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X ray spectroscopy tools for the characterization of nanoparticles

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This document discusses various x-ray spectroscopy techniques for characterizing nanoparticles, focusing on x-ray diffraction (XRD) spectroscopy. It provides an overview of XRD principles and applications, including Bragg's law, instrumentation, peak analysis to determine structure and composition, and limitations when analyzing nanomaterials due to lack of long-range order. The document also discusses other x-ray techniques like XPS and XRF spectroscopy before concluding that XRD is a powerful tool for determining properties like phase, orientation, stress, and crystallite size in nanoparticle samples.

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X-Ray Spectroscopy Tools for the Characterization of Nanoparticles Presented By Md. Sayedul Islam Ph. D Student ID: 1016034001 Department of Chemistry Bangladesh University of Engineering & Technology 1
There are various techniques for the characterization of nanoparticles on the basis of the x-ray such as- • XRD SPECTROSCOPY • XPS SPECTROSCOPY • XRF SPECTROSCOPY etc. 2
• The contents of the topic are as follows- • what is XRD? • History of XRD • Basic Principle of XRD • Instrumentation • Peak analysis • What type of information obtain from XRD? • Conclusion • References 3 XRD spectroscopy technique for the characterization of nanoparticles
What is XRD? • X-ray diffraction is based on the scattering of x-ray by crystal. • “ Every crystalline substance always gives a pattern, the same substance always gives the same pattern and in a mixture of substance each produces its pattern independently of other”. • So x-ray diffraction pattern of a pure substance is called the finger print of that substance. 4
A Brief History of XRD • 1895- Röntgen publishes the discovery of X-rays. • 1912- Laue observes diffraction of X-rays from a crystal. The father and son team of Sir William Henry and William Lawrence Bragg were awarded the Nobel prize for physics "for their services in the analysis of crystal structure by means of X-rays“ in 1915. 5 Wilhelm Conrad Röntgen (1845- 1923)
Bragg’s law is a simplistic model to understand what conditions are required for diffraction. 6
Information from Bragg’s law for XRD We can know the following two main informations from Bragg law- • The space between diffracting planes of atoms determines peak positions. • The peak intensity is determined by what atoms are in the diffracting plane. 7
Basic Principle of XRD 8
9
Challenge of applying XRD to nanotechnology • Traditional X-ray powder-diffraction techniques rely on the long-range order in crystals to produce sharp "Bragg peaks" in a diffraction pattern. • But in case of nanocrystal due to lack of long-range order, their diffraction patterns are much more diffused Bragg peaks. • "This poses a real challenge to the traditional techniques for the structure determination of nanoparticle," -- Valeri Petkov of Michigan State. 10
Due to overcome this problem Scientist Scherrer use X-rays to estimate the crystallite size of nanophase materials by the following equation. The Scherrer Equation was published in 1918 • Peak width (B) is inversely proportional to crystallite size (L) • P. Scherrer, “Bestimmung der Grösse und der inneren Struktur von Kolloidteilchen mittels Röntgenstrahlen,” Nachr. Ges. Wiss. Göttingen 26 (1918) pp 98-100. • J.I. Langford and A.J.C. Wilson, “Scherrer after Sixty Years: A Survey and Some New Results in the Determination of Crystallite Size,” J. Appl. Cryst. 11 (1978) pp 102-113. 11      cos 2 L K B 
Factors that affect K and crystallite size analysis- • how the peak width is defined • how crystallite size is defined • the shape of the crystal • the size distribution 12
Peak Width Broadening 13 66 67 68 69 70 71 72 73 74 2(deg.) Intensity(a.u.) Peak Width varies inversely with crystallite size as the crystallite size gets smaller, the peak gets broader. The peak width varies with 2ө as cos ө.
How is Crystallite Size Defined • For a distribution of sizes, the mean size can be defined as – the mean value of the cube roots of the individual crystallite volumes. 14
Crystallite Size is Different than Particle Size • A particle may be made up of several different crystallites. • Crystallite size often matches grain size, but there are exceptions. 15
Crystallite Shape • Though the shape of crystallites is usually irregular, we can often approximate them as: – sphere, cube, tetrahedra, or octahedra – needles or plates – prisms or cylinders 16
Non-Uniform Lattice Distortions of nanocompound • Non-Uniform Lattice Distortions produces a broader observed diffraction peak. • Such distortions can be introduced by: – surface tension of nanocrystals – morphology of crystal shape, such as nanotubes – interstitial impurities 17 26.5 27.0 27.5 28.0 28.5 29.0 29.5 30.0 2(deg.) Intensity(a.u.)
Sample Deposition – Flat Plate (Bragg- Brentano) • plastic, aluminum or glass sample holder: dry sample in hollow space • avoid vertical loading (preferred orientation effects) 18
fig: Bruker D8 Analytical X-ray Systems 19
Information from XRD XRD gives the information of a nanosample about the following - Structure determination Phase identification Percent of crystallinity Crystallite size and microanalysis Texture analysis 20
Conclusion • XRD is a powerful tool for answering some specific questions about a given nanosample- • Phase present • Orientation • Residual stress • Texturing • QPA • Crystallite size analysis. • XRD is extremely efficient for the characteristic of the sample due to data acquisition is straight forward and short set up time is required. 21
Textbook References • HP Klug and LE Alexander, X-Ray Diffraction Procedures for Polycrystalline and Amorphous Materials, 2nd edition, John Wiley & Sons, 1974. – Chapter 9: Crystallite Size and Lattice Strains from Line Broadening • BE Warren, X-Ray Diffraction, Addison-Wesley, 1969 – reprinted in 1990 by Dover Publications – Chapter 13: Diffraction by Imperfect Crystals • DL Bish and JE Post (eds), Reviews in Mineralogy vol 20: Modern Powder Diffraction, Mineralogical Society of America, 1989. – Chapter 6: Diffraction by Small and Disordered Crystals, by RC Reynolds, Jr. – Chapter 8: Profile Fitting of Powder Diffraction Patterns, by SA Howard and KD Preston • A. Guinier, X-Ray Diffraction in Crystals, Imperfect Crystals, and Amorphous Bodies, Dunod, 1956. – reprinted in 1994 by Dover Publications 22
Articles • D. Balzar, N. Audebrand, M. Daymond, A. Fitch, A. Hewat, J.I. Langford, A. Le Bail, D. Louër, O. Masson, C.N. McCowan, N.C. Popa, P.W. Stephens, B. Toby, “Size-Strain Line-Broadening Analysis of the Ceria Round-Robin Sample”, Journal of Applied Crystallography 37 (2004) 911- 924 • S Enzo, G Fagherazzi, A Benedetti, S Polizzi, – “A Profile-Fitting Procedure for Analysis of Broadened X-ray Diffraction Peaks: I. Methodology,” J. Appl. Cryst. (1988) 21, 536-542. – “A Profile-Fitting Procedure for Analysis of Broadened X-ray Diffraction Peaks. II. Application and Discussion of the Methodology” J. Appl. Cryst. (1988) 21, 543-549 23
• B Marinkovic, R de Avillez, A Saavedra, FCR Assunção, “A Comparison between the Warren-Averbach Method and Alternate Methods for X-Ray Diffraction Microstructure Analysis of Polycrystalline Specimens”, Materials Research 4 (2) 71-76, 2001. • D Lou, N Audebrand, “Profile Fitting and Diffraction Line-Broadening Analysis,” Advances in X-ray Diffraction 41, 1997. • A Leineweber, EJ Mittemeijer, “Anisotropic microstrain broadening due to compositional inhomogeneities and its parametrisation”, Z. Kristallogr. Suppl. 23 (2006) 117-122 • BR York, “New X-ray Diffraction Line Profile Function Based on Crystallite Size and Strain Distributions Determined from Mean Field Theory and Statistical Mechanics”, Advances in X-ray Diffraction 41, 1997. 24
Thank You to All 25

More Related Content

X ray spectroscopy tools for the characterization of nanoparticles

  • 1. X-Ray Spectroscopy Tools for the Characterization of Nanoparticles Presented By Md. Sayedul Islam Ph. D Student ID: 1016034001 Department of Chemistry Bangladesh University of Engineering & Technology 1
  • 2. There are various techniques for the characterization of nanoparticles on the basis of the x-ray such as- • XRD SPECTROSCOPY • XPS SPECTROSCOPY • XRF SPECTROSCOPY etc. 2
  • 3. • The contents of the topic are as follows- • what is XRD? • History of XRD • Basic Principle of XRD • Instrumentation • Peak analysis • What type of information obtain from XRD? • Conclusion • References 3 XRD spectroscopy technique for the characterization of nanoparticles
  • 4. What is XRD? • X-ray diffraction is based on the scattering of x-ray by crystal. • “ Every crystalline substance always gives a pattern, the same substance always gives the same pattern and in a mixture of substance each produces its pattern independently of other”. • So x-ray diffraction pattern of a pure substance is called the finger print of that substance. 4
  • 5. A Brief History of XRD • 1895- Röntgen publishes the discovery of X-rays. • 1912- Laue observes diffraction of X-rays from a crystal. The father and son team of Sir William Henry and William Lawrence Bragg were awarded the Nobel prize for physics "for their services in the analysis of crystal structure by means of X-rays“ in 1915. 5 Wilhelm Conrad Röntgen (1845- 1923)
  • 6. Bragg’s law is a simplistic model to understand what conditions are required for diffraction. 6
  • 7. Information from Bragg’s law for XRD We can know the following two main informations from Bragg law- • The space between diffracting planes of atoms determines peak positions. • The peak intensity is determined by what atoms are in the diffracting plane. 7
  • 9. 9
  • 10. Challenge of applying XRD to nanotechnology • Traditional X-ray powder-diffraction techniques rely on the long-range order in crystals to produce sharp "Bragg peaks" in a diffraction pattern. • But in case of nanocrystal due to lack of long-range order, their diffraction patterns are much more diffused Bragg peaks. • "This poses a real challenge to the traditional techniques for the structure determination of nanoparticle," -- Valeri Petkov of Michigan State. 10
  • 11. Due to overcome this problem Scientist Scherrer use X-rays to estimate the crystallite size of nanophase materials by the following equation. The Scherrer Equation was published in 1918 • Peak width (B) is inversely proportional to crystallite size (L) • P. Scherrer, “Bestimmung der Grösse und der inneren Struktur von Kolloidteilchen mittels Röntgenstrahlen,” Nachr. Ges. Wiss. Göttingen 26 (1918) pp 98-100. • J.I. Langford and A.J.C. Wilson, “Scherrer after Sixty Years: A Survey and Some New Results in the Determination of Crystallite Size,” J. Appl. Cryst. 11 (1978) pp 102-113. 11      cos 2 L K B 
  • 12. Factors that affect K and crystallite size analysis- • how the peak width is defined • how crystallite size is defined • the shape of the crystal • the size distribution 12
  • 13. Peak Width Broadening 13 66 67 68 69 70 71 72 73 74 2(deg.) Intensity(a.u.) Peak Width varies inversely with crystallite size as the crystallite size gets smaller, the peak gets broader. The peak width varies with 2ө as cos ө.
  • 14. How is Crystallite Size Defined • For a distribution of sizes, the mean size can be defined as – the mean value of the cube roots of the individual crystallite volumes. 14
  • 15. Crystallite Size is Different than Particle Size • A particle may be made up of several different crystallites. • Crystallite size often matches grain size, but there are exceptions. 15
  • 16. Crystallite Shape • Though the shape of crystallites is usually irregular, we can often approximate them as: – sphere, cube, tetrahedra, or octahedra – needles or plates – prisms or cylinders 16
  • 17. Non-Uniform Lattice Distortions of nanocompound • Non-Uniform Lattice Distortions produces a broader observed diffraction peak. • Such distortions can be introduced by: – surface tension of nanocrystals – morphology of crystal shape, such as nanotubes – interstitial impurities 17 26.5 27.0 27.5 28.0 28.5 29.0 29.5 30.0 2(deg.) Intensity(a.u.)
  • 18. Sample Deposition – Flat Plate (Bragg- Brentano) • plastic, aluminum or glass sample holder: dry sample in hollow space • avoid vertical loading (preferred orientation effects) 18
  • 19. fig: Bruker D8 Analytical X-ray Systems 19
  • 20. Information from XRD XRD gives the information of a nanosample about the following - Structure determination Phase identification Percent of crystallinity Crystallite size and microanalysis Texture analysis 20
  • 21. Conclusion • XRD is a powerful tool for answering some specific questions about a given nanosample- • Phase present • Orientation • Residual stress • Texturing • QPA • Crystallite size analysis. • XRD is extremely efficient for the characteristic of the sample due to data acquisition is straight forward and short set up time is required. 21
  • 22. Textbook References • HP Klug and LE Alexander, X-Ray Diffraction Procedures for Polycrystalline and Amorphous Materials, 2nd edition, John Wiley & Sons, 1974. – Chapter 9: Crystallite Size and Lattice Strains from Line Broadening • BE Warren, X-Ray Diffraction, Addison-Wesley, 1969 – reprinted in 1990 by Dover Publications – Chapter 13: Diffraction by Imperfect Crystals • DL Bish and JE Post (eds), Reviews in Mineralogy vol 20: Modern Powder Diffraction, Mineralogical Society of America, 1989. – Chapter 6: Diffraction by Small and Disordered Crystals, by RC Reynolds, Jr. – Chapter 8: Profile Fitting of Powder Diffraction Patterns, by SA Howard and KD Preston • A. Guinier, X-Ray Diffraction in Crystals, Imperfect Crystals, and Amorphous Bodies, Dunod, 1956. – reprinted in 1994 by Dover Publications 22
  • 23. Articles • D. Balzar, N. Audebrand, M. Daymond, A. Fitch, A. Hewat, J.I. Langford, A. Le Bail, D. Louër, O. Masson, C.N. McCowan, N.C. Popa, P.W. Stephens, B. Toby, “Size-Strain Line-Broadening Analysis of the Ceria Round-Robin Sample”, Journal of Applied Crystallography 37 (2004) 911- 924 • S Enzo, G Fagherazzi, A Benedetti, S Polizzi, – “A Profile-Fitting Procedure for Analysis of Broadened X-ray Diffraction Peaks: I. Methodology,” J. Appl. Cryst. (1988) 21, 536-542. – “A Profile-Fitting Procedure for Analysis of Broadened X-ray Diffraction Peaks. II. Application and Discussion of the Methodology” J. Appl. Cryst. (1988) 21, 543-549 23
  • 24. • B Marinkovic, R de Avillez, A Saavedra, FCR Assunção, “A Comparison between the Warren-Averbach Method and Alternate Methods for X-Ray Diffraction Microstructure Analysis of Polycrystalline Specimens”, Materials Research 4 (2) 71-76, 2001. • D Lou, N Audebrand, “Profile Fitting and Diffraction Line-Broadening Analysis,” Advances in X-ray Diffraction 41, 1997. • A Leineweber, EJ Mittemeijer, “Anisotropic microstrain broadening due to compositional inhomogeneities and its parametrisation”, Z. Kristallogr. Suppl. 23 (2006) 117-122 • BR York, “New X-ray Diffraction Line Profile Function Based on Crystallite Size and Strain Distributions Determined from Mean Field Theory and Statistical Mechanics”, Advances in X-ray Diffraction 41, 1997. 24
  • 25. Thank You to All 25