Experimental methods in the physical sciences, vol 46

Experimental Methods in the Physical Sciences Thomas Lucatorto, Albert C Parr and Kenneth Baldwin Editors in Chief Academic Press is an imprint of Elsevier Radarweg 29, PO Box 211, 1000 AE Amsterdam, The Netherlands 225 Wyman Street, Waltham, MA 02451, USA The Boulevard, Langford Lane, Kidlington, Oxford, OX5 1GB, UK Copyright © 2014 Elsevier Inc All rights reserved No part of this publication may be reproduced, stored in a retrieval system or transmitted in any form or by any means electronic, mechanical, photocopying, recording or otherwise without the prior written permission of the publisher Permissions may be sought directly from Elsevier’s Science & Technology Rights Department in Oxford, UK: phone (+ 44) (0) 1865 843830; fax (+ 44) (0) 1865 853333; email: permissions@elsevier.com Alternatively you can submit your request online by visiting the Elsevier web site at http://elsevier.com/locate/permissions, and selecting Obtaining permission to use Elsevier material Notice No responsibility is assumed by the publisher for any injury and/or damage to persons or property as a matter of products liability, negligence or otherwise, or from any use or operation of any methods, products, instructions or ideas contained in the material herein Because of rapid advances in the medical sciences, in particular, independent verification of diagnoses and drug dosages should be made Library of Congress Cataloging-in-Publication Data Spectrophotometry : accurate measurement of optical properties of materials / edited by Thomas A Germer, Joanne C Zwinkels, Benjamin K Tsai pages cm — (Experimental methods in the physical sciences ; volume 46) Includes bibliographical references and index ISBN 978-0-12-386022-4 Spectrophotometry I Germer, Thomas A., editor of compilation II Zwinkels, Joanne C., 1955- editor of compilation III Tsai, Benjamin K., editor of compilation IV Series: Experimental methods in the physical sciences ; v 46 QD117.S64S64 2014 5430 55–dc23 2014015452 British Library Cataloguing in Publication Data A catalogue record for this book is available from the British Library ISBN: 978-0-12-386022-4 ISSN: 1079-4042 For information on all Academic Press publications visit our website at store.elsevier.com Printed and bound in United States of America 14 15 16 17 10 Contributors Numbers in Parentheses indicate the pages on which the author’s contributions begin Carol J Bruegge (457), Jet Propulsion Laboratory, California Institute of Technology, Pasadena, California, USA Roger Davies (457), Department of Physics, University of Auckland, Auckland, New Zealand Paul C DeRose (221), National Institute of Standards and Technology (NIST), NIST, Material Measurement Laboratory, Gaithersburg, Maryland, USA Michael B Eyring (489), Micro Forensics, Ltd., and Arizona Department of Public Safety Crime Laboratory, Phoenix, Arizona, USA Arnold A Gaertner (67), National Research Council Canada, Ottawa, Ontario, Canada Thomas A Germer (1, 11, 67, 291), National Institute of Standards and Technology, Gaithersburg, Maryland, USA John P Hammond (409), Starna Scientific Limited, Hainault, Essex, United Kingdom Leonard Hanssen (333), National Institute of Standards and Technology, Gaithersburg, Maryland, USA Andreas Hoăpe (179), Physikalisch-Technische Bundesanstalt, Braunschweig, Germany Juntaro Ishii (333), National Metrology Institute of Japan, AIST, Tsukuba, Japan Simon G Kaplan (97), National Institute of Standards and Technology, Gaithersburg, Maryland, USA Tomoyuki Kumano (333), Kobe City College of Technology, Kobe, Japan James E Leland (221), Copia LLC, Goshen, New Hampshire, USA Paul C Martin (489), CRAIC Technologies, San Dimas, California, USA Maria E Nadal (367), National Institute of Standards and Technology, Gaithersburg, Maryland, USA Manuel A Quijada (97), NASA Goddard Space Flight Center, Code 551, Greenbelt, Maryland, USA Sven Schroăder (291), Fraunhofer Institute for Applied Optics and Precision Engineering, Jena, Germany Florian M Schwandner (457), Jet Propulsion Laboratory, California Institute of Technology, Pasadena, California, USA Felix C Seidel (457), Jet Propulsion Laboratory, California Institute of Technology, Pasadena, California, USA xv xvi Contributors John C Stover (291), The Scatter Works, Inc., Tucson, Arizona, USA Benjamin K Tsai (1, 11), National Institute of Standards and Technology, Gaithersburg, Maryland, USA Peter A van Nijnatten (143), OMT Solutions BV, Eindhoven, Netherlands Hidenobu Wakabayashi (333), Kyoto University, Kyoto, Japan Hiromichi Watanabe (333), National Metrology Institute of Japan, AIST, Tsukuba, Japan Dave Wyble (367), Avian Rochester, LLC, Webster, New York, USA Howard W Yoon (67), National Institute of Standards and Technology, Gaithersburg, Maryland, USA Clarence J Zarobila (367), National Institute of Standards and Technology, Gaithersburg, Maryland, USA Joanne C Zwinkels (1, 11, 221), National Research Council Canada, NRC, Measurement Science and Standards, Ottawa, Ontario, Canada Volumes in Series Experimental Methods in the Physical Sciences (Formerly Methods of Experimental Physics) Volume Classical Methods Edited by lmmanuel Estermann Volume Electronic Methods, Second Edition (in two parts) Edited by E Bleuler and R O Haxby Volume Molecular Physics, Second Edition (in two parts) Edited by Dudley Williams Volume Atomic and Electron Physics - Part A: Atomic Sources and Detectors; Part B: Free Atoms Edited by Vernon W Hughes and Howard L Schultz Volume Nuclear Physics (in two parts) Edited by Luke C L Yuan and Chien-Shiung Wu Volume Solid State Physics - Part A: Preparation, Structure, Mechanical and Thermal Properties; Part B: Electrical, Magnetic and Optical Properties Edited by K Lark-Horovitz and Vivian A Johnson Volume Atomic and Electron Physics - Atomic Interactions (in two parts) Edited by Benjamin Bederson and Wade L Fite Volume Problems and Solutions for Students Edited by L Marton and W F Hornyak Volume Plasma Physics (in two parts) Edited by Hans R Griem and Ralph H Lovberg Volume 10 Physical Principles of Far-Infrared Radiation Edited by L C Robinson Volume 11 Solid State Physics Edited by R V Coleman Volume 12 Astrophysics - Part A: Optical and Infrared Astronomy Edited by N Carleton Part B: Radio Telescopes; Part C: Radio Observations Edited by M L Meeks xvii xviii Volumes in Series Volume 13 Spectroscopy (in two parts) Edited by Dudley Williams Volume 14 Vacuum Physics and Technology Edited by G L Weissler and R W Carlson Volume 15 Quantum Electronics (in two parts) Edited by C L Tang Volume 16 Polymers - Part A: Molecular Structure and Dynamics; Part B: Crystal Structure and Morphology; Part C: Physical Properties Edited by R A Fava Volume 17 Accelerators in Atomic Physics Edited by P Richard Volume 18 Fluid Dynamics (in two parts) Edited by R J Emrich Volume 19 Ultrasonics Edited by Peter D Edmonds Volume 20 Biophysics Edited by Gerald Ehrenstein and Harold Lecar Volume 21 Solid State Physics: Nuclear Methods Edited by J N Mundy, S J Rothman, M J Fluss, and L C Smedskjaer Volume 22 Solid State Physics: Surfaces Edited by Robert L Park and Max G Lagally Volume 23 Neutron Scattering (in three parts) Edited by K Skold and D L Price Volume 24 Geophysics - Part A: Laboratory Measurements; Part B: Field Measurements Edited by C G Sammis and T L Henyey Volume 25 Geometrical and Instrumental Optics Edited by Daniel Malacara Volume 26 Physical Optics and Light Measurements Edited by Daniel Malacara Volume 27 Scanning Tunneling Microscopy Edited by Joseph Stroscio and William Kaiser Volume 28 Statistical Methods for Physical Science Edited by John L Stanford and Stephen B Vardaman Volumes in Series xix Volume 29 Atomic, Molecular, and Optical Physics - Part A: Charged Particles; Part B: Atoms and Molecules; Part C: Electromagnetic Radiation Edited by F B Dunning and Randall G Hulet Volume 30 Laser Ablation and Desorption Edited by John C Miller and Richard F Haglund, Jr Volume 31 Vacuum Ultraviolet Spectroscopy I Edited by J A R Samson and D L Ederer Volume 32 Vacuum Ultraviolet Spectroscopy II Edited by J A R Samson and D L Ederer Volume 33 Cumulative Author lndex and Tables of Contents, Volumes 1-32 Volume 34 Cumulative Subject lndex Volume 35 Methods in the Physics of Porous Media Edited by Po-zen Wong Volume 36 Magnetic Imaging and its Applications to Materials Edited by Marc De Graef and Yimei Zhu Volume 37 Characterization of Amorphous and Crystalline Rough Surface: Principles and Applications Edited by Yi Ping Zhao, Gwo-Ching Wang, and Toh-Ming Lu Volume 38 Advances in Surface Science Edited by Hari Singh Nalwa Volume 39 Modern Acoustical Techniques for the Measurement of Mechanical Properties Edited by Moises Levy, Henry E Bass, and Richard Stern Volume 40 Cavity-Enhanced Spectroscopies Edited by Roger D van Zee and J Patrick Looney Volume 41 Optical Radiometry Edited by A C Parr, R U Datla, and J L Gardner Volume 42 Radiometric Temperature Measurements I Fundamentals Edited by Z M Zhang, B K Tsai, and G Machin Volume 43 Radiometric Temperature Measurements II Applications Edited by Z M Zhang, B K Tsai, and G Machin Volume 44 Neutron Scattering – Fundamentals Edited by Felix Fernandez-Alonso, and David L Price xx Volumes in Series Volume 45 Single-Photon Generation and Detection Edited by Alan Migdall, Sergey Polyakov, Jingyun Fan, and Joshua Bienfang Volume 46 Spectrophotometry: Accurate Measurement of Optical Properties of Materials Edited by Thomas A Germer, Joanne C Zwinkels, and Benjamin K Tsai Preface Spectrophotometry is the quantitative measurement of the optical properties of materials over a wide wavelength range encompassing the ultraviolet, visible, and infrared spectral regions These spectral measurements include reflectance, transmittance, absorptance/emittance, scattering, and fluorescence, and their accurate measurement has an impact on a wide field of science and technology The design and performance of optical instruments, ranging from low cost cellphone cameras to high cost microlithography projection tools and satellite telescopes, requires knowledge of the optical properties of the components, such as their refractive index, roughness, subsurface scatter, and contamination The pharmaceutical and chemical industries use optical absorption and fluorescence measurements to quantify concentration which is required for accurate dosing and elimination of contaminants Global climate change simulations require accurate knowledge of the optical properties of materials, gases, and aerosols to calculate the net energy balance of our planet The properties of thin films, even when they are not intended for optical applications, are often related to their optical reflection, transmission, and scattering properties Commercial products are often selected by consumers based upon their appearance, a complex attribute that encompasses more specific attributes, such as color, gloss, and texture Renewed interest in solar energy has driven the need to maximize the light capture efficiency of solar collectors This book is intended to be a hands-on text for those seeking to perform precise and accurate spectrophotometry of the optical properties of materials Based on teaching experiences at our respective institutes, it is our aim to present material that helps the practitioner to set up and optimize the spectrophotometer to perform these various measurements, validate the instrument performance, and be aware of the various sources of errors that can impact the results A number of our students have been from institutes interested in developing an independent capability for realizing spectrophotometric scales, and it is our intention to also provide the researcher the necessary framework for designing and characterizing reference instruments for traceable measurements of these optical quantities Chapter introduces the topic of spectrophotometry and a short history of its development and present-day challenges It includes a section outlining the standard methods and terminology used for evaluating and expressing uncertainty in any measurement This will provide the reader the background needed to follow the examples of uncertainty analysis that are given for specific spectrophotometric measurements in some of the following chapters xxi xxii Preface Chapter describes some theoretical concepts underlying spectrophotometry and the optical properties of materials It begins by defining the different radiometric quantities of radiance, irradiance, and intensity These quantities are then related to the corresponding electromagnetic field quantities This theoretical foundation allows the definition of the spectrophotometric quantities: reflectance, transmittance, emittance, diffuse reflectance, diffuse transmittance, and the bidirectional reflectance distribution function (BRDF) Relationships between these quantities are derived and explained A review of the Fresnel relations is given, including expressions appropriate for thin films and thick films The Kirchhoff relationship between the reflectance and emittance is derived While the topic of BRDF modeling is beyond the scope of this text, Chapter describes the theory of Kubelka and Munk, which is applicable to highly diffuse materials and used widely in color formulation and for determining molecular optical properties (absorption and scattering coefficients) Chapter also describes two theories for scattering from rough surfaces, one appropriate for very rough surfaces and one appropriate for very smooth surfaces Chapters and discuss the means of obtaining wavelength separation and spectral resolution in spectrophotometry Chapter provides an overview of the use of grating and prism spectrometers in spectrophotometry, while Chapter discusses the use of Fourier transform interferometric methods Each of these methods has its advantages and disadvantages Included in these chapters are discussions of how measurement noise is propagated, how nonlinearities affect results, how stray light or interreflections produce artifacts, and what determines the spectral resolution or bandpass of the measured spectrophotometric quantities Methods to identify and alleviate these problems are described Chapter covers the topic of specular reflectance of nonscattering samples such as mirrors and other samples with mirror-like reflection, and of regular transmittance of transparent samples such as glass filters The instrumentation and procedures for measuring these properties via both absolute and relative methods are discussed and practical methods are given for improving the measurement accuracy Sources of error are treated and representative uncertainty budgets are given for various examples As a special topic, methods for accurate reflectance measurement at oblique incidence of very high reflectance materials like reference mirrors and laser mirrors are discussed Examples are given for both Fourier transform infrared (FTIR) and ultraviolet, visible, and near-infrared (UV/Vis/NIR) spectrophotometry Chapter describes the basic principles of diffuse reflectance and transmission measurements Unlike the measurement of specular reflection, where the angle of incidence equals the angle of reflection, in the case of diffuse reflection, the incoming radiation is spread over the half-space above the surface, with a certain distribution specific to the surface or material under test The integrating sphere with its ability to collect all or the diffuse-only ... Canada Volumes in Series Experimental Methods in the Physical Sciences (Formerly Methods of Experimental Physics) Volume Classical Methods Edited by lmmanuel Estermann Volume Electronic Methods, ... arrangements with the General Electric Company [6] to commercialize the instrument In the intervening years, there have been significant advances in the design of spectrophotometers including the emergence... uncertainty While the factors in the first term in Eq (1.3) always increase the uncertainty, those in the second term not necessarily so and in some cases can reduce the combined standard uncertainty It