Crystal Growth and

Characterization
P. Shiny Christina
 Table of contents

1. Introduction
2. Methods for growing crystals
3. Characterization techniques
 INTRODUCTION
The definition of a crystal is an arrangement of molecules, usually a
solid, in which the atoms, ions, or molecules are regularly arranged in
three dimensions. A crystal usually has flat faces, sharp edges, and
specific symmetry patterns.
Crystal growth involves the controlled deposition of atoms/molecules
from liquid phase to a solid phase. It starts from the collection of atoms
to acquire a critical size called nuclei followed by the growth of nuclei to
a macroscopic crystal size.
 METHODS FOR GROWING CRYSTALS
Crystal growth

Solid growth Vapour growth Solution growth Melt growth

Gel growth Low temperature High temperature

Slow cooling Slow evaporation

 CHARACTERIZATION TECHNIQUES

Characterization involves evaluation of the chemical composition,

structure, optical, mechanical, electrical and thermal properties of the
grown crystals.
Different types of characterization techniques are available to study the
physical and chemical properties of the crystal.
 Single crystal XRD studies
● Single-crystal X-ray diffraction is most commonly used for precise
determination of a unit cell, including cell dimensions and positions
of atoms within the lattice. Bond-lengths and angles are directly
related to the atomic positions
● This technique is directly connected to a single-crystal refinement
module, where the data generated from the X-ray analysis is
interpreted and refined to obtain the crystal structure. This technique
is technically similar to the XRD
 Powder XRD studies
● X-ray powder diffraction (XRD) is a rapid analytical technique
primarily used for phase identification of a crystalline material and
can provide information on unit cell dimensions.
● The analyzed material is finely ground, homogenized, and average
bulk composition is determined.
 Microhardness studies
● Microhardness testing or microindentation hardness testing is often
applied to measure the hardness of a sample on a microscopic scale
● The estimation of mechanical strength of the grown crystal plays an
important role in device fabrication
● Microhardness Testing is a method used here to find out the
material’s hardness or it’s resistance to undergoing deformation
 FTIR analysis
● Fourier Transform Infrared Spectroscopy (FTIR) is a powerful tool
for identifying types of chemical bonds in a molecule by producing
an Infrared absorption spectrum
● This technique measures the absorption of various infrared light
wave lengths by the material of interest. These Infrared absorption
bands identify specific molecular component and structures.
 UV analysis
● UV-Vis Spectroscopy (or Spectrophotometry) is a quantitative
technique used to measure how much a chemical substance absorbs
light.
● This is done by measuring the intensity of light that passes through a
sample with respect to the intensity of light through a reference
sample or blank.
● UV-Spectroscopy is used to study the optical properties of materials
 SEM analysis
● The scanning electron microscope is a tool for the characterization
of nanostructures
● With nanoscale and even sub-nanoscale resolutions available, SEMs
can provide you with extensive information on a sample's
topography, morphology and chemical composition.
 TEM analysis
● Transmission electron microscopic techniques that use highly
energetic electrons to visualize the highly magnified image of a
sample at the atomic level. This technique is used for the
determination of the size, shape, structure, dispersion, uniformity of
material, and crystal phase.
● TEM has two advantages over scanning electron microscopy; it
can provide better spatial resolution and provide additional analytical
measurements
 TGA analysis
● Thermogravimetric analysis (TGA) is a powerful technique for the
measurement of thermal stability of materials
● A TGA device is a tool for diagnosing and analyzing processes
occurring in a material under different temperature conditions. The
thermal gravimetric analysis (TGA) technique determines the change
in the sample mass as a function of temperature or time under
different gas atmosphere conditions
 EDAX analysis
● Energy dispersive X-ray analysis (EDAX) is an analysis method that
can be coupled with several applications including SEM, TEM, and
STEM
● EDAX, when combined with electron microscopes, can
provide elemental analysis on areas as small as several nanometers