In situ lift-out dedicated techniques using FIB–SEM system for TEM specimen preparation

Tomus, Dacian; Ng, Hoi Pang

doi:10.1016/j.micron.2012.05.006

Cited by 81 publications

(35 citation statements)

References 10 publications

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“…STEM-HAADF images and selected area diffraction patterns (SADPs) were captured on a 200-keV FEI Tecnai G 2 F-20 Supertwin scanning-transmission electron microscope. TEM samples were prepared using a variation of the focused-ion-beam (FIB) lift-out method in an FEI Quanta 200 3D Dual Beam FIB microscope (FEI Company, Hillsboro, OR, USA) [48]. Discontinuous isothermal oxidation tests of the as-cast and annealed specimens were conducted at 1050 • C in a tube furnace under ambient laboratory air.…”

Section: Methodsmentioning

confidence: 99%

Influence of Annealing on the Microstructures and Oxidation Behaviors of Al8(CoCrFeNi)92, Al15(CoCrFeNi)85, and Al30(CoCrFeNi)70 High-Entropy Alloys

Butler

Weaver

2016

Metals

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Abstract:The understanding of the oxidation behaviors of as-cast and annealed high-entropy alloys (HEAs) is currently limited. This work systematically investigates the influence of annealing on the microstructures and oxidation behaviors of AlCoCrFeNi-based HEAs. Annealing was found to alter the distribution of Al-rich phases which caused a change in the oxidation mechanisms. In general, all three of the investigated HEAs displayed some degree of transient oxidation at 1050 • C that was later followed by protective, parabolic oxide growth. The respective oxidation behaviors are discussed relative to existing oxide formation models for Ni-Cr-Al alloys.

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Section: Methodsmentioning

confidence: 99%

Influence of Annealing on the Microstructures and Oxidation Behaviors of Al8(CoCrFeNi)92, Al15(CoCrFeNi)85, and Al30(CoCrFeNi)70 High-Entropy Alloys

Butler

Weaver

2016

Metals

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“…The initial steps of the TEM sample preparation procedure is identical to traditional lift out method, as explained elsewhere [21,22]. The only deviation from traditional liftout required for this particular application was the "welding" of the foil, using platinum, to the end of the TEM grid post along the entire length of the sample as shown in Fig.…”

Section: Materials and Experimental Proceduresmentioning

confidence: 99%

Micromechanical and in situ shear testing of Al–SiC nanolaminate composites in a transmission electron microscope (TEM)

Mayer

Mara

et al. 2015

Materials Science and Engineering: A

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a b s t r a c tNanolaminate composites show promise as high strength and toughness materials. However, due to the limited volume of these materials, micron scale mechanical testing methods must be used to determine the properties of these films. To this end, a novel approach combining a double notch shear testing geometry and compression with a flat punch in a nanoindenter was developed to determine the mechanical properties of these films under shear loading. To further elucidate the failure mechanisms under shear loading, in situ TEM experiments were performed using a double notch geometry cut into the TEM foil. Aluminum layer thicknesses of 50 nm and 100 nm were used to show the effect of constraint on the deformation. Higher shear strength was observed in the 50 nm sample (690 7 54 MPa) compared to the 100 nm sample (423 728.7 MPa). Additionally, failure occurred close to the Al-SiC interface in the 50 nm sample as opposed to failure within the Al layer in the 100 nm sample.

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“…8,9 These two approaches were boosted by the focused ion beam (FIB) technique, which made specimen preparation significantly easier compared to conventional techniques. 10 These techniques have advanced our understanding Ó 2015 The Minerals, Metals & Materials Society of the fundamentals of mechanical deformation and damage mechanisms. 3,11,12 They also have inspired the development of a new breed of in situ TEM techniques involving scanning probe microscopy, 13 electrochemistry 14 and chemical reactors for materials synthesis, 15 to name a few.…”

Section: Introductionmentioning

confidence: 99%

In Situ Microstructural Control and Mechanical Testing Inside the Transmission Electron Microscope at Elevated Temperatures

Wang

Haque

2015

JOM

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With atomic-scale imaging and analytical capabilities such as electron diffraction and energy-loss spectroscopy, the transmission electron microscope has allowed access to the internal microstructure of materials like no other microscopy. It has been mostly a passive or post-mortem analysis tool, but that trend is changing with in situ straining, heating and electrical biasing. In this study, we design and demonstrate a multi-functional microchip that integrates actuators, sensors, heaters and electrodes with freestanding electron transparent specimens. In addition to mechanical testing at elevated temperatures, the chip can actively control microstructures (grain growth and phase change) of the specimen material. Using nano-crystalline aluminum, nickel and zirconium as specimen materials, we demonstrate these novel capabilities inside the microscope. Our approach of active microstructural control and quantitative testing with real-time visualization can influence mechanistic modeling by providing direct and accurate evidence of the fundamental mechanisms behind materials behavior.

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In situ lift-out dedicated techniques using FIB–SEM system for TEM specimen preparation

Cited by 81 publications

References 10 publications

Influence of Annealing on the Microstructures and Oxidation Behaviors of Al8(CoCrFeNi)92, Al15(CoCrFeNi)85, and Al30(CoCrFeNi)70 High-Entropy Alloys

Influence of Annealing on the Microstructures and Oxidation Behaviors of Al8(CoCrFeNi)92, Al15(CoCrFeNi)85, and Al30(CoCrFeNi)70 High-Entropy Alloys

Micromechanical and in situ shear testing of Al–SiC nanolaminate composites in a transmission electron microscope (TEM)

In Situ Microstructural Control and Mechanical Testing Inside the Transmission Electron Microscope at Elevated Temperatures

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