Characterization Methods and Systems

X-Ray Diffraction

4 Apr 2007

XRD char.ppt

Methods of Characterization
Characterization methods can be categorized into several general categories.
These include (but arent limited to):
1. Physical--determination of the structural, topographical, morphological state of
the sample. Includes SEM, TEM, AFM.
2. Chemical/compositional--characterization of the chemical elements or
compounds present in the sample, possibly including location on the
surface or with depth into the sample. Includes XRD, EDX, SIMS,
XRF, XPS.
3. Electrical--measurement of the resistivity/conductivity of a sample, carrier
concentration, mobility of charge carriers. Includes 4PP.
4. Optical--measurement of the optical properties or behavior of the sample.
Includes ellipsometry, interference spectroscopy, FTIR, PL.
5. Magnetic--measurement of the magnetic properties or behavior of the sample.
Includes VSM, Hall.
6. Mechanical--determination of the mechanical properties (strength, elastic
modulus, etc) of the sample.

Characterization Techniques

~0.350
keV

Surface morphology

Surface composition

Electron microprobe

EDX

x-ray

130 keV

Transmission electron
microscopy

TEM

50400 keV

Secondary ion mass

spectroscopy

SIMS

ion

ion

115 keV

X-ray diffraction

XRD

x-ray

x-ray

> 1 keV

Crystal structure,
composition

X-ray fluorescence

XRF

x-ray

x-ray

> 1 keV

Composition near
surface

X-ray photoelectron
spectroscopy

XPS

x-ray

> 1 keV

Surface composition

High-resolution
structure
Composition vs depth

X-ray Diffraction
X-ray diffraction can be used to characterize film structure (degree of crystallinity),
intermixing of multiple films, & epitaxial composition, among others.
X-rays are electromagnetic radiation with a very short wavelength.
They are produced when electrically charged particles of sufficient energy are
decelerated. In an X-ray tube, the high voltage maintained across the electrodes
draws electrons toward a metal target (the anode).
X-rays are produced at the point of impact, and radiate in all directions. Tubes with
copper targets, which produce their strongest characteristic radiation (K1) at a
wavelength of about 1.5. (0.15 nm).

X-ray Diffraction
If an incident X-ray beam encounters a crystal lattice, general scattering occurs.
Most scattering is destructively interfered and is lost (destructive interference).
Diffraction occurs when scattering in a certain direction from one atomic plane is in
phase with scattered rays from other atomic planes. Under this condition the
reflections combine to form enhanced wave fronts that mutually reinforce each other
(constructive interference). The relation by which diffraction occurs is known as the
Bragg law. Each crystalline material has a characteristic atomic structure and it will
diffract X-rays in a unique characteristic pattern.

Braggs Law:
2dsin = n
= X-ray wavelength
= X-ray incident angle
d = lattice spacing of atomic
planes (assuming a crystal)

X-ray Diffraction
The basic geometry of an X-ray diffractometer includes
a. a source of monochromatic radiation
and
b. an X-ray detector situated on the
circumference of a graduated circle
centered on the powder specimen.
c. divergent slits, located between the Xray source and the specimen, and
divergent slits, located between the
specimen and the detector, limit
scattered (non-diffracted) radiation,
reduce background noise, and
collimate the radiation.
d. the detector and specimen holder are
mechanically coupled with a
goniometer giving a detector rotation of
2 for a specimen rotation of .

X-ray Diffraction
A curved-crystal monochromator containing a graphite crystal is used to ensure that
the detected radiation is monochromatic.
When positioned properly just in front of the detector, only K radiation is directed
into the detector, and the K radiation is directed away.
The signals from the detector are filtered by pulse-height analysis, scaled to
measurable proportions, and sent to a linear ratemeter for conversion into a
continuous current.

X-ray Diffraction
For crystalline specimens, XRD can determine the lattice spacing d. A crystalline
specimen will produce a characteristic diffraction pattern of spots. This diffraction
pattern can be analyzed to give the crystal structure.

Since the method can determine the lattice parameter d, it can also be used in
mechanical characterization such as to characterize strain, d/d0, inside an
epitaxial sample.

X-ray Diffraction
XRD can be used to identify crystal structures. Individual atomic planes (families)
can be identified.

X-ray diffraction patterns of (a) BaLa2ZnO5 and (b) BaNd2ZnO5.

These patterns can be used for compositional analysis in an unknown sample.

XRD can be used to investigate the crystal environment of particular atoms.

Ta displaying cubic symmetry in the

mineral microlite.

Ta showing hexagonal symmetry in the

mineral calciotantite.

Can use XRD to generate a time series to follow changes in a sample under
experimentation.

This sample undergoes

a phase transition as a
function of T between
150C and 170C.
high T phase
low T phase

X-ray Diffraction
For polycrystalline or noncrystalline materials, X-rays may be diffracted into a
number of different directions.