Синтез и свойства замещённых Hg-содержащих сложных оксидов меди тема диссертации и автореферата по ВАК РФ 02.00.21, кандидат химических наук Павлов, Дмитрий Алексеевич

• Павлов, Дмитрий Алексеевич
• кандидат химических наук
• 2004

Оглавление диссертации кандидат химических наук Павлов, Дмитрий Алексеевич

Введение

Литературный обзор

Кристаллохимия сложных оксидов меди AmZ2Qn-iCunOm+i+2n

Типы слоев и структурных блоков Номенклатура. Четырёхзначная система обозначений

Кристаллохимия соединений HgBa2Ca„.iCun02n+2+5 (n = 1,2 и 3)

Введение и общие особенности строения Кристаллическая структура HgBa2Cu04+5 (Hg-1201)

Кристаллическая структура НдВагСаСигОб+б (Hg-1212) <

Кристаллическая структура HgBa2Ca2Cu30s+5 (Hg-1223)

Синтез соединений ряда HgBa2Can.iCun02n+2+s

Особенности синтеза в запаянных ампулах Оптимизация процесса синтеза в запаянных ампулах

Замещения в структурах Hg-содержащих купратов

Замещения в катионной подрешётке

Структуры с замещением атомов ртути Структуры с замещением атомов бария Замещения в анионной подрешётке Методы синтеза оксофторидов

Исследование оксофторидов Hg-содержащих купратов

Допирование Hg-содержащих купратов носителями заряда

Механизмы допирования Hg-содержащих купратов

Взаимосвязь "структура - сверхпроводящие свойства"

Введение. Некоторые общие определения Влияние структурных факторов на Гс Влияние структурных факторов на Нт.

Экспериментальная часть

Методы синтеза

Получение исходных веществ Синтез Hg-содержащих купратов

Использование флюса Термическая обработка полученных соединений Окисление Восстановление Фторирование

Методы исследования

Рентгенофазовый анализ

Локальный рентгеноспектральный анализ

ИК-спектроско11 ия

Исследование протяжённой тонкой структуры рентгеновского спектра Магнитные измерения

Методы определения р и vcp.cu

Термогравиметрия и титриметрия Рентгеновская и нейтронная дифракция Исследование тонкой структуры края поглощения

Синтез в запаянных кварцевых ампулах

Синтез с использованием флюса LiF

Исследование анион-замещённых Hg-содержащих купратов

Оксофториды на основе Hg-1212 Оксофториды на основе Hg

Оксофторид состава (Hgo sTlo.2)Ba2Ca2Cu3Os(0,F)s Оксофториды HgBa2Ca2Cu3Os(0,F)snod высоким давлением

Исследование линий необратимости Hg-содержащих купратов

Линии необратимости для купратов на основе Hg-1223 Зависимости х(Т) Магнитная фазовая диаграмма Линии необратимости для купратов на основе Hg-1212 Дифференциальный парамагнитный эффект Зависимости х(Т) Магнитная фазовая диаграмма

Исследование катион-замещснных купратов на основе Hg

РФА и JIPCA

Метод анализа ПТСРС и ИК-спектроскопия Метод анализа ТСКП

Идентификация пиков в спектрах

Количественный анализ концентрации носителей заряда Исследование линий необратимости для купратов на основе Hg

Зависимости хСО Магнитные фазовые диаграммы

Обсуждение результатов

Влияние фактора анизотропии

Влияние степени допирования носителями заряда

Благодарности

Выводы

Заключение диссертации по теме «Химия твердого тела», Павлов, Дмитрий Алексеевич

Выводы

1. Разработан метод синтеза Hg-содержащих сверхпроводников в запаянных кварцевых ампулах с использованием флюса LiF, в результате чего получены образцы с высоким содержанием фазы HgBaaCaCi^Oe+s.

2. С использованием в качестве фторирующего агента дифторида ксенона (XeF2) получены оксофториды на основе Hg-1212 с различными значениями Тс. Впервые получены фторированные образцы Hg-1212 в переокисленном состоянии. Показано, что зависимость Тс от величины параметра а для фторированного Hg-1212 имеет куполообразный характер, аналогичный установленному ранее для Hg-1201 и Hg-1223.

3. Оксофторид HgBa2Ca2Cu30g(0,F)5 впервые исследован под высоким давлением. Показано, что данное соединение проявляет рекордное среди всех известных сверхпроводников значение Тс = 166К при давлении ~ 23 ГПа.

4. Изучение зависимостей Hm{Т) для соединений на основе фаз Hg-1212 и Hg-1223 показано, что образцы с замещениями в катиоиной и анионной подрешётках обладают улучшенным положением линий необратимости по сравнению с незамещёнными аналогами.

5. Проведённое комплексное физико-химическое исследование соединений состава (Hgo.9Mo.i)Ba2Cu04+5 (где М = Tl, Pb, W, Мо, Nb и V) показало, что изменение степени допирования носителями заряда является важным структурным фактором, определяющим положение линии необратимости данных соединений. На основании исследований ряда катион-замещённых образцов (IIg,M)-1201 было установлено, что наилучшим положением линии необратимости среди них обладает (Hgo.9Moo.i)Ba2Cu04+s

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