RU2004103976A - Способ получения тетрафторсилана, метод анализа примесей в тетрафторсилане и газ на его основе - Google Patents

Способ получения тетрафторсилана, метод анализа примесей в тетрафторсилане и газ на его основе Download PDF

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RU2004103976A
RU2004103976A RU2004103976/15A RU2004103976A RU2004103976A RU 2004103976 A RU2004103976 A RU 2004103976A RU 2004103976/15 A RU2004103976/15 A RU 2004103976/15A RU 2004103976 A RU2004103976 A RU 2004103976A RU 2004103976 A RU2004103976 A RU 2004103976A
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tetrafluorosilane
stage
gaseous
gas
impurities
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RU2004103976/15A
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RU2274603C2 (ru
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Хитоси АТОБЕ (JP)
Хитоси АТОБЕ
Масаказу ОКА (JP)
Масаказу ОКА
Тораити КАНЕКО (JP)
Тораити КАНЕКО
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Сова Денко К.К. (Jp)
Сова Денко К.К.
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Claims (25)

1. Способ получения тетрафторсилана, включающий стадию (1) нагревания гексафторсиликата, стадию (2-1) реакции газообразного тетрафторсилана, содержащего гексафтордисилоксан, образовавшийся на стадии (1) с газообразным фтором, стадию (2-2) реакции газообразного тетрафторсилана, содержащего гексафтордисилоксан, образовавшийся на стадии (1) с фтористым соединением многовалентного металла, или стадию (2-1) реакции газообразного тетрафторсилана, содержащего гексафтордисилоксан, образовавшийся на стадии (1) с газообразным фтором, и стадию (2-3) реакции газообразного тетрафторсилана, полученного на стадии (2-1) с фтористым соединением многовалентного металла.
2. Способ по п.1, в котором стадию (1) проводят при температуре 400°С или выше.
3. Способ по п.1, в котором стадию (2-1) проводят при температуре 100-350°С.
4. Способ по п.1, в котором стадию (2-2) или стадию (2-3) проводят при температуре 50-350°С.
5. Способ по любому из пп.1-4, в котором гексафторсиликат представляет собой, по меньшей мере, одно соединение, выбранное из группы, состоящей из гексафторсиликата щелочного металла или гексафторсиликата щелочноземельного металла.
6. Способ по п.1, в котором гексафторсиликат измельчают и сушат перед проведением стадии (1).
7. Способ по п.1, в котором фтористое соединение многовалентного металла представляет собой, по меньшей мере, одно соединение, выбранное из группы, состоящей из CoF3, MnF3, MnF4, AgF2, CeF4, PbF4 и K3NiF7.
8. Способ по п.1, в котором используют фтористое соединение многовалентного металла на носителе.
9. Способ по п.8, в котором носитель получают фторированием, по меньшей мере, одного соединения, выбранного из группы, состоящей из оксида алюминия, оксида титана и оксида циркония.
10. Способ по п.1, в котором стадию (2-2) или стадию (2-3) проводят в присутствии газообразного фтора.
11. Способ по п.1, включающий стадию (3) контактирования кремния с газообразным тетрафторсиланом, полученным на стадии (2-1), стадии (2-2) или стадиях (2-1)и(2-3).
12. Способ по п.11, в котором стадию (3) проводят при температуре 50°С или выше.
13. Способ по п.11 или 12, в котором перед проведением стадии (3) кремний подвергают термообработке в присутствии инертного газа при 400°С или выше.
14. Способ по п.1, включающий стадию (4), заключающуюся в контактировании газа, полученного на стадии (2-1), стадии (2-2), стадиях (2-1) и (2-3), стадиях (2-1) и (3), стадиях (2-2) и (3), или стадиях (2-1), (2-3) и (3), с газоразделительной мембраной и/или молекулярно-ситовым углеродом.
15. Способ по п.14, в котором газоразделительная мембрана представляет собой SiO2-ZrO2 керамическую мембрану и/или поли(4-метилпентен-1) гетерогенизированную мембрану.
16. Способ по п.14, в котором молекулярно-ситовой углерод имеет размер пор 5Å или менее.
17. Высокочистый тетрафторсилан, содержащий гексафтордисилоксан в количестве 1 об.млн-1 или менее, полученный способом по любому из пп.1-16.
18. Высокочистый тетрафторсилан по п.17, содержащий гексафтордисилоксан в количестве 0,1 об.млн-1 или менее.
19. Метод анализа примесей в высокочистом тетрафторсилане, заключающийся в контактировании тетрафторсилана, содержащего в качестве примесей газообразный H2, газообразный O2, газообразный N2, газообразный СО, газообразный СН4 и/или газообразный СО2, с адсорбентом с целью отделения указанных примесей от тетрафторсилана, и введении указанных примесей совместно с газом-носителем в газовый хроматограф с целью анализа примесей.
20. способ по пункту 19, в котором адсорбент представляет собой активированный уголь, сферический активированный уголь на основе нефтяного пека и/или молекулярно-ситовой углерод с размером пор 6Å или более.
21. Метод анализа примесей в высокочистом тетрафторсилане, заключающийся в введении тетрафторсилана, содержащего гексафтордисилоксан в качестве примеси в оптическую ячейку, окно которой изготовлено из галогенида металла, и анализе гексафтордисилоксана и/или фтористого водорода методом инфракрасной спектрометрии.
22. Способ по п.1, в котором способ по любому из пп.19-21 используется для контроля процесса.
23. Газ, предназначенный для производства оптического волокна, включающий газообразный тетрафторсилан, полученный способом по любому из пп.1-16.
24. Газ, предназначенный для производства полупроводников, включающий газообразный тетрафторсилан, полученный способом по любому из пп.1-16.
25. Газ, предназначенный для производства элемента солнечной батареи, включающий газообразный тетрафторсилан, полученный способом по любому из пп.1-16.
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