X-Ray Diffraction Analysis

Rigaku X-Ray Diffraction System at AME laboratories.
Rigaku MiniFlex 6G XRD System at AME laboratories

X-ray Diffraction Analysis

X-ray diffraction (XRD) analysis is used to identify crystalline materials based on the x-ray diffraction pattern they produce. When multiple crystalline phases are present, the percentage of each can be determined by x-ray diffraction. The percent of crystalline materials versus the percent of amorphous material can also be measured by XRD. Our XRD system works with both powder and solid materials.


Rigaku XRD System Features

  • 600W Copper X-ray (8.041 KeV) Source, Normal Focus
  • 8-Position Sample Changer with Sample Spinner
  • Diffracted Beam Monochromator
  • D/teX Ultra 0D/1D High Speed Detector
  • Variable Knife Edge for low-angle optimization without blind spot at high-angle
  • Continuously Variable, Theta-Compensating Divergence Slit
  • Scattering Slit, 8 mm
  • Soller Slits, 5-Degrees Incident and Receiving
  • Receiving Slit, 0.3 mm
  • X-ray Tube Take-Off Angle 6 Degrees
  • Goniometer Range -3 to 145 Degrees 2-Theta

Applications of XRD Analysis

  • Identification of the chemical phase of a powder sample
  • Determining the percentage of each of several chemical phases in a powder sample
  • Determining the chemical phase identity of an inorganic fill particulate added to a polymer
  • Determining the chemical phases in a metal alloy
  • Determining the degree of crystallinity of a polymer
  • Determining the chemical phases in a metal oxide or other surface layer
  • Determining the chemical phase composition of a thin or thick film

Comparison to Other Analyses

Because of its 8.041 KeV x-ray, our XRD probes a more standard distance into a material than does our XRF. The XRF has a more energetic excitation source (Rh K-alpha at 20.167 eV), making it possible to detect heavy elements from deeper into a sample. However, in XRF, the signal depth is largely determined by the characteristic x-ray emission of a given element. Consequently, carbon and nitrogen with their very low x-ray energies are only detected when within about 20 micrometers of a surface, while tin or similarly heavy elements may be detected from more than 1 mm deep into a sample. The EDS analysis method has a detection depth which is mostly determined by the excitation electron beam of the SEM. This is commonly 15 to 25 KeV. Its sampling depth is about 1 to 2 micrometers. The XPS surface analysis technique uses a low excitation x-ray energy of 1487 eV, but even though this is low, the detection depth is determined by the photoelectron energy of the element in question. XPS gets nearly all of its signal from the outer 20 nm of a surface.

Case History Examples

Mineral Composition Analysis by XRF and XRD