ES2251294A1 - Vacuum semi-automatic system for amorphous alloy samples or vitreous powder, comprises vacuum chamber that is assisted by vacuum pump and nitrogen line, where vacuum chamber is conveniently regulated by pressure sensor - Google Patents
Vacuum semi-automatic system for amorphous alloy samples or vitreous powder, comprises vacuum chamber that is assisted by vacuum pump and nitrogen line, where vacuum chamber is conveniently regulated by pressure sensorInfo
- Publication number
- ES2251294A1 ES2251294A1 ES200401136A ES200401136A ES2251294A1 ES 2251294 A1 ES2251294 A1 ES 2251294A1 ES 200401136 A ES200401136 A ES 200401136A ES 200401136 A ES200401136 A ES 200401136A ES 2251294 A1 ES2251294 A1 ES 2251294A1
- Authority
- ES
- Spain
- Prior art keywords
- vacuum
- vacuum chamber
- semi
- assisted
- pressure sensor
- 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.)
- Granted
Links
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 8
- 230000001105 regulatory effect Effects 0.000 title claims abstract 3
- 239000000843 powder Substances 0.000 title claims description 5
- 229910000808 amorphous metal alloy Inorganic materials 0.000 title description 2
- 229910045601 alloy Inorganic materials 0.000 claims description 7
- 239000000956 alloy Substances 0.000 claims description 7
- 239000011521 glass Substances 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 description 7
- 229910052760 oxygen Inorganic materials 0.000 description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 239000000428 dust Substances 0.000 description 6
- 238000000034 method Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 3
- 231100000331 toxic Toxicity 0.000 description 3
- 230000002588 toxic effect Effects 0.000 description 3
- 238000003915 air pollution Methods 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 238000004880 explosion Methods 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- 238000005304 joining Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 150000002926 oxygen Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/006—Processes utilising sub-atmospheric pressure; Apparatus therefor
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Sampling And Sample Adjustment (AREA)
- Manipulator (AREA)
Abstract
Description
Sistema semiautomático de vacío para muestras de aleaciones amorfas o vítreas en polvo.Semi-automatic vacuum system for samples of Amorphous or vitreous powder alloys.
Esta invención se refiere a un sistema para eliminara el oxígeno de muestras para la fabricación de aleaciones. Tiene su campo de aplicación principal en laboratorios de investigación.This invention relates to a system for remove oxygen from samples for alloy manufacturing. It has its main field of application in laboratories of investigation.
Para evitar explosiones en el horno encargado de fundir los elementos constitutivos de cada aleación amorfa o vítrea, es necesario extraer el oxígeno de los citados elementos.To avoid explosions in the oven in charge of melt the constituent elements of each amorphous alloy or vitreous, it is necessary to extract the oxygen from the aforementioned elements.
Para esta extracción de oxígeno se emplean diversos sistemas que permiten hacer vacío en un recipiente donde se encuentre la muestra.For this oxygen extraction they are used various systems that allow emptying in a container where The sample is found.
Sin embargo, al hacer vacío surgen diferentes
problemas que algunos sistemas resuelven de forma muy gravosa. En
estos sistemas, las conexiones entre los equipos se realizan
mediante unas mangueras de silicona que permiten hacer un vacío muy
alto. Esta característica, necesaria para que funcione la
instalación, hace que sea muy difícil operar con las mangueras
(desconectar, limpiar, etc.), siendo frecuente la rotura accidental
de alguna válvula. Este problema es de vital importancia debido a
que esta rotura puede producir accidentes por contaminación
atmosférica con productos tóxicos y peligrosos, así como pérdidas
de parte de las muestras cuando estas se introducen en la bomba
de
vacío.However, when emptying, different problems arise that some systems solve in a very burdensome way. In these systems, the connections between the equipment are made by means of silicone hoses that allow a very high vacuum. This characteristic, necessary for the installation to work, makes it very difficult to operate with the hoses (disconnect, clean, etc.), the accidental breakage of a valve being frequent. This problem is of vital importance because this breakage can cause accidents due to air pollution with toxic and dangerous products, as well as losses of part of the samples when they are introduced into the pump
empty.
En consecuencia se ha ideado un nuevo sistema que elimina los problemas mencionados y cuyas características son el objeto de la presente invención.Consequently a new system has been devised that eliminates the mentioned problems and whose characteristics are the object of the present invention.
La presente invención se refiere a un sistema que, haciendo uso de una cámara de vacío, permite extraer el oxígeno de los elementos que serán utilizados para fabricar aleaciones de materiales amorfos y cristalinos, para evitar posibles explosiones en el horno encargado de fundir los elementos constitutivos de cada aleación.The present invention relates to a system which, using a vacuum chamber, allows to extract the oxygen of the elements that will be used to manufacture alloys of amorphous and crystalline materials, to avoid possible explosions in the oven responsible for melting the elements constitutive of each alloy.
Consta de una cámara de vacío, con 4 válvulas de
paso lento, que conectan esta cámara con el resto de los elementos
del sistema, esto es, la bomba de vacío, la línea de N_{2} el
sensor de presión y el recipiente donde se encuentra la
mues-
tra.It consists of a vacuum chamber, with 4 slow-pass valves, which connect this chamber with the rest of the system elements, that is, the vacuum pump, the N2 line, the pressure sensor and the container where is the sample
tra.
Las mangueras de goma de vacío, utilizadas ampliamente en este tipo de instalaciones, habitualmente se conectan directamente a la válvula correspondiente. En este caso, para evitar la rotura de la válvula, cuando se manipula sobre ella, las conexiones entre las válvulas y cada una de las mangueras de los cuatro elementos del sistema se hacen mediante un dispositivo compuesto por un tubo de goma flexible, en cuyo interior se insertan dos cilindros huecos de vidrio, que a su vez se inserta en cada manguera, ajustando el conjunto mediante un par de bridas.Vacuum rubber hoses, used widely in this type of facility, usually connect directly to the corresponding valve. In this case, to prevent the breakage of the valve, when handled on it, the connections between the valves and each of the hoses the four elements of the system are made by a device composed of a flexible rubber tube, inside which are inserted two hollow glass cylinders, which in turn is inserted into each hose, adjusting the assembly by means of a pair of flanges.
Esta instalación mantiene la cantidad de muestra intacta en el porta-muestras de cuarzo y evita que el polvo de la misma sea aspirado por la bomba de vacío, o escape al exterior, evitando por tanto, el riesgo de contaminación con productos altamente tóxicos.This installation maintains the sample quantity intact in the quartz sample holder and prevents Dust from it is sucked by the vacuum pump, or exhaust abroad, thus avoiding the risk of contamination with highly toxic products
Además, permite mayor agilidad en el procedimiento de vacío de la muestra y desmontar cómoda y rápidamente todo el sistema, en caso de avería o limpieza del mismo.In addition, it allows greater agility in the Sample vacuum procedure and disassemble comfortable and quickly the entire system, in case of breakdown or cleaning of the same.
\vskip1.000000\baselineskip\ vskip1.000000 \ baselineskip
Figura 1.- Esquema general del sistema.Figure 1.- General scheme of the system.
\newpage\ newpage
Figura 2.- Detalle de los dispositivos de unión de las válvulas a las mangueras del resto de los elementos del sistema.Figure 2.- Detail of the joining devices from the valves to the hoses of the rest of the elements of the system.
En el proceso de fabricación de aleaciones amorfas, antes de fundir en un horno los productos en polvo contenidos en un tubo de cuarzo (5) cerrado al vacío, es necesario extraer el oxígeno del mismo. Para ello se realizan, con el tubo abierto por un extremo, varios ciclos de vacío y gas inerte. Esta operación implica riesgos de contaminación atmosférica por salida de la muestra al exterior y contaminación de la bomba de vacío por escape del polvo de la muestra. Para evitar ambos riesgos, hemos diseñado un sistema que, siguiendo el procedimiento de trabajo, elimina los riesgos citados.In the alloy manufacturing process amorphous, before melting the powdered products in an oven contained in a vacuum closed quartz tube (5), it is necessary extract oxygen from it. For this they are done, with the tube open at one end, several cycles of vacuum and inert gas. This operation implies risks of air pollution by exit of the sample outside and contamination of the vacuum pump by Sample dust leakage. To avoid both risks, we have designed a system that, following the work procedure, Eliminate the mentioned risks.
El sistema está formado por un recipiente transparente (1), que denominamos cámara de vacío, que permite ver en su interior del mismo si se produce un escape de la muestra y soporta ciclos alternativos de vacío y sobre presión. El volumen de este recipiente (1) debe ser lo suficientemente para que la separación entre las válvulas o llaves (6c) y (6a) impida el paso del polvo de la muestra contenida en el recipiente portamuestras (5) a la bomba (2), y que por el contrario, se deposite en el fondo del recipiente.The system consists of a container transparent (1), which we call vacuum chamber, which allows us to see inside it if there is an escape of the sample and Supports alternative cycles of vacuum and over pressure. The volume of this container (1) must be enough for the separation between valves or keys (6c) and (6a) prevents passage of the sample powder contained in the sample holder (5) to the pump (2), and that on the contrary, be deposited in the bottom of the container.
Al recipiente se sueldan 4 válvulas o llaves de paso lento (6a, 6b, 6c y 6d), fabricadas en vidrio con cierre de teflón. La llave (6c), cierra y abre el paso al porta muestras (5) y se debe instalar hacia 1/3 del fondo del recipiente (1). Las llaves (6a) (cierra y abre el paso a la bomba de vacío (2)) y (6b) (cierra y abre el paso al depósito de nitrógeno) se instalan en la parte opuesta del recipiente (1), de modo que la llave (6a) quede en la parte más alta posible y la (6b) por debajo del eje de la llave (6c). De este modo, si sale polvo por la llave (6c) choca contra la pared del recipiente (1) y se precipita al fondo, no llegando al exterior ni a la bomba (2). La llave (6d) cierra y abre el paso al sensor digital de presión (4).4 valves or keys are welded to the vessel slow step (6a, 6b, 6c and 6d), made of glass with closing Teflon The key (6c), close and open the passage to the sample holder (5) and must be installed towards 1/3 of the bottom of the container (1). The keys (6a) (close and open the passage to the vacuum pump (2)) and (6b) (closes and opens the passage to the nitrogen tank) are installed in the opposite part of the container (1), so that the key (6a) is in the highest possible part and the (6b) below the axis of the key (6c). In this way, if dust comes out of the key (6c) it crashes against the wall of the container (1) and rushes to the bottom, not reaching outside or the pump (2). The key (6d) closes and opens the passage to the digital pressure sensor (4).
El procedimiento de trabajo es el siguiente:The work procedure is as follows:
1°.- Teniendo cerradas las llaves (6c) y (6b) se pone en marcha la bomba de vacío (2) y cuando el sensor (4) indique vacío en el recipiente (1) se cierra la llave (6a) y se abre muy despacio la llave (6c). El vacío existente en el recipiente (1) hará que el polvo de la muestra (5) intente subir hacia el tubo (7c) pero controlando el paso de la llave (6c) se impide que pase a dicho tubo.1 .- Having the keys (6c) and (6b) closed starts the vacuum pump (2) and when the sensor (4) indicates empty in the container (1) the key (6a) is closed and very open Slowly the key (6c). The vacuum in the container (1) will make the sample dust (5) try to rise towards the tube (7c) but controlling the passage of the key (6c) prevents it from passing to said tube.
2°.- Cuando se estabiliza la depresión en el porta muestras (5) y la muestra se mantiene apelmazada en el fondo del tubo (5), se cierra la llave (6c) y se procede a abrir la llave (6a) repitiendo íntegramente el punto 1° de este procedimiento.2 .- When the depression stabilizes in the sample holder (5) and the sample remains caked in the bottom of the tube (5), the key (6c) is closed and the key is opened (6a) repeating in full the 1st point of this procedure.
Estos puntos se repiten las veces necesarias hasta que se vea que el polvo del porta muestras (5) no se inmuta cuando se hace vacío. Cuando esto ocurre, se dejan abiertas las llaves (6c) y (6a) con la bomba de vacío (2) en marcha durante varias horas.These points are repeated as many times as necessary. until you see that the dust in the sample holder (5) does not change When it becomes empty. When this occurs, the keys (6c) and (6a) with the vacuum pump (2) running during several hours.
3°.- Posteriormente, se cierra la llave (6c) y unos segundos antes de cerrar la llave (6a) se abre la llave (6b) para que entre el nitrógeno en el recipiente sin que llegue a entrar oxígeno. A continuación se abre la llave (6c) para que el nitrógeno entre en el porta muestras (5). Se tiene así dos horas para que el nitrógeno penetre bien en todos los resquicios de la muestra.3 .- Afterwards, the key (6c) is closed and a few seconds before closing the key (6a) the key (6b) is opened so that nitrogen enters the vessel without reaching Enter oxygen Then the key (6c) is opened so that the nitrogen enters the sample holder (5). You have two hours like that so that the nitrogen penetrates well in all the cracks of the sample.
4º.- Seguidamente, se cierra la llave (6b) y (6c) y con la bomba de vacío (2) en marcha se repiten los puntos 1° y 2° para hacer un nuevo ciclo de vacío. A continuación, se repite el paso 3° para hacer una nueva inertización de la muestra y así sucesivamente hasta realizar todos los ciclos necesarios para que la muestra no contenga oxígeno.4º.- Next, the key (6b) and (6c) are closed and with the vacuum pump (2) running, the 1st and 2nd points are repeated to make a new vacuum cycle. Then repeat the step 3 to make a new inertization of the sample and so successively until all the necessary cycles are carried out so that The sample does not contain oxygen.
Posteriormente, manteniendo la bomba de vacío (2) funcionando se procede al cierre del tubo porta muestras (5).Subsequently, maintaining the vacuum pump (2) When working, the sample holder tube (5) is closed.
Siguiendo este procedimiento no escapará ninguna partícula de la muestra. Sin embargo, si no se operasen adecuadamente las llaves (6), la configuración del sistema impediría el escape del polvo tóxico al exterior o a la bomba citada.Following this procedure will not escape any Sample particle. However, if they were not operated properly keys (6), system configuration prevent the escape of toxic dust to the outside or to the pump cited
Claims (2)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| ES200401136A ES2251294B1 (en) | 2004-05-12 | 2004-05-12 | SEMIAUTOMATIC VACUUM SYSTEM FOR SAMPLES OF AMORPH ALLOYS OR VITREAS IN POWDER. |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| ES200401136A ES2251294B1 (en) | 2004-05-12 | 2004-05-12 | SEMIAUTOMATIC VACUUM SYSTEM FOR SAMPLES OF AMORPH ALLOYS OR VITREAS IN POWDER. |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| ES2251294A1 true ES2251294A1 (en) | 2006-04-16 |
| ES2251294B1 ES2251294B1 (en) | 2009-01-01 |
Family
ID=36201221
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| ES200401136A Expired - Fee Related ES2251294B1 (en) | 2004-05-12 | 2004-05-12 | SEMIAUTOMATIC VACUUM SYSTEM FOR SAMPLES OF AMORPH ALLOYS OR VITREAS IN POWDER. |
Country Status (1)
| Country | Link |
|---|---|
| ES (1) | ES2251294B1 (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB729871A (en) * | 1952-07-18 | 1955-05-11 | Leitz Ernst Gmbh | Improved method of evacuating vessels |
| US5466765A (en) * | 1995-03-09 | 1995-11-14 | Eastman Chemical Company | Vaccum system for controlling pressure in a polyester process |
| DE19823163A1 (en) * | 1998-05-23 | 1999-05-06 | Bundesrep Deutschland | Decontamination of equipment involved in chemical warfare |
| US6455718B1 (en) * | 1996-11-22 | 2002-09-24 | Albemarle Corporation | Halogen exchange reactions in preparing catalysts and their precursors |
-
2004
- 2004-05-12 ES ES200401136A patent/ES2251294B1/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB729871A (en) * | 1952-07-18 | 1955-05-11 | Leitz Ernst Gmbh | Improved method of evacuating vessels |
| US5466765A (en) * | 1995-03-09 | 1995-11-14 | Eastman Chemical Company | Vaccum system for controlling pressure in a polyester process |
| US6455718B1 (en) * | 1996-11-22 | 2002-09-24 | Albemarle Corporation | Halogen exchange reactions in preparing catalysts and their precursors |
| DE19823163A1 (en) * | 1998-05-23 | 1999-05-06 | Bundesrep Deutschland | Decontamination of equipment involved in chemical warfare |
Also Published As
| Publication number | Publication date |
|---|---|
| ES2251294B1 (en) | 2009-01-01 |
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