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X-ray Diffraction (XRD)

X-ray diffraction (XRD) is the most extensive tool to analyze crystalline materials or sample composition. This versatile analytical non-destructive technique allows the calculation of the structure of atoms, phases, and preferred crystal alignments (texture).
chemical analysis lab
The phenomenon in which light slightly bends as it passes around the obstacle or corner of an object is called Diffraction. For diffraction that has to occur it depends upon the wavelength used by the light compared to the size of the obstacle for which it has to be passed or object encountered and it should be a few angstroms (approx. 1 Å). The best possible way to study X-Ray diffraction patterns is through Crystal and its atomic spacing is approximately a few Å.

Principle:

X-rays are electromagnetic radiations in nature. Monochromatic X-rays pass through a crystalline sample. Crystal is an ordered array of atoms. The elastic Scattering phenomenon occurs when X-rays are scattered by the interaction of the crystal atom’s electrons. In different directions, these scatters produce spherical waves. In the majority of directions, these spherical waves map out each other through destructive interference. Constructive interference is produced when incident X-rays interact with the sample and these conditions satisfy Braggs law
2dsinθ = nλ
Where d is the intervals between diffracting planes that cause diffraction peaks θ is the angle between the incident ray and scatter plane called as incident angle, λ specifies the wavelength of the incident X-Ray beam, and n is an integer referred to as an order of diffraction. In specific directions, spots appear on diffraction called Reflections. Electromagnetic waves exert influence on a regular array of scatters therefore they result in the X-Ray diffraction pattern. You can analyze the sample structure by collecting Diffracted X Rays showing that each mineral has a unique set of d-spacings. And Sample Structure is identified by comparing standard reference patterns of d-spacings. X-Ray tube generates X-Rays and all diffraction methods are based on it. Single Crystal and Powder diffraction varies in instrumentation.
The phenomenon in which light slightly bends as it passes around the obstacle or corner of an object is called Diffraction. For diffraction that has to occur it depends upon the wavelength used by the light compared to the size of the obstacle for which it has to be passed or object encountered and it should be a few angstroms (approx. 1 Å). The best possible way to study X-Ray diffraction patterns is through Crystal and its atomic spacing is approximately a few Å.

Data Analysis:

Many rare isotopes, such as Be-10, C-14, Al-26, Cl-36, Ca-41, I-129 and several isotopes of Uranium and Plutonium can be analysed with AMS. One of the most common applications of the method is radiocarbon dating. The technique is widely used for determining the age of carbon-containing samples by measuring the amount of radioactive C-14 isotope in them. In addition to archaeology and historical research, AMS is also commonly used for determining the bioportion (the proportion of biobased content in a sample) of different kinds of fuels.

The isotopes analysed with AMS have a wide range of dating applications and they are used in a variation of chronometers and tracers. Therefore, AMS is utilized in many disciplines, such as geological and planetary sciences, geomorphology, quaternary science, environmental and atmospheric research, archaeology, historical research, global climate change control, nuclear safeguards and biomedicine.

Sample requirements and preparation

XRD is a non-destructive analytical technique. The outcome of XRD measurement is a Diffractogram showing:

The Structural properties:

▪️ Strain

▪️ Stress in the sample

▪️ Grain size of the sample

▪️ Identifies the orientation of a single crystal or grain

1.      As  Crystal lattice  has a three-dimensional diffraction pattern of atoms  Defects have a dominating influence on crystalline solid properties so the XRD technique is used to provide information about those defects.

2.      XRD identifies phase quantification, preferred orientation, Peak positions, peak heights, and % Crystallinity. Sharp peaks are the reason for large crystallites and as crystallite size reduces peak width increases.

3.      It examines a diverse range of materials from solid objects and powders and thin films to nanomaterials.

4.      It measures the interplanar spacings

5.      Unit cell dimensions are also identified

6.      The latest Technology gets an upper hand in the technique where diffractometer systems are programmed to measure record and interpret every particular diffractogram even of highly complex mixtures.

7.      Chemical phases are determined qualitatively and quantitively in Powders.

8.      Layer parameters such as width, density, and roughness are discovered through High-Resolution X-Ray Diffraction.

9.      Micro X-ray diffraction is used for very small sample analysis containing less than 1mm crystal constituents (µ-XRD).

Applications:

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