DE2103066C3 - Apparatus for the production of high-purity arsenic - Google Patents
Apparatus for the production of high-purity arsenicInfo
- Publication number
- DE2103066C3 DE2103066C3 DE19712103066 DE2103066A DE2103066C3 DE 2103066 C3 DE2103066 C3 DE 2103066C3 DE 19712103066 DE19712103066 DE 19712103066 DE 2103066 A DE2103066 A DE 2103066A DE 2103066 C3 DE2103066 C3 DE 2103066C3
- Authority
- DE
- Germany
- Prior art keywords
- arsenic
- tube
- production
- resistant material
- abrasion
- 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.)
- Expired
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/04—Obtaining arsenic
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Description
Für die Herstellung von Galliumarsenid-Verbindungshalbleitern wird Arsen mit einem hohen Reinheitsgrad benötigt. Im Patent 20 21332 wird vorgeschlagen, hochreines, insbesondere silicium- und sauerstoffarmes Arsen durch Sublimation in Gegenwart von oberflächenaktiven und/oder reaktiven Stoffen herzustellen.Arsenic with a high degree of purity is used for the production of gallium arsenide compound semiconductors needed. In the patent 20 21332 it is proposed, highly pure, in particular silicon and low-oxygen arsenic by sublimation in the presence of surface-active and / or reactive To manufacture fabrics.
Bei Anwendung dieses Verfahrens, das in Quarzgefäßen durchgeführt wird, hat sich gezeigt, daß ein geringer Abrieb der Quarzwände auftreten kann und daß dadurch der Siliciumgehalt in sublimierten Arsen erhöht wird und leicht schwankt.When using this method, which is carried out in quartz vessels, it has been shown that a less abrasion of the quartz walls can occur and that thereby the silicon content in sublimed arsenic is increased and fluctuates slightly.
Es wurde nun eine Vorrichtung zur Durchführung des Verfahrens zur Herstellung von hochreinem, insbesondere silicium- und sauerstoffarmen Arsen durch Sublimation in Gegenwart von oberflächenaktiven und/oder reaktiven Stoffen gemäß Patent 20 21 332 gefunden, gekennzeichnet durch ein Rohr, bei dem mindestens die innere Oberfläche aus abriebfestem Material besteht.There has now been an apparatus for carrying out the process for the production of highly pure, in particular low-silicon and low-oxygen arsenic by sublimation in the presence of surface-active substances and / or reactive substances found according to patent 20 21 332, characterized by a tube in which at least the inner surface is made of abrasion-resistant material.
Das Rohr, in dem die Sublimation durchgeführt wird, ist insbesondere konisch. In einer bevorzugten Ausführungsform besteht das konijche Rohr aus Quarz und ist mit einem abriebfesten Material, vorzugsweise aus Bornitrid, überzogen. Es kann auch mit einem Rohr aus dem abriebfesten Material ausgelegt sein, oder das gesamte Rohr, in dem die Sublimation durchgeführt wird, besteht aus einem abriebfesten Material.The tube in which the sublimation is carried out is in particular conical. In a preferred Embodiment, the konijche tube is made of quartz and is covered with an abrasion-resistant material, preferably made of boron nitride, coated. It can also be designed with a tube made of the wear-resistant material be, or the entire tube in which the sublimation is carried out consists of an abrasion-resistant Material.
Als abriebfeste Materialien kommen beispielsweiseExamples of abrasion-resistant materials are
ίο Aluminiumnitrid oder Aluminiumoxyd, vorzugsweise Bornitrid, in Frage.ίο aluminum nitride or aluminum oxide, preferably Boron nitride, in question.
Diese Materialien haften als Beschichtungen besonders gut auf Quarzrohren. Als Rohrmaterialien können auch andere Stoffe, beipielsweise Keramik oder Kohle verwendet werden.As coatings, these materials adhere particularly well to quartz tubes. As pipe materials Other materials, for example ceramics or carbon, can also be used.
Die Herstellung der Rohre oder Beschichtungen kann durch Gasphasenabscheidung erfolgen. Dabei werden reine und kompakte Körper erhalten. Beispielsweise eignet sich für die Bornitridabscheidung besonders das Verfahren gemäß DT-OS 19 43 582, wobei aus Borsäurealkylestern und Ammoniak reines Bornitrid abgeschieden wird.The pipes or coatings can be produced by gas phase deposition. Included pure and compact bodies are obtained. For example, it is suitable for boron nitride deposition especially the method according to DT-OS 19 43 582, whereby pure boric acid and ammonia Boron nitride is deposited.
Die Beschichtungen werden meistenteils in Dicken von 5 bis 300 (im, vorzugsweise 10 bis 150 um, aufgetragen. Vor der Beschichtung wird das Rohr aufgerauht, beispielsweise durch Sandstrahlen oder bei Quarzgefäßen durch Anätzen mit Fluorwasserstoffsäure. The coatings are mostly applied in thicknesses of 5 to 300 µm, preferably 10 to 150 µm. Before coating, the pipe is roughened, for example by sandblasting or at Quartz vessels by etching with hydrofluoric acid.
Die Durchführung der Arsensublimation erfolgt wie im Hauptpatent 20 21 332 beschrieben.The arsenic sublimation is carried out as described in main patent 20 21 332.
Ein Quarzrohr von 1,20 m Länge und 45 mm Durchmesser wurde durch Umsetzung von Borsäuretrimethylester mit Ammoniak mit einer Bornitridschicht von etwa 100 [im Dicke beschichtet. In dem einseitig verschlossenen Rohr werden 250 g Arsen mit 50 g spektralreinem Kohlepulver überschichtet. Durch Beheizung mit einem Widerstandsofen wird bei einer Temperatur der Arsen-Quelie von 500° C und einer Abscheidungstemperatur von 420° C das Arsen unter Vakuum umsublimiert. Der Siliciumgehalt ging von 3 auf 0,3 ppm zurück; ein Gehalt an Bor war spektralanalytisch nicht festzustellen.A quartz tube 1.20 m long and 45 mm in diameter was made by reacting trimethyl borate coated with ammonia with a layer of boron nitride about 100 [in thickness. By doing With a tube closed on one side, 250 g of arsenic are covered with 50 g of spectrally pure carbon powder. The arsenic source is heated with a resistance furnace at a temperature of 500 ° C and a deposition temperature of 420 ° C, the arsenic sublimates under vacuum. The silicon content decreased from 3 to 0.3 ppm; a boron content could not be determined by spectral analysis.
Bei einem weiteren Versuch wurden 250 g ArsenOn another attempt, 250 g of arsenic were found
mit 50 g spektralreinem Borpulver überdeckt und unter den im Beispiel 1 genannten Bedingungen sublimiert. Es wurde eine Abnahme des Siliciumgehaltes von 50 auf 0,5 ppm gefunden.Covered with 50 g of spectrally pure boron powder and under the conditions mentioned in Example 1 sublimated. A decrease in the silicon content from 50 to 0.5 ppm was found.
Claims (5)
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19712103066 DE2103066C3 (en) | 1971-01-22 | 1971-01-22 | Apparatus for the production of high-purity arsenic |
| NL7105564A NL7105564A (en) | 1970-04-30 | 1971-04-23 | |
| US137588A US3700413A (en) | 1970-04-30 | 1971-04-26 | Process for making extra-pure arsenic by sublimation in the presence of carbon or boron |
| JP46029394A JPS515639B1 (en) | 1970-04-30 | 1971-04-30 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19712103066 DE2103066C3 (en) | 1971-01-22 | 1971-01-22 | Apparatus for the production of high-purity arsenic |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| DE2103066A1 DE2103066A1 (en) | 1972-07-27 |
| DE2103066B2 DE2103066B2 (en) | 1975-05-15 |
| DE2103066C3 true DE2103066C3 (en) | 1976-01-08 |
Family
ID=5796669
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DE19712103066 Expired DE2103066C3 (en) | 1970-04-30 | 1971-01-22 | Apparatus for the production of high-purity arsenic |
Country Status (1)
| Country | Link |
|---|---|
| DE (1) | DE2103066C3 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2467342A1 (en) * | 1979-10-12 | 1981-04-17 | Alsthom Atlantique | DISCHARGE VALVE OF A HYDRAULIC INSTALLATION |
-
1971
- 1971-01-22 DE DE19712103066 patent/DE2103066C3/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| DE2103066B2 (en) | 1975-05-15 |
| DE2103066A1 (en) | 1972-07-27 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C3 | Grant after two publication steps (3rd publication) | ||
| E77 | Valid patent as to the heymanns-index 1977 | ||
| EGZ | Application of addition ceased through non-payment of annual fee of main patent |