Comprehensive Thin Film Analysis

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XRD vs Ellipsometry and Raman

Welcome
Today’s Topics Introduction to X-ray Diffraction (XRD) Comparison of XRD with other Metrology Methods Semiconductor Application Examples
Uwe Preckwinkel Webinar Host

Guest Speakers
Mike Lyubchenko – Applications Scientist, XRD, Madison, WI Dr. Assunta Vigliante – Head of Business Development, Semiconductor Industry, Karlsruhe, Germany

Introduction What Can XRD “See”?

When x-rays are scattered from nanoscale structures – such as atoms, molecules, films, grains or pores – a diffraction pattern will appear that carries information about the structure and morphology of the illuminated sample volume

X-ray Applications for Materials in the Semiconductor Field

XRD Metal layers Diffusion stop layers Low-k layers Silicides High-k materials Channel materials Substrate

Phase, Orientation, Stress, Thickness, Composition, Texture, Strain, Density Profiling Crystallinity Mis-cut Relaxation

Grain Size, Porosity, Roughness

Advanced Technology Platform

D8 DISCOVER

D8 DISCOVER for Thin Film Analysis Eulerian Cradle Detector KEC Göbel Mirror X-ray Source Secondary Optics 4-bounce Monochromator Ge 022 asym. D8 Goniometer .

Detectors for XRD Dimension GF >1000 GF >1500 GF >150 GF >500 Gain factor 3 Capabilities .

XRD3 – Diffraction Space Viewer .

LEPTOS Material Database .

allow straightforward analysis of: small sample features and thin films in high.Introduction XRD in the Semiconductor Field Advanced sources. optics and detectors. as well as goniometers and software. we will compare XRD to other analytical techniques and show application examples related to thin films . medium and low resolution for high-end research and fully integrated metrology During this webinar.

Semiconductor Metrology Methods & Applications Mike Lyubchenko .

phase Gate oxide / High-k: SiO2. NiSi Thickness. Al-Cu. sSOI Oxide thickness / depth. Ti/TiN. HfO2 Thickness. strained Si Thickness. composition. stress Barrier layers: Ta/TaN. orientation. phase. CoSi. TiSi. SOI. W Thickness. SiNO. porosity Silicide: WSi. crystallinity Channel: epi-SiGe. Ge profile. relaxation Substrate: Si. phase Low-k layers: Black Diamond.Semiconductor Applications Metal layers: Cu. density. phase. Ta2O5. mis-cut angle . SiLK Thickness. W/WN Thickness.

Metrology Techniques for Thin Films Film Thickness Measurement Transmission Electron Microscopy (TEM) Spectroscopic Ellipsometry (SE) X-ray Reflectivity (XRR) X-ray Fluorescence (XRF) X-ray Diffraction (XRD) Secondary Ion Mass Spectrometry (SIMS) Auger Electron Spectrometry (AES) Rutherford Backscattering Spectrometry (RBS) Elemental Composition X-ray Fluorescence (XRF) X-ray Diffraction (XRD) Auger Electron Spectrometry Spectroscopic Ellipsometry (SE) Secondary Ion Mass Spectrometry (SIMS) Rutherford Backscattering Spectrometry (RBS) Energy Dispersive Spectroscopy (EDS/TEM) .

Metrology Techniques for Thin Films Lattice Strain Characterization X-ray Diffraction (XRD) UV Raman Spectroscopy High Resolution Lattice Image (HRTEM) Surface/Interface Roughness X-ray Reflectivity (XRR) Atomic Force Microscopy (AFM) Transmission Electron Microscopy (TEM) .

..Your Turn… Use your mouse to answer the question on the right of your screen: What methods do you currently use for thin films analysis? (Check all that apply): Transmission Electron Microscopy Spectroscopic Ellipsometry Raman Spectroscopy X-ray Reflectivity X-ray Fluorescence X-ray Diffraction Other And the results are..

TEM Capabilities Multi-layer thickness capability Excellent defect detection Elemental composition (with EDS) Advantages Provides accurate film thickness Excellent contrast between films Provides film interface information Provides information on crystallinity High resolution (higher than SEM) Disadvantages Destructive. samples need thinning. down to <50 μm Specimen preparation is time and labor intensive (2-3 hrs typical) Image artifacts require expert interpretation of micrographs Samples may be sensitive to electron beam damage Sample may not be representative .Metrology Techniques .

it undergoes some changes in its amplitude and phase. . As the light shining on the sample passes through and bounces out. such as their refractive indices and thicknesses. These two parameters are analyzed to derive information about the layers.Spectroscopic Ellipsometry Ellipsometry is an optical technique used to analyze thin transparent layers.

thickness. roughness. optical constants Advantages Rapid Non-destructive Insensitive to light intensity fluctuations & losses Many in-line systems available Small spot size (25 μm) for features Disadvantages Requires transparent films Does not measure quantities directly Quantifiable only with standards Analysis can be difficult Difficult for thin conformal Si layer on rough relaxed SiGe Problems with fits when substrate stress is different from model stress Optical constants change as a function of strain.Metrology Techniques . .SE Capabilities Uses polarized light for stacked film optical thickness (refractive index) Elemental composition.

Rayleigh scattering . The energy of the re-emitted photon can be either higher or lower than the original depending on a chemical state of he molecule. gets absorbed exciting the molecule. The molecule then relaxes to one of the lower energy states by emitting another photon of energy different from the incident one. it can interact with it in many different ways. . Raman scattering .The photon strikes the molecule.Raman – Principles When a photon strikes a molecule. The two main ones are: 1.The photon bounces off of the molecule without any energy exchange 2.

4 μm) Not affected much by roughness Control of penetration depth (325nm <10 nm) Disadvantages No in-line monitoring tools available for patterned wafers Requires complex data interpretation Ge composition variation (out-diffusion) affects accuracy of derived strain value. . strain. Ge out-diffusion. nonuniformity Advantages Non-destructive. disorder.Metrology Techniques – UV Raman Capabilities Composition. crystallinity. strain/stress Phonon frequency shift in Si used to determine strain in Si channel Peak broadening related to defects: dislocations. no sample preparation Rapid (364 nm Ar-ion laser resonance Raman 10X faster than 325 nm He-Cd laser non-resonance Raman) Small spot size (0.

XRF Capabilities Multi-element composition Good precision Fluorescence intensity is proportional to atomic density Thickness measurements Advantages Spot size (40-50μm) ppm capability in a few cases.Metrology Techniques . more commonly.01% detection limits Simple spectra – No fitting or models required High Throughput (~10 sec per site) Whole wafer analysis Non-destructive Disadvantages Calibration standards required Some elements (e. 0. same peak) Diffraction background depends on substrate type . Ge) have low fluorescence yield (long acquisition times) Matrix effects (fluorescence absorption and enhancement) must be compensated Only elements beyond O detectable Interference (different element.g.

Metrology Techniques – High Resolution X-ray Diffraction Capabilities Strain/stress Film thickness Composition Advantages In-line monitoring tools available Non-destructive Rapid High-accuracy Disadvantages Strain measurement straight-forward only on bulk Si wafers Strain measurement on SOI wafers is time-consuming Requires triple-axis reciprocal space maps .

What Can Be Measured with X-rays? Thin Film Real Structure .

Analytical Tasks X-ray Reflectometry AC A BxC1-x AB Layer thickness Chemical Composition Roughness Lateral structure .

fluids Specular reflection of X-rays • film thickness of single. etc.1nm → 1000nm) • density profiles of near surface regions (~1%) • roughness of surfaces and interfaces (0.1nm → 5nm) Diffuse scattering of X-rays • roughness structure of surfaces and interfaces • morphology.and multilayer systems (0. correlation length.X-ray Reflectometry General Remarks Based on reflection of X-rays at interfaces – no crystal lattices needed Non-destructive method for the investigation of the near surface region of different sample systems • single crystalline. polycrystalline and amorphous samples • polymers. fractal parameters . organic samples (Langmuir Blodgett.).

a portion of X-rays is reflected. the penetration rises quickly with an angle. Below the critical angle. The measurements are done around a “critical angle” (an angle of total reflection). the X-rays don’t penetrate the sample surface. Above it. At every interface.XRR – X-ray Reflectometry thickness density Slope = roughness A technique which utilizes the effect of total external reflection of X-rays. Interference of these partially reflected X-ray beams creates a reflectometry pattern. .

5 μm) . 80μm x ~3mm Ge diffusion reduces density contrast Doesn’t work well with very rough interfaces There is an upper limit on thickness (<0. roughness. density. surface/interface roughness Most accurate in-line thin film metrology Advantages Can accurately determine thickness. crystalline.XRR – X-ray Reflectometry Capabilities Stacked film thickness. opaque) Complex multilayer structures can be measured Doesn’t require a prior knowledge of material composition Disadvantages Modeling can be difficult Fairly slow Spot size. density of layers Any type of material can be analyzed (amorphous.

XRR – X-ray Reflectometry Typical Experimental Setup .

Comparison of X-ray and Optical Analytical Techniques Thickness XRR is a direct method XRR is material independent Can resolve complex layer stacks Crystallinity XRD is the ideal technique to probe crystal structure Strain HRXRD can determine strain and concentration independently with precision <1% HRXRD analysis is simple and can be automated .

Semiconductor Industrial Applications Assunta Vigliante .

Bruker AXS D8 FABLINE with UMC300 STAGE .

single-crystal film structure • Thickness. thickness. density. grain size . amorphous.Industrial Applications Measurement Schemes High-Resolution X-ray Diffraction (HRXRD) • Single-crystal / epitaxial layer structure • Composition. relaxation X-ray Reflectivity (XRR) • Polycrystalline. surface / interface roughness Grazing Incidence Diffraction (GID) • Polycrystalline thin film • Crystallinity phase.

Please Tell Us… Use your mouse to answer the question on the right of your screen: What is your biggest challenge in analyzing semiconductor or thin film samples? Choose one: Integrating analysis instruments into my fabrication processes Determining the best measurement method for my application Being able to apply multiple analytical methods with one instrument Logistical and environmental constraints of placing an instrument in my facility And the results are… .

0 1.6 0.8 0.4 0.11 0.7 0.9 1.5 0. [au] 100 10 5 0.Limits of X-ray Reflectometry Thick Layers Example: SiO2 on Si 1e4 1014 nm SiO2:H Si 1000 Int.2 0.3 0.1 2θ [°] .

7 nm LaZrO Si (111) -2 -3 -4 -5 -6 -7 -8 2 4 6 2θ [°] 8 10 12 14 .Limits of X-ray Reflectometry Thin Layers Example: LaZrO on Si 1*10 1*10 1*10 Intensity [au] 1*10 1*10 1*10 1*10 1*10 1*10 0 -1 6.

0 1.5 3.5nm InP InP InGaAs InP InP 10 -8 0.0 o 2.0 Incidence angle [ ] .5nm 4.X-ray Reflectometry 0 Example of Sensitivity to Layer Thickness 10 10 10 -1 -2 10x 5x 50nm 5nm 4nm 4nm InP InP InGaAs InP InP Reflectivity 10 10 10 10 10 -3 -4 -5 -6 -7 10x 5x 50nm 5nm 3.5 2.0 0.5 1.

62 ± 0.55 16.93 0.00 ± 0.57 experimental simulation0.91 ± 0.47 1.04 Density (g cm-3) 2.Metal / Barrier Layers (Cu Process) 30 nm Cu/10 nm Ta/Si Material Thickness (nm) 2.05 --Roughness (nm) 0.23 ± 0.70 9.33 100 Cu2O 10-1 Cu Relative intensity 10-2 10-3 10-4 10-5 10-6 10-7 1 2 3 Ta Si 4 5 2θ (degrees) .35 ± 0.38 ± 1.20 ± 0.48 ± 0.14 ± 8.09 0.56 29.80 ± 0.55 2.

Titanium Silicon .3° Lin (Counts) 4000 3000 2000 1000 0 20 30 40 50 60 70 80 90 2-Theta .Start: 20.Osbornite.d x by Detected Phases: TiSi2.Ti5Si3 .Scale File: VLR40077-05.50 00-029-1362 (*) .000 ° Operations: Background 0.raw .raw .Type: 2Th alone .TiN .Start: 20.Titanium Silicon .000 ° Operations: Import File: VLR40077-05.05 6000 5000 Θ=0.75 % . syn .1.Type: 2Th alone .Y: 18.Silicide Layers TiSi / TiN / Si VLR40077.Y: 50.00 % .Y: 12.d 00-038-1420 (*) .alpha-TiSi2 .000. Ti5Si3. TiN .000 | Import 00-035-0785 (*) .

Pattern or Product Wafers .

Si structure pseudomorphic layer partially relaxed layer completely relaxed layer R=0 R=1 Δd d || R= Δa a rel Δd ≠0 d || || d L ≠ aS Δd Δa Δd = = d || d ⊥ a ⊥ || d L = d L = aL .Heterostructures Relaxation Degree R Example: Si1-xGex .

6 68.4 68.2 68.8 .4 Raw Curve 67.2 Sim Curve 67.Measurement Scheme (I) High-Resolution X-ray Diffractometry (HRXRD) Applicable semiconductor processes • SiGe and SiC epitaxial thin film • Strained Si film • SOI and sSOI Analysis parameters • Composition • Thickness • Relaxation 1*10 -4 1*10 0 1*10 -1 1*10 Intensity -2 1*10 -3 1*10 -5 67.4 69.2 69.8 68 68.8 2theta / omega (degree) 69 69.6 69.6 67.

Pattern Recognition Cognex Pattern Recognition Autofocus function 7 zoom factors Laser video system .

2 34.Start: 33.1 34.Step: 0.002 ° .Type: Rocking curve .0 34.3 34.Scale File: PatternedSiGe_VS0i1_HS0i2_SiGe004_06.9 34.6 33.5 34 Theta .7 33.8 33.Temp.600 ° .Time Started: 1074 s .2-Theta: 68.4 34.raw .1 s .Step time: 2.: 25 °C (Room) .SiGe on Si 2e4 1e4 1000 Log (Cps) 100 10 6 5 4 3 2 1 33.600 ° . Operations: Import .End: 34.

92 3.98 3.9994.038 deg) 1e4 1.99 3.99 3.raw .95 (0.97 3.03 4.96 3.94 (1.00 4.9457) 3.00 2.9975.92 3.01 4.96 3.98 l [001] 3.SiGe on SOI 4.915 h [110] 1 10 10 100 100 1000 Miscut=0.raw .9437) 3.97 l [001] 3.Start: -0 Counts [001] .93 (1.915 0 3.03 4.95 3.94 3.986 1. 3.File: m004 [001].9436) 3.File: m224+ [001]. 3.0018.0 h [110] 1 10 100 1000 1000 1e4 Cps [001] .00 3.Type: General Scan .02 4.99 2. 3.Type: General Scan .93 3.01 4. .02 4.9436) (-0. 3.Start: 1.

about 400 seconds per point .SOI 200μm collimeter.

DIFFRACplus LEPTOS 3 Automatic Fitting Extended Genetic Algorithm .

analytic profile fitting .simulation & fitting.D8 FABLINE Automated Operation and Analysis Measurement tasks automated using Visual Basic scripts Automatic alignment for reflectometry and Bragg reflections First task .LEPTOS • unified program for XRR &HRXRD • script automation .TOPAS BBQ • Choice of profile shape function: Pseudo-Voigt and Pearson VII • Crystallite size determination by Scherrer method Second task .

Texture Measurements on Cu Lines Beam spot 100μm Texture measurement can be done in 15 min (111) and (200) Cu reflections are collected simultaneously .

Stress Measurements on Cu Lines Beam spot 100 μm Stress measurement can be done in 2 hrs (331) and (420) Cu reflections are collected simultaneously .

Stress Measurements on Cu Lines .

Industrial Applications High-Resolution X-ray Diffraction (HRXRD) X-ray Reflectivity (XRR) Grazing Incidence Diffraction (GID) Grazing Incidence Small Angle Scattering (GI-SAXS) In-Plane Grazing Incidence Diffraction (IP-GID) Texture Stress All in one instrument! .

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2007 Salt Lake City.bruker-axs. UT .com See us at: International Conference on Crystal Growth (ICCG-15) August 12-17.www.

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