X-ray diffraction techniques for thin films

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1 X-ray diffraction techniques for thin films Rigaku Corporation Application Laboratory Takayuki Konya 1 Today s contents (PM) Introduction X-ray diffraction method Out-of-Plane In-Plane Pole figure Reciprocal space mapping High resolution rocking curve X-ray reflectivity 2 1

2 Advantage of X-ray diffraction (XRD) method Probed depth control by incidence angle Nondestructive Measurement under atmosphere pressure 3 What can we see? a,b,c Thickness, Density, Roughness Phase Identification Interface, transition layer, etc Crystal structure Crystal quality, lattice parameter, etc Crystal orientation Single: orientation relation of substrate & film Poly: preferred orientation? (hkl) ρ, σ d 4 2

3 What XRD reveals Position and coordinate of reciprocal lattice points lattice constant crystal orientation lattice distortion K spread of reciprocal lattice points degree of preferred orientation Shape of a reciprocal lattice distribution crystal perfection defects mosaicity 5 Structure parameters Structure Parameter Order Analysis Method Thickness 1~10 3 nm Precision :~several % Xray Reflectivity Density H 2 O~Heavy Metals Xray Reflectivity Roughness 0.2~several nm Xray Reflectivity Phase ID - In-Plane XRD Out-of-Plane XRD etc Crystal System - In-Plane XRD Out-of-Plane XRD etc Lattice Constant ~several nm Precision : 0.05~ nm In-Plane XRD Out-of-Plane XRD etc Crystal quality Poly~Single, Perfect In-Plane XRD Crystals Out-of-Plane XRD etc Preferred Random~Preferred Orientation Orientation ~Single Crystal Pole Figure ect Orientation Relation Relation between Film & Substrate Rocking Curve Reciprocal Space Map etc Layer Structure Crystal Structure 6 3

4 Today s contents (PM) Introduction X-ray diffraction method Out-of-Plane In-Plane Pole figure Reciprocal space mapping High resolution rocking curve X-ray reflectivity 7 Today s contents (PM) Introduction X-ray diffraction method Out-of-Plane In-Plane Pole figure Reciprocal space mapping High resolution rocking curve X-ray reflectivity 8 4

5 Difference between Scan Modes The orientation of observed crystal plane depends on scanning mode. Out-of-Plane scan Film scan In-Plane scan Observed plane is.. Observed plane is.. parallel to the surface tilting (changing during a scan) perpendicular to the surface 9 What is In-Plane XRD? The detector moves parallel to the surface. Incident x-ray Diffracted x-ray α Diffraction angle 2θ B Reflected x-ray Grazing incidence (fixed angle) Observing planes are perpendicular to the surface. 10 5

6 Outward of In-Plane Attachment Scanning motion is completely perpendicular to θ/2θ scan. θ/2θ scan In-Plane measurement (2θχ/φ scan) 11 In-plane effect Intensity (cps) In Plane θχ/φ (degree) In-Plane 220 Intensity (cps) Out of Plane θ/ω (degree) Out-of-plane poly-si Glass 12 6

7 Probed depth control? 1 extinction distance (nm) incident angle (degree) Sample:Al Wavelength: Å(CuKα1) 13 Surface & Interface Structure 250 In-Plane XRD Intensity (cps) Al(111) 40 Al+Cu Al+Cu Cu(111) Cu(200) θχ/φ(degree) Incident angle 0.2 deg. 0.5 deg. Al(220) Al(311) Cu(220) Al(222) ~300nm Transition layer Al Al+Cu SiO 2 Si (substrate) Cu Ta 14 7

8 Today s contents (PM) Introduction Advantage of reciprocal lattice vector X-ray diffraction method Out-of-Plane In-Plane Pole figure Reciprocal space mapping High resolution rocking curve X-ray reflectivity 15 Single crystal and random orientation Single crystal Fiber orientation Random orientation 16 8

9 Orientation conditions and pole figure (111) pole figure (220) pole figure α=90 β=0 α=90 β=0 Random orientation β=90 β=270 β=90 β=270 β=180 β=180 {111} fiber orientation α=90 β=0 β=90 β=270 β=180 α=90 β=0 α=70.5 α=90 β=0 β=90 β=270 β=180 α=90 β=0 α=35.3 (111) single crystal β=90 β=270 β=90 β=270 β=180 β= Today s contents (PM) Introduction Advantage of reciprocal lattice vector X-ray diffraction method Out-of-Plane In-Plane Pole figure Reciprocal space mapping High resolution rocking curve X-ray reflectivity 18 9

10 Reciprocal space mapping Diffraction intensity distribution is plotted on reciprocal space. 2θ/ω g hkl Δω k g 2θ/ω k o ω 19 Epitaxial layer structures Relaxation Strain Misorientation 00l cubic[112] 00l substrate[001] cubic[112] 00l film[001] tetragonal[112] hh0 hh0 hh

11 Reciprocal space mapping Mosaic spread GaAs115 q y / -1 AlGaAs115 Broadening in direction of sample rotation Mismatch (strained) q x / -1 Broadening in direction of radial scan 21 Today s contents (PM) Introduction Advantage of reciprocal lattice vector X-ray diffraction method Out-of-Plane In-Plane Pole figure Reciprocal space mapping High resolution rocking curve X-ray reflectivity 22 11

12 High- resolution rocking curve The differences of lattice spacing between the substrate and epitaxial films are observed. Thickness and composition ratio of epitaxial films (when the degree of relaxation is known. ) 2θ/ω K ghkl k g log(i ) k o Δ2θ/ω 23 When the sample has multilayer structure Complicated oscillation composed of oscillation from each layer is observed. Reflectivity GeSi GeSi Si (004) Ge x Si (1-x) 50nm Ge x Si (1-x) 300nm x=0.015 Si substrate Deviation Angle (arcseconds) x=0.050 x=

13 When the sample has superlattice structure Satellite peaks are observed GaAs (004) Reflectivity GaAs 5nm In x Ga (1-x) As 5nm GaAs substrate 10L Deviation Angle (arcseconds) x= How to interpret the profile Si substrate (004) SiGe mismatch Reflectivity Intensity SiGe mismatch 10-3 Oscillation period SiGe thickness 10-5 Ge x Si (1-x) 50nm x=0.050 Ge x Si (1-x) 300nm x=0.015 Si substrate Oscillation period 2SiGe thickness diffraction Deviation Angle angle (arcseconds) (Δarcsec.) 26 13

14 Today s contents (PM) Introduction X-ray diffraction method Out-of-Plane In-Plane Pole figure Reciprocal space mapping High resolution rocking curve X-ray reflectivity 27 What reflectivity reveals X-ray reflectivity nondestructively reveals - layer structure of multi layers - thickness (1 to 1000nm) - density as an absolute value - surface and interface roughness Interface roughness thickness layer 1 thickness layer 2 density substrate 28 14

15 How to interpret the profile Critical angle c Density Reflectivity Amplitude of 10-4 oscillation Contrast 10-5 of density 0 2 Period of oscillation Thickness 4 2θ/θ (degree) roughness 1 roughness 2 roughness 3 Decay of amplitude Interface roughness 6 8 density 1 density 2 density 3 layer 1 layer 2 substrate Decay of reflectivity Surface roughness thickness 1 thickness 2 29 X-ray reflectivity measurement of TiN film 10 0 TiN SiO 2 Si Reflectivity Simulation Experimental Layer density (g/cm 3 ) Thickness (nm) Roughness (nm) TiN TiN SiO Si substrate Grancing angle α (degree) 1.5 Coating layer

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