G.

PULLA REDDY DENTAL COLLEGE AND HOSPITAL,

KURNOOL
DEPARTMENT OF ORTHODONTICS AND DENTOFACIAL
ORTHOPEDICS

SEMINAR
ON
INSTRUMENTAL TECHNIQUES FOR
STUDY OF ORTHODONTIC MATERIALS

PRESENTED BY : GUIDED BY:

B.Sailusha Dr. Y. Muralidhar Reddy.

CONTENTS:
1) INTRODUCTION

2)X-RAY FLUORESCENCE SPECTROMETRY (XRF)

3)X-RAY DIFFRACTION(XRD)

4) RAMAN MICRO SPECTROSCOPY

5)AUGER ELECTRON SPECTROSCOPY(AES)

6)X-RAY PHOTO ELECTRON SPECTROSCOPY

7)SECONDARY ION MASS SPECTROMETRY

8)DIFFERENTIAL SCANNING CALORIMETRY(DSC)

9)AIR FORCE MICROSCOPY

REFERENCES
  INTRODUCTION:
Analytical instrumentation offer powerful tools for the study of
orthodontic biomaterials and for the characterization of tissue-
material interactions.
 Computer-controlled systems has greatly expanded the use of
various spectroscopic methods in the field, providing important
in- formation for the elemental, molecular, and structural
characteristics of biomaterials.

SPECTROSCOPY:
 It is the study of interaction between the matter and electromagnetic
radiation
 Historically spectroscopy originated through the study of visible light
dispersed according to its wavelength by a prism.
SPECTROMETER:

 It is a device for measuring wavelengths of light over a wide range of the

electromagnetic spectrum is called spectrometer and the process is called
spectrometry.
 It is widely used spectroscopic analysis of sample materials.

X-RAY FLOURESCENCE SPECTROMETRY(XRF):

 Photoelectric effect
 Charecteristic X- Rays
 Energy source of XRF X-Ray Tube.

X-RAY TUBE

Charecteristics of X-Ray Tube:

 Tubes do not require high vacuum or con ductive samples as do

electron beams
  Does not require accelerators as does particle-induced X-ray
emission.
 X ray tube with a single source many elements can be excited
efficiently.
 X Ray tube anode:
Charecteristic lines emitted by the anode should always have
higher energy than the absorption energy of elements of
interest,without creating spectral interfereneces.

Elemental identificattiion in XRF spectrometry:

 It is accomplished by spectrometers that resolve the spectral lines emitted

into separate components.
 XRF spectrometer operates with sample chamber kept at atmospheric
condition with vaccum (or)under helium.
SPECTROMETERS

Wide Dispersive Spectrometry Energy dispersive spectrometry

 X-Rays emitted are dispersed  Semiconductors used to create

into specific wavelengths by the
mechanical movement of
analyzing crystals attached to a
goniometer and detected by
scintillation counters.
 Demonstrate high resolution
 Higher sensitive detection
 Higher counting rates
 Single channel detection
 Slow because of goniometer
arrangement
Range of acceleration voltage:
0-100keV
signals proportional to X-ray
energy
 Lower resolution
 Lower sensitive detection
 Lower counting rates
 Multi channel detection
 High speed provides
simultaneous multielement
analysis capable.
0-40KeV
X-Ray spectrometry can be applied to analyse

a)solid samples like bulk ,powder,briquette.

b)liquids

c)thin films and

d)filtered aerosol sample.

This technique will detect the elements with atomic number Z>11

Oxygen and fluorine can be measured by the detectors.

X-RAY FLOURESCENCE SPECTROMETRY OF NiTi :

X-RAY FLOURESCENCE SPECTROMETRY OF TYPE 304 STAINLESS
STEEL:

Detection limits:

Bulk:From afew ppm to few tens of ppm

Thin films:100 ng /cm2

Bulk materials can be analysed by placing in a special cups or holders.

Smaller samples-beam collimators are required

 Sample should have a surface roughness less than 100 micrometers

 POLISHING has to be done carefully on sample in order to prevent
interactions with x rays emitted.
 Powder particle size should be <100µm.
 XRF spectrometry can be applied for measuring film thickness and
composition of coatings .
X-RAY DIFFRACTION:

 X-ray diffraction (XRD), which is used to study the crystal

structures of materials and related matters, is one of the major
traditional la boratory tools employed in materials science.
 A beam of parallel X-rays that are incident upon atomic
planes at the surface of a crystalline material.
 If the difference in path length for X-rays reflected from
adjacent planes is an integral number of wavelengths, these
reflected X-rays will be in phase and produce a strong signal at
some detector.

 The diffraction angle (2θ) is the angle between the incident

and transmitted X-ray beams.
 The number of wavelengths in the path length dif- ference is
designated by n, which is termed the order of diffraction.

 In XRD studies of arch wires, a series of parallel wire

segments may be placed in contact to obtain an
acceptable specimen for the diffractometer.

 shows that the diffracted X-rays from an atomic plane in a

 polycrystalline powder specimen form a cone when the
powder contains a very large number of randomly oriented
crystals.
 The diffracted X-rays from a powder specimen may be
detected with a Debye-Scherrer camera that contains film or
with a diffractometer.
 For some materials the surface atomic planes giving rise to the
XRD peaks can be under a state of uniform residual elastic
strain.
 For uniform tensile strain, the interplanar spacing (d) will be
increased, and consideration of Bragg's law shows that the
diffraction angle (2e) for the reflection from these planes is
decreased;
 the diffraction angles are increased if the surface planes are
under uniform compressive strain.
 Substantial peak broadening is often observed in XRD
patterns from archwires owing to residual plastic
deformation arising from the wire processing sequence.
 When two materials, such as iron and nickel, have the
same crystal structure then the pattern of the XRD peaks
is the same, although the peak positions (2e values) differ
because of the different lattice parameters
 X-ray diffraction is inherently a near-surface
analytical technique, since the depth of penetration
of the X-ray beam is typically no greater than 50 µm and
frequently much less for the metals of usual interest.

XRD can be applicable to identification of phases in zirconia

ceramic brackets.
X RAY DIFFRACTION PATTERN OF NiTi alloy:
RAMAN MICROSPECTROSCOPY:

 In this method,radiation from the monochromatic source,such as a

laser is focused on a sample microregion.
 RAYLEIGH LINE:
 The fraction of radiation scattered by the sample consists of a
component of the exciting ion.
 RAMAN LINES:
Other weak lines are called Raman lines.
 The frequency of shifts of raman lines from Rayleigh
linecorresponds to molecular vibration frequencies within sample
molecules.
 Sample is viewed through a optical microscope under bright field
(or)dark –field illumination.
 Analysis can be in a spot mode with high spatial resolution/in
molecular imaging mode.
 The entire vibrational spectrum is probed with one instrument at
increased sensitivity and at high spatial resolution especially for
metal oxide systems.
 Water demonstrates weak raman scattering and thus it is ideal
solvent,
 Solids and crystals contain contributions from lattice vibrations at
low frequencies that provide important information on crystal
structure.
X-RAY PHOTOELECTRON SPECTROSCOPY(XPS):

 In X-ray photoelectron spectroscopy (XPS) a core electron is

ejected from a sample upon irradiation with X-rays of known
energy.
 Usually Mg, Al or combined Mg/Al sources are used to produce
photoelectrons having energies of 5 - 15 keV. Dual anodes are
very useful for the analysis of samples emitting photoelectrons
and Auger electrons of the same energy.
 XPS detects all elements except helium
 The photoemitted electrons are characterized by a binding energy,
the difference between the total energies of the initial and final
states, which is energy-resolved under UHV.

 Upon relaxation of the atom, characteristic X-rays or Auger

electrons are produced.
 XPS is essentially a surface analysis technique with a depth of
analysis ranging from 2 to 10nm for photoelectrons with binding
energies of 0- 1100KeV and, as with other surface- specific
techniques, requires UHV.
 XPS detects all elements except helium and can be applied for
organic materials.
 XPS provides information about bonding state, oxidation state,
change in crystal structure and formation of new compounds.
 XPS is used extensively ins study of biomaterial surfaces-impant,
amalgams, prosthodonticalloys, polymers and adhesives.

DIFFERENTIAL SCANNING CALORIMETRY:

 DSC is extensively used characteristic industrial polymer mainly in

orthodontics for NiTi arch wire alloys and polyurethane elastomer.
 In conventional DSC two small pans, one containing the material to be
analysed and the other for I inert material such as indium are heated at same
 rate 5° upto 10°per minute.

 Thermal energy supplied to each pan to maintain equal heating rate is plotted
as a function of temperature over the scanning range to yield the DSC
CURVE.
  A schematic DSC plot for a polymeric material undergoing typical structural
transformation is shown in the diagram.
Glass transition temperature(Tg):
 Point deflection where the sense of curvature changes on the sigmoid.
 EXOTHERMIC PEAK
 ENDOTHERMIC PEAK
 Temperature Modulated Differential Scanning Clorimetry has provided new
insight into polymeric phase
transformations in elastomeric maxillofacial and impression materials.
Whether they are reversible or irreversible character.

AUGER ELECTRON SPECTROSCOPY:

 Is a highly sensitive surface nalytical technique that utilizes a high energy
electron beam as an excitation soure.
 Electron beam ATOM relax emission of auger
electrons.
 The kinetic energy of characteristic auger electrons depends on the chemical
state of surface atoms participating in ionic bonding and oxidation.
 Excellent tool for study of surface contamination of biomaterials, with
additional applications for corrosion, wear and tribology by comparision
with subsurface spectra obtained from depth profiling AES.

SECONDARY ION MASS SPECTROMETRY:

 It is a technique used to analyse composition of solid surfaces and thin films
by sputtering the specimens with a foused primary ion beam.
 Collecting and analyzing ejected secondary ions
DIRECT IMAGING

Ion microprobes Ion microscopes

USES:
 Study of biomineralisation in bone and teeth using concentration
profile analysis and molecular and ionic imaging.
 To dectect trace elements are very high sensitivity (ppm-ppb) and
high spatial resolution(µm-nm)
  Implant-tissue interactions, remineralisation potential of fluoride-
containing solutions.

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Bradley TG, Brantley WA, Culbertson BM. Differential scanning calorimetry

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Quantitative analysis of the dentin ad- hesive interface by Auger
spectroscopy. J Dent Res
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Hanawa T, Takahashi H, Ota M, Pinizzotto R, Ferracane JL, Okabe T.
Surface characterization of amalgams using
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Suzuki M, Koto H, Wakumoto S. Vibrational analysis by Ra- man

spectroscopy of the interface between dental ad- hesive resin and dentin.
J Dent Res 1992; 70: 1092 - 7.
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mineralized tissues. Scanning Electron Micro-
scopy 1983; 83: 1229 – 42