Thermochemical Etching Method for Ceramics

Owate, I. O.; Freer, Robert

doi:10.1111/j.1151-2916.1992.tb05567.x

Cited by 15 publications

(5 citation statements)

References 8 publications

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“…Both methods require either the use of hazardous chemicals [2] or long heat treatments that often have to be optimised when working with new materials [3]. Finally, thermal etching could bias the measurements of grain sizes, particularly when grain growth, surface modifications [4,5,6,7], and/or secondary phase precipitation at the grain boundaries [8] occur during the heat treatment.…”

Section: Introductionmentioning

confidence: 99%

SEraMic: A semi-automatic method for the segmentation of grain boundaries

Podor

Goff

Lautru

et al. 2021

Journal of the European Ceramic Society

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The SEraMic method, implemented in the SEraMic plugin for Fiji or ImageJ software, was developed to calculate a segmented image of a ceramic cross section that shows the grain boundaries. This method was used to accurately and automatically determine grain boundary positions and further assess the grain size distribution of monophasic ceramics, metals, and alloys. The only required sample preparation is polishing the cross section to a mirror-like finish. The SEraMic method is based on at least six backscattered electron scanning electron microscopy images of a unique region of interest with various tilt angles ranging from -5° to +5°, which emphasises the orientation contrasts of the grains.Because the orientation contrast varies with the incident beam angle on the sample, the set of images contains information related to all the grain boundaries. The SEraMic plugin automatically calculates and builds a segmented image of the grain boundaries from the set of tilted images. The SEraMic method was compared with classical thermal etching methods, and it was applied to determine the grain boundaries in various types of materials (oxides, phosphates, carbides, and alloys). The method remains easy to use and accurate when the average grain diameter is greater than or equal to 0.25 µm.

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Section: Introductionmentioning

confidence: 99%

SEraMic: A semi-automatic method for the segmentation of grain boundaries

Podor

Goff

Lautru

et al. 2021

Journal of the European Ceramic Society

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“…For a ceramic that fractures in the intergranular fracture mode, the contrast between the grains and grain boundaries cannot be easily distinguished on the fracture surface due to the existence of glassy phases and impurities segregated on grain boundaries. In this case, similar post-processing steps, including grinding, polishing, and etching, are needed for successful imaging [5][6][7]. However, during the grinding and polishing processes, the practical morphology of the microstructure could be somehow destroyed [8][9][10].…”

Section: Introductionmentioning

confidence: 99%

A Polishing-free Etching Method for Microstructure Observation of Fine-grained Ceramics

Liu¹,

Shimai²,

Zhao³

et al. 2020

Preprint

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Microstructural studies are very important because of their decisive role in the properties of advanced ceramics. During the sample preparation process, it is critical to grind, polish, and etch the fracture surface of the ceramic for effective microstructure observation. Here, a sample preparation process is proposed by directly etching the fracture surface of the ceramic without the time-consuming grinding and polishing. We used this method to create micrographs for MgAl2O4, Al2O3, and ZrO2 ceramics with an average grain size less than 1 μm; these were clearly resolved by SEM. More importantly, the damage resulting from grinding or polishing is minimized and SEM images taken from samples prepared via this new method are closer to the original morphology of the microstructures. This method also greatly simplifies the sample preparation process and is especially suitable for fine-grained ceramics.

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“…There are several publications presenting recommended conditions for various dense materials. The general recommendation is that the thermal etching should be performed at 50-200 °C below the sintering temperature for a certain amount of time [1][2][3][4][5][6][7]. In addition, there are recommendations which advice to utilize absolute etching temperatures -for an example the thermal etching of alumina: 1500 °C for 20-30 min [1], 1100-1300 °C for 120 min [1], 1300-1400 °C for 15-20 min [6], 1500 °C for 120 min [7].…”

Section: Introductionmentioning

confidence: 99%

The comprehensive study of the thermal etching conditions for partially and fully dense ceramic samples

2019

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An alternative approach to the thermal etching of oxide ceramic materials (αalumina, t-zirconia, and c-zirconia) is presented and compared with the standardly used regime for thermal etching. The given approach was tested on partially (93.8 -96.3 % t.d.) and fully (99 -100 % t.d.) dense samples with the criterion of minimizing the density difference after and before etching and with the criterion of clear visibility of grain boundaries. The presented results show, that 900 °C/1 h etching regime is sufficient to reveal the studied microstructure for analysis of the surface of the samples sintered above 1355 °C without affecting the density and without thermal effect on the measured average grain size. The modern approaches as digital analysis of the images can help to reveal the thin grain boundaries after thermal etching at low temperatures.

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Thermochemical Etching Method for Ceramics

Cited by 15 publications

References 8 publications

SEraMic: A semi-automatic method for the segmentation of grain boundaries

SEraMic: A semi-automatic method for the segmentation of grain boundaries

A Polishing-free Etching Method for Microstructure Observation of Fine-grained Ceramics

The comprehensive study of the thermal etching conditions for partially and fully dense ceramic samples

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