DE1161868B - Process for the production of high purity silicon halides - Google Patents
Process for the production of high purity silicon halidesInfo
- Publication number
- DE1161868B DE1161868B DEW30706A DEW0030706A DE1161868B DE 1161868 B DE1161868 B DE 1161868B DE W30706 A DEW30706 A DE W30706A DE W0030706 A DEW0030706 A DE W0030706A DE 1161868 B DE1161868 B DE 1161868B
- Authority
- DE
- Germany
- Prior art keywords
- production
- silicon halides
- graphite
- high purity
- purity silicon
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229910052710 silicon Inorganic materials 0.000 title claims description 10
- 239000010703 silicon Substances 0.000 title claims description 10
- 238000000034 method Methods 0.000 title claims description 8
- -1 silicon halides Chemical class 0.000 title claims description 6
- 238000004519 manufacturing process Methods 0.000 title claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- 229910002804 graphite Inorganic materials 0.000 claims description 6
- 239000010439 graphite Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 238000004508 fractional distillation Methods 0.000 claims description 3
- 230000008022 sublimation Effects 0.000 claims description 3
- 238000009835 boiling Methods 0.000 claims description 2
- 238000000260 fractional sublimation Methods 0.000 claims description 2
- 239000000126 substance Substances 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 150000004820 halides Chemical class 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- RTCGUJFWSLMVSH-UHFFFAOYSA-N chloroform;silicon Chemical compound [Si].ClC(Cl)Cl RTCGUJFWSLMVSH-UHFFFAOYSA-N 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/04—Hydrides of silicon
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/107—Halogenated silanes
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Description
Verfahren zur Herstellung von hochreinen Siliciumhalogeniden Die Herstellung von reinen Halogeniden wird in bekannter Weise so durchgeführt, daß das Rohprodukt, vom eigentlichen Herstellungsvorgang kommend, einer fraktionierten Destillation oder Sublimation unterworfen wird. Diese bekannten Operationen sind jedoch nicht ausreichend, wenn extreme Reinheitsgrade verlangt werden; vor allem dann, wenn die Halogenide als Ausgangsprodukt zur Herstellung von besonders reinen Stoffen wie Katalysatoren oder Halbleitermetallen benutzt werden, bei denen noch Verunreinigungsmengen, stören, die unterhalb der spektroskopischen Nachweisgrenze liegen.Process for the preparation of high purity silicon halides The preparation of pure halides is carried out in a known manner so that the crude product, coming from the actual manufacturing process, a fractional distillation or is subjected to sublimation. However, these operations are not known sufficient if extreme degrees of purity are required; especially when the Halides as a starting product for the production of particularly pure substances such as Catalysts or semiconductor metals are used in which there are still amounts of impurities, interfere, which are below the spectroscopic detection limit.
Im Gegensatz zu den genannten Arbeitsweisen wurde ein einfaches, schnell und sicher arbeitendes Verfahren gefunden, das erlaubt, extrem reine Siliciumhalogenide unter Verwendung von Graphit herzustellen. Das Verfahren ist dadurch gekennzeichnet, daß die Siliciumhalogenide vor oder nach einer fraktionierten Destillation oder Sublimation flüssig oder verdampft mit aktiviertem Graphit bei Temperaturen vom Siedepunkt der flüssigen Luft bis 300° C behandelt werden.In contrast to the above-mentioned working methods, a simple, fast one became and found a safe working process which allows extremely pure silicon halides using graphite. The procedure is characterized by that the silicon halides before or after a fractional distillation or Sublimation liquid or vaporized with activated graphite at temperatures from Boiling point of liquid air up to 300 ° C can be treated.
Es wurde beobachtet, daß die Wirkung des Graphits hinsichtlich Intensität und Quantität steigt, wenn er vor der Verwendung mit Luft bei Rotglut oder tiefer kurzzeitig behandelt wird. Diese Aktivierung kann auch mit anderen bekannten Stoffen, z. B. flüssigen Oxydationsmitteln, durchgeführt werden.It was observed that the effect of the graphite in terms of intensity and quantity increases if it is red heat or lower before use with air is treated briefly. This activation can also be done with other known substances, z. B. liquid oxidants are carried out.
Der aktivierte Graphit kann auf Trägermaterial wie Graphit, Kohle, Silicium in brauner und metallischer Form, Quarzglas oder andere Gläser und sonstige inerte Stoffe aufgebracht werden.The activated graphite can be applied to carrier material such as graphite, carbon, Silicon in brown and metallic form, quartz glass or other glasses and others inert substances are applied.
Die Temperatur während der Behandlung mit dem reinigend wirkenden Stoff ist abhängig von der Form, Menge und Art des Stoffes und der Menge und Art der Verunreinigungen sowie von dem zu reinigenden Halogenid. Die Verweilzeit ist bei gegebenem Kontaktstoff abhängig von Art und Menge der Verunreinigungen und der Temperatur.The temperature during treatment with the cleansing agent Substance depends on the shape, amount and type of substance and the amount and type the impurities and the halide to be cleaned. The dwell time is for a given contact substance depending on the type and amount of impurities and the Temperature.
Das Verfahren kann bei Normal-, Über- oder Unterdruck durchgeführt werden. Als günstiger Druckbereich hat sich das Gebiet von Normaldruck bis zu mehreren Atmosphären erwiesen. Beispiel Schuppenförmiger Graphit mit einem Schuppendurchmesser von 0,3 bis 2 mm wird in konzentrierter Salpetersäure bei einer Temperatur von 30° C aufgeschlämmt. Unter Rühren wird die Temperatur langsam auf 50° C erhöht und bis zur vollständigen Aktivierung auf dieser Höhe gehalten. Die Salpetersäure wird dann durch Abnutschen abgetrennt und der aktivierte Graphit mit destilliertem Wasser gewaschen.The process can be carried out under normal, positive or negative pressure will. The range from normal pressure to several has proven to be a favorable pressure range Atmospheres proven. Example of flaky graphite with a flake diameter from 0.3 to 2 mm is in concentrated nitric acid at a temperature of 30 ° C slurried. While stirring, the temperature is slowly increased to 50 ° C. and up to held at this level for full activation. The nitric acid will then separated by suction and the activated graphite with distilled water washed.
Über den aktivierten Graphit, der sich in einem senkrecht stehenden Quaxzglasrohr befindet, läßt man flüssiges Siliciumchloroform, hergestellt aus technisch reinem Silicium und Chlorwasserstoff, einmal fraktioniert, bei 20° C und mit einer Strömungsgeschwindigkeit von etwa 0,5 cm pro Minute von oben nach unten hindurchströmen. Das unten ausfließende Siliciumchloroform hat die für die Halbleitertechnik störenden Verunreinigungen an den Graphit abgegeben und kann unmittelbar zu Halbleitersilicium, z. B. durch thermisches Spalten an heißen Siliciumträgern, verarbeitet werden.About the activated graphite, which is in a vertical position Quaxzglasrohr is, one lets liquid silicon chloroform, produced from technical pure silicon and hydrogen chloride, once fractionated, at 20 ° C and with a Flow through a flow rate of about 0.5 cm per minute from top to bottom. The silicon chloroform flowing out below has the disruptive elements for semiconductor technology Impurities are released to the graphite and can lead directly to semiconductor silicon, z. B. processed by thermal cleavage on hot silicon substrates.
Diese Reinigungsmethode läßt sich in gleicher Weise bei SiliciumtetrachIorid anwenden, wobei eine Durchlaufgeschwindigkeit von 0,1 cm pro Minute eingehalten wird.This cleaning method can be used in the same way for silicon tetrachloride apply, maintaining a throughput speed of 0.1 cm per minute will.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEW30706A DE1161868B (en) | 1958-07-15 | 1958-07-15 | Process for the production of high purity silicon halides |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEW30706A DE1161868B (en) | 1958-07-15 | 1958-07-15 | Process for the production of high purity silicon halides |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE1161868B true DE1161868B (en) | 1964-01-30 |
Family
ID=7599574
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DEW30706A Pending DE1161868B (en) | 1958-07-15 | 1958-07-15 | Process for the production of high purity silicon halides |
Country Status (1)
| Country | Link |
|---|---|
| DE (1) | DE1161868B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4374182A (en) * | 1980-07-07 | 1983-02-15 | Dow Corning Corporation | Preparation of silicon metal through polymer degradation |
-
1958
- 1958-07-15 DE DEW30706A patent/DE1161868B/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4374182A (en) * | 1980-07-07 | 1983-02-15 | Dow Corning Corporation | Preparation of silicon metal through polymer degradation |
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