks becomes-3000 second of arcs by 3000 second of arcs, and the angular separation at 2 and 3 peaks remains unchanged substantially, and the angular separation at 1 and 2 peaks then becomes-5000 second of arcs by 1000 second of arcs.Known Δ θ=1/2 (Δ ωA+ Δ ωB) and
Wherein θ is the Bragg angle of diffraction surfaces,
Be the angle of diffraction surfaces with the surface, Δ ωAWith Δ ωBThe angular separation of representing two diffraction peaks in the same rocking curve in sample Rotate 180 ° front and back respectively.Infer that in view of the above 2 peaks come from SiGe layer diffraction, 3 peaks are from Si layer diffraction.The angular separation at 1 and 2 peaks is owing to the different of BESOI body Si substrate and SiGe layer (004) diffraction surfaces interplanar distance and the misorientation between them, the angular separation at 1 and 3 peaks is to exist due to the pitch angle between BESOI body Si substrate and Si layer (004) diffraction surfaces, 2 with 3 peak angular separation different owing to Si layer and SiGe layer diffraction surfaces interplanar distance.
(2) below strain Si layer and the SiGe layer among the different Fig. 2 of making a, Fig. 2 b of Si layer (004) diffractionsurfaces interplanar distance 3 peak-to-peak shapes present asymmetry.Because epitaxy layer thickness is than existing the crystal face distortion or the bending that are caused by dislocation strain field to make diffraction peak under double crystal diffraction ω or ω-2 θ scan pattern broadening take place in thin and the diffraction crystal, make that Si layer diffraction peak broadening becomes a peak---3 peaks in the twin crystal rocking curve, from the diffracted intensity difference of different Si layers, finally cause the asymmetry of 3 peak-to-peak shapes in addition.Utilize three axialite X-ray diffractions that the Si layer is done 2 θ-ω scanning, owing to removed diffraction peak peak shape broadening effects such as the crystal face distortion introduced by defective or bending, make Si layer diffraction peak present the double-peak feature (see figure 4), this result verification to the analysis of Si layer diffraction peak asymmetry.
(3) the synchrotron radiation twin crystal pattern picture of halfwidth A, B-C, D-E place shooting Si/SiGe/Si-SOI strain silicon heterojunction in Fig. 2 a.Owing to occur on the interface of deformation relaxation between SiGe layer and the Si layer below it in the SiGe layer or/and introduce dislocation in the Si layer, cause the defects count in the Si cap layer of the defects count in the Si layer below the SiGe layer.The cross-like contrast of quadrature and being parallel in the synchrotron radiation twin crystal pattern picture＜011〉direction is relevant with the misfit dislocation strain field, so the synchrotron radiation twin crystal pattern image pattern 3d that takes at D and E place is corresponding with Si layer below strain Si layer and the SiGe layer respectively with Fig. 3 e.The SiGe layer is the process that (004) interplanar distance reduces gradually by complete strain to deformation relaxation takes place.After deformation relaxation took place, (004) interplanar distance at close interface down changed maximum in the SiGe layer, and changes minimum near the lattice at last interface owing to being subjected to Si cap lamination stress.The image space of Fig. 3 b is corresponding to the relatively large position of (004) interplanar distance in the SiGe layer, interplanar distance changes less, so be to close SiGe layer and strain Si bed interface lattice imaging in the SiGe layer, the image space of Fig. 3 c on rocking curve is corresponding to the less relatively position of (004) interplanar distance in the SiGe layer, interplanar distance changes greatly, thus be in the SiGe layer near Si bed interface lattice imaging below SiGe layer and the SiGe layer.
The experimental result of above-mentioned synchrotron radiation twin crystal topography and the consistent (see figure 5) of high-resolution electron microscopic imaging results that sample is carried out, that is: the relaxation of misfit strain mainly by on the interface between SiGe layer and the Si layer below it or/and introduce misfit dislocation in the Si layer below the SiGe layer and realize, concrete analysis, see " the high-resolution Electronic Micro-Analysis of Si/SiGe-OI strained heterostructure " (semiconductor journal, 2004,25 (9), 1123～1127).
Embodiment 2 (sample is isolated the strain silicon heterojunction Si/SiGe/Si-SOI that obtains on SOI (SIMOX SOI) substrate for injecting at oxygen)
According to existing data as can be known, the twin crystal rocking curve feature of the strain silicon heterojunction Si/SiGe/Si-SOI ofembodiment 2 methods acquisition is: SIMOX SOI body Si substrate peak bases high corner side presents asymmetry.There is not misorientation between SIMOX SOI top layer Si and the body Si substrate; On SIMOX SOI, in the process of preparation strain silicon heterojunction,, thereby may between strain Si layer and SOI top layer Si, introduce misorientation because deformation relaxation has taken place the SiGe layer.In addition, the deformation relaxation of SiGe layer makes Si cap layer generation strain obtain strain Si layer, and meanwhile, the strain in the SiGe layer also takes place to transmit downwards to make SOI top layer Si generation strain.Generally, the dependent variable of strain Si layer is greater than the dependent variable of SOI top layer Si, and on asymmetrical diffraction twin crystal rocking curve, the angle of elevation end at SOI body Si substrate diffraction peak is followed successively by the diffraction peak of SOI top layer Si and strain Si layer.Yet owing to may have misorientation between strain Si layer and the SOI top layer Si, the broadening effect at the peak of thickness effect and defective strain field introducing in addition finally causes the corresponding relation of Si layer diffraction peak and Si layer diffraction structure to be difficult to confirm.For the corresponding relation of clear and definite Si layer diffraction peak and Si layer diffraction structure, need differentiate the corresponding relation of diffraction peak and diffraction structure according to step of the present utility model, then on each diffraction, obtain the synchrotron radiation twin crystal pattern picture of corresponding diffraction structure.
5 sum up
Utilize synchrotron radiation twin crystal looks physiognomy, according to design proposal of the present invention, obtained twin crystal rocking curve through the heat treated Si/SiGe/Si-SOI heterojunction of in-situ low-temperature sample Rotate 180 ° front and back, judged the corresponding relation of diffraction peak and each diffraction structure of heterojunction, and taken the synchrotron radiation twin crystal looks picture that comprises strain Si layer at each diffraction peak halfwidth place of synchrotron radiation twin crystal rocking curve.The experimental result of high-resolution three axialite X-ray diffractions and high-resolution electron microscopy shows that the result that design proposal of the present utility model obtained is reliable.
Claims (3)
1. the lossless detection method of a strain silicon heterojunction in insulator is characterized in that:
(1), according to the crystallography architectural feature of the strain silicon heterojunction that will detect, by how much layouts that experimentize of X ray twin crystal asymmetrical diffraction;
(2), utilizing synchrotron radiation monochromatic light that sample is carried out asymmetrical diffraction obtains the twin crystal rocking curve, obtains the diffraction peak of strain silicon heterojunction;
(3), be a Rotate 180 ° with sample with surface normal, obtain the twin crystal rocking curve once more;
(4), the twin crystal rocking curve of Rotate 180 ° front and back relatively, judge the corresponding relation of each diffraction peak and diffraction structure;
(5), adjust the incident angle of incident ray present asymmetry or discrete peak occurs so that Si layer diffraction closes the peak;
(6), be fixed into the incident angle of ray, at the synchrotron radiation pattern picture of the corresponding diffraction structure of each diffraction peak photographs.
2. the lossless detection method of a kind of strain silicon heterojunction in insulator according to claim 1 is characterized in that: the strain silicon heterojunction Si/SiGe/Si-SOI of described sample for obtaining on bonding back of the body erosion SOI (BESOI) or smart peeling SOI (Smart-cutSOI) substrate; Described synchrotron radiation pattern at the corresponding diffraction structure of each diffraction peak photographs looks like to be respectively:
(1), is the synchrotron radiation pattern picture that Si layer below strain Si layer and the SiGe layer is taken at asymmetry or discrete Si layer diffraction peak halfwidth place respectively in peak shape;
(2), take respectively near near the synchrotron radiation pattern picture the SiGe layer upper and lower interface at halfwidth place, SiGe layer diffraction peak both sides;
(3), take the pattern picture of SOI body Si substrate at the halfwidth place of SOI body Si substrate.
3. the lossless detection method of a kind of strain silicon heterojunction in insulator according to claim 1 is characterized in that: the strain silicon heterojunction Si/SiGe/Si-SOI of described sample for obtaining on oxygen injection isolation SOI (SIMOX SOI) substrate; Described synchrotron radiation pattern at the corresponding diffraction structure of each diffraction peak photographs looks like to be respectively:
(1), the high arm of angle one side of SOI body Si substrate diffraction peak bases that is asymmetry in peak shape is taken the synchrotron radiation pattern picture of Si layer below strain Si layer and the SiGe layer respectively;
(2), take the pattern picture of SOI body Si substrate at the halfwidth place of SOI body Si substrate;
(3), take respectively near near the synchrotron radiation pattern picture the SiGe layer upper and lower interface at halfwidth place, SiGe layer diffraction peak both sides.
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| CF01 | Termination of patent right due to non-payment of annual fee | Granted publication date:20101110 Termination date:20171215 |