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  • L 16 CHN 425 Analysis Techniques 3 BET XRD 3

    Enviado por

    Harsha Vardhan
    43 visualizações17 páginas
    This document provides an overview of various analytical techniques used to characterize nanomaterials, including microscopy, spectroscopy, and physical methods. Specifically, it discusses BET analysis for measuring surface area, X-ray diffraction (XRD) for determining crystal structure and sizes, and UV-vis spectroscopy. For XRD, it explains Bragg's law and how diffraction patterns provide information about atomic arrangements. It also shows how the Scherrer equation relates nanoparticle sizes to peak broadening in XRD patterns. Examples are given of using these techniques to analyze ZnS nanoparticles. The document was presented by Dr. T. Das to students at IIT Roorkee on nanotechnology analysis methods.

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    Analysis Techniques

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    This document provides an overview of various analytical techniques used to characterize nanomaterials, including microscopy, spectroscopy, and physical methods. Specifically, it discusses BET analysis for measuring surface area, X-ray diffraction (XRD) for determining crystal structure and sizes, and UV-vis spectroscopy. For XRD, it explains Bragg's law and how diffraction patterns provide information about atomic arrangements. It also shows how the Scherrer equation relates nanoparticle sizes to peak broadening in XRD patterns. Examples are given of using these techniques to analyze ZnS nanoparticles. The document was presented by Dr. T. Das to students at IIT Roorkee on nanotechnology analysis methods.

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    © All Rights Reserved
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    Sinalizar o conteúdo como inadequado
    43 visualizações17 páginas

    L 16 CHN 425 Analysis Techniques 3 BET XRD 3

    Enviado por

    Harsha Vardhan
    This document provides an overview of various analytical techniques used to characterize nanomaterials, including microscopy, spectroscopy, and physical methods. Specifically, it discusses BET analysis for measuring surface area, X-ray diffraction (XRD) for determining crystal structure and sizes, and UV-vis spectroscopy. For XRD, it explains Bragg's law and how diffraction patterns provide information about atomic arrangements. It also shows how the Scherrer equation relates nanoparticle sizes to peak broadening in XRD patterns. Examples are given of using these techniques to analyze ZnS nanoparticles. The document was presented by Dr. T. Das to students at IIT Roorkee on nanotechnology analysis methods.

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    © All Rights Reserved
    Baixe no formato PDF, TXT ou leia online no Scribd
    Sinalizar o conteúdo como inadequado
    de 17

    NanotechnologyinChemicalEngineering

    (CHN425)

    LL16AnalysisTechniquesIII
    16 Analysis Techniques III
    (BET/XRD/UVvis/FTIR/Raman)
    (Surfacearea/crystalsizesofsamples)

    byDr.T.Das

    Date:17/10/2016
    DepartmentofChemicalEngineering
    IndianInstituteofTechnologyRoorkee,India

    Content
    Analysis Techniques

    Microscopes
    Mi
    SEM/TEM/ SPM/STM/AFM/SNOM
    Diffraction Techniques
    q
    XRD
    Spectroscopies
    UV Vis NIR/FTIR/Raman/XPS
    UVVisNIR/FTIR/Raman/XPS
    Physical methods
    BET

    BET
    Multilayer adsorption theory:

    Langmuir equation is valid for adsorption less than monolayer coverage


    Brunauer, Emmette and Teller derived an relationship between the volume of gas
    physically adsorbed and the partial pressure of the adsorbate which is valid for
    multilayer
    ltil
    adsorption
    d
    ti

    BET
    BETequation:

    v0 =v, is volume of gas adsorbed per unit area of adsorbent surface and
    vm is the volume of gas adsorbed when the entire adsorbent surface is covered with a
    complete unimoleculer layer
    p0 : saturation pressure of gas ( infinite no of layers can build up on the surface)
    c: constant

    BET
    Isothermsmostcommonlyusedincatalysis
    y
    y

    Type

    Langmuir

    Freundlich

    Temkin

    Brunauer Emmet Teller


    BrunauerEmmetTeller

    Isotherm equations

    Type of adsorption
    Chemisorption
    Physisorption
    Chemisorption
    and
    physisorption at low coverage
    Ch i
    Chemisorption
    i

    Multilayer
    u t aye p
    physical
    ys ca adso
    adsorption
    pt o

    BET
    The equilibrium adsorption of N2 on an oxide sample at 77.4K, b.pt of N2

    X RayDiffraction(XRD)
    XRayDiffraction(XRD)
    (crystalstructureofpolycrystallinesamples,thinfilmsandnanoparticles)

    XRayDiffraction(XRD)
    X
    tt d by
    b atoms
    t
    bl us to
    t understand
    d t d about
    b t arrangementt off atoms
    t
    i solids
    lid
    X-rays
    scattered
    enable
    in
    X-rays are scattered by atoms i.e that they are scattered by electrons of atoms
    The scattered intensity at point P is given as (by JJ Thomson)

    Ie:IntensityofXraysatpointP
    e:chargeofanelectron
    I:IntensityoftheXraybeamatorigin
    y
    y
    g
    r:distanceofpointPfromtheorigin
    n:numberofelectron
    m:massofanelectron
    :anglebetweenincidentandscattered
    beam
    c:velocityoflight

    XRayDiffraction(XRD)
    X
    diff t
    t
    X-ray
    diffractometer

    For crystal structure analysis


    Used for nanomaterials analysis
    Commonly used diffractometer is known as Powder Diffractometer or DebyeScherrer Diffractometer

    XRayDiffraction(XRD)
    A monochromatic source of X-rays
    A Cu (copper) target or anode giving CuK (=0.154nm)
    (=0 154nm)
    A sample holder
    An X-ray detector(Geiger Muller tube)

    Both sample and detector move around an axis passing through sample center
    and normal plane of the paper
    Diffracted rays make an angle 2 at the detector
    A plot
    l t off intensity
    i t it (counts)
    (
    t ) as a function
    f ti off angle
    l 2
    2 (usually
    (
    ll 20 to
    t 160 o) is
    i a
    diffraction pattern ready for analysis

    XRayDiffraction(XRD)
    B
    Law
    L off diffraction
    diff ti
    Braggs

    A beam of X-rays fall on crystal planes at some grazing incidence,


    B
    Beam
    off parallel
    ll l rays is
    i assumedd
    Parallel rays of AO and BP are incident on atoms O and P and making an angle
    Rays are scattered as OA and PB.
    Distance between O and P is d
    is the path difference between rays AOA and BPB

    XRayDiffraction(XRD)
    Diff ti from
    f
    diff
    t types
    t
    l
    Diffraction
    different
    off samples
    Dont have infinite
    ordered of arrangement
    of atoms and have few
    atoms and few planes
    Scattering
    without
    diffraction peaks

    Diffraction peaks are


    sharp and broadened,
    since nano particles and
    i planes
    its
    l
    are small
    ll
    Dont have infinite
    arrangement of atoms

    XRayDiffraction(XRD)
    Diff ti from
    f
    ti l and
    d Scherrer
    S h
    ti
    Diffraction
    nanoparticles
    equation

    FWHM

    Nanoparticles are similar to single crystals and diffraction peaks are broadened
    Particle sizes (T) decreases with increasing width of peak

    XRayDiffraction(XRD)
    Spacing between atomic planes of a crystal:
    The plane spacing of cubic crystal is related to the lattice parameter (a) by the
    following equation

    XRayDiffraction(XRD)
    ZnS nanoparticles: Diffraction peak at 30 degree is due to ZnS nanoparticles

    UVvisNIRspectrometer

    Thanksforyourattention

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