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Chapter 5 – Materials Characterization – IR Spectroscopy

Infrared Spectroscopy

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Chapter 5 – Materials Characterization – IR Spectroscopy

Infrared Spectroscopy

• Energy absorption by molecule in infrared region


• Transition between two vibrational levels
• Extract molecular structural information by measuring molecular
vibrations spectra
• Molecular fingerprints, characterize and identify the molecule
• Used in conjunction with Raman Spectroscopy
Chapter 5 – Materials Characterization - IR Spectroscopy

Infrared Spectroscopy Instrumentation

• Dispersive – prism or grating


• Non-dispersive – interference filters, tunable lasers sources, an
interferometer (Fourier Transform Infrared Spectrometer
• For IR region, front faced mirrors
• Glass and quartz absorb opaque to IR
Chapter 5 – Materials Characterization - IR Spectroscopy

Infrared Spectroscopy Instrumentation


1. Source of Infrared radiation
• IR, heat radiation
• Heat transfer direct, do not require a direct physical medium
• Converted to heat, only on absorption by object
• Source, an incandescent solid material which has a radiant energy
distribution
• Similar to theoretical black body
• Tungsten filament lamp, Glober, Nernst Glower, Nichrome heater
Chapter 5 – Materials Characterization - IR Spectroscopy

Infrared Spectroscopy Instrumentation


2. Infrared monochromator
• Means of separating source radiation wavelengths
• Prisms and gratings
• Prisms of alkali halides
• Large crystals, Prisms, windows and cells are cut from them
• NaCl 4000-650 cm-1
• Potassium bromide 1000-400 cm-1
• Cesium iodide 1000-260 cm-1
• Below 250 cm-1, gratings are used, disperse the energy
Chapter 5 – Materials Characterization - IR Spectroscopy

Infrared Spectroscopy Instrumentation


3. Infrared Detector
• Thermal radiant energy into electrical energy
• Selective – response dependent on wavelength incident radiation
• Photographic plates, photocells, photoconductive cells, infrared
phosphors
• Photoconductive important, rapid response and high sensitivity
• PbS, PbSe, Lead telluride, selenium
• Increase in conductivity, with increase in IR illumination
• 0.5 – 3.5 microns
Chapter 5 – Materials Characterization - IR Spectroscopy

Infrared Spectroscopy Instrumentation


3. Infrared Detector
• Non-selective – response independent of wavelength of incident
radiation
• Directly proportional to incident energy
• Thermocouples, bolometers, pneumatic cell
• Thermocouples: evaporating bismuth antimony, semiconductor
alloys, on thin film cellulose nitrate, in evacuated chamber with KBr
window
Chapter 5 – Materials Characterization - IR Spectroscopy

Infrared Spectroscopy Instrumentation


3. Infrared Detector
• Bolometer: Electrical signal, change in resistance of a metallic
conductor with temperature
• Faster response time due to small thermal capacity
• Thermistor bolometer, increased sensitivity
• Fused mixture of metal oxides : Ni, Co, Mn, exponential decrease in
resistance with temperature
Chapter 5 – Materials Characterization - IR Spectroscopy

Infrared Spectroscopy Instrumentation


3. Infrared Detector
• Pneumatic detector cell : Two cells, first 3 mm filled with a gas (Xe),
connected to second cell through a tube
• One end closed with a curved diaphragm, acting as mirror
• Heat on gas changes the volume, expansion due to IR absorption
• Thereby moving mirror in other cell proportionally
Chapter 5 – Materials Characterization - IR Spectroscopy

Preparation of samples
1. Gaseous samples
• No special preparation
• 10 cm long cell for gaseous samples
• Vacuum tight cells
• Connection problems
• Proper operation, due to heating and cooling cycles
Chapter 5 – Materials Characterization - IR Spectroscopy

Preparation of samples
2. Liquid or solution samples
• Pure liquid samples
• No solvents, as they have their own absorption spectra
• Liquid and solution, same type of cell
• Non-corrosive and not too viscous liquids, normally in sealed cells
• Highly viscous liquids, sandwiched as a layer between two salt
plates
• Cavity cells
Chapter 5 – Materials Characterization - IR Spectroscopy

Preparation of samples
3. Solids
• Solid Films: solid samples into thin films, on IR transmitting
window, or solid melted and cooled into thin film, not
recommended for crystalline substances
• Mull-Technique: Powdered sample mixed with a little heavy
paraffin oil, nujol, mulled into paste, transferred to rock salt plate
• Pressed Pellet Technique: Weighed solid material thoroughly mixed
with KBr, pressed into pellet under high pressure in evacuated die,
resulting in transparent discs
Chapter 5 – Materials Characterization – IR Spectroscopy

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