Neutrons, X-rays, and Light

Scattering Methods Applied to Soft Condensed Matter

2nd Edition - December 6, 2024
Imprint: Elsevier
Editors: Peter Lindner, Julian Oberdisse
Language: English
Hardback ISBN:
9 7 8 - 0 - 4 4 3 - 2 9 1 1 6 - 6
eBook ISBN:
9 7 8 - 0 - 4 4 3 - 2 9 1 1 7 - 3

This book addresses the possibilities provided by scattering techniques in the study of soft matter. It fills the gap between the fundamental scattering processes, which are… Read more

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This book addresses the possibilities provided by scattering techniques in the study of soft matter. It fills the gap between the fundamental scattering processes, which are described by the general theoretical framework of elastic and quasi-elastic interaction of radiation with matter, and state-of-the-art applications to specific soft matter systems. Three probes are discussed in detail: neutrons, X-ray photons, and visible light.

Part 1 of the book is dedicated to the use of general principles for the measurement and analysis of scattered intensity: elementary scattering process, data reduction, general theorems, the concept of reciprocal space, and its link to structural and dynamical information in direct space. In Part 2, methods and techniques are further discussed, including resolution effects, contrast variation, static and dynamic light scattering, quasielastic neutron scattering, and reflectometry and grazing incidence techniques. Part 3 deals with the state of the art of scattering studies of typical soft matter systems (polymers, self-assembled surfactant systems and liquid crystals, microemulsions, colloids, aggregates, biological systems) with dedicated chapters for particle interactions and modeling. Part 4 highlights special applications, from light scattering in turbid media to scattering under external constraints, applications of neutron reflectometry, characterization of relaxation modes by neutron spectroscopy, and industrial applications.

This new edition, written by the lecturers of the Bombannes Summer School, will be most useful as a learning tool for masters and PhD students, postdocs, and young researchers moving into the field. As with the previous edition, it will also be a reference for any scientist working in soft matter, where scattering techniques are ubiquitous, used in both small laboratories and large-scale research facilities.

Neutrons, X-rays, and Light
Cover image
Title page
Table of Contents
Copyright
Contributors
About the Editors
Preface to the Lecture Notes (1991)
Preface to the First Edition (2002)
Preface to the Second Edition
Part I: Using general principles
Chapter 1 General Introduction to Soft Matter and Scattering Experiments
Abstract
Keywords
1 Definition of soft condensed matter
2 The scattering experiment in practice
2.1 Setup and momentum transfer
2.2 Relating the scattered intensity to the differential scattering cross section
2.3 From the differential scattering cross section to structure and dynamics
2.4 The scattering experiment in practice_ experimental aspects
2.5 Summary of a general method for solving structural problems
3 Conception of the book and summary of the chapters
References
Chapter 2 General Theorems, Differential Scattering Cross-Section, and Initial Data Treatment
Abstract
Keywords
Acknowledgments
1 Introduction
2 General theorems
2.1 General expressions for the scattering of waves
2.2 Scattering by particle systems
2.3 Scattering at low q (where q tends to zero)
2.4 Scattering at high q
3 Differential scattering cross-section and initial data treatment
3.1 Definition of differential scattering cross-section
3.2 Scattering experiment in practice
3.3 Initial reduction of scattering data
References
Chapter 3 The Inverse Scattering Problem
Abstract
Keywords
1 Introduction
2 Rayleigh-Debye-Gans theory
3 Dilute systems
3.1 Monodisperse, dilute systems
3.2 The radius of gyration Rg, Guinier approximation
4 Particles with spherical symmetry
5 Shape and structure of particles
6 Rod-like particles
7 Flat particles
8 Hollow and inhomogeneous particles
8.1 Hollow spheres
8.2 Inhomogeneous spherical particles
8.3 Inhomogeneous rod-like particles
8.4 Inhomogeneous lamellar particles
9 Polydisperse systems
References
Chapter 4 Indirect Fourier Transformation, Deconvolution, and Generalized Indirect Fourier Transformation
Abstract
Keywords
1 Introduction
2 Indirect Fourier transformation
2.1 Introduction
2.2 The indirect Fourier transformation method
2.3 Basic principles of the IFT method
2.4 Stabilization
2.5 Choice of Dmax
2.6 IFT for rod-like, lamellar, or polydisperse systems
3 Deconvolution – Convolution square root operation
3.1 Spherical symmetry
3.2 Circular cylinders and centrosymmetric lamellae
3.3 Principles of the deconvolution technique – DECON
4 Interacting systems
5 Generalized indirect Fourier transformation
5.1 Basics of the GIFT method
5.2 GIFT method applied to uncharged, hard-sphere systems
5.3 GIFT method applied to charged systems
5.4 GIFT method applied to lamellar systems
5.5 GIFT method applied to hexagonal phases
5.6 GIFT method applied to systems with attractive interaction
5.7 GIFT summary
6 Software
References
Part II: Methods
Chapter 5 Instrumentation and Resolution Effects for Small-Angle X-ray and Neutron Scattering
Abstract
Keywords
Acknowledgments
1 Introduction
2 Instrumental smearing
3 Small-angle X-ray scattering instrumentation
3.1 Introduction
4 Examples of SAXS instruments
4.1 Simple pinhole SAXS systems
4.2 Pinhole SAXS system with multi-layer optics
4.3 Synchrotron SAXS beamlines
4.4 Bonse–Hart camera for USAXS
5 Small-angle neutron scattering instrumentation
5.1 Pin-hole SANS instruments
5.2 Time-of-flight SANS
5.3 Ultra-small-angle neutron scattering (USANS)
6 Summary and conclusions
References
Chapter 6 Contrast and Contrast Variation in Neutron, X-ray, and Light Scattering
Abstract
Keywords
Acknowledgments
1 Introduction
2 Scattering length and cross section
3 Light scattering
3.1 The physical basis of light scattering
3.2 Scattering length, polarizability, and index of refraction
4 Neutron scattering
4.1 Coherent and incoherent scattering
4.2 Overall contrast and molar mass determination with light and neutron scattering
5 X-ray scattering
5.1 Scattering length
5.2 Anomalous scattering and contrast variation
6 Selected examples
6.1 Polymer conformation and flexibility
6.2 Zero-average contrast: Single-chain conformation in crowded environments
6.3 Highlighting domain structures in biological systems
6.4 Local structure of polymer-like micelles: X-rays vs neutrons
6.5 Size and polydispersity of microemulsions: An optical contrast variation study
6.6 Nucleation and phase separation in microemulsions: SANS contrast variation experiments
References
Chapter 7 Static Light Scattering
Abstract
Keywords
1 Introduction
2 Static light scattering set-ups
3 Basic theory of light scattering
4 Discrete scatterers
4.1 Dilute systems: Form factor
4.2 Concentrated systems: Structure factor
5 Absolute intensities
6 Mie scattering
6.1 Homogeneous spheres
6.2 Layered spheres
6.3 Non-spherical objects
6.4 Particle sizing of polydisperse systems with static light scattering
7 Addressing multiple scattering
8 Practical issues: An experimentalist’s checklist
Appendix
References
Chapter 8 Dynamic Light Scattering
Abstract
Keywords
Acknowledgment
1 Introduction
2 Speckle and correlation functions
3 Sizing of spherical particles by DLS
3.1 Dilute suspension of identical spheres in Brownian motion
3.2 Dilute suspension of polydisperse spheres in Brownian motion
4 Concentrated systems
5 Suppression of multiple-scattering
6 Non-ergodic samples
7 Equipment for light scattering
8 X-ray photon correlation spectroscopy
9 Other topics
9.1 Non-spherical particles
9.2 Depolarized scattering
9.3 Scattering in the heterodyne mode
Appendix: Simple derivation of Eqs. (31) and (34)
References
Chapter 9 Inelastic Neutron Scattering
Abstract
Keywords
1 Introduction
2 Time-of-flight spectrometer
3 Backscattering spectrometer
4 Inverse TOF spectrometer
5 Neutron spin-echo spectrometer
6 Conclusion
References
Chapter 10 Neutron and X-ray Reflectometry and Grazing Incidence Scattering
Abstract
Keywords
1 Introduction
2 Specular reflectometry
2.1 Introduction
2.2 Exact solution
3 Instrumentation
3.1 Resolution smearing
4 Off-specular scattering within the distorted wave Born approximation
4.1 Introduction and theory
4.2 Off-specular scattering integrated over y
5 Grazing incidence scattering
5.1 Introduction and theory
5.2 Grazing incidence small-angle scattering
5.3 Grazing incidence X-ray diffraction
References
Part III: Revealing microstructures and dynamics of soft condensed matter
Chapter 11 Introduction to Polymers: Static Scattering
Abstract
Keywords
1 Polymer molecules
1.1 Single chains: Random and self-avoiding walk
2 Polymer conformation in solution and bulk
3 Polymer morphology
3.1 Semi-crystalline polymers
3.2 Block copolymers
References
Chapter 12 Self-assembled Aggregates: Form and Structure Factors in Surfactant Systems and Lyotropic Liquid Crystals
Abstract
Keywords
Acknowledgments
1 Introduction
2 The physics of surfactant self-assembly
2.1 Amphiphilic molecules and self-assembly
2.2 Sequence of morphologies
2.3 Free energy of bending: The Helfrich Hamiltonian
3 Lyotropic liquid crystalline phases
4 A simple view of form factor scattering
4.1 Basics of scattering processes
4.2 Form factor scattering
4.3 Small-angle scattering of typical surfactant phases
5 Some practical considerations about interparticle structure factors
6 Conclusion
References
Chapter 13 Small-Angle Scattering by Microemulsions
Abstract
Keywords
Acknowledgments
1 Introduction
2 Phase diagrams
2.1 Phase prism and cuts
2.2 Other types of microemulsions
3 Small-angle scattering of classical microemulsion structures
3.1 Evolution of microemulsion morphologies and scattering with monolayer curvature
3.2 Droplet microemulsions: Bulk and film contrast, and swelling of the droplets
3.3 Bicontinuous microemulsions
4 Complementary techniques
5 Some applications of microemulsions
6 Outlook: Where are we heading?
References
Chapter 14 Interacting Colloidal Systems, Gels, Glasses
Abstract
Keywords
1 Introduction
2 Effective interactions
3 Predictions of structure of interacting colloidal systems
3.1 Basic definitions
3.2 Ornstein–Zernike equation: Closures and solutions
3.3 Mixtures and polydispersity effects
4 Predictions of dynamical properties of interacting colloidal systems: Mode-coupling theory and other approaches
5 Experimental challenges
5.1 Non-ergodicity
5.2 Time-evolving systems: Aging and aggregation
5.3 Temporal and spatial heterogeneity of the dynamics
5.4 Driven systems
6 Scattering studies of interacting colloids
6.1 Hard and soft repulsive glasses
6.2 Attractive glasses
6.3 Gels
7 Concluding remarks
References
Chapter 15 Model Fitting and Simulation Techniques in Small-Angle Scattering Data Analysis
Abstract
Keywords
Acknowledgments
1 Introduction
2 Least-squares fitting
3 Models
3.1 Form factors
3.2 Structure factors
3.3 Structure factors of oligomers, aggregates, and clusters
4 Application of Monte Carlo methods for the calculation of form factors
4.1 MC methods for solid particle form factors
4.2 MC and simulation for polymer form factors
5 Example of analysis on absolute scale: Block copolymer micelles
6 Summary and conclusions
References
Chapter 16 Polymer Dynamics
Abstract
Keywords
1 Introduction
2 Free chain dynamics (Rouse model)
3 Entangled chain dynamics (reptation)
4 Advanced studies
4.1 Limits of reptation
4.2 Polymer architecture: Stars
5 Conclusion
Appendix: Rouse dynamics scattering function
References
Chapter 17 Analysis of Small-Angle Scattering Data of Complex Biological Systems
Abstract
Keywords
1 Introduction
2 Fundamental challenges in SAS data analysis
3 Archetypal modeling schemes
4 Recent developments and advanced modeling schemes
4.1 Advances in sample handling and preparation
4.2 Examples of specialized analysis methods
4.3 Toward more complex samples and modeling schemes
5 Current challenges and perspectives
6 Final remarks
References
Chapter 18 Macromolecular and Supramolecular Assemblies
Abstract
Keywords
1 Introduction
2 Macromolecular and supramolecular assembly
2.1 Surfactant micelles
2.2 Complex coacervate core micelles
2.3 What can we learn about macromolecular and supramolecular assembly through scattering techniques?
3 Studying macromolecular and supramolecular assembly with scattering tools
3.1 Molar mass
3.2 Critical micelle concentration
3.3 Aggregation number
3.4 Sizing and scaling laws
3.5 Complex colloids: From “simple” core–shell architectures to Janus micelles, multi-compartment micelles, core–shell-corona micelles, and other hierarchical nanostructures
3.6 Polymorphism
3.7 Thermoresponsive systems
3.8 Kinetics
3.9 Exchange dynamics
4 Conclusion
References
Part IV: Special applications
Chapter 19 Soft Matter Studies Under Non-equilibrium Conditions
Abstract
Keywords
1 Introduction
2 External constraints
2.1 Osmotic pressure
2.2 Stopped-flow
2.3 High pressure
3 External fields
3.1 Flow fields
3.2 Examples
3.3 Recent other developments
4 Conclusions
References
Chapter 20 Polymer Processing: Application of Scattering Methods to Polyurethane Materials
Abstract
Keywords
1 Introduction
2 Reaction-induced microphase separation of PU foam
2.1 Structure development during polymerization
2.2 Experimental methods
2.3 Reaction kinetics and hydrogen bonding from FT-IR
2.4 Microphase separation kinetics from SAXS
3 PU structure by contrast variation SANS
3.1 PU elastomers
3.2 Experimental methods
3.3 Results
4 PU and PU/polyacrylic dispersions
4.1 Aqueous PUDs
4.2 Hybrid PU/acrylic dispersions
5 Contrast variation SAXS on PU/PA aqueous dispersions
5.1 Experimental methods
5.2 Particle morphology from SAXS distance distribution functions
6 Reaction-induced phase separation in PU/PA polymerization
6.1 Structure development in nanoparticles by time-resolved SAXS
6.2 Experimental methods
6.3 Evolution of morphology from time-resolved SAXS data collection
References
Chapter 21 Light Scattering and Propagation in Turbid Media
Abstract
Keywords
1 Introduction
2 Multiple light scattering and photon diffusion
2.1 Mean free path and extinction
2.2 The random walk picture
2.3 Light diffusion equation
3 DWS
3.1 Theory
3.2 DWS from non-ergodic, solid-like media
3.3 Backscattering DWS and particle sizing
3.4 DWS-based optical microrheology
4 Summary and conclusion
References
Chapter 22 From Real to Reciprocal Space_ Scattering Information From Real Space Images
Abstract
Keywords
Acknowledgments
1 A Fourier optics perspective on scattering experiments
1.1 Far-field scattering experiments are typically performed at sufficiently large distances from the sample
1.2 Far-field scattering experiments can also be performed in the back focal plane of a lens
2 The traditional role of speckles in scattering experiments
2.1 In the Fraunhofer regime, the speckle size does not depend on the sample properties
2.2 In the Fraunhofer regime, the speckle spatio-temporal distribution depends on sample properties
3 A new role for speckles in scattering experiments
3.1 In the deep Fresnel regime, the speckle pattern is achromatic, invariant upon propagation, and depends solely on the sample correlation
3.2 Experimental observation of deep-Fresnel speckles
3.3 Fourier transforming the diffracted field at a close distance from the sample is equivalent to Fraunhofer diffraction
4 A new type of scattering experiment can be performed in the deep-Fresnel regime
4.1 The importance of the transmitted beam in deep Fresnel experiments
4.2 Heterodyne detection of the freely propagated field
4.3 Quantitative shadowgraphy
4.4 Near-field scattering
4.5 Probing dynamics in shadowgraphy and near-field scattering
5 Differential dynamic microscopy: Extracting scattering information with or without scattering
5.1 There is no need for scattering to extract scattering information in microscopy experiments
5.2 Connecting the dynamics of the 2D Fourier modes of the image intensity with the dynamics of the 3D modes of the sample generalized density
5.3 Differential dynamic microscopy and the image structure function
6 Conclusion
References
Chapter 23 Use of Scattering Techniques in Industry
Abstract
Keywords
Acknowledgments
1 The use of scattering techniques in industry from the university perspective
2 Preparation of polymer nanofoams studied by DLS, SANS, SAXS, SEM
2.1 Polymer nanoparticles of adjustable size and polydispersity and their packing
2.2 Addition of scCO2, continuity inversion, and expansion
3 Formation kinetics of water–oil microemulsions studied by TR-SANS
3.1 Phase behavior of w/o microemulsions and stopped-flow SANS setup
3.2 Analysis of TR-SANS data to reveal the mechanism of w/o-microemulsion formation
4 Approaches toward a wider use of scattering methods in industry
References
Chapter 24 Applications of Neutron Reflectometry to Soft Matter and Biological Systems
Abstract
Keywords
1 Introduction
2 Gas–liquid interfaces
2.1 Sample environment
2.2 Sample preparation methods
2.3 NR from surfactant monolayers
2.4 NR from lipid monolayers
2.5 NR from protein and polymer films
2.6 NR from nanoparticle layers
3 Solid–liquid interfaces
3.1 Sample environment
3.2 Sample preparation methods
3.3 Bio-membranes
3.4 NR from polymer layers at solid–liquid and solid–air interfaces
4 Liquid–liquid interfaces
4.1 Sample environment
4.2 Sample preparation
4.3 Lipid layers at an oil–water interface
5 Key considerations when preparing and analyzing NR measurements
5.1 Isotopic substitution and contrast variation
5.2 Bulk-like films
5.3 Determination of absolute z-position in contrast-match conditions
References
Chapter 25 Using Weak Aggregation for Solubilization and Separation
Abstract
Keywords
1 Context
2 The colloidal view of weak aggregation
2.1 Weak aggregation in water
2.2 Weak aggregation in other solvents
3 Phase diagrams
4 Characterizing weak aggregation via X-ray, neutron, and light scattering
4.1 Small-angle scattering
4.2 Overwhelming effect of critical fluctuations
4.3 The case of charged clusters
4.4 Weak aggregation as studied by light scattering
5 Weak aggregation in practical applications
5.1 Using weak aggregation in hydrometallurgy
5.2 Weak aggregation induced by a hydrotrope in quantitative lipid extraction
5.3 Mesoscale solubilization in ternary systems used for the analysis of traces
6 Conclusion
6.1 Key points to remember
References
Chapter 26 Quasi-Elastic Neutron Scattering Spectroscopy: Characterization of Relaxation Modes at the Molecular Scale
Abstract
Keywords
1 Principles of time-of-flight and backscattering-based quasi-elastic neutron scattering spectroscopy
1.1 The observable physics: Brief notes on diffusion
1.2 Principles of instrumentation
2 Quasi-elastic neutron spectroscopy as an experimental tool
2.1 Generalities
2.2 Most common models
2.3 The elastic incoherent structure factor confinement
2.4 Example QENS spectrum and practical approach to fitting
3 QENS scientific case and examples
3.1 Case study n.1: Ionic liquids
3.2 Case study n.2: Self- and collective dynamics in simple liquids
3.3 Case study n.3: Protein dynamics
4 Conclusion
References
List of Most Used Abbreviations
List of Most Used Variables
Index

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Health

Neutrons, X-rays, and Light

Scattering Methods Applied to Soft Condensed Matter

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Peter Lindner

Julian Oberdisse

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