SU327781A1 - The method of obtaining monosilane - Google Patents
The method of obtaining monosilaneInfo
- Publication number
- SU327781A1 SU327781A1 SU1440706A SU1440706A SU327781A1 SU 327781 A1 SU327781 A1 SU 327781A1 SU 1440706 A SU1440706 A SU 1440706A SU 1440706 A SU1440706 A SU 1440706A SU 327781 A1 SU327781 A1 SU 327781A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- monosilane
- obtaining
- tetraethoxysilane
- sodium hydride
- hydride
- Prior art date
Links
- 238000000034 method Methods 0.000 title claims description 13
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 title claims description 9
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 claims description 6
- 229910000104 sodium hydride Inorganic materials 0.000 claims description 6
- 239000012312 sodium hydride Substances 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- 150000004678 hydrides Chemical class 0.000 claims 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- MCULRUJILOGHCJ-UHFFFAOYSA-N triisobutylaluminium Chemical compound CC(C)C[Al](CC(C)C)CC(C)C MCULRUJILOGHCJ-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Silicon Compounds (AREA)
Description
Изобретение относитс к химической и электронной промышленности, в частности к получению моносилана особой степени чистоты, пригодного дл использовани эпитаксиальной технологии изготовлени полупроводниковых приборов.The invention relates to the chemical and electronic industries, in particular, to obtaining monosilane of special purity suitable for the use of epitaxial technology for the manufacture of semiconductor devices.
Известен способ получени моносилана путем восстановлени соединений кремни , в частности тетраэтоксисилана, комплексным алюмогидридами в среде растворителей. Процесс ведут при ISG-IGO C в течение нескольких часов.A known method of producing monosilane by reducing silicon compounds, in particular tetraethoxysilane, with complex aluminum hydrides in the medium of solvents. The process is carried out at ISG-IGO C for several hours.
Недостатками известного способа вл ютс довольно высока температура процесса , его длительность и дефицитность указанных восстановителей.The disadvantages of this method are quite high process temperature, its duration and deficiency of these reducing agents.
Дл упрощени процесса, а также повышени степени чистоты получаемого продукта предлагаетс восстанавливать тетра- алкоксисиланы, например тетраэтоксисилан, гидридом натри , который вл етс дешевым и легкодоступным продуктом. Кроме того, гидрид натри не содержит примесей углерода и элементов III и V групп, посTo simplify the process, as well as to increase the purity of the product obtained, it is proposed to reduce tetra-alkoxysilanes, for example tetraethoxysilane, with sodium hydride, which is a cheap and readily available product. In addition, sodium hydride does not contain carbon impurities and elements of the III and V groups, after
кольку их летучие соединени удал ютс в процессе его получени .since their volatile compounds are removed during its preparation.
Восстановление тетраэтоксисилана гидридом натри до моносилана происходит в присутствии алюминийалкилов, вз тыхThe reduction of tetraethoxysilane with sodium hydride to monosilane occurs in the presence of aluminum alkyls taken
шению к гидриду натри to sodium hydride
4NQiH-v4AtP +Si()-.-SiH 44NaAEPj-OC.H. Реакци протекает в интервале темпера0 тур 4-1ОО°С с высоким выходом ( не ни же 96% от теоретического), который зависит от пор дка смешени компонентов. Процесс может проводитьс без растворител в избытке тетраэтоксисилана, что . 4NQiH-v4AtP + Si () -.- SiH 44NaAEPj-OC.H. The reaction takes place in a temperature range of 4-1OO ° C in high yield (not less than 96% of the theoretical), which depends on the order of mixing the components. The process can be carried out without solvent in excess of tetraethoxysilane, which.
5 способствует получению более чистого моносилана . Поскольку освоено производство очень чистых алкоксисиланов, например тетраэтоксисилана с суммарным содержанием определ емых примесей до , 5 contributes to a cleaner monosilane. Since the production of very pure alkoxysilanes is mastered, for example, tetraethoxysilane with a total content of detectable impurities up to
0 процесс дает возможность получать моносилан высокой степени чистоты.The 0 process makes it possible to obtain high purity monosilane.
в нелетучие боргидриды,что обеспечивает глубокую очистку мои осилена от дибор на в процессе получени и значительно упрощает стадию очистки продукта.into nonvolatile borohydrides, which ensures deep cleaning of my sediment from dibor in the process of obtaining and greatly simplifies the stage of purification of the product.
Пример, В кварцевый реактор, предварительно заполненный сухим аргоном с магнитной мешалкой, обратньм холодильником , соединенным с двум ловушками, охлаждаемыми смесью из сухого льда, ацетона и спирта, термометром и капельной воронкой заливают 2О мл толуола и 22,2 г триизобутилалюмини . При помощи дозатора в реактор при комнатной температуре добавл ют измельченный гидрид натри в количестве 4,82 г. К полученному раствору при перемешивании постепенно прибавл ют 5,2 г тетраэтоксисилана марки ОСЧ. В ходе реакции температура поднимаетс от 2О до . Выдел ющийс моносилан дл очистки от паров тетраэтоксисилана и толуола пропускают через охлажденные до -78°С ловушки. Выход моExample: In a quartz reactor, pre-filled with dry argon with a magnetic stirrer, an inverse cooler connected to two traps cooled with a mixture of dry ice, acetone and alcohol, a thermometer and a dropping funnel, pour 2 O ml of toluene and 22.2 g of triisobutyl aluminum. Using a metering device, crushed sodium hydride was added to the reactor at room temperature in an amount of 4.82 g. To the resulting solution, 5.2 g of tetraethoxysilane grade OCh was gradually added to the resulting solution. During the reaction, the temperature rises from 2O to. Separated monosilane for purification from tetraethoxysilane vapor and toluene is passed through traps cooled to -78 ° C. Exit mo
носилана, определ емый по весу кремни , полученного термическим разложением моносилана при ЭОО-С, 97% от теоретического . Реакци заканчиваетс в течение 5 мин.the nosilane, determined by the weight of silicon obtained by thermal decomposition of monosilane at EOO-C, is 97% of the theoretical value. The reaction is complete within 5 minutes.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU1440706A SU327781A1 (en) | 1970-06-05 | 1970-06-05 | The method of obtaining monosilane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU1440706A SU327781A1 (en) | 1970-06-05 | 1970-06-05 | The method of obtaining monosilane |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU327781A1 true SU327781A1 (en) | 1976-10-05 |
Family
ID=20453198
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| SU1440706A SU327781A1 (en) | 1970-06-05 | 1970-06-05 | The method of obtaining monosilane |
Country Status (1)
| Country | Link |
|---|---|
| SU (1) | SU327781A1 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4959200A (en) * | 1987-02-10 | 1990-09-25 | Chisso Corporation | Process for manufacturing silane |
| US6103942A (en) * | 1999-04-08 | 2000-08-15 | Midwest Research Institute | Method of high purity silane preparation |
-
1970
- 1970-06-05 SU SU1440706A patent/SU327781A1/en active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4959200A (en) * | 1987-02-10 | 1990-09-25 | Chisso Corporation | Process for manufacturing silane |
| US6103942A (en) * | 1999-04-08 | 2000-08-15 | Midwest Research Institute | Method of high purity silane preparation |
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