EP1244823A1 - Dispositif permettant de produire un melange gazeux - Google Patents

Dispositif permettant de produire un melange gazeux

Info

Publication number
EP1244823A1
EP1244823A1 EP00990701A EP00990701A EP1244823A1 EP 1244823 A1 EP1244823 A1 EP 1244823A1 EP 00990701 A EP00990701 A EP 00990701A EP 00990701 A EP00990701 A EP 00990701A EP 1244823 A1 EP1244823 A1 EP 1244823A1
Authority
EP
European Patent Office
Prior art keywords
column
gas
central
gas mixture
hmdso
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.)
Withdrawn
Application number
EP00990701A
Other languages
German (de)
English (en)
Inventor
Rodney Moore
Andreas LÜTTRINGHAUS-HENKEL
Patrik Hoffmann
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Tetra Laval Holdings and Finance SA
Original Assignee
Tetra Laval Holdings and Finance SA
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Tetra Laval Holdings and Finance SA filed Critical Tetra Laval Holdings and Finance SA
Publication of EP1244823A1 publication Critical patent/EP1244823A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/448—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
    • C23C16/4481—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by evaporation using carrier gas in contact with the source material

Definitions

  • the invention relates to a device for producing a gas mixture from a liquid starting compound, for example HMDSO, and a carrier gas, for example oxygen (0 2 ), as the process gas.
  • a liquid starting compound for example HMDSO
  • a carrier gas for example oxygen (0 2 )
  • the invention is therefore based on the object of providing a device of the type mentioned at the outset with which a large volume of process gas can be produced continuously and can be removed at practically processable temperatures. Temperatures that can be processed practically require a product gas (gas mixture) that is on the order of room temperature, whereby temperatures of the gas mixture between 0 ° C. and 20 ° C. are also considered to be practically processable.
  • the further condition for the solution according to the invention was the provision of a gas flow with a large volume per unit time, with 0.05 to 5 m 3 per hour, preferably 0.1 to 0.5 m 3 per hour, particularly preferably 0.2 up to 0.5 m 3 per hour (the volume flow is converted to standard conditions - 1 bar pressure, 20 ° C).
  • the object is achieved in that in an elongated, essentially vertically arranged, coolable column, several filling packs are arranged one above the other, that in the upper region of the column, an inlet connection from outside into the column and a are attached to the outside gas outlet connection and that devices for measuring the temperature, pressure and amount of the exiting gas mixture are provided.
  • HMDSO is particularly preferred as the liquid starting compound for producing a gas mixture with a carrier gas in the device according to the invention.
  • the device according to the invention is also suitable for producing a gas mixture from a large number of other liquid starting compounds and a carrier gas.
  • the liquid starting compounds typically used to produce a plasma contain a metal or semimetal such as tin, zinc, silicon, zirconium, titanium or aluminum.
  • the compounds are organic or organometallic formations, such as alcoholates, acetates, alkyls or aryls.
  • Organosilicon compounds such as tetramethoxysilane, are preferably used. Tetramethyldisiloxane or silazanes, such as hexamethyldisiiazane, are particularly preferred.
  • a large number of further starting compounds suitable for this purpose are specified in US Pat. No. 4,041,303.
  • the invention aimed to generate steam from the HMDSO at a lower temperature. It was therefore necessary to evaporate the liquid HMDSO by means other than increasing the temperature.
  • the invention makes use of the distillation or extraction columns. Appropriate changes and measures have been provided to evaporate the HMDSO, which has been introduced liquidly into a substantially vertically arranged column at the top, at moderate temperatures.
  • the invention hereby goes the way to use filling packs with honeycomb structure which are known per se from another context, whereby the distribution of the liquid HMDSO is improved even at lower temperatures.
  • the known filling packs with a honeycomb structure preferably consist of metal and are arranged one above the other in such a way that they lie under an inlet connection of the liquid HMDSO.
  • the flow of the liquid HMDSO can be converted into drops which drip onto the upper packing and gradually get into the packing below, where the offered large surfaces are wetted.
  • the viscosity of the liquid HMDSO which is approximately in the range of water, allows this distribution.
  • this can be implemented by providing the column with a cooling jacket through which coolant flows.
  • the coolant itself - water is particularly easy to use here - can then be tempered in a conventional thermostat.
  • the other gas in the lower region of the column for example oxygen, which can also be replaced by argon, for example.
  • oxygen which can also be replaced by argon, for example.
  • a gas outlet connection led to the outside is attached at a correspondingly favorable point, through which the desired gas mixture of HMDSO and a carrier gas, such as oxygen, is led out.
  • devices are provided on or in the column according to the invention in order to measure the temperature and the pressure of the liquid and / or the gases or the gas mixture, because their setting can optimize the production process of the gas mixture.
  • the same also applies to the amount of the emerging gas mixture, which should be adapted to the further processing method, but to which the other parameters within the manufacturing device according to the invention must also be adapted.
  • the new manufacturing device makes it possible to continuously produce a large volume flow of process gas, in particular at temperatures in the order of room temperature, so that further processing, for example continuing through longer pipelines, through distribution devices, etc., is practically and without technical difficulties become possible.
  • the column It has proven to be practical to make the column about 15 cm to 1.5 m and preferably 30 cm long. In this case, diameters in the range from 30 to 300, preferably 40 to 200 and particularly preferably 50 mm to 80 mm are provided. In such columns, 2 to 10 and preferably 3 to 8 filling packs with the honeycomb structure are arranged one above the other.
  • the invention has gone the other way for particularly high outputs, to further design the device of the type described above in such a way that a distributor shell with gas throughflow openings spanning the cross section of the column is fitted under the inner outlet end of the inlet connection.
  • a distributor shell must of course be gas-permeable, because the quantities of steam rising from below and generated by the filling packs must be able to pass through this distributor shell to the top.
  • a central floor provided with through holes is arranged in the central area of the distributor shell and is surrounded on the outside by the gas throughflow openings.
  • the column of the device according to the invention is circular in cross section, because then the industrially offered filling packs are easier to use.
  • the circumference of the flat or slightly arched distributor shell can then expediently be attached to the inner wall of the column in such a way that the distributor shell spans the entire cross section of the column.
  • the mentioned central floor is provided, which has through holes for the passage of the liquid HMDSO.
  • the free passage cross-section of the holes is 1 to 20%, preferably 5 to 10%, with respect to the closed area of the central floor.
  • the proportion of the area arranged outside around the central plate, which is predetermined by the gas throughflow openings, is greater; for example in the range of 50 - 80% of the total column cross section. It has been shown that the liquid (HMDSO) supplied from the inlet nozzle drips onto the distributor shell in the region of its central bottom and tries to get down through the individual through holes into the top filling pack. As a result, the filling pack is already offered a much better distributed liquid flow than in the first-mentioned device without the distributor shell.
  • the central floor of the distributor shell between the through holes is closed and is supported by a central ring element.
  • the central plate fastened on the cylindrical jacket-shaped inner surface of the column has in its central region the mentioned central ring element, within which the central plate is located. It is closed in the above-mentioned percentage ratios or open through the through holes.
  • the manufacture of such a distributor shell is simple.
  • the central floor can be arched towards the center, a particularly favorable curvature being the one in which the highest point of the central floor lies in the central area thereof.
  • the central ring element can be connected by spoke-shaped connecting struts to an outer ring of the distributor shell, which is fastened to the inner wall of the column.
  • the central floor is designed as a sieve floor, the central floor also being supported by a central ring element.
  • the sieve bottom can be imagined from any suitable sieve made of metal or plastic, preferably sintered metal. A glass frit would also be conceivable.
  • the device of the type described above for coating the inner surfaces of hollow bodies is particularly advantageous according to the invention.
  • hollow bodies which have only a single opening can be coated on the inside in this way if the desired gas mixture produced with the correct and practically processable temperature is introduced and, after its treatment and after its precipitation on the inner surfaces of the hollow body, the remaining process gas is removed again can be.
  • FIG. 1 shows a basic diagram of an overall system in which the device for producing the gas mixture is shown schematically in the middle
  • FIG. 2 shows a cross section of the column according to the invention without a distributor shell
  • FIG. 3 shows a cross section of another embodiment of the column with distributor shell
  • FIG. 4 shows an enlarged detail from FIG. 3,
  • Figure 5 is a perspective view of a distributor shell with a closed central floor and through holes located therein, and
  • Figure 6 shows another embodiment of a distributor shell with an inserted sieve bottom.
  • the device for producing the product gas mixture described here which is generally designated by 1, is located approximately in the middle. It represents the elongated, vertically arranged column 1 and is filled with five filling packs 2, each of which has a honeycomb structure and consists of a nickel-chromium-molybdenum alloy (trade name: Hastelloy) which is chemically less susceptible to attack.
  • an inlet connection 3 is introduced into the column from the outside. Its inner outlet end 4 ends approximately in the region of the vertical longitudinal central axis 5 of the column 1.
  • arrow 6 ′ illustrates the direction of flow of the gas mixture produced, namely the process gas which leaves the column 1 at its head through the gas outlet connection 6 which is led to the outside.
  • the process gas is a mixture of carrier gas and vaporized HMDSO and, after passing through a pressure regulator 7, reaches the distribution system 9 via a valve 8.
  • this is a distributor 10, of which ten inlet lines 11 in the inside of hollow bodies, in this case bottles 12 open at the top, are introduced.
  • the column 1 itself is coolable, ie it is surrounded on the outside with a cooling jacket 13 through which water as a cooling medium flows. This passes through the inlet 14 according to arrow 14 'from a thermostat into the cavity of the cooling jacket 13 and leaves via the outlet 15 according to arrow 15'. In the manufacturing process carried out here, the cooling water is kept at a temperature in the range between 5 and 11 ° C. by the thermostat.
  • the liquid HMDSO hexamethyldisiloxane
  • the process gas is not solely vaporized HMDSO, but rather a mixture with a carrier gas, which here is oxygen (0 2 ), but in other versions can also be argon (Ar), krypton (Kr) and the like.
  • the oxygen as the carrier gas is also introduced into the bottom 20 of the column 1 through the introduction line 18 and via the mass flow controller 19, as indicated by arrow 18 '.
  • the downstream end 21 of the gas introduction line 18 is shown in FIGS provided with a cap 22, which is provided to prevent liquid HMDSO from dripping into the gas introduction line 18.
  • Unevaporated HMDSO can be drawn off at the bottom of the column through the discharge line 23, controlled by a valve 24, and fed to a recovery system (which is not shown here).
  • an auxiliary gas can be fed via the inlet line 25 into the top of the column 1 if it is desired to add another gas component in the column 1.
  • This inlet line 25 can also be used to rinse column 1.
  • thermocouple 26 In the middle at the top of the column 1 there is also shown a thermocouple 26 by means of which the temperature of the gas in the column can be measured.
  • a liquid sensor shown here can also be provided at the bottom 20 of the column in order to sense whether and, if appropriate, how much unevaporated HMDSO has formed at the bottom 20 of the column.
  • Figures 2 and 3 show column 1 in its more concrete structure with the packing 2 and the clamping rings 28 at the top and bottom of column 1. While Figure 2 is similar to the embodiment of Figure 1 and there from the outlet end 4 of the inlet nozzle 3 liquid HMDSO is dropped onto the packing 2 in relatively large drops, because the drops are largely distributed in the packing 2, the embodiment of FIG. 3 represents an additional auxiliary measure, namely a distributor shell 29, which is essentially perpendicular to the vertical longitudinal central axis 5, is arranged horizontally and spans the entire inner cross section of column 1. This distributor shell 29 is attached at a short distance of 0.1 to 10 mm and preferably about 2 mm below the lower part of the inner outlet end 4 of the inlet connection 3.
  • FIG. 4 a first embodiment of a distributor shell 29 is shown enlarged in a column 1 shown broken off at the top and bottom.
  • the aforementioned distance of the distributor shell from the inner outlet end 4 of the inlet nozzle 3 is measured in the central region 30 of the distributor shell, because the vertical longitudinal central axis 5 extends through this central region 30 and essentially touches the lower part of the outlet end 4 of the inlet nozzle 3.
  • such an elevation 31 is also shown and is provided there with a central passage hole 32.
  • This passage hole is missing in FIG 32.
  • the raised part 31 in the central region 30 of the distributor shell 29 is solid in the case of the embodiment in FIG. 4, while in FIG. 5 it is produced in the form of a curved, curved sheet.
  • the distributor shell 29 has a circular cross section which is adapted to the interior of the column and which can be seen particularly clearly from the perspective representations of FIGS. 5 and 6.
  • this central floor 33 is designed with the raised part 31 and solid; in the example of FIG. 5 as an upwardly curved sheet metal with the central passage hole 32; and in the case of FIG. 6 a flat sieve.
  • the middle floor 33 is supported by a middle ring element 35.
  • This ring element 35 is in turn fastened to an outer ring 37 at a distance via spokes 36 which are evenly distributed over the circumference and are radially attached.
  • the distance between the outer ring 37 and the central ring element 35 results in a free ring area which is composed of four segments which represent gas throughflow openings 38.
  • the HMDSO which is finely distributed and partially evaporated in the packing, must flow up through these gas throughflow openings 38 through the distributor shell 29 to the top of column 1, so that the product gas mixture can then be fed to the consumer via line 6.
  • mass flow controller 18 gas introduction line 18 'direction of introduction of the carrier gas 19 mass flow controller 20 bottom of the column

Landscapes

  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Feeding, Discharge, Calcimining, Fusing, And Gas-Generation Devices (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Chemical Vapour Deposition (AREA)

Abstract

L'invention concerne un procédé de production d'un mélange gazeux contenant du HMDSO et de l'oxygène permettant d'obtenir un gaz de traitement. Pour pouvoir produire en continu un gros volume de gaz de traitement avec ce dispositif et le soustraire à des températures quasiment d'aptitude au traitement, plusieurs emballages de remplissage (2) sont empilés en colonne (1) allongée, sensiblement verticale et refroidissable de telle façon qu'un raccord d'arrivée (3) introduit dans la colonne (1) depuis l'extérieur et un raccordement de sortie de gaz (6) débouchant à l'extérieur sont fixés à la colonne (1) et de telle façon que des dispositifs (26) permettent la mesure de la température, de la pression et de la quantité du mélange gazeux sortant. De plus, une coque de répartition (29) dotée d'orifices de passage de gaz (38) recouvre la section de la colonne (1) sous l'extrémité de sortie interne (4) du raccord d'arrivée (3).
EP00990701A 1999-12-15 2000-12-14 Dispositif permettant de produire un melange gazeux Withdrawn EP1244823A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19960333A DE19960333C2 (de) 1999-12-15 1999-12-15 Vorrichtung zum Herstellen eines Gasgemisches und deren Verwendung
DE19960333 1999-12-15
PCT/EP2000/012493 WO2001044538A1 (fr) 1999-12-15 2000-12-14 Dispositif permettant de produire un melange gazeux

Publications (1)

Publication Number Publication Date
EP1244823A1 true EP1244823A1 (fr) 2002-10-02

Family

ID=7932657

Family Applications (1)

Application Number Title Priority Date Filing Date
EP00990701A Withdrawn EP1244823A1 (fr) 1999-12-15 2000-12-14 Dispositif permettant de produire un melange gazeux

Country Status (7)

Country Link
US (1) US20030094711A1 (fr)
EP (1) EP1244823A1 (fr)
JP (1) JP2003517102A (fr)
AU (1) AU3009101A (fr)
DE (1) DE19960333C2 (fr)
TW (1) TW458805B (fr)
WO (1) WO2001044538A1 (fr)

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19963122A1 (de) * 1999-12-24 2001-06-28 Tetra Laval Holdings & Finance Anordnung zum Einkoppeln von Mikrowellenenergie in eine Behandlungskammer
DE10010642B4 (de) * 2000-03-03 2007-07-26 Tetra Laval Holdings & Finance S.A. Maschine zum Beschichten von Hohlkörpern
DE10114401B4 (de) 2001-03-23 2005-03-17 Tetra Laval Holdings & Finance S.A. Verfahren zum Blasformen eines Behälters aus Kunststoff und zum Beschichten des Behälterinneren
DE102004017241B4 (de) 2004-04-05 2012-09-27 Schott Ag Verbundmaterial und Verfahren zu seiner Herstellung
DE102004043384B4 (de) * 2004-09-08 2010-06-17 Schott Ag Verfahren zur Herstellung eines beschichteten Hohlkörper-Substrates aus zumindest Polyethylenterephthalat
DE102007062977B4 (de) 2007-12-21 2018-07-19 Schott Ag Verfahren zur Herstellung von Prozessgasen für die Dampfphasenabscheidung
US9431238B2 (en) * 2014-06-05 2016-08-30 Asm Ip Holding B.V. Reactive curing process for semiconductor substrates

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Also Published As

Publication number Publication date
JP2003517102A (ja) 2003-05-20
WO2001044538A1 (fr) 2001-06-21
WO2001044538A9 (fr) 2001-10-25
DE19960333A1 (de) 2001-06-21
AU3009101A (en) 2001-06-25
DE19960333C2 (de) 2002-12-19
TW458805B (en) 2001-10-11
US20030094711A1 (en) 2003-05-22

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