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Thermal and Rheological Measurement Techniques for Nanomaterials Characterization

Thermal and Rheological Measurement Techniques for Nanomaterials Characterization

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Thermal and Rheological Measurement Techniques for Nanomaterials Characterization

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May 23, 2017


Thermal and Rheological Measurement Techniques for Nanomaterials Characterization, Second Edition covers thermal and rheological measurement techniques, including their principle working methods, sample preparation and interpretation of results.

This important reference is an ideal source for materials scientists and industrial engineers who are working with nanomaterials and need to know how to determine their properties and behaviors.

  • Outlines key characterization techniques to determine the thermal and rheological behavior of different nanomaterials
  • Explains how the thermal and rheological behavior of nanomaterials affect their usage
  • Provides a method-orientated approach that explains how to successfully use each technique
May 23, 2017

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Thermal and Rheological Measurement Techniques for Nanomaterials Characterization - Elsevier Science

Thermal and Rheological Measurement Techniques for Nanomaterials Characterization

Volume Three


Sabu Thomas

Raju Thomas

Ajesh K. Zachariah

Raghvendra Kumar Mishra

Table of Contents

Cover image

Title page


List of Contributors

Editor Biographies

Chapter 1. Instrumental Techniques for the Characterization of Nanoparticles

1.1. Nanotechnology and Nanomaterials

1.2. Classification of Nanomaterials

1.3. Advantages and Disadvantages of Nanomaterials

1.4. Opportunities Presented by Nanomaterials

1.5. Characterization Techniques of Nanomaterials

1.6. Conclusions

Chapter 2. Dynamic Light Scattering (DLS)

2.1. Introduction

2.2. Light Scattering Theory

2.3. Dynamic Light Scattering Basics

2.4. Depolarized Fabry–Pérot Interferometry

2.5. Conclusion

Chapter 3. Size-Exclusion Chromatography

3.1. Introduction

3.2. Instrumentation

3.3. Size-Exclusion Chromatographic Techniques

3.4. Applications of Size-Exclusion Chromatography

3.5. Drawbacks

Chapter 4. Thermogravimetric Analysis for Characterization of Nanomaterials

4.1. Introduction

4.2. Instrumental Setup for Thermogravimetric Analysis

4.3. Classification of Thermogravimetric Analysis

4.4. Thermogravimetry Curve

4.5. Advanced Thermogravimetric Analysis Instruments

4.6. Case Studies for Applications of Thermogravimetric Analysis

4.7. Conclusions

Chapter 5. Differential Scanning Calorimetry in Nanoscience and Nanotechnology

5.1. Introduction

5.2. Applications

5.3. Differential Scanning Calorimetry for Nanomaterials

5.4. Conclusion


Chapter 6. Dynamic Mechanical Thermal Analysis of Polymer Nanocomposites

6.1. Introduction

6.2. Thermoplastic Nanocomposites

6.3. Thermoset Nanocomposites

6.4. Elastomeric Nanocomposites

6.5. Effects of Nanofillers on the Dynamic Mechanical Properties of Polymer Blends

6.6. Theoretical Modeling of Dynamic Mechanical Properties

6.7. Conclusion

Chapter 7. Thermomechanical Analysis and Its Applications

7.1. Introduction

7.2. Instrumentation

7.3. Procedure

7.4. Applications of Thermomechanical Analysis

7.5. Comparison With Other Thermal Analysis Techniques

7.6. Conclusions

Chapter 8. Contact Angle Measurement Techniques for Nanomaterials

8.1. Introduction

8.2. Calculation of Surface Energy

8.3. Measurement of Contact Angle

8.4. Applications of Contact Angle Measurement

8.5. Conclusion

Chapter 9. Surface Area Analysis of Nanomaterials

9.1. Introduction

9.2. Theory Behind Adsorption and Desorption

9.3. Different Theories About Adsorption

9.4. Instrumentation of Surface Area Analyzer

9.5. The Brunauer–Emmett–Teller Adsorption

9.6. Applications

9.7. Conclusion

Chapter 10. Small-Angle Light and X-ray Scattering in Nanosciences and Nanotechnology

10.1. Introduction

10.2. Nature of Scattering

10.3. Small-Angle Scattering

10.4. Applications of Small-Angle Scattering

10.5. Conclusions




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List of Contributors

Jiji Abraham,     Mahatma Gandhi University, Kottayam, India

Elaheh Allahyari

Mahatma Gandhi University, Kottayam, India

Islamic Azad University, Tehran, Iran

Gudimamilla Apparao,     Acharya Nagarjuna University, Guntur, India

Jayesh Cherusseri,     Mahatma Gandhi University, Kottayam, India

Cintil Jose Chirayil,     Newman College, Thodupuzha, India

Soney C. George,     Amal Jyothi College of Engineering, Kottayam, India

Gurram Giridhar,     Acharya Nagarjuna University, Guntur, India

Jose James,     St. Joseph's College, Moolamattom, India

Karingamanna Jayanarayanan,     Amrita Vishwa Vidyapeetham, Amrita University, Coimbatore, India

Nandakumar Kalarikkal,     Mahatma Gandhi University, Kottayam, India

Obey Koshy,     Mahatma Gandhi University, Kottayam, India

Sravanthi Loganathan,     Mahatma Gandhi University, Kottayam, India

R.K.N.R. Manepalli,     The Hindu College, Machilipatnam, India

Raghvendra Kumar Mishra

Mahatma Gandhi University, Kottayam, India

Indian Institute of Space Science and Technology, Thiruvananthapuram, India

Oluwatobi S. Oluwafemi,     University of Johannesburg, Johannesburg, South Africa

G. Pugazhenthi,     Indian Institute of Technology Guwahati, Guwahati, India

Nanoth Rasana,     Amrita Vishwa Vidyapeetham, Amrita University, Coimbatore, India

El Hadji Mamour Sakho,     Mahatma Gandhi University, Kottayam, India

Ashin Shaji,     Mahatma Gandhi University, Kottayam, India

Lakshmanan Subramanian,     Amrita Vishwa Vidyapeetham, Amrita University, Kollam, India

Sabu Thomas,     Mahatma Gandhi University, Kottayam, India

Ravi Babu Valapa,     Centre for Biopolymer Science and Technology, A Unit of Central Institute of Plastics Engineering and Technology (CIPET), Kochi, India

Ajesh K. Zachariah,     Mar Thoma College, Tiruvalla, India

Editor Biographies

Professor (Dr.) Sabu Thomas is the Director of International and Interuniversity Center for Nanoscience and Nanotechnology, Mahatma Gandhi University, Kottayam, Kerala, India. He is also a full professor of Polymer Science and Engineering and School of Chemical Science of the same University. He is a fellow of many professional bodies. Professor Thomas has co-authored many papers in international peer-reviewed journals in the area of polymer processing. He has organized several international conferences. Professor Thomas's research group is in specialized areas of polymers, which includes polymer blends, fiber-filled polymer composites, particulate-filled polymer composites and their morphological characterization, aging, and degradation, pervaporation phenomena, sorption, and diffusion, interpenetrating polymer systems, recyclability and reuse of waste plastics and rubbers, elastomeric cross-linking, and dual porous nanocomposite scaffolds for tissue engineering. Professor Thomas's research group has extensive exchange programs with different industries, research, and academic institutions all over the world and is performing world-class collaborative research in various fields. The Professor's Center is equipped with various sophisticated instruments and has established state-of-the-art experimental facilities which cater to the needs of researchers within the country and abroad. He has more than 700 publications, 50 books, H Index-78 and 3 patents to his credit. He is a reviewer to many international journals. Professor Thomas has attained 5th Position in the list of Most Productive Researchers in India in 2008–16.

Professor (Dr.) Raju Thomas is currently Vice Chancellor of Middle East University FZE, Al Hamra, Ras Al Khaimah, United Arab Emirates. Dr. Thomas started his Professorship from the Research and Postgraduate Department of Chemistry, Mar Thoma College, Thiruvalla-3, Kerala, India. Dr. Thomas procured his PhD under the supervision of Professor (Dr.) Sabu Thomas, Director of International and Interuniversity Center for Nanoscience and Nanotechnology, Mahatma Gandhi University, Kottayam, Kerala, India. He has extensive research experience in Nanoscience and Nanotechnology. He has 12  years of research experience in the Organic Chemistry and Polymer Chemistry laboratories of the School of Chemical Sciences, Mahatma Gandhi University, Kottayam, Kerala, India. He has also worked in the laboratory of Applied Rheology and Polymer processing of Katholieke University, Leuven, Belgium, and in the laboratory at Leibniz Institute of Polymer Research, Dresden, Germany. He has widely studied the kinetics of curing, morphology development, and structural characteristics of in situ-cured nanocomposites based on epoxy resin and reactive rubbers. His research is reflected in his six published research articles in international journals, and additional articles which are currently under review. In addition, many articles have been published in popular journals. He has co-authored many chapters and is co-editor of a book entitled Micro and Nanostructured Epoxy/Rubber Blends which was recently published by Wiley and Sons. He has attended many national and international seminars/conferences and presented many research papers. He is an approved research guide in Chemistry at Mahatma Gandhi University, Kottayam, India and has availed projects from University Grants Commission (UGC), Department of Science and Technology–Science and Engineering Research Board (DST–SERB) and Kerala Science Council for Science, Technology, and Environment (KSCSTE).

Dr. Ajesh K. Zachariah is working as Assistant Professor in the Department of Chemistry, Mar Thoma College, Kerala, India. He has many publications in the field of materials chemistry, and polymer nanocomposites and has one national patent. He is an expert in sophisticated techniques such as Atomic Force Microscopy (AFM), X-ray diffraction Technique (XRD), Gas Permeability Tester, and Dynamic Mechanical Analyzer (DMA). He has many years' experience in the field of nanoscience and nanotechnology.

Raghvendra Kumar Mishra is currently working as Senior Research Fellow at the International and Interuniversity Center for Nanoscience and Nanotechnology, Mahatma Gandhi University, India. He has received India's most prestigious Visvesvaraya Research Fellowship, and he is currently serving as Visvesvaraya Fellow. He has widely studied the processing of blends, in situ generation micro- and nanofibrillar composites, electromagnetic shielding effect of nanocomposites, decorating and alignment of carbon nanotubes, and thermal, dynamic mechanical, and structural relationships in polymer blends and nanocomposites. He has won several awards from different organizations and technology events. He is serving as reviewer in many international journals, for example, Environmental Chemistry Letters (Springer). He has research experience in Mechanical Engineering, Materials Science and Technology, and Nanoscience and Nanotechnology. His areas of research are multidisciplinary, which include thermodynamics, heat transfer, refrigeration and air-conditioning, fluid mechanics, machine design, solid mechanics, machine theory, power plant engineering, metal and ceramic processing. In addition, he specializes in polymers, which include polymer recycling, polymer blends, fiber-filled polymer composites, particulate-filled polymer composites and their morphological characterization, aging and degradation, nanomaterials e.g., metallic, metallic oxide, carbon nanotubes, graphene, conducting polymer blends, composites and nanocomposites, biodegradable polymer blends and composites. He has expertise in sophisticated characterization techniques such as dynamic mechanical analyzer, differential scanning calorimetry, thermogravimetric analysis, spectroscopy, vector network analyzer, scanning electron microcopy, and atomic force microscopy (AFM).

Chapter 1

Instrumental Techniques for the Characterization of Nanoparticles

Cintil Jose Chirayil¹, Jiji Abraham², Raghvendra Kumar Mishra², Soney C. George³, and Sabu Thomas²     ¹Newman College, Thodupuzha, India     ²Mahatma Gandhi University, Kottayam, India     ³Amal Jyothi College of Engineering, Kottayam, India


Advances in nanomaterials have opened a new era in various fields such as industrial, medical, commercial, and consumer products owing to their unique and novel physical and chemical properties. A wide variety of techniques can be used to analyze and characterize nanoparticles depending on the application of interest. Characterization refers to the study of material features such as composition, structure, and various properties such as physical, chemical, electrical, magnetic, etc. This chapter summarizes the techniques that are commonly used to investigate the size, shape, surface properties, composition, purity, and stability of nanomaterials, along with their benefits and drawbacks. Various characterization techniques such as optical (imaging), electron probe, photon probe, ion particle probe, and thermodynamic techniques are discussed briefly in this chapter.


Electron probe characterization techniques; Ion particle; Nanomaterials; Optical (imaging); Photon probe characterization techniques; Probe characterization techniques; Thermodynamic characterization techniques

Chapter Outline

1.1 Nanotechnology and Nanomaterials

1.2 Classification of Nanomaterials

1.3 Advantages and Disadvantages of Nanomaterials

1.4 Opportunities Presented by Nanomaterials

1.5 Characterization Techniques of Nanomaterials

1.5.1 Optical (Imaging) Characterization Techniques Confocal Laser-Scanning Microscopy Scanning Near-Field Optical Microscopy Two-Photon Fluorescence Microscopy Dynamic Light Scattering Brewster Angle Microscopy

1.5.2 Electron Probe Characterization Techniques Scanning Probe Electron Microscopy Electron Probe Microanalysis Transmission Electron Microscopy Scanning Transmission Electron Microscopy

1.5.3 Photon Probe Characterization Techniques Photoelectron Spectroscopy UV–Visible Spectroscopy Atomic Absorption Spectroscopy Inductively Coupled Plasma Spectroscopy Fluorescence Spectroscopy Localized Surface Plasmon Resonance

1.5.4 Ion Particle Probe Characterization Techniques Rutherford Backscattering Small-Angle Scattering Nuclear Reaction Analysis Raman Spectroscopy X-Ray Diffraction Cathodoluminescence Nuclear Magnetic Resonance Spectroscopy Matrix-Assisted Laser Desorption/Ionization Time-of-Flight Mass Spectrometry

1.5.5 Thermodynamic Characterization Techniques Thermogravimetric Analysis Differential Thermal Analysis Evolved Gas Analysis Differential Scanning Calorimetry Nanocalorimetry Brunauer–Emmett–Teller Method

1.5.6 Other Important Techniques Nanoparticle Tracking Analysis Tilted Laser Microscopy Turbidimetry Field-Flow Fractionation Size-Exclusion Chromatography Hydrophobic Interaction Chromatography ζ Potential Measurements

1.6 Conclusions



1.1. Nanotechnology and Nanomaterials

Nanotechnology is the art and science of handling matter at the nanoscale (down to 1/10,000,000 the width of a human hair) to create new and unique materials and products with properties that differ significantly from those on a larger scale [1]. Early developments in nanotechnology were initiated by Nobel Laureate Richard Feynman, who introduced the idea of molecular machines in 1959. The importance of nanotechnology comes from the tunability of material properties by assembling such materials at the nanoscale level. Norio Taniguchi's 1974 paper is the first scientific publication in which the term nanotechnology was used [2]. Now nanotechnology can be identified as the driving force behind the industrial revolution. Owing to its enormous potential to change society, both public and private sectors are spending a lot of money on this new technology. At the same time, scientists have anxieties about the adverse effects of the basic building blocks of nanotechnologies—particles smaller than one-billionth of a meter—on health and the environment. By using nanotechnology we can design, characterize, produce, and apply nanostructures, nanodevices, and nanosystems by controlling shape and size at the nanometer scale. A nanometer is one-billionth of a meter. The difference in the properties of materials at nanoscale compared to bulk is due to two main reasons. First is the increased chemical reactivity of nanomaterials due to their large surface area compared to bulk. The second is the quantum confinement effect. A nanomaterial is an object that has at least one dimension on the nanometer scale (approximately 1–100  nm). There are several ways to classify nanomaterials based on their origin, dimensions, and structural configuration.

1.2. Classification of Nanomaterials

According to their origin nanomaterials are classified as follows:

1. Natural nanomaterials

    Natural nanomaterials belong to the natural nanoworld and originate from animals or minerals without any human modification or processing. Some important examples of natural nanomaterials include inorganic natural nanomaterials (minerals, clays, etc.), natural carbon nanoparticles (diamond and graphite), nanoparticles from space, nanomaterials from the animal and plant kingdoms (cotton, collagen, bacterial fibers, exoskeleton, and endoskeleton), and nanomaterials in insects (chitin, sponge fibers) [3].

2. Artificial nanomaterials

    These are fabricated by experimental and well-defined mechanical and fabrication processes. Examples include carbon nanotubes, graphene, metal oxides, quantum dots, etc.

According to their number of dimensions, which are not confined to the nanoscale range (<100  nm), nanomaterials are classified as follows:

▪ Zero-dimensional

    For this kind of material all the dimensions measured are within the nanosize range. The most common demonstration of zero-dimensional nanomaterials is nanoparticles. They are amorphous or crystalline, single crystalline or polycrystalline; composed of single or multiple chemical elements; exist individually or incorporated in a matrix; exhibit various shapes and forms; and can be metallic, ceramic, or polymeric.

▪ One-dimensional

    For these materials one dimension is outside the nanoscale, which leads to needle-like-shaped nanomaterials. One-dimensional materials include nanotubes, nanorods, and nanowires.

▪ Two-dimensional

    Two of the dimensions are not confined to the nanoscale in two-dimensional materials and they exhibit a plate-like geometry. Two-dimensional nanomaterials include nanofilms, nanolayers, and nanocoatings. Thickness is in the nanometer range.

▪ Three-dimensional

    Bulk nanomaterials are materials that are not confined to the nanoscale in any dimension. These materials are thus characterized by having three arbitrary dimensions above 100  nm. Three-dimensional nanomaterials can contain dispersions of nanoparticles, bundles of nanowires, and nanotubes as well as multiple nanolayers.

According to their structural configuration nanomaterials can be classified into four types:

1. Carbon-Based Nanomaterials

    Carbon-based materials have captured broad interest in the materials science community for decades because of the versatility and extremely low weight of carbon. Examples include carbon nanotubes, graphene, fullerenes, etc. [4].

2. Metal-Based Materials

    The main component of these materials is metal. Examples include nanoplatinum, nanogold, nanosilver, metal oxides, quantum dots, etc. [5].

3. Dendrimers

    Dendrimers are nanosized, radially symmetric molecules with a well-defined, homogeneous, and monodispersed structure that has a typically symmetric core, an inner shell, and an outer shell [6].

4. Composites

    Nanocomposites are multiphase solid materials in which at least one phase is in the nano range. Composites are of three types, namely, ceramic matrix nanocomposite, metal matrix nanocomposite, and polymer matrix nanocomposite.

1.3. Advantages and Disadvantages of Nanomaterials

▪ Advantages

▪ small size

▪ high surface area

▪ easy to suspend in liquids

▪ deep access to cells

▪ tunable/tailorable physical, chemical, and mechanical properties due to extremely small size (1–100  nm)

▪ high strength, toughness, and ductility

▪ reduced energy costs

▪ enhanced activity (extremely large specific surface area), surface-dependent material properties

▪ Challenges

▪ The main challenges are to develop instruments to assess exposure to engineered nanomaterials in the air and water.

▪ The second challenge is to develop and validate methods to evaluate the toxicity of engineered nanomaterials by 2020–2030.

▪ The last challenge is to develop tools to properly assess risks to human health and to the environment.

1.4. Opportunities Presented by Nanomaterials

Now, nanotechnology is described as a revolutionary discipline because of its possible impression on industrial applications. Through the use of emerging nano techniques, nanotechnology can offer possible remedies to many problems. Because nanotechnology is an interdisciplinary area there are many research fields and several potential applications that involve nanotechnology. Because nanomaterials possess unique, beneficial physical, chemical, and mechanical properties, they can be used for a wide variety of applications. Fig. 1.1 shows some key applications of nanomaterials.

1.5. Characterization Techniques of Nanomaterials

Nanomaterials commonly consist of at least two of the following units: metallic, semiconducting, and organic particles or molecules. Additionally, nanomaterials are generally coated with polymers or biorecognition molecules to improve biocompatibility and selective targeting of biologic molecules. A common feature of all nanomaterials is their large ratio of surface area to volume, which may be orders of magnitude greater than that of macroscopic materials. Still, the final size and structure of nanomaterials depend on the salt and surfactant additives, reactant concentrations, reaction temperatures, and solvent conditions used during their synthesis. Thus, the comprehension of these physicochemical properties as well as the fundamentals of the associated measuring methods is necessary before characterizing nanomaterials and developing reproducible synthesis procedures to optimize the medical application of nanomaterials.

Figure 1.1  Potential applications of nanomaterials.

Characterization refers to the study of a material's features such as its composition, structure, and various properties such as physical, chemical, electrical, magnetic, etc. There are plenty of techniques available on the market that were initially used for colloidal particles (e.g., microscopy, spectroscopy, and magnetic resonance), but each of these techniques has a certain degree of uncertainty. Particle size distribution (PSD) plays a fundamental role in controlling the properties of different nanomaterials. For example, the chemical reactivity of nanomaterials, which mostly differs from that of macroscale or microscale materials, is usually affected by the nanoparticle (NP) surface/volume ratio. Particle size also determines NP diffusivity and the ability of NPs to permeate cell membranes. PSD analysis thus allows monitoring of NP aggregation or release of NP-surface modifiers. There are plenty of techniques available in the literature covering specific ranges of NP size distribution, as shown in Fig. 1.2 [7].

1.5.1. Optical (Imaging) Characterization Techniques Confocal Laser-Scanning Microscopy

Confocal microscopy, most frequently confocal laser scanning microscopy (CLSM), is a powerful technique to produce sharp images of a sample that would otherwise appear blurred when viewed under a conventional microscope. Reconstruction of three-dimensional structures from images obtained by this technique is possible by taking a large number of images at different depths (a process known as optical sectioning) within a thick object. Scanning by one or more focused beams of light, usually from a laser or arc-discharge source, across the specimen is used to obtain images by confocal microscopy. An objective lens is used to focus the light beam on the specimen and then the object is scanned using some form of scanning device under computer control. The sequences of points of light from the specimen are detected by a photomultiplier tube (PMT) and the output from the PMT is built into an image and displayed by the computer [8].

Figure 1.2  Performance of various particle size measurement techniques (note: only a few techniques can measure particles in the nanoscale region) [7] . AFM , atomic force microscopy; NP , nanoparticle; SEM , scanning electron microscopy; TEM , transmission electron microscopy.

▪ Advantages

▪ The ability to serially produce thin (0.5–1.5  μm) optical sections through fluorescent specimens that have a thickness ranging up to 50  μm or more

▪ The ability to control depth of field

▪ The ability to isolate and collect a plane of focus from the sample, thus eliminating the out-of-focus haze normally seen with a fluorescent sample

▪ Elimination or reduction of background information away from the focal plane

▪ The ability to compensate for autofluorescence

▪ Minimum specimen preparation and instrument reconfiguration

▪ Disadvantage

▪ A disadvantage of CLSM is colocalization of fluorophores in the confocal microscope—two or more fluorescence emission signals can often overlap in digital images recorded by confocal microscopy because of their close proximity within the specimen

▪ Applications

▪ This technique has gained popularity in the scientific and industrial communities and typical applications are in life sciences, semiconductor inspection, and materials science. It is widely used in numerous biological science disciplines, from cell biology and genetics to microbiology and developmental biology. It is also used in quantum optics and nanocrystal imaging and spectroscopy [9]. Scanning Near-Field Optical Microscopy

Scanning near-field optical microscopy (SNOM) gives simultaneous measurements of topography and optical properties (fluorescence) and provides a direct correlation between surface nano features and optical/electronic properties. SNOM is based on scanning with an arbitrarily small aperture, which is illuminated from the back side at a close but constant distance, across a sample surface and recording optical information pixel by pixel, collecting transmitted, reflected, or fluorescent light to form an image. In SNOM, the excitation laser light is focused through an aperture with a diameter smaller than the excitation wavelength, resulting in an evanescent field (or near field) on the far side of the aperture. When the sample is scanned at a small distance below the aperture, the optical resolution of transmitted or reflected light is limited only by the diameter of the aperture. The optical resolution attainable is in the range of 60–100  nm. The optical image is generated by scanning the sample's surface point by point and line by line. A standard SNOM setup is shown in Fig. 1.3 [10].

▪ Advantages

▪ High resolution (up to 25  nm)

▪ Analysis of various properties made possible through contrast

▪ No special sample preparation needed

▪ Can be used for different kinds of samples (conductive, nonconductive, and transparent)

Figure 1.3  Standard scanning near-field optical microscopy setup consisting of (A) an illumination unit, (B) a collection and redistribution unit, and (C) a detection module [10] .

▪ Disadvantages

▪ Very low working distance and extremely shallow depth of field

▪ Limited to study of surfaces

▪ Not conducive to studying soft materials, especially under shear-force mode

▪ Long scan times for large sample areas or high-resolution imaging

▪ Applications

    This technique can be ideally suited to quickly and effortlessly imaging the optical properties of a sample with resolution below the diffraction limit. It can be used in various fields such as nanotechnology research, nanophotonics and nanooptics, life sciences, and materials research—for optical detection of the

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