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In Situ and Operando

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Transmission Electron Microscopy

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References

General References

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Specific References – In-Situ TEM Collections

ETEM

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Deformation

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DTEM and UEM

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Temperature Control

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  • Gai PL, Boyes ED (2009) Advances in Atomic Resolution In Situ Environmental Transmission Electron Microscopy and 1Å Aberration Corrected In Situ Electron Microscopy. Microsc Res Techn 72:153–164

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  • Li YB, Bando Y, Golberg D, Liu ZW (2003) Ga-Filled Single Crystalline MgO Nanotube: Wide-Temperature Range Nanothermometer. Appl Phys Lett 83(5):999–1001

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  • Mortensen PM, Hansen TW, Wagner JB, Jansen AD (2015) Modeling of temperature profiles in an environmental transmission electronmicroscope using computational fluid dynamics. Ultramicroscopy 152:1–9 (Measuring T in a TEM with gas around the specimen)

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  • Saka H, Kamino T, Arai S, Sasaki K (2008) In Situ Heating Transmission Electron Microscopy. MRS Bull 33:93–100 (Nice description of the filament heating holder)

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Magnetic Fields (section 2.7.2)

  • Arita M, Tokuda R, Hamada K, Takahashi Y (2014) Development of TEM Holder Generating In-Plane Magnetic Field Used for In-Situ TEM Observation. Mater Transact 55(3):403–409

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  • Budruk A, Phatak C, Petford-Long AK, De Graef M (2011) In situ Lorentz TEM magnetization studies on a Fe-Pd-Co martensitic alloy. Acta Mater 59:6646–6657

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  • Budruk A, Phatak C, Petford-Long AK, De Graef M (2011) In situ Lorentz TEM magnetization study of a Ni-Mn-Ga ferromagnetic shape memory alloy. Acta Mater 59:4895–4906

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  • Inoue M, Tomita T, Naruse M, Akase Z, Murakami Y, Shindo D (2005) Development of a magnetizing stage for in situ observations with electron holography and Lorentz microscopy. J Electron Microsc 54(6):509–513

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  • Lau JW, Schofield MA, Zhu Y (2007) A straightforward specimen holder modification for remnant magnetic-field measurement in TEM. Ultramicroscopy 107:396–400

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  • Lau JW, Schofield MA, Zhu Y, Neumarl GF (2003) In-situ Magnetodynamic Experiments Achieved with the Design of an In-plane Magnetic Field Specimen Holder. Microsc Microanal 9(Suppl 2):130–131

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  • Uhlig T, Heumann M, Zweck J (2003) Development of a specimen holder for in situ generation of pure in-plane magnetic fields in a transmission electron microscope. Ultramicroscopy 94(3–4):193–196 (Beam deflection using the Lorentz force; using an in-situ magnetization holder)

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  • Yi G, Nicholson WAP, Lim CK, Chapman JN, McVitie S, Wilkinson CDW (2004) A new design of specimen stage for in situ magnetising experiments in the transmission electron microscope. Ultramicroscopy 99:65–72

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  • Zweck J (2012) Lorentz Microscopy. In: Dehm G, Howe JM, Zweck J (eds) In-Situ Electron Microscopy: Applications in Physics, Chemistry and Materials Science. Wiley-VCH Verlag & Co KGaA, Weinheim, Germany (Specific numbers for the field in a 300 kV TEM)

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Electric Fields (section 2.7.3)

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  • Costas PMFJ, Golberg D, Shen G, Mitome M, Bando Y (2008) ZnO low-dimensional structures: electrical properties measured inside a transmission electron microscope. J Mater Sci 43:1460–1470

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  • Liu XH, Huang JY (2011) In situ TEM electrochemistry of anode materials in lithium ion batteries, Energy Environ. Sci 4:3844

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Optical Effects

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  • Miller BK, Crozier PA (2013) System for In Situ UV-Visible Illumination of Environmental Transmission Electron Microscopy Samples. Microsc Microanal 19:461–469

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  • Picher M, Mazzucco S, Blankenship S, Sharma R (2015) Vibrational and optical spectroscopies integrated with environmental transmission electron microscopy. Ultramicroscopy 150:10–15

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  • Shindo D, Takahashi K, Murakami Y, Yamazaki K, Deguchi S, Suga H, Kondo Y (2009) Development of a multifunctional TEM specimen holder equipped with a piezodriving probe and a laser irradiation port. J Elect Microsc 58(4):245–249

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  • Yoshida K, Yamasaki J, Tanaka N (2004) In situ high-resolution transmission electron microscopy observation of photodecomposition process of poly-hydrocarbons on catalytic TiO 2 films. Appl Phys Lett 84(14):2542–2544

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Electron and Ion Irradiation

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Image capture software

  • Camtasia allows you to record the images on your monitor as you see them with 1,024-by-1,024 resolution. Versions for Mac and PC are available. http://www.techsmith.com/camtasia.html

  • VirtualDub is a video capture and processing utility that works on the PC that came with your TEM. It runs on both 32-bit and 64-bit Windows platforms, but sadly not on a Mac. http://www.virtualdub.org

  • Commercial programs like VideoStudio Pro X8, or the Apple equivalent, can be used to polish your videos for the supplementary material section. www.videostudiopro.com

  • Spacetime is a code that can link data from an external stimulus to the corresponding images in time. spacetime.uithetblauw.nl

  • Different research groups are willing to share their own codes for image analysis, Lewys Jones included. http://www.lewysjones.com

Companies

  • http://www.attolight.com Manufactures cathodoluminescence detectors for S/TEM. Accessed in August 2015

  • http://www.comsol.com Multiphysics modeling software. Accessed in August 2015

  • http://www.denssolutions.com Solutions for in-situ microscopy: Stages for MEMS heating, gas and liquid cells. Accessed in August 2015

  • http://www.directelectron.com Producing high-speed and high DQE cameras for TEM. Accessed in August 2015

  • http://www.expresslo.com EXpressLO LLC: Quick FIB sample lift out and grid placement using visible optics. Accessed in August 2015

  • http://www.fei.com Producing ETEMs, temperature control stages, and former Nanofactory STM-TEM and Nanoindentation stage designs. Accessed in August 2015

  • http://www.fischione.com/products/holders Tomography holders and a heated gas stage. Accessed in August 2015

  • http://www.gatan.com/products/tem-specimen-holders Stages for temperature control, vacuum transfer, straining, and tomography. Producing high-frame-rate direct-electron-detection cameras, in addition to software and spectrometers. Accessed in August 2015

  • http://www.hitachi-hightech.com E-TEM products: MEMS heating gas injection, bulk heating gas injection, MEMS biasing, liquid-cell electrochemistry/static and flow, and zone holders. Accessed in August 2015

  • http://www.hummingbirdscientific.com Hummingbird Scientific designs and manufactures pioneering in-situ TEM specimen holders that enable electrical probing, sample heating, cooling and magnetizing, tomographic imaging, nano-manipulation and environmental TEM in liquids and gases. Accessed in August 2015

  • http://www.hysitron.com/products/pi-series Quantitative nanomechanics stages. The design for JEOL and FEI instruments have an important difference, which results from the diameter of the rod, and which we leave you to discover. Accessed in August 2015

  • http://www.IDES-inc.com Retrofitting TEMs for ultrafast imaging. Accessed in August 2015

  • http://www.nanofactory-user-group.org NanoFactory is now owned by FEI; this group supports users of non-FEI equipment. Accessed in August 2015

  • http://www.ni.com/labview System design software, graphical programming to code engineering systems. Accessed in August 2015

  • http://www.protochips.com Protochips provides complete in-situ TEM systems including Atmosphere for gas control and heating, Poseidon for liquid and electrochemistry, and Aduro for heating and electrical analysis. Accessed in August 2015

User Facilities

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Author information

Authors and Affiliations

  1. Sandia National Laboratories, CINT, Albuquerque, USA

    Katherine Jungjohann

  2. University of Connecticut, Storrs, Connecticut, USA

    C. Barry Carter

Authors
  1. Katherine Jungjohann
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  2. C. Barry Carter
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Corresponding author

Correspondence to Katherine Jungjohann .

Editor information

Editors and Affiliations

  1. University of Connecticut, Storrs, Connecticut, USA

    C. Barry Carter

  2. Ohio State University, Columbus, Ohio, USA

    David B. Williams

Appendix

Appendix

2.1.1 People

Gertrude Fleming Rempfer was born in Seattle in 1912 and died on October 4, 2011, in Portland, OR, aged 99. She worked in her lab with her microscopes until weeks before she died. She was working on photoemission TEMs when most people had forgotten that they existed. See Ultramicroscopy 119, pages 1–110 to learn more of her work.

Peter Roland Swann (February 4, 1935–July 14, 2013) made an e-cell TEM holder in ~1960. Interested in straining experiments at controlled temperatures when most wanted one or the other! He introduced CBC to TEM in 1970 and MGB to TEM a little later.

Ugo Valdrè was born on February 4, 1936 in Faenza Italy (also the birthplace of faience pottery), trained as a physicist and designed many early holders for in-situ studies; in 1971 he wrote “… we cherish the time when, reversing the present criteria, the electron microscope will be made to fit a predesigned universal specimen stage containing the facilities of a laboratory for specimen treatment.” Prescient.

Ahmed Hassan Zewail (born February 26, 1946 in Damanhur, Egypt, died 2 August 2016) won the 1999 Nobel Prize for Chemistry for his work on femtochemistry and made UEM work.

2.1.2 Self-Assessment Questions

Q2.1:

What is the pressure at the specimen in a conventional TEM – the one you use most days?

Q2.2:

Define nanoparticle.

Q2.3:

What is the difference between in situ and operando? What does ex situ TEM mean?

Q2.4:

You’ve seen several Latin terms, including those in the title. Do you think in silico experiments have a place in materials research?

Q2.5:

Why are nearly all TEM made for side-entry holders? Which are top-entry?

Q2.6:

Summarize the most important features of recording the data.

Q2.7:

What is a direct-detection camera and why are these cameras expensive?

Q2.8:

What is ImageJ and who provides it?

Q2.9:

What is DTEM and what is UEM?

Q2.10:

How many electrons do you need to produce a DP?

Q2.11:

For environmental TEM, we can use a holder or an ETEM. Explain the difference, suggest which you would prefer and explain your reasons.

Q2.12:

What voltage is preferred for operando studies?

Q2.13:

What is the challenge when you want to perform XEDS in an ETEM?

Q2.14:

For high-resolution imaging in an operando study, do you want to use STEM or TEM?

Q2.15:

Operando TEM is new. When were TEMs first used to study reactions in gases?

Q2.16:

What are the windows made from in modern gas or liquid operando holders?

Q2.17:

Why does window bowing happen when you are using a “liquid” holder.

Q2.18:

What are the advantages of using a MEMS device for heating your specimen.

Q2.19:

What is the BGPL?

Q2.20:

Why do we include UHV in the discussion of environment?

Q2.21:

Why do we call it Klug’s approach ?

Q2.22:

Why might you want to cool your specimen? Is this operando?

Q2.23:

Can you do operando experiments in specimens prepared by plunge freezing?

Q2.24:

How cold can the specimen be in cryo-TEM?

2.1.3 Text-Specific Questions

T2.1:

If you were to custom build a TEM holder, what considerations to the TEM are necessary to prevent damage to the instrument and have a operational stage? What additional requirements would you consider based on safety?

T2.2:

What is adaptive threshholding?

T2.3:

Discuss the state-of-the-art in drift correction, identify which method you favor (and why) and guess how this will improve in the future.

T2.4:

Compare and contrast DTEM and UEM.

T2.5:

Compare the difficulties of operando studies in gases versus in liquids.

T2.6:

Operando studies present a major challenge to the TEM manufacturers. Explain this statement.

T2.7:

How do we measure the partial pressure around the specimen in a TEM.

T2.8:

How much energy is needed to heat a 3-mm TEM specimen to 500 °C? Be sure to state your assumptions about the specimen geometry.

T2.9:

How much energy must be removed to change the temperature of a 1-µm-long nanowire of Si.

T2.10:

Discuss window bowing when you are using a liquid-cell holder and what to do about it.

T2.11:

Consider the schematic in Fig. 2.12. Why is there a pressure gap?

T2.12:

Discuss the reliability and accuracy of temperature measurement in the TEM.

T2.13:

Discuss how you would use the nanothermometer shown in Fig. 2.25.

T2.14:

Discuss how to stop the reaction and dewetting shown in Fig. 2.26.

T2.15:

Discuss the artifacts that might occur in the experiment illustrated in Fig. 2.36.

T2.16:

Compare the pros and cons of the crucible and filament-wire heating stages.

T2.17:

Discuss the advantages and disadvantages of using dog-bone specimens versus MEMS specimens for studying mechanical behavior.

T2.18:

What is a comb-drive electrostatic actuator and how does it function?

T2.19:

Summarize with bullets the challenges and considerations you must keep in mind when studying mechanical properties in the TEM.

T2.20:

Explain the contrast seen in Fig. 2.41.

T2.21:

Use bullets to summarize the pros and cons of studying mechanical properties using the method illustrated in Fig. 2.39.

T2.22:

Explain the contrast that we see in Fig. 2.43.

T2.23:

Why is the contrast in Fig. 2.47 in the lithiation of Ge so different from the Ge–Si core–shell structure?

T2.24:

Using the literature describe five other systems that have used the geometry shown in Fig. 2.52 to study the growth of nanowires.

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Jungjohann, K., Carter, C.B. (2016). In Situ and Operando . In: Carter, C., Williams, D. (eds) Transmission Electron Microscopy. Springer, Cham. https://doi.org/10.1007/978-3-319-26651-0_2

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