Abstract
The paper presents the research results of the fine structure of coke which was received on the basis of coal tar pitch after oxidation in thin layers on the surface of graphite foam bubble walls. After oxidation the mixture of expanded graphite and pitch (8%) was milled, and workpieces obtained from powder were baked and gained the density of 1.5 g/cm3 due to shrinkage. The thickness of bubble walls is 5 nm, the thickness of pitch coke layers between bubble walls is one order of magnitude greater. The fine structure of coke was examined by X-ray diffraction and transmission electron microscopy. Peaks of 002 lines, narrow for the graphite foam and broad for the baked coke, show that the material consists of two phases, the coke 002 line is broadened towards small angles. Coke structure in baked workpieces is formed by single graphite-like layers of limited sizes. Separate layers are curved and form a polydisperse fullerene-like and closed globular structure with a globule size up to 20 nm. Pitch coke layers and bubble walls are sintered without cracking. Sequences of onion-like multilayer structures of up to 5 nm were detected on the wall surface of the graphite foam bubbles. The mechanism of oxidized pitch degradation during the formation of globular non-graphitized structures was suggested. During coking aromatic molecules of adjacent layers are joined by carbon-carbon chemical bonds in curved graphite-like layers. Curving of the graphite-like layers synthesized near the walls is possible in the direction from bubble walls thus leading to the formation of onion-like structures.
Highlights
Ключевые слова: кокс; пенографит; каменноугольный пек; окисление; слой; турбостратная структура; просвечивающий электронный микроскоп; замкнутые глобулярные структуры; луковичные структуры
After oxidation the mixture of expanded graphite and pitch (8%) was milled, and workpieces obtained from powder were baked and gained the density of 1.5 g/cm3 due to shrinkage
Bulletin of the South Ural State University
Summary
Экспериментальная часть Для исследования тонкой структуры слоев обожженного кокса между стенками пузырьков пенографита в качестве образцов использовали углеродный материал, полученный согласно [3] с окислением пека в тонких слоях на поверхности стенок пузырьков пенографита при ~ 275 °С. 1. Прочность обожженного материала значительно превышает прочность графитированного, после графитации возрастают dk и в меньшей мере di. Для характеристики тонкой структуры кокса в составе углеродного материала использовали методы просвечивающей электронной микроскопии и рентгеноструктурного анализа. 1), типичны для углеродных материалов с невысокой степенью упорядоченности; отсутствуют линии, характерные для трехмерно упорядоченного графита. Также виден сдвинутый в сторону больших углов острый пик пенографита, площадь пика значительно меньше площади сильно размытой линии 002 пекового кокса. Специально проведенные рентгенографические исследования графитированного материала показали, что отдельная линия 002 пенографита на фоне более интенсивной линии 002 графитированного пекового кокса не выделяется. Прочность на сжатие (σсжатие), кажущаяся (dk) и пикнометрическая (di) плотности углеродного материала после обжига и после графитации
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