Presentation on XRD

Presented By
Md. Alamin Haque
Sales & Service Engineer
Bsc. in Electrical & Electronics Engineer (AIUB)
 What is XRD?

X-ray diffractography (XRD) is the experimental science determining the atomic and molecular structure of
a crystal, in which the crystalline structure causes a beam of incident X-rays to diffract into many specific
directions. By measuring the angles and intensities of these diffracted beams, a diffractographer can
produce a three-dimensional picture of the density of electrons within the crystal. From this electron
density, the mean positions of the atoms in the crystal can be determined, as well as their chemical bonds,
their crystallographic disorder, and various other information.
 Principle

Olympus XRD Technology

1.Microfocus X-Ray Tube
2.X-Ray Beam
3.Collimator
4.Sample
5.CCD Detector
 Olympus XRD

Portable TERRA™ II Benchtop BTX III

Features

1. Faster analysis times.

2. Easy sample preparation.
3. faster and offers more intensity, leading to lower LODs.
4. SwiftMin automated phase ID and quantitative software provides real-time data
directly on the XRD analyzer.
5. Quick decisions with confidence.
6. One dashboard for data.
7. Preset calibrations with privacy.
8. Easy data export.
9.Smart Sense XRD detector
Ease of Use

1. Easy sample preparation.

2. Fully compacted so no connections to be made separately.
3. Need two days training to operate.
4. No need expert to operate it. Less experts can operate it smoothly.
Applications

1. Identification of unknown crystalline materials (e.g. minerals, inorganic compounds).

2. Determination of unknown solids is critical to studies in geology, environmental science, material science,
engineering and biology.
3. Characterization of crystalline materials
4. Identification of fine-grained minerals such as clays and mixed layer clays that are difficult to determine optically
5. Determination of unit cell dimensions
6. Measurement of sample purity
7. Qualitative & Quantitative analysis.
8. Phase and crystalline analysis.
Advantages

1. Easy sample preparation. Need only 15mg of sample powder.

2. The process is so easy that even non-lab personnel can quickly acquire important data.
3. Onsite analysis.
4. Qualitative & Quantitative results.
5. Cost-effective with a low cost of ownership.
Limitations

1. Homogeneous and single phase material is best for identification of an unknown

2. Must have access to a standard reference file of inorganic compounds
3. The sample must be ground into a powder
4. For mixed materials, detection limit is ~ 2% of sample
5. For unit cell determinations, indexing of patterns for non-isometric crystal systems is
complicated
6. Peak overlay may occur and worsens for high angle 'reflections'
X-ray Source: Cobalt Vs. Copper
A high peak-to-noise ratio enables accurate identification of the XRD pattern. Two of the phenomena
that can affect this ratio are secondary fluorescence and absorption, which occur as a function of the
energy of the X-rays and of the major elements composition of the sample. The choice of tube will
influence both absorption and secondary fluorescence so it is important to consider these two effects
when choosing your tube. For instance, high Fe/Co containing samples will strongly absorb and
fluoresce under Cu radiation, while high Mn/Ti/Ca-containing samples will strongly absorb and
fluoresce under Co radiation.

Cobalt and Copper Tube Options: Olympus XRD analyzers come standard with a rugged cobalt (Co)
target X‐ray tube. This anode is the preferred choice of geologists and mineralogists, as it is excellent
at analyzing samples with high iron (Fe) content. However, some applications (i.e. high manganese
content), require a copper (Cu) target X‐ray tube. Olympus supplies either X-ray tube anode,
depending on application needs.
Co vs Cu
Why 2θ ?
Detector
The Olympus TERRA® and BTX II™ XRD analyzers utilize a specially designed charge coupled device
(CCD) detector to provide results. The analyzer derives quantitative mineralogy by sending X-rays into
a crystalline sample. Each crystal has a unique shape and diffracts the energy as light in a specific
pattern. The CCD captures a portion of the Debye-Scherrer cone (a way of locating the position of the
light) and converts this image into a classical two-theta diffraction pattern. The detector is both
position sensitive and energy sensitive, enabling both accurate phase identification as well as energy
discrimination. The detector has no moving parts, so it works well both in the lab and in the field.

Advantages of a CCD detector for XRD The benefits of the Smart Sense CCD detector include:
• Reduced background noise from fluorescence • Particle statistics
• Higher peak to background noise • Reliable (no moving parts)
• Higher sensitivity
• Ability to quickly determine sample effects
• Preferred orientation
Results
Customers…

Steel Companies
Purpose of Use XRD in steel Industries

The quality of iron ore is defined by the total iron content and also by the quantitative content of iron-
containing phases such as-

1. Hematite (Fe2O3), magnetite (Fe3O4), or goethite (FeOOH) and gangue minerals like quartz (SiO2),
kaolinite (Al2Si2O5(OH)4), gibbsite (Al(OH)3), or calcite (CaCO3). Quantification of these minerals
gives important information for the manufacturing process.
2. Especially, the analysis of hematite and magnetite, and subsequently, the Fe2+/Fe3+ ratio, affects
the control of the energy consumption and thereby the CO2 emissions. Magnetite is oxidized to
hematite in an exothermic chemical reaction which produces heat and reduces the energy needed.
Customers…

Ceramics Companies
Purpose of Use XRD in ceramics Industries
Customers..

Oil & Gas

Purpose of Use XRD in Oil & Gas Industries
Customers…

Aluminum Companies
Purpose of Use XRD in Aluminum Industries
Customers…

Cement Companies
Purpose of Use XRD in Cement Industries
Customers…

Fertilizer Companies
Purpose of Use XRD in Fertilizer Industries
Customers…

Universities
 Customers...

Ministry Of Defence

.
Customers…

Mining
Purpose of Use XRD in Mining Industries
Contd..
Customers…

Other Industrial Companies

 . Thank You…