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Lecture 4 Application of X-ray diffraction (XRD) technique on the characterization of in nano materials

History of X-ray and XRD


Wilhelm Conrad Rntgen discovered X-Rays in 1895. 1901 Nobel prize in Physics

Wilhelm Conrad Rntgen (1845-1923)

Bertha Rntgens Hand 8 Nov, 1895

A modern radiograph of a hand

History of X-ray and XRD


Radiographs like the ones in the last slide are simply shadowgrams. The X-rays either pass straight through or are stopped by the object. The diagram on the upper left illustrates the principle and shows a perfect shadow. In reality, a large fraction of the X-rays are not simply absorbed or transmitted by the object but are scattered. The diagram on the bottom left illustrates this effect and illustrates the fuzzy edge of the object that is produced in the image by the scattered X-rays.

Schematic for X-ray Diffraction

A continuous beam of X-rays is incident on the crystal The diffracted radiation is very intense in certain directions These directions correspond to constructive interference from waves reflected from the layers of the crystal

The diffraction pattern is detected by photographic film

History of X-ray and XRD


The first kind of scatter process to be recognised was discovered by Max von Laue who was awarded the Nobel prize for physics in 1914 "for his discovery of the diffraction of X-rays by crystals". His collaborators Walter Friedrich and Paul Knipping took the picture on the bottom left in 1912. It shows how a beam of X-rays is scattered into a characteristic pattern by a crystal. In this case it is copper sulphate. The X-ray diffraction pattern of a pure substance is like a fingerprint of the substance. The powder diffraction method is thus ideally suited for characterization and identification of polycrystalline phases.

Max von Laue (1897-1960)

Production of X-rays
X-rays are produced when highspeed electrons are suddenly slowed down Can be caused by the electron striking a metal target

A current in the filament causes electrons to be emitted These freed electrons are accelerated toward a dense metal target The target is held at a higher potential than the filament

Equipment

Bruker D8 Analytical X-ray Systems

Goniometer

2-Theta:Theta Setup

X-ray spectrum

Braggs Law

The beam reflected from the lower surface travels farther than the one reflected from the upper surface If the path difference equals some integral multiple of the wavelength, constructive interference occurs Braggs Law gives the conditions for constructive interference 2 d sin = m , m = 1, 2, 3

Problem: X-ray diffraction

X-rays of wavelength 0.140 nm are reflected from a certain crystal, and the first-order maximum occurs at an angle of 14.4. What value does this give for the interplanar spacing of this crystal?

Photo of X-ray Diffraction Pattern The array of spots is called a Laue pattern The crystal structure is determined by analyzing the positions and intensities of the various spots This is for NaCl

Nano-Kompozitler

Nano-Kompozitler Nanoteknolojinin z, molekler boyutta alarak, molekler yaps yenilenmi byk yaplar elde etmektir. Malzemelerin nanometrik boyuttaki zellikleri, ayn malzemenin makro boyuttaki zelliklerine gre deiiklik gstermektedir. Nano kompozitler, bir matris ierisinde nanometre byklnde paracklarn dalmas ile oluan malzemelerdir. Nano kompozitlerin malzemeye getirdii stnlkler; modl arttrmas, glendirmesi, s direncini arttrmas, malzemeye gaz szmasn engellemesi, yancln azaltmas olarak sralanabilir.

NANO-KOMPOZTLER
metal / seramik metal / metal seramik / seramik
Nano Kompozitler

polimer / seramik
inorganik/ polimer

polimer / polimer

NANO-KOMPOZTLER
1. Nanokompozitler seramik/seramik
Al2O3/(SiC, Si3N4, TiC, TiN, TiB2, BN), MgO/SiC, Si3N4/(SiC, TiN, BN), Sialon/SiC, B4C/SiC, B4C/SiC/TiB2

2. Nanokompozitler seramik/metal
Al2O3/(W, Mo, Ti, Ni, Co, Fe, FeNi), ZrO2/(Mo, Ni. Co) MgO/(Fe, Ni)

3. Nanokompozit temelli fonksiyonel seramikler


BaTiO3, ZnO, c-ZrO2 based nanocomposites

4. Nanokompozitler metal/seramic
Ti-Al Intermetalic based nanocomposites, MoSi2 based nanocomposites

5. Nanokompozitler polimer/seramik ve polimer/metal

Toz

Mikroyap

Makroyap

Arzu edilen zelliklere Sahip KOMPOZT MALZEME

Mukavemet, tokluk, srnme, kimyasal kararllk, Yksek scaklk zellikleri

NANO-KOMPOZTLER Nanoboyuttaki tozlar, gelimi zelliklere sahip nanokompozitleri oluturmak zere seramik, metal ya da polimer gibi malzemeler iinde destekleyici olarak kullanlmaktadr. Nano toz / Nano toz seramik kompozitler iin kullanlacak tozlar; Yksek kimyasal saflk Homojen toz boyut dalm Dk topaklama Nano boyutta homojen olarak dalm tozlarn elde edilmesi gerekir. BU NEDENLE TOZ RETM YNTEM NEML BR BASAMAKTIR.

DOLGU MADDELER

KL
Yksek iyon deiim kapasitesi Yksek yzey alan/hacim oran, Kolay ilenebilirlik, Dk maliyet
Polimerlerin termal, mekanik ve yanmazlk zelliklerini, kilin yap iinde kolay dalm ve kil tabakalarnn birbirinden ayrlmasyla gelitirir.

MONTMORLLONT (MMT)

MONTMORLLONT (MMT)

3 tip yap olumaktadr:


1. Mikro kompozit; Polimer kil tabakas arasna giremez. Killer yn halinde bulunur. 2. Intercalated nanokompozit; Polimer zincirleri kil tabakalar arasna yerlemitir.
nm

nm

3. Exfoliated nanokompozit; Kil tabakalar birbirinden tamamen ayrlm ve polimer matriksine dalmtr. Polimer/nanokil etkileimi maksimumdur.

Nanokompozit Karakterizasyon Yntemleri


X In Krnm (XRD) Taramal Elektron Mikroskopu (SEM) Geirimli Elektron Mikroskopu (TEM) Taramal Sonda Mikroskobu (SPM) Yakn Alan Taramal Optik Mikroskop