Application of X-Ray Diffraction (XRD) Technique in Nano Composite Materials

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    History of X-ray and XRD

    Wilhelm Conrad Rntgen discoveredX-Rays in 1895.

    1901 Nobel prize in Physics

    Wilhelm Conrad Rntgen (1845-1923)

    A modern radiograph of a handBertha Rntgens Hand 8 Nov, 1895

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    History of X-ray and XRD

    Radiographs like the ones in thelast slide are simplyshadowgrams.

    The X-rays either pass straightthrough or are stopped by the

    object. The diagram on the upperleft illustrates the principle andshows a perfect shadow.

    In reality, a large fraction of theX-rays are not simply absorbedor transmitted by the object butare scattered. The diagram onthe bottom left illustrates thiseffect and illustrates the fuzzyedge of the object that isproduced in the image by thescattered X-rays.

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    Schematic for X-ray Diffraction

    A continuous beam of X-rays isincident on the crystal

    The diffracted radiation is veryintense in certain directions

    These directionscorrespond to constructiveinterference from wavesreflected from the layers ofthe crystal

    The diffraction pattern isdetected by photographic film

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    The first kind of scatter process to berecognised was discovered by Max vonLauewho was awarded the Nobel prize for physicsin 1914 "for his discovery of the diffraction ofX-rays by crystals". His collaborators WalterFriedrich and Paul Knipping took the picture

    on the bottom left in 1912. It shows how abeam of X-rays is scattered into acharacteristic pattern by a crystal. In thiscase it is copper sulphate.

    The X-ray diffraction pattern of a pure

    substance is like a fingerprint of thesubstance. The powder diffraction method isthus ideally suited for characterization andidentification of polycrystalline phases.

    History of X-ray and XRD

    Max von Laue (1897-1960)

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    Production of X-rays

    X-rays are produced when high-speed electrons are suddenlyslowed down

    Can be caused by theelectron striking a metaltarget

    A current in the filament causeselectrons to be emitted

    These freed electrons areaccelerated toward a dense

    metal target The target is held at a higher

    potential than the filament

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    Equipment

    Bruker D8 Analytical X-ray Systems

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    Goniometer

    2-Theta:Theta Setup

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    X-ray

    spectrum

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    Braggs Law

    The beam reflected from the lowersurface travels farther than theone reflected from the uppersurface

    If the path difference equals someintegral multiple of the wavelength,constructive interference occurs

    Braggs Lawgives the conditions

    for constructive interference

    2 d sin = m , m = 1, 2, 3

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    Problem: X-ray diffraction

    X-rays of wavelength 0.140 nm are reflected from acertain crystal, and the first-order maximum occursat an angle of 14.4. What value does this give for

    the interplanar spacing of this crystal?

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    Photo of X-ray Diffraction Pattern

    The array of spots is called aLauepattern

    The crystal structure isdetermined by analyzing thepositions and intensities of thevarious spots

    This is for NaCl

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    Nano-Kompozitler

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    Nanoteknolojinin z, molekler boyutta alarak,

    molekler yaps yenilenmi byk yaplar elde etmektir.Malzemelerin nanometrik boyuttaki zellikleri, aynmalzemenin makro boyuttaki zelliklerine gre deiiklikgstermektedir. Nano kompozitler, bir matris ierisinde

    nanometre byklnde paracklarn dalmas ileoluan malzemelerdir.

    Nano kompozitlerin malzemeye getirdii stnlkler;

    modl arttrmas, glendirmesi, s direncini arttrmas,malzemeye gaz szmasn engellemesi, yanclnazaltmas olarak sralanabilir.

    Nano-Kompozitler

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    NanoKompozitler

    metal / seramik

    seramik / seramik

    metal / metal

    polimer / seramik

    inorganik/ polimer

    polimer / polimer

    NANO-KOMPOZTLER

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    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 seramiklerBaTiO3, ZnO, c-ZrO2 based nanocomposites

    4. Nanokompozitler metal/seramicTi-Al Intermetalic based nanocomposites, MoSi2based nanocomposites

    5. Nanokompozitler polimer/seramik ve polimer/metal

    NANO-KOMPOZTLER

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    Toz

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

    Mikroyap Makroyap

    Arzu edilen zelliklereSahip KOMPOZT MALZEME

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    Nanoboyuttaki tozlar, gelimi zelliklere sahip nanokompozitleri

    oluturmakzere seramik, metal ya da polimer gibi malzemeler iindedestekleyici 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.

    NANO-KOMPOZTLER

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    DOLGU MADDELER

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    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 tabakalarnnbirbirinden ayrlmasyla gelitirir.

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    MONTMORLLONT(MMT)

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    MONTMORLLONT(MMT)

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    3 tip yap olumaktadr: m

    1. Mikro kompozit;Polimer kil tabakas arasnagiremez. Killer yn halindebulunur.

    nm

    2. Intercalated nanokompozit;Polimer zincirleri kil tabakalararasna yerlemitir.

    3. Exfoliated nanokompozit;Kil tabakalar birbirindentamamen ayrlm ve polimermatriksine dalmtr.Polimer/nanokil etkileimimaksimumdur.

    nm

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    Nanokompozit KarakterizasyonYntemleri

    X In Krnm (XRD)

    Taramal Elektron Mikroskopu (SEM)

    Geirimli Elektron Mikroskopu (TEM) Taramal Sonda Mikroskobu (SPM)

    Yakn Alan Taramal Optik Mikroskop

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