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- Herausgeber: John Wiley & Sons
- Kategorie: Wissenschaft und neue Technologien
- Sprache: Englisch
Nanomaterial Characterization
Providing various properties of nanomaterials and the various methods available for their characterization
Over the course of the last few decades, research activity on nanomaterials has gained considerable press coverage. The use of nanomaterials has meant that consumer products can be made lighter, stronger, esthetically more pleasing, and less expensive. The significant role of nanomaterials in improving the quality of life is clear, resulting in faster computers, cleaner energy production, target-driven pharmaceuticals, and better construction materials. It is not surprising, therefore, that nanomaterial research has really taken off, spanning across different scientific disciplines from material science to nanotoxicology. A critical part of any nanomaterial research, however, is the need to characterize physicochemical properties of the nanomaterials, which is not a trivial matter.
Nanomaterial Characterization: An Introduction is dedicated to understanding the key physicochemical properties and their characterization methods. Each chapter begins by giving an overview of the topic before a case study is presented. The purpose of the case study is to demonstrate how the reader may make use of the background information presented to them and show how this can be translated to solve a nanospecific application scenario. Thus, it will be useful for researchers in helping them design experimental investigations. The book begins with a general overview of the subject, thus giving the reader a solid foundation to nanomaterial characterization.
Nanomaterial Characterization: An Introduction features:
- Nanomaterial synthesis and reference nananomaterials
- Key physicochemical properties and their measurements including particle size distribution by number, solubility, surface area, surface chemistry, mechanical/tribological properties, and dustiness
- Scanning tunneling microscopy methods operated under extreme conditions
- Novel strategy for biological characterization of nanomaterial methods
- Methods to handle and visualize multidimensional nanomaterial characterization data
The book is written in such a way that both students and experts in other fields of science will find the information useful, whether they are in academia, industry, or regulation, or those whose analytical background may be limited.There is also an extensive list of references associated with every chapter to encourage further reading.
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Veröffentlichungsjahr: 2016
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TABLE OF CONTENTS
TITLE PAGE
COPYRIGHT
DEDICATION
LIST OF CONTRIBUTORS
EDITOR'S PREFACE
CHAPTER 1: INTRODUCTION
1.1 OVERVIEW
1.2 PROPERTIES UNIQUE TO NANOMATERIALS
1.3 TERMINOLOGY
1.4 MEASUREMENT OF GOOD PRACTICE
1.5 TYPICAL METHODS
1.6 POTENTIAL ERRORS DUE TO CHOSEN METHODS
1.7 SUMMARY
ACKNOWLEDGMENTS
REFERENCES
CHAPTER 2: NANOMATERIAL SYNTHESES
2.1 INTRODUCTION
2.2 BOTTOM–UP APPROACH
2.3 Synthesis: Top–Down Approach
2.4 BOTTOM–UP AND TOP–DOWN: LITHOGRAPHY
2.5 BOTTOM–UP OR TOP–DOWN? CASE EXAMPLE: CARBON NANOTUBES (CNTs)
2.6 PARTICLE GROWTH: THEORETICAL CONSIDERATIONS
2.7 CASE STUDY: MICROREACTOR FOR THE SYNTHESIS OF GOLD NANOPARTICLES
2.8 SUMMARY
ACKNOWLEDGMENTS
REFERENCES
CHAPTER 3: REFERENCE NANOMATERIALS
3.1 DEFINITION, DEVELOPMENT, AND APPLICATION FIELDS
3.2 CASE STUDIES
3.3 SUMMARY
ACKNOWLEDGMENTS
REFERENCES
CHAPTER 4: PARTICLE NUMBER SIZE DISTRIBUTION
4.1 INTRODUCTION
4.2 MEASURING METHODS
4.3 SUMMARY OF CAPABILITIES OF THE COUNTING TECHNIQUES
4.4 EXPERIMENTAL CASE STUDY
4.5 SUMMARY
REFERENCES
CHAPTER 5: SOLUBILITY PART 1: OVERVIEW
5.1 INTRODUCTION
5.2 SEPARATION METHODS
5.3 QUANTIFICATION METHODS: FREE IONS (AND LABILE FRACTIONS)
5.4 QUANTIFICATION METHODS TO MEASURE TOTAL DISSOLVED SPECIES
5.5 THEORETICAL MODELING USING SPECIATION SOFTWARE
5.6 WHICH METHOD?
5.7 CASE STUDY: MINIATURIZED CAPILLARY ELECTROPHORESIS WITH CONDUCTIVITY DETECTION TO DETERMINE NANOMATERIAL SOLUBILITY
5.8 SUMMARY
ACKNOWLEDGMENTS
REFERENCES
CHAPTER 6: SOLUBILITY PART 2: COLORIMETRY
6.1 INTRODUCTION
6.2 MATERIALS AND METHOD
6.3 RESULTS AND INTERPRETATION
6.4 CONCLUSION
ACKNOWLEDGMENTS
A6.1 MATERIALS AND METHOD
A6.6 RESULTS AND INTERPRETATION
REFERENCES
CHAPTER 7: SURFACE AREA
7.1 INTRODUCTION
7.2 MEASUREMENT METHODS: OVERVIEW
7.3 CASE STUDY: EVALUATING POWDER HOMOGENEITY USING NMR VERSUS BET
7.4 SUMMARY
ACKNOWLEDGMENTS
REFERENCES
CHAPTER 8: SURFACE CHEMISTRY
8.1 INTRODUCTION
8.2 MEASUREMENT CHALLENGES
8.3 ANALYTICAL TECHNIQUES
8.4 CASE STUDIES
8.5 SUMMARY
REFERENCES
CHAPTER 9: MECHANICAL, TRIBOLOGICAL PROPERTIES, AND SURFACE CHARACTERISTICS OF NANOTEXTURED SURFACES
9.1 INTRODUCTION
9.2 FABRICATING NANOTEXTURED SURFACES
9.3 MECHANICAL PROPERTY CHARACTERIZATION
9.4 CASE STUDY: NANOSCRATCH TESTS TO CHARACTERIZE MECHANICAL STABILITY OF PS/PMMA SURFACES
9.5 CASE STUDY: STRUCTURAL INTEGRITY OF MULTIWALLED CNT FOREST
9.6 CASE STUDY: MECHANICAL CHARACTERIZATION OF PLASMA-TREATED POLYLACTIC ACID (PLA) FOR PACKAGING APPLICATIONS
9.7 CONCLUSIONS
ACKNOWLEDGMENTS
REFERENCES
CHAPTER 10: METHODS FOR TESTING DUSTINESS
10.1 INTRODUCTION
10.2 CEN TEST METHODS (UNDER CONSIDERATION)
10.3 CASE STUDIES: APPLICATION OF DUSTINESS DATA
10.4 SUMMARY
ACKNOWLEDGMENTS
REFERENCES
CHAPTER 11: SCANNING TUNNELING MICROSCOPY AND SPECTROSCOPY FOR NANOFUNCTIONALITY CHARACTERIZATION
11.1 INTRODUCTION
11.2 EXTREME FIELD STM: A BRIEF HISTORY
11.3 STM/STS FOR THE EXTRACTION OF SURFACE LOCAL DENSITY OF STATES (LDOS): THEORETICAL BACKGROUND
11.4 SCANNING TUNNELING SPECTROSCOPY (STS) AT LOW TEMPERATURES: BACKGROUND
11.5 STM INSTRUMENTATION AT EXTREME CONDITIONS: SPECIFICATION REQUIREMENTS AND DESIGN
11.6 STM/STS IMAGING UNDER EXTREME ENVIRONMENTS: A REVIEW ON APPLICATIONS
11.7 SUMMARY AND FUTURE OUTLOOK
ACKNOWLEDGMENTS
REFERENCES
CHAPTER 12: BIOLOGICAL CHARACTERIZATION OF NANOMATERIALS
12.1 INTRODUCTION
12.2 MEASUREMENT METHODS
12.3 EXPERIMENTAL CASE STUDY
12.4 SUMMARY
ACKNOWLEDGMENTS
REFERENCES
CHAPTER 13: VISUALIZATION OF MULTIDIMENSIONAL DATA FOR NANOMATERIAL CHARACTERIZATION
13.1 INTRODUCTION
13.2 CASE STUDY: STRUCTURE–ACTIVITY RELATIONSHIP (SAR) ANALYSIS OF NANOPARTICLE TOXICITY
13.3 SUMMARY
REFERENCES
INDEX
END USER LICENSE AGREEMENT
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Guide
Table of Contents
Preface
Begin Reading
List of Illustrations
CHAPTER 1: INTRODUCTION
Figure 1.1 Schematic illustration of the process in standards development, publication, and uptake.
CHAPTER 2: NANOMATERIAL SYNTHESES
Figure 2.1 Schematic of common apparatus used in the arc-discharge synthesis of carbon nanotubes.
Figure 2.2 Illustration of microemulsion synthesis. Aqueous precursors (A and B) are encapsulated in nanomicelles, which collide and coalesce, mixing the precursors and leading to the formation of nanoparticles.
Figure 2.3 An example of a complex structure with nanoscale features generated by lithography using a focused ion beam (FIB) and assembled using nanomanipulation, showing the possibilities of this technique.
Figure 2.4 Change in free energy plotted against particle radius. The maximum value of corresponds to the critical radius of a cluster of atoms, .
Figure 2.5 Schematic microreactor set-up under different synthesis strategies: (a) continuous flow, (b) microdroplet.
Figure 2.6 Typical DLS particle size distributions and the corresponding
Z
-average particle diameter of gold nanoparticles of six samples, as prepared by: traditional batch, microfluidic continuous flow, and microfluidic microdroplet flow. Each data point in the plot is the average of triplicate measurements; error bars represent the SD of those measurements.
Figure 2.7 Polydispersity index from DLS measurements of six samples. Results compare the different types of nanoparticle synthesis methods of traditional batch, microfluidic continuous flow, and microfluidic microdroplet flow synthesis. Each data point in the plot is the average of triplicate measurements; error bars represent the SD of those measurements.
Figure 2.8 Mean RSD % of
Z
-average and PDI values for six samples, when nanoparticles are synthesized with (a) batch, (b) microreactor continuous flow, and (c) microreactor microdroplet.
CHAPTER 3: REFERENCE NANOMATERIALS
Figure 3.1 Determination of film thickness for SiO
2
on Si-wafer referring to (100) lattice spacing of Si (Unpublished work, see acknowledgements).
Figure 3.2 (a) Specimens and methods used in MechProNO [27] for the determination of mechanical properties of nanosized features. European Metrology Research Programme [27]. Reproduced with permission of European Metrology Research Programme. (b) Transmission electron micrograph showing silica nanoparticles embedded homogeneously in epoxy matrix. Thin foil prepared by ultramicrotomy of EP + 5% SiO
2
nanocomposite.
Figure 3.3 Illustration of other characteristics of nanoparticles (protein corona, agglomeration), which may influence nanoparticle toxicity.
CHAPTER 4: PARTICLE NUMBER SIZE DISTRIBUTION
Figure 4.1 Schematic representation of the PTA (NTA) principle. Carr and Wright [18], Figure 4.1. Reproduced with permission of Wiley.
Figure 4.2 Schematic illustration of the Coulter counter (a) and TRPS principle (b), adapted from [23].
Figure 4.3 Schematic illustration of the ICP-MS principle.
Figure 4.4 Schematic illustration of TEM (a) and SEM (b) principles.
Figure 4.5 Schematic illustration of AFM principle.
Figure 4.6 Representative TEM images of crude (a and b) and precleaned (c) coffee creamer suspension with corresponding number-based size distribution histogram (d) and EDX spectra (e).
CHAPTER 5: SOLUBILITY PART 1: OVERVIEW
Figure 5.1 CE-conductivity microchip analysis.
Figure 5.2 ZnO dissolution study showing the feasibility of the CE-conductivity device to detect free zinc from a dispersion of nano-ZnO in fish medium.
CHAPTER 6: SOLUBILITY PART 2: COLORIMETRY
Figure 6.1 UV–Vis absorption spectra of 5-Bromo PAPS when (a) in deionized water, (b) digestive blank media, and (c) extracted supernatant after 2.56 mg/ml of ZnO (NM 110) has been dispersed and exposed to the digestion protocol.
Figure 6.2 [Zn
2+
] concentration calibration plot using 5-Bromo-PAPS (
λ
max
= abs peak at 556 nm). Each data point is the mean of triplicate measurements; note that the standard deviation is too small to be visible.
Figure 6.3 Estimated [Zn
2+
] as a function of ZnO (NM 110) particle concentration. The [Zn
2+
] reported arises from the dissolution of ZnO (NM 110) particle concentration as a result of digestive juice experiment.
Figure 6.4 SEM images showing ZnO (NM 110) nanomaterials after dispersion using NanoGenotox protocol. Three different images were acquired, taken at different magnifications, showing (a) the presence of particle agglomerates, (b) size of the smallest agglomerates, and (c) polydispersity in primary particle size.
Figure 6.5 SEM images showing ZnO (NM 110) nanomaterial (a) after saliva addition. Results also show (b) the corresponding digestive blank after saliva addition.
Figure 6.6 SEM images showing ZnO (NM 110) nanomaterial at the end of digestion (a). Results also show the corresponding digestive blank (b) at the end of the digestion protocol.
Figure A6.1 Plot of amplitude versus acoustic power to establish the performance of the ultrasonic probe.
CHAPTER 7: SURFACE AREA
Figure 7.1 Illustration of common surface features (internal, external, and total surface area) of a particle.
Figure 7.2 Plot of specific surface area values of NM 110. A comparison between BET and NMR; the values plotted are the mean of three replicates (±1 SD).
CHAPTER 8: SURFACE CHEMISTRY
Figure 8.1 Illustrative overview of spatial resolution and types of information that can be obtained by a range of tools important for nanoanalysis, including AES, AFM, desorption electrospray ionization (DESI), dynamic SIMS (dSIMS), electron probe microanalysis (EPMA), gentle SIMS (G-SIMS), low-energy ion scattering (LEIS), micro thermal analysis (μTA), scanning near-field optical microscopy (SNOM), STM, static SIMS (sSIMS), tip-enhanced Raman spectroscopy (TERS), transmission electron microscopy (TEM), parallel electron energy-loss spectrometry (PEELS), and XPS. The diagram also shows the techniques for bulk analysis of materials of electron ionization (EI), electrospray and inductively coupled plasma (ICP) mass spectrometry (MS) [44].
Figure 8.2 XPS Survey (a, c, and e) and C 1s narrow spectra (b, d, and f) of 40 nm gold nanoparticles coated with citrate (a and b), BSA (c and d) and IgG molecules (e and f), deposited on PTFE-wrapped silicon wafer.
Figure 8.3 Average number of (a) IgG and (b) BSA molecules,
N
, plotted against nanoparticle diameter (calculated from Eq. (8.7) (XPS) and Eq. (8.8) (opt)). Data show excellent agreement of
N
values independently estimated from a combination of DLS and LSPR shift measurements and XPS measurements.
Figure 8.4 Assessment of sample preparation protocol for TOF-SIMS analysis performed on sample E (ZnO nanomaterial). (a) TOF-SIMS spectrum of the sample.(b) Enlargement of the spectrum showing the
69
Zn
+
peak. The spectrum exhibits a satellite peak shifted 0.045 mass units from the Zn
+
peak. (c) Total ion image of the analyzed sample surface. The dark areas refer to regions of the sample where little signal was detected. (d) Region-of-interest TOF-SIMS spectra regenerated from two areas of the image that are shown in the inset. This shows that the higher intensity peak originates from the central area of the sample, and the shifted peak originates from the bright area surrounded by dark circular regions on the left. Similar features are observed in other samples, and it is concluded that this is a typical artifact due to sample topography.
Figure 8.5 Normalized secondary ion emission of (a and b) CeO
2
and (c and d) ZnO nanopowders. The emission is normalized to the Ce
+
and Zn
+
peaks, respectively (Bi
+
beam was operated at 25 kV).
CHAPTER 9: MECHANICAL, TRIBOLOGICAL PROPERTIES, AND SURFACE CHARACTERISTICS OF NANOTEXTURED SURFACES
Figure 9.1 SEM image of 4 min nanotextured COP surface. A higher magnification (×20,000) image is given as inset.
Figure 9.2 SEM images of micro–nanotextured, water-immersed and dried PEEK (a) and PMMA (b) surfaces after perfluorosilane modification in cyclohexane (70° tilted). Curved microhills (re-entrant-like structures) are produced after etching and grafting of the polymeric surfaces.
Figure 9.3 SEM images of 10 min SF6 plasma-nanotextured PDMS surfaces before silanization and (as inset) after silanization.
Figure 9.4 SEM images of PMMA surfaces (60° tilted) displaying the hierarchical, hexagonally ordered packed pillars obtained upon plasma etching using 1 µm (left) and 3 µm polystyrene particles (right).
Figure 9.5 SEM image of CNT carpet consisting of well-aligned carbon nanotubes.
Figure 9.6 Representative (a) load versus time curve and (b) depth-displacement versus time curve during the load-control experiment.
Figure 9.7 Typical load–depth displacement curve from a nanoindentation experiment.
Figure 9.8 (a) Representative scheme of scratch segments and (b) scratch load protocol (with increasing load).
Figure 9.9 Scratch and postscratch load protocol: (1) preload, (2) constant load stage (for various maximum loads 10–100 μN), and (3) unloading.
Figure 9.10 Coefficient of friction (CoF) as a function of scratch path: (a) for uncoated and (b) perfluorodecyltrichlorosilane (FDTS)-coated 1 µm PS/PMMA samples.
Figure 9.11 SPM images of the CNT forest (a) in 3D, and (b) from top view (5 µm × 5 µm), where the edges of CNT forest surface are observed.
Figure 9.12 Representative load–displacement data from a loading–unloading cycle: (a) full cycle and (b) loading part).
Figure 9.13 (a) Input function of CNT forest nanoindentation experiment, following repeating loading cycles and (b) representative load–unload curves.
Figure 9.14 AFM imaging (30 × 30 µm
2
) of plasma-treated PLA surface.
Figure 9.15 Schematic trapezoidal of load–time function for nanoindentation experiment.
Figure 9.16 Hardness versus displacement for oxygen plasma-etched PLA, with displacement scale ranging between (a) 0 and 1000 nm (b) 0 and 100 nm.
Figure 9.17 Elastic modulus versus displacement for oxygen plasma-etched PLA, with displacement scale ranging between (a) 0 and 1000 nm (b) 0 and 100 nm.
Figure 9.18 Hardness versus etching time for oxygen-plasma etched PLA, at ∼100 nm of displacement.
Figure 9.19 Hardness to modulus ratio for oxygen plasma-etched PLA.
CHAPTER 10: METHODS FOR TESTING DUSTINESS
Figure 10.1 Standardized particle size-selective criteria (inhalable, thoracic, and respirable) for health-related aerosol sampling according to the EN 481 (1994) and ISO 7708 (1995) standards, and the total aerosol deposition curve in the human respiratory tract according to the ICRP model [9]. Calculations assume a spherical particle of density
ρ
= 1 g/cm
3
and a standard worker according to the ICRP [9].
Figure 10.2 Principle sketch and photograph of the EN 15051 standard rotating drum with a modified sampling train. In the illustration given here, real-time size-distribution measurements were acquired using a Differential Mobility Particle Sizer (DMPS) and an Aerodynamic Particle Sizer (APS). Previously, an Electrical Low-Pressure Impactor (ELPI) has also been used to acquire real-time size-distribution measurements in a similar setup. The inset photograph shows a commercial version of the EN 15051 rotating drum.
Figure 10.3 Principle sketch and photograph of the EN 15051 continuous drop method. In this illustration, real-time size-distribution measurements using a Scanning Mobility Mobility Particle Sizer and an Aerodynamic Particle Sizer, are shown. The inset photograph shows a version of the EN 15051 continuous drop method.
Figure 10.4
Figure 10.5 Particle size-distributions of five TiO
2
samples acquired from the OECD Working Party on Manufactured Nanomaterials test programme. The FMPS and APS particle size ranges are given in terms of electrical mobility and aerodynamic particle sizes, respectively.
Figure 10.6 The two experimental configurations used in the vortex shaker method according to Witschger et al. [32]: (a) for measuring respirable number concentration and its corresponding particle size-distribution, and for collecting airborne particles for subsequent electron microscopy observations; (b) for collecting respirable mass fraction of the emitted aerosol.
Figure 10.7 Respirable mass and number dustiness
indexes
of 15 NMs from the JRC nanomaterial repository tested with the VS method (data from Witschger et al. [32]).
Figure 10.8 Scatter-plot of respirable dustiness data generated by the RD (left
y
-axis) and VS (right
Y
-axis) plotted against the respirable dustiness data generated by the SRD. The black line shows the 1:1 relationship for the RD and SRD data, while the gray line shows the 1:1 relationship between the VS and SRD data.
CHAPTER 11: SCANNING TUNNELING MICROSCOPY AND SPECTROSCOPY FOR NANOFUNCTIONALITY CHARACTERIZATION
Figure 11.1 Schematic representation of STM nanoscale characterization under extreme environments for novel nanofunctionality research.
Figure 11.2 Schematic representation of geometry of STM tip in Tersoff–Hamann model. Tip apex with distance
d
from sample surface is assumed to have a hemispherical shape with a curvature radius
R
.
Figure 11.3 Dependence of convolution function on temperature obtained by convoluting FDDF with itself.
Figure 11.4 Schematic view of UHV-LT-HMF STM based on single-shot
3
He refrigeration system. Load-lock and preparation chambers are not shown
Figure 11.5 Atomic-resolution STM images taken by UHV-LT-HMF STM using
3
He refrigeration. (a) Constant current STM image of reconstructed Si(001) surface at 670 mK, exhibiting single phase of c(4×2) reconstruction. (b) Constant current STM image of highly oriented pyrolytic graphite (0001) surface at 500 mK and 5 T.
Figure 11.6 (a) Atomic resolution imaging of Au(111) 22 × √3 surface at 650 mK using VLT-UHV STM with
3
He refrigeration system. (b) Schematic representation of cross-sectional profile of reconstruction.
Figure 11.7 Constant-current STM images and simultaneously obtained
dI/dV
images of reconstructed Au(111) surface at very low temperatures and under different perpendicular magnetic fields. (a)
T
= 650 mK and
B
= 0 T (
V
= +10 mV,
I
= 100 pA). (b)
T
= 833 mK and
B
= 6 T. Inset 2D FFT of
dI/dV
image. (c)
T
= 897 mK and
B
= 10 T (
V
= +10 mV,
I
= 150 pA).
Figure 11.8 Schematic representation of Landau quantization of 2D electron system. By applying high-magnetic field perpendicular to
x–y
plane, continuous DOS collapses from constant for 2D system to series of discrete levels called Landau levels.
CHAPTER 12: BIOLOGICAL CHARACTERIZATION OF NANOMATERIALS
Figure 12.1 The principle of the acetylcholinesterase (AChE) reaction according to Ellman et al. [55].
Figure 12.2 Experimental setup for measurement of AChE inhibition.
Figure 12.3 Experimental setup for measurement of AChE adsorption.
CHAPTER 13: VISUALIZATION OF MULTIDIMENSIONAL DATA FOR NANOMATERIAL CHARACTERIZATION
Figure 13.1 An example showing a straight line being translated into parallel coordinates [36].
Figure 13.2 Parallel coordinate plot of the cytotoxicity data; four NPs that have high toxicity (N3, N6, N12, and N14) are highlighted.
Figure 13.3 Parallel coordinate plot of the BET and DTT data analysis of the 14 dry samples only.
Figure 13.4 Parallel coordinate plot of the structural properties of zinc oxide (N14) and nickel oxide (N12), excluding BET and DTT data, plotted together with the structural properties of low-toxicity particles.
Figure 13.5 Parallel coordinate plot of the metal content analysis of the 18 samples, excluding structural descriptors.
Figure 13.6 Parallel coordinate plot of the toxicity data of diesel exhaust particles (N2), plotted together with data representing lower toxicity.
Figure 13.7 Parallel coordinate plot of the structural properties of nanotubes (N3) analysis, without including BET and DTT data, plotted together with structural properties of low-toxicity particles.
Figure 13.8 Parallel coordinate plot of the structural properties of N6 (aminated beads), N5 (unmodified), and N7 (carboxylated), excluding BET and DTT data, plotted together with structural properties of low-toxicity particles, showing no signs of difference of N6 from N5 and N7.
List of Tables
CHAPTER 1: INTRODUCTION
Table 1.1 Nanomaterial as Defined by Different Organizations
Table 1.2 Physicochemical Properties of Relevance to Nanotoxicology Community, as Defined by ISO and OECD Guidelines
Table 1.3 A Comparison of Powder Sample Reduction Methods
CHAPTER 3: REFERENCE NANOMATERIALS
Table 3.1 List of Existent and in Progress Reference nanomaterials
CHAPTER 4: PARTICLE NUMBER SIZE DISTRIBUTION
Table 4.1 Summary of Capabilities of the Counting Techniques
CHAPTER 5: SOLUBILITY PART 1: OVERVIEW
Table 5.1 Components of the Fish (Ecotox) Medium
Table 5.2 Substrate Batches and Corresponding Microchip ID
CHAPTER 6: SOLUBILITY PART 2: COLORIMETRY
Table 6.1 Composition of Four Different Juices for the Fed
In Vitro
Digestion [18], made up on Day 1
Table 6.2 A Summary of UV–Vis Absorbance Signal (
λ
max
= abs peak at 556 nm) and Corresponding Estimated [Zn
2+
] Found in the Extracted Supernatant from ZnO (NM 110) Digestive Juice Experiment
Table 6.3 SiO
2
(NM 200) Benchmark Data: Our Values versus the Expected Benchmark Values
Table 6.4 ZnO (NM 110) Data: NPL Values Versus Indicated Benchmark Value
CHAPTER 7: SURFACE AREA
Table 7.1 Surface Area Measurement Methods, Evaluated Against Some of the Demanding Analytical Requirements, Found in Nanotoxicology Research
CHAPTER 8: SURFACE CHEMISTRY
Table 8.1 Photoelectron Attenuation Lengths and Calculated Values for Terms B and C
Table 8.2 Shell Thickness Determined by DLS versus XPS
Table 8.3 Specification of Nanopowders Analyzed by TOF-SIMS
CHAPTER 10: METHODS FOR TESTING DUSTINESS
Table 10.1 Examples of Dustiness Data and Specific Surface Areas of Nine Nanomaterials with Indication on the Type of Real-Time Measurements that were Conducted for the Dust Characterization
Table 10.2 Examples of Dustiness Data Using the SRD Obtained on 13 Nanomaterials Associated Material
CHAPTER 12: BIOLOGICAL CHARACTERIZATION OF NANOMATERIALS
Table 12.1 Summary of Data: The Physicochemical Properties of NMs, Their AChE Inhibition and Adsorption Potentials to Recombinant AChE (from
Drosophila melanogaster
). In the case of enzyme activity inhibition the IC20 denotes the concentration of NMs where 20% inhibition of activity in comparison to control was found. In the case of adsorption efficiency the IC20 means the concentration where 20% of the enzyme has adsorbed NMs and is hence inactive
CHAPTER 13: VISUALIZATION OF MULTIDIMENSIONAL DATA FOR NANOMATERIAL CHARACTERIZATION
Table 13.1 The 18 Nanoparticles Used in this Study
Table 13.2 Characterization of Physicochemical Properties of the 18 Nanoparticles
Table 13.3 The Cytotoxicity Assays Performed
Nanomaterial Characterization
An Introduction
Edited by
Ratna Tantra
Copyright © 2016 by John Wiley & Sons, Inc. All rights reserved
Published by John Wiley & Sons, Inc., Hoboken, New Jersey
Published simultaneously in Canada
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Library of Congress Cataloging-in-Publication data has been applied for
ISBN: 9781118753590
This book is gratefully dedicated to my father, I Wayan Tantra
LIST OF CONTRIBUTORS
D. Bartczak
, LGC Limited, Middlesex TW11 0LY, UK
N. A. Belsey
, Analytical Science Division, National Physical Laboratory, Teddington TW11 0LW, UK
E. Bolea
, Group of Analytical Spectroscopy and Sensors (GEAS), Institute of Environmental Sciences (IUCA), Universidad de Zaragoza, 50009 Zaragoza, Spain
H. Bouwmeester
, Toxicology and Bioassays, RIKILT – Wageningen University & Research Center, 6708 WB Wageningen, The Netherlands
C.A. Charitidis
, School of Chemical Engineering, Laboratory Unit of Advanced Composite, Nanomaterials and Nanotechnology, National Technical University of Athens, Athens 15780, Greece
C. A. David
, Departament de Química and Agrotecnio, Universitat de Lleida, 25198 Lleida, Spain
J-M Dogné
, Department of Pharmacy, University of Namur (UNamur), 5000 Namur, Belgium
D.A. Dragatogiannis
, School of Chemical Engineering, Laboratory Unit of Advanced Composite, Nanomaterials and Nanotechnology, National Technical University of Athens, Athens 15780, Greece
D. Drobne
,
Biotechnical Faculty
, Department of Biology, University of Ljubljana, 1000 Ljubljana, Slovenia
D. Fujita
, Advanced Key Technologies Division, National Institute for Materials Science, Tsukuba 305-0047, Japan
H. Goenaga-Infante
, LGC Limited, Middlesex TW11 0LY, UK
D. Gohil
, Advanced Engineered Materials Group, Materials, National Physical Laboratory, Teddington TW11 0LW, UK
J. C. Jarman
, Quantitative Surface Chemical Spectroscopy Group, Analytical Science, National Physical Laboratory, Teddington TW11 0LW, UK
A. Jemec
,
Biotechnical Faculty
, Department of Biology, University of Ljubljana, 1000 Ljubljana, Slovenia
K. A. Jensen
, Danish Centre for Nanosafety, National Research Centre for the Working Environment, Copenhagen, Denmark
E.P. Koumoulos
, School of Chemical Engineering, Laboratory Unit of Advanced Composite, Nanomaterials and Nanotechnology, National Technical University of Athens, Athens 15780, Greece
F. Laborda
, Group of Analytical Spectroscopy and Sensors (GEAS), Institute of Environmental Sciences (IUCA), Universidad de Zaragoza, 50009 Zaragoza, Spain
J. Laloy
, Department of Pharmacy, University of Namur (UNamur), 5000 Namur, Belgium
M. Levin
, Danish Centre for Nanosafety, National Research Centre for the Working Environment, Copenhagen, Denmark; Department of Micro- and Nanotechnology, Technological University of Denmark, Lyngby, Denmark
J. Li
, School of Chemistry and Chemical Engineering, South China University of Technology, Guangzhou 510640, PR China
J. J. Liu
, School of Chemistry and Chemical Engineering, South China University of Technology, Guangzhou 510640, PR China; Institute of Particle Science and Engineering, School of Chemical and Process Engineering, University of Leeds, Leeds LS2 9JT, UK
C. Y. Ma
, Institute of Particle Science and Engineering, School of Chemical and Process Engineering, University of Leeds, Leeds LS2 9JT, UK
T. Mesarič
,
Biotechnical Faculty
, Department of Biology, University of Ljubljana, 1000 Ljubljana, Slovenia
C. Minelli
, Analytical Science Division, National Physical Laboratory, Teddington TW11 0LW, UK
W. Österle
, Department of Materials Engineering, BAM Federal Institute for Materials Research and Testing, 12200 Berlin, Germany
C. Oksel
, Institute of Particle Science and Engineering, School of Chemical and Process Engineering, University of Leeds, Leeds LS2 9JT, UK
G. Orts-Gil
, European Office – Spanish Foundation for Science and Technology, Spanish Embassy, 10787 Berlin, Germany
D. Perivoliotis
, School of Chemical Engineering, Laboratory Unit of Advanced Composite, Nanomaterials and Nanotechnology, National Technical University of Athens, Athens 15780, Greece
C. Rey-Castro
, Departament de Química and Agrotecnio, Universitat de Lleida, 25198 Lleida, Spain
K. N. Robinson
, Quantitative Surface Chemical Spectroscopy Group, Analytical Science, National Physical Laboratory, Teddington TW11 0LW, UK
T. Sainsbury
, Materials Processing and Performance Group, Materials, National Physical Laboratory, Teddington TW11 0LW, UK
K. Sepčić
,
Biotechnical Faculty
, Department of Biology, University of Ljubljana, 1000 Ljubljana, Slovenia
A.G. Shard
, Analytical Science Division, National Physical Laboratory, Teddington TW11 0LW, UK
M. Sopotnik
,
Biotechnical Faculty
, Department of Biology, University of Ljubljana, 1000 Ljubljana, Slovenia
R. Tantra
, Quantitative Surface Chemical Spectroscopy Group, Analytical Science, National Physical Laboratory, Teddington TW11 0LW, UK
A. K. Undas
, Toxicology and Bioassays, RIKILT – Wageningen University & Research Center, 6708 WB Wageningen, The Netherlands
M. van der Zande
, Toxicology and Bioassays, RIKILT – Wageningen University & Research Center, 6708 WB Wageningen, The Netherlands
X. Z. Wang
, School of Chemistry and Chemical Engineering, South China University of Technology, Guangzhou 510640, PR China; Institute of Particle Science and Engineering, School of Chemical and Process Engineering, University of Leeds, Leeds LS2 9JT, UK
O. Witschger
, Laboratoire de Métrologie des Aérosols Département Métrologie des Polluants, Institute National de Recherche et de Sécurité, Nancy, France
EDITOR'S PREFACE
To measure is to know. If you cannot measure it, you cannot improve it
Lord Kelvin (1824–1907)
Since joining the National Physical Laboratory (NPL) (UK's national measurement institute) in 2004, I have been fortunate enough to have worked in numerous projects related to nanoscience and nanotechnology. During this time, the nature of my research activities varied widely across different disciplines, from the applications of nanomaterials in surface-enhanced Raman spectroscopy to understanding their potential toxicological implications. A critical part of the research throughout the years, however, has been the need to characterize physicochemical properties of the nanomaterials. This has not always been trivial.
The idea for this book came from my involvement in a European Commission Framework 7 research project entitled MARINA (Managing Risks of Nanomaterials). One of the goals of this project was to harmonize activities and to establish a common platform to ultimately support the scientific infrastructure for risk management of nanomaterials. Although the relevance of MARINA is for nanosafety, the idea of having a common approach can be extended to other application areas. This, coupled with my interest in measurement science, ultimately laid the foundation for this multi-authored book.
The book begins with a general introduction, which aims to give the reader a solid foundation to nanomaterial characterization. Chapters 2 and 3 focus on two principal topics: nanomaterial synthesis and reference nanomaterials, which serve as useful background for the rest of the book. Chapters 4–10 constitute the very heart of this book, dedicated to key physicochemical properties and their measurements. Undoubtedly, it is beyond the scope of the book to cover all properties and only several key properties, such as particle size distribution by number, solubility, surface area, surface chemistry, mechanical/tribological, and dustiness, are covered. Chapters 11–13 are devoted to state-of-the-art techniques, in which three very different sets of characterization tools are presented: (i) scanning tunneling microscopy operated under extreme conditions; (ii) novel strategy for biological characterization of nanomaterials; and (iii) methods to handle and visualize multidimensional nanomaterial characterization data.
Most of the chapters this book begin by giving an overview of the topic area before a case study is presented. The purpose of the case study is to demonstrate how the reader may make use of background information presented to them and show how this can be translated to solve a nano-specific application scenario. Thus, it will be useful for researchers to help them design experimental investigations.
The book is written in such a way that both students and experts in other fields of science will find the information useful. My intention is that it will appeal to a range of audience outside the research field, whether they are in academia, industry, or regulation and is particularly useful for readers whose analytical background may be limited. There is also an extensive list of references associated with every chapter, to encourage further reading.
Finally, it has taken me just less than 2 years to complete this book and so, I must say a few words of thanks. First, I am grateful to all of the authors for their chapter contributions. Second, I thank the many people who have encouraged me to publish this book: my Wiley editor, my husband Keith F. E. Pratt, family, and friends. Special thanks go to Sinta Tantra, for her generosity in donating her artwork, which has been used for the cover of this book. The cover is abstract art that depicts the image of a nanomaterial surface at atomic resolution!
Portsmouth, England
16 December, 2015
CHAPTER 1INTRODUCTION
R. Tantra, J. C. Jarman and K. N. Robinson
Quantitative Surface Chemical Spectroscopy Group, Analytical Science, National Physical Laboratory, Teddington, TW11 0LW, UK
1.1 OVERVIEW
Over the course of the past few decades, the word “nanomaterial” started to shine in reporting and publishing; nanomaterial thus became the new buzzword, giving the impression of a new type of technology. In fact, nanomaterials are not new at all and can be found in everyday lives, with most people not being aware of their existence. Nanomaterials exist in nature, for example, in volcanic ashes, sea sprays and smoke [1]. In relation to manufactured nanomaterials, they have existed as early as the 4th century. The Lycurgus Cup, a glass cup made with tiny proportions of gold and silver nanoparticles is an example of Roman era nanotechnology. The use of nanoparticles for beautiful art continued ever since, and by 1600s it is not uncommon for alchemists to create gold nanoparticles for stained glass windows. These days, there are far more uses; nanomaterials thus represent a growing class of material already introduced into multiple business sectors. For example, in early 20th century, tire companies used carbon black in car tires, primarily for physical reinforcement (e.g., abrasion resistance, tensile strength) and thermal conductivity to help spread heat load. Although nanomaterials have been around for a long time, it was only the invention of the scanning tunneling microscope in 1981 and the discovery of fullerenes in 1986 that really marked the beginning of the current nanoscience revolution. This led nanoscientists to conduct research, to study their behavior, so as to control their properties and harness their power.
Lesen Sie weiter in der vollständigen Ausgabe!
Lesen Sie weiter in der vollständigen Ausgabe!
Lesen Sie weiter in der vollständigen Ausgabe!
Lesen Sie weiter in der vollständigen Ausgabe!
Lesen Sie weiter in der vollständigen Ausgabe!
Lesen Sie weiter in der vollständigen Ausgabe!
Lesen Sie weiter in der vollständigen Ausgabe!
Lesen Sie weiter in der vollständigen Ausgabe!
Lesen Sie weiter in der vollständigen Ausgabe!
Lesen Sie weiter in der vollständigen Ausgabe!
Lesen Sie weiter in der vollständigen Ausgabe!
Lesen Sie weiter in der vollständigen Ausgabe!
Lesen Sie weiter in der vollständigen Ausgabe!
Lesen Sie weiter in der vollständigen Ausgabe!
