Electron microscopy of ceramic materials based on thermal power plant fly ash

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Resumo

The importance of studying ceramic materials microstructure for controlling sintering processes which provide ceramic masses required performance characteristics is shown. The scanning electron microscopy (SEM) informativity in carrying out parametric structural analysis of building materials is noted. The physical principles that ensure electron microscopy high resolution and the various optical systems characteristics used in microscopic research methods are given. The samples prepared on modern equipment with application of a conductive layer on their surface were investigated, SEM and energy dispersive spectroscopy (EDS) were carried out using a KYKY EM 6900 electron microscope. Microstructure and features of pore space of the ceramic materials based on thermal power plant fly ash have been studied. A step-by-step procedure for setting up and conducting experiments is described, including study of the matrix structure at microscope resolution different limits, study of the matrix composite nuclei pore microstructure and the sample scanned surface elemental composition. The total elements concentration of EDS spectrum of the ceramic sample based on fly ash is presented. The SEM studies results are described indicating the peculiarities of the ceramic composite matrix structure formation that is a boundary layer forming a transition zone between the matrix and the core of the composite material. Features of the nuclei pore space fiber structure formation with fibers disorderly arrangement and abundance of air spaces between them.

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Sobre autores

A. Stolboushkin

Siberian State Industrial University

Autor responsável pela correspondência
Email: stanyr@list.ru

Doctor of Sciences (Engineering)

Rússia, 42, Kirova Street, Novokuznetsk, 654007

E. Isterin

Siberian State Industrial University

Email: eisterin@gmail.com

Engineer

Rússia, 42, Kirova Street, Novokuznetsk, 654007

O. Fomina

Mechanical Engineering Research Institute of the Russian Academy of Sciences

Email: soa2@mail.ru

Candidate of Sciences (Engineering)

Rússia, 4, Maly Kharitonyevsky Pereulok, Moscow, 101990

Bibliografia

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2. Fig. 1. Abrasive cutting machine METACUT-250: а – general view; b – double work table with T-shaped slots; 1 – diamond cutting disk; 2 – vice-type clamping device; 3 – liquid supply nozzles; 4 – metal guides; 5 – ceramic sample for SEM examination

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3. Fig. 2. Zenko Plasma tabletop carbon coating system: а – general view of the device; b – loading a ceramic sample into a vacuum chamber; c – pulsed heating of the chamber; d – 7-inch color touch screen with vacuum diagram, pulsed heating current and deposition of carbon fiber layers

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4. Fig. 3. Scanning electron microscope KYKY EM 6900: а – general view of the device; b – vacuum chamber; c – energy dispersive analyzer Oxford Xplore; d – loading the sample into the microscope; e – installing the ceramic sample on the working table: 1 – electron gun; 2 – sample positioning system; 3 – reflected electron detector; 4 – working table; 5 – sample with a dedicated area for observations

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5. Fig. 4. Image of the structure of a ceramic sample based on fly ash: а – zone B is a core covered with a shell; b – zone C is a shell (matrix) formed from the coating layer of the granule, and zone D is a core formed from an aggregated granule. Shooting conditions: SEM, 20 (а); 65 (b)

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6. Fig. 5. Image of the microstructure of a ceramic sample based on fly ash: (а, b, c) zone C is the matrix of the composite material; (d, e, f) zone D is the core of the composite material. Shooting conditions: SEM, 160 (а); 400 (b); 2000 (c); 80 (d); 400 (e); 1800 (f)

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7. Fig. 6. Image of the pore structure of the cores of a ceramic sample based on fly ash: 1 – pore; 2 – ash microsphere. Shooting conditions: SEM, 120 (а); 400 (b); 200 (c); 550 (d)

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8. Fig. 7. Energy dispersive microanalysis of a ceramic sample based on fly ash: а – electron image of the map; b – multilayer image of the EDS map; c – total spectrum of the EDS map

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9. Fig. 8. Layered color image of the EDS map of a ceramic sample based on fly ash for the main chemical elements: 1 – Fe; 2 – Ca; 3 – Si; 4 – Al; 5 – O; 6 – Mg

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