Investigation of the aluminium-aluminium oxide reversible transformation as observed by hot stage electron microscopy

Grove, C. A.; Judd, G.; Ansell, G. S.

doi:10.1007/bf02403402

Cited by 62 publications

(3 citation statements)

References 8 publications

(7 reference statements)

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“…The effects of alloying additions on the oxidation of A1 over a range of temperatures and pressures has been studied by Scamans andButler (1975, 1976). Oxidation of pure A1 at 0.01 N m-2 pressure produced homogeneously nucleated crystals of yA1203 whose density was 1012 m-2 at 750 K and 6 x 1012 m-2 at 790 K. No evidence was found for the formation of A1 islands within the amorphous oxide in those areas exposed to the electron beam, as had previously been reported during in situ oxidation studies of high-purity AI (Grove et al 1972). The addition of 5% Mg resulted in complete coverage within 1 min at 750 K of 50-75 nm crystals of MgA1204 spinel.…”

Section: Oxidaiion and Reductionsupporting

confidence: 71%

In situ experiments in the transmission electron microscope

Butler

1979

Rep. Prog. Phys.

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The possibility of using the objective region of a transmission electron microscope as a microlaboratory has long intrigued electron microscopists. They recognised that experiments conducted on specimens inside the microscope could provide direct evidence for the way in which a material responded to a change in state or environment. Such sophisticated experiments cannot be undertaken lightly. They involve the use of special stages designed to alter the state of a specimen in a controlled and measurable way, while at the same time permitting the continuous observation of the microstructure of the material. It is the purpose of this article to review the principles and practice of in situ experimentation in both conventional 100 kV microscopes and those operating at a higher accelerating potential, to provide a practical guide to the electron microscopist.The introductory sections deal with the important question of selecting the optimum image recording technique for the process being studied, and a discussion of the factors that can affect the validity of in situ observations. A description of the design and construction of in situ stages follows and serves to highlight the ingenuity of stage designers faced with the problem of providing services to the specimen in the restricted pole-piece gap region of a microscope without compromising microscope performance. Here an attempt has been made to describe selected stages which fulfil the basic principles of good stage design and which have been successfully employed to carry out in situ experiments. Discussion is confined to the four main types of stages fulfilling the functions of heating and cooling, deformation, environmental control and Lorentz imaging. The experimental application of in situ techniques forms the major part of this review. Emphasis has been placed on investigations producing results which could not have been obtained using other techniques, such as the direct observation of the movement, multiplication and interaction of dislocations, and the development of microstructural instabilities in crystalline solids subjected to electron irradiation. This section illustrates the unique nature of the information that can be obtained both at the qualitative and quantitative level by in situ experimentation.

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Section: Oxidaiion and Reductionsupporting

confidence: 71%

In situ experiments in the transmission electron microscope

Butler

1979

Rep. Prog. Phys.

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“…The effect of the microstructure on the spall (damage) response has been studied extensively. The body of literature spans from the classic works by Barbee, Curran and Seaman, [10][11][12] to Meyers et al, 13 Gray et al, [6][7][8] and recently by Minich et al, [14][15][16] among many others. [17][18][19] However, most of the cited work has focused on the effects of microstructure on pull-back measurements in experiments in which the sample experienced complete failure.…”

Section: Introductionmentioning

confidence: 99%

Effects of grain size and boundary structure on the dynamic tensile response of copper

Escobedo¹,

Dennis-Koller²,

Cerreta³

et al. 2011

Journal of Applied Physics

164

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Plate impact experiments have been carried out to examine the influence of grain boundary characteristics on the dynamic tensile response of Cu samples with grain sizes of 30, 60, 100, and 200 lm. The peak compressive stress is $1.50 GPa for all experiments, low enough to cause an early stage of incipient spall damage that is correlated to the surrounding microstructure in metallographic analysis. The experimental configuration used in this work permits real-time measurements of the sample free surface velocity histories, soft-recovery, and postimpact examination of the damaged microstructure. The resulting tensile damage in the recovered samples is examined using optical and electron microscopy along with micro x-ray tomography. The free surface velocity measurements are used to calculate spall strength values and show no significant effect of the grain size. However, differences are observed in the free surface velocity behavior after the pull-back minima, when reacceleration occurs. The magnitude of the spall peak and its acceleration rate are dependent upon the grain size. The quantitative, postimpact, metallographic analyses of recovered samples show that for the materials with grain sizes larger than 30 lm, the void volume fraction and the average void size increase with increasing grain size. In the 30 and 200 lm samples, void coalescence is observed to dominate the void growth behavior, whereas in 60 and 100 lm samples, void growth is dominated by the growth of isolated voids. Electron backscatter diffraction (EBSD) observations show that voids preferentially nucleate and grow at grain boundaries with high angle misorientation. However, special boundaries corresponding to Rl (low angle, < 5) and R3 ($60 <111> misorientation) types are more resistant to void formation. Finally, micro x-ray tomography results show three dimensional (3D) views of the damage fields consistent with the two dimensional (2D) surface observations. Based on these findings, mechanisms for the void growth and coalescence are proposed. V

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“…Above ~327°C the sticking probability decreases. This explains the observation that at higher temperatures the formation of the amorphous oxide layer proceeds through formation of oxide "islands" and complete surface oxidation takes longer than at lower temperatures [50,51].…”

Section: Aluminum Oxidationmentioning

confidence: 88%

Evaluation of Aluminum-Boron Carbide Neutron Absorbing Materials for Interim Storage of Used Nuclear Fuel

Wierschke¹

2015

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Investigation of the aluminium-aluminium oxide reversible transformation as observed by hot stage electron microscopy

Cited by 62 publications

References 8 publications

In situ experiments in the transmission electron microscope

In situ experiments in the transmission electron microscope

Effects of grain size and boundary structure on the dynamic tensile response of copper

Evaluation of Aluminum-Boron Carbide Neutron Absorbing Materials for Interim Storage of Used Nuclear Fuel

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