In-Situ Transmission Electron Microscopy Experiments

Design and Practice

Inbunden, Engelska, 2023

1 719 kr

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In-Situ Transmission Electron Microscopy Experiments Design and execute cutting-edge experiments with transmission electron microscopy using this essential guide In-situ microscopy is a recently-discovered and rapidly-developing approach to transmission electron microscopy (TEM) that allows for the study of atomic and/or molecular changes and processes while they are in progress. Experimental specimens are subjected to stimuli that replicate near real-world conditions and their effects are observed at a previously unprecedented scale. Though in-situ microscopy is becoming an increasingly important approach to TEM, there are no current texts combining an up-to-date overview of this cutting-edge set of techniques with the experience of in-situ TEM professionals. In-Situ Transmission Electron Microscopy Experiments meets this need with a work that synthesizes the collective experience of myriad collaborators. It constitutes a comprehensive guide for planning and performing in-situ TEM measurements, incorporating both fundamental principles and novel techniques. Its combination of technical detail and practical how-to advice makes it an indispensable introduction to this area of research. In-Situ Transmission Electron Microscopy Experiments readers will also find: Coverage of the entire experimental process, from method selection to experiment design to measurement and data analysisDetailed treatment of multimodal and correlative microscopy, data processing and machine learning, and moreDiscussion of future challenges and opportunities facing this field of researchIn-Situ Transmission Electron Microscopy Experiments is essential for graduate students, post-doctoral fellows, and early career researchers entering the field of in-situ TEM.

Produktinformation

Utgivningsdatum2023-06-21
Mått170 x 244 x 24 mm
Vikt907 g
FormatInbunden
SpråkEngelska
Antal sidor384
FörlagWiley-VCH Verlag GmbH
ISBN9783527347988

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Renu Sharma, PhD, is an NIST Emeritus Fellow and worked as project leader there from 2009 to 2019. Before working at NIST, she was Senior Research Scientist in the LeRoy Eyring Center for Solid State Science at Arizona State University, as well as an affiliated faculty member in multiple departments. She is a pioneer in the field of transmission electron microscopy who has published extensively on the subject.

Preface xiiiAcknowledgments xviiList of Abbreviations xixAbout the Author xxiii1 In-Situ TEM 11.1 Introduction 11.2 General Scope of the Book 21.3 Why In-Situ TEM 31.4 TEM: Overview 41.4.1 Historical Perspective 41.4.2 Electron–Sample Interactions 41.4.3 Overview of Modern TEM 51.4.3.1 Electron Source or Electron Gun 51.4.3.2 Lenses 71.4.3.3 Lens Aberrations 71.4.3.4 Aberration Correctors 91.4.4 Data Acquisition Systems 91.4.4.1 Types of Detectors 91.5 TEM/STEM-Based Characterization Techniques 111.5.1 Diffraction 111.5.2 TEM Imaging Modes 121.5.3 Stem 141.5.4 Analytical TEM 141.5.4.1 Chemical Analysis 151.5.4.2 Eftem 191.5.4.3 Spectrum Imaging (SI) 201.6 Other Techniques 201.6.1 Lorentz Microscopy 201.6.2 Holography 221.6.2.1 In-Line Holography 221.6.2.2 Off-Axis Holography 221.6.3 UEM and DTEM 231.7 Introduction to Different Stimuli Used for In-Situ TEM 241.7.1 Heating (Chapter 3) 241.7.2 Cooling (Cryo TEM – Chapter 4) 241.7.3 Interactions with Liquid/Electrochemistry (Chapter 6) 241.7.4 Interaction with Gas Environment/Catalysis (Chapter 7) 251.7.5 Other Stimuli Not Included in this Book 251.7.5.1 Mechanical Testing 251.7.5.2 Ion Radiation/Implantation 251.7.5.3 Biasing 271.7.5.4 Magnetization 281.8 Potential Limitations and Cautions 291.9 Take-Home Messages 31References 312 Experiment Design Philosophy 412.1 General 412.2 Choice of Technique and the Microscope 442.2.1 Stimulus and Technique Selection 442.2.2 Microscope Selection 452.2.2.1 Operating Voltage 452.2.2.2 TEM/STEM and Pole-Piece Gap 462.2.2.3 Image Acquisition System and Detectors 462.2.3 Development or Modification of New Tool 472.3 TEM Holder Design and Selection 472.4 Specimen Design and Preparation 482.4.1 Direct Dispersion on a TEM Grid 482.4.2 Sintering Pallets 492.4.3 Ultramicrotomy 502.4.4 Electropolishing 502.4.5 Mechanical and Ion Milling 502.4.6 Focused Ion Beam (FIB) 522.4.7 Tripod Polishing 542.4.8 Cryo Sample Preparation 542.5 Guidelines for Experimental Setup 552.5.1 Electron Beam Effects 552.5.2 Choice of TEM Grid and Support Material 562.5.2.1 Reactivity of Sample with Grid and/or Support Material 562.5.2.2 Reactivity of TEM Grids Upon Heating 572.5.2.3 Reactivity of TEM Grids in Gaseous Environment 582.5.2.4 Reactivity of Liquids with the Windows 592.5.2.5 Reactivity of Gases/Liquids with the TEM Holder Parts 592.5.3 Purity of Gases 602.5.4 Liquid Cell Experiments 622.5.5 Experiments Using Other Stimuli 632.6 Practical Example of Designing In-Situ TEM Experiment 632.6.1 Growth of GaN Nanowires Using ETEM 632.6.2 Applications of Quantitative Data 642.6.2.1 Physical and Materials Science 662.6.2.2 Catalysis 672.7 Review 67References 683 In-Situ Heating 773.1 History 773.2 Currently Available Heating Holders 783.2.1 Direct Heating Holder 793.2.2 Indirect Heating Holders 793.2.2.1 Furnace Heating Holders 793.2.2.2 MEMS-Based Heating Holders 823.3 Experimental Considerations 843.3.1 General 843.3.2 Electron Beam 863.3.3 Sample Temperature at Nanoscale 883.3.4 Specimen Design and Selection 903.3.5 Thermal Drift 913.4 Select Applications 923.4.1 Dislocation Motion 933.4.2 Nucleation, Precipitation, and Crystallization 943.4.3 Sintering 983.4.4 Thermal Stability of Materials 1003.4.4.1 Alloys 1003.4.4.2 Core–Shell Structures 1003.4.4.3 2-D Materials 1023.4.5 Phase Transformation 1023.4.6 Materials Synthesis 1043.5 Limitations and Possibilities 1053.6 Chapter Summary 106References 1064 In-Situ Cryo-TEM 1154.1 Historical Perspective 1164.2 Specimen Holder Design and Function 1164.3 Specimen Design and Preparation 1194.4 Practical Aspects of Performing Cryogenic Cooling 1214.5 Some Noteworthy Applications 1224.5.1 Mitigating Radiation Damage 1234.5.1.1 Structure of Polymers 1244.5.1.2 Structure of MOF and Zeolites 1254.5.1.3 Cryo-TEM for Energy Materials 1264.5.1.4 Reactions in Liquids 1284.5.1.5 Quantum and 2-D Materials 1294.5.2 Phase Transformations Below RT 1324.5.3 Correlative In-Situ Experiments at Low Temperature 1354.5.3.1 Mechanical Testing 1354.5.3.2 Magnetic Field 1364.6 Benefits and Limitations 1374.7 Chapter Summary 138References 1385 Designing Liquid and Gas Cell Holders 1455.1 Historical Perspective 1465.2 Design Philosophy 1465.3 Windows 1495.3.1 Image Resolution: Thickness and Material Properties of the Windows 1495.3.2 Strength and Flexibility 1505.3.3 Tolerance for the Pressure Difference 1515.3.4 Inert or Corrosion Resistant 1535.4 Microfabricated Window Cell (Microchips) 1545.4.1 Static Cells 1575.4.2 Flow Cells 1595.4.3 Incorporation of Other Stimuli 1615.4.4 Monolithic Microchips 1625.5 Examples of Modified Window Holders 1635.5.1 Redesigning the Microchips for Commercial Holder 1645.5.2 Modified Window Microchips and TEM Holder Combination 1665.5.3 Non-window Cell Holder to Incorporate Other Stimuli 1665.6 Take Home Message 167References 1686 In-Situ Solid–Liquid Interactions 1736.1 Historical Perspective 1736.2 Holder Design and Selection 1756.2.1 Closed Cells 1756.2.1.1 Graphene Cells 1756.2.1.2 Microfabricated Window Cell 1786.2.2 Limitations of Closed Cells and Need for External Stimuli 1786.2.3 Flow Reactors: Microfluidic Design 1786.2.4 Electrochemical Cell: Biasing 1816.2.5 Heating in Liquids 1826.3 Specimen Design and Preparation 1846.4 Data Acquisition 1856.5 Practical Challenges 1856.5.1 Sample Loading 1856.5.2 Electron Beam Effects 1876.5.3 Windows Bulging 1886.5.4 Interaction of Sample with Windows 1896.6 Select Examples of Applications 1906.6.1 Nucleation and Growth of Nanoparticles 1906.6.2 Corrosion/Oxidation 1926.6.3 Galvanic Replacement Reactions 1936.6.4 Growth of Core–Shell Nanoparticles 1946.6.5 Soft Nanomaterials Analyzed by In-Situ Liquid TEM 1956.6.6 Quantitative Electrochemical Measurements 1976.6.7 Battery Research 1986.6.7.1 Open Cell 1996.6.7.2 Closed Liquid Cell 2006.7 Limitations 2016.8 Take-Home Messages 202References 2037 In-Situ Gas–Solid Interactions 2157.1 Historical Perspective 2157.2 Current Strategies 2187.2.1 Window Holders 2187.2.1.1 Incorporation of Other Stimuli 2217.2.1.2 Specimen Design and Preparation 2217.2.1.3 Practical Challenges for Gas-Cell Holders 2217.2.1.4 Review of Benefits and Limitations of Gas-Cell Holders 2227.2.2 Environmental Microscopes (Open Cell) 2237.2.2.1 ETEM Combined with Gas Injection Sample Holder 2237.2.2.2 Differentially Pumped TEM 2247.3 Gas Manifold Design and Construction 2277.4 Practical Aspects of Performing Experiments in Gas Environment 2287.4.1 Electron Beam Effects 2297.4.2 Gas Pressure and Resolution 2317.4.3 Sample Temperature and Cell Pressure 2327.4.4 Anticontamination Device 2337.5 Select Examples of Applications 2347.5.1 Effect of Gas Environment on Catalyst Nanoparticles 2347.5.2 Carbon Nanotube (CNT) Growth 2367.5.3 Nanowire Growth 2377.5.4 Electron-Beam-Induced Deposition 2387.5.5 REDOX Reactions 2397.5.6 Gas Adsorption Sites 2417.6 Review of Benefits and Limitations 2437.7 Take-Home Messages 244References 2458 Multimodal and Correlative Microscopy 2558.1 Multimodal TEM 2568.1.1 Parallel Ion Electron Spectrometry (PIES) 2578.1.2 Hybrid Microscope 2588.1.3 Alternatives to Free Space Approach 2608.1.4 Introducing Light for Other Applications 2638.1.4.1 Through Sample Chamber Port 2638.1.4.2 Through Sample Holder 2648.1.5 Laser Alignment 2698.2 Correlative Approaches 2698.2.1 TEM and SEM 2708.2.2 Electron and X-ray Microscopies and Spectroscopies 2728.2.2.1 Portable Reactor for Various Platforms 2748.2.2.2 Independent Correlative Measurements 2788.3 Take Home Messages 280References 2809 Data Processing and Machine Learning 2859.1 History of Image Simulation and Processing 2859.1.1 Image Simulations 2869.1.2 Image Processing 2869.2 Current Status 2899.2.1 Progress for Image Simulations 2899.2.2 Progress in Data (Image) Processing 2909.3 Data Management 2919.4 Data Processing and Machine Learning (ML) 2929.4.1 What Is Machine Learning? 2939.4.1.1 Unsupervised ml 2939.4.1.2 Supervised ml 2949.4.2 Motivation 2969.4.3 Current Status 2989.5 Select Applications 3009.5.1 Noise Reduction 3009.5.2 Structure Determination 3019.5.2.1 Diffraction Pattern Analysis 3029.5.2.2 Image Analysis 3039.5.2.3 Atomic Column Heights (3-D Structure) 3059.5.2.4 Other Applications 3059.6 Future Needs 3079.7 Limitations 3099.8 Take Home Messages 309References 31010 Future Vision 31710.1 Historical Aspect 31810.2 Current Status 31810.2.1 Etem 31810.2.2 UEM and DTEM 31910.2.3 Stroboscopic TEM 31910.2.4 Pies 31910.3 Technical Challenges 31910.3.1 List of Major Workshops 32010.3.2 Open Challenges and Technical Roadmaps 32310.3.2.1 Specific for Battery Research 32310.3.2.2 Specific for Liquid-Cell TEM 32410.3.2.3 Specific for Catalysis 32410.3.2.4 Specific for Quantum Materials 32510.4 Developing Relevant Strategies 32610.4.1 Modifying Base TEM/STEM Unit 32710.4.2 TEM Holders with Multiple Stimuli 33210.4.3 Automation and Autonomous Operation 33610.4.3.1 Automation 33610.4.3.2 Autonomous Experiments 33810.5 Take Home Messages 340References 340Index 349