EP1476585A1 - Gas quenching installation and the corresponding quenching method - Google Patents

Gas quenching installation and the corresponding quenching method

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Publication number
EP1476585A1
EP1476585A1 EP03720608A EP03720608A EP1476585A1 EP 1476585 A1 EP1476585 A1 EP 1476585A1 EP 03720608 A EP03720608 A EP 03720608A EP 03720608 A EP03720608 A EP 03720608A EP 1476585 A1 EP1476585 A1 EP 1476585A1
Authority
EP
European Patent Office
Prior art keywords
quenching
buffer
gas
pressure
cell
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
Application number
EP03720608A
Other languages
German (de)
French (fr)
Other versions
EP1476585B1 (en
Inventor
Bruno Roques
Linda Lefevre
Jean-Martial Leger
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.)
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Original Assignee
Air Liquide SA
LAir Liquide SA a Directoire et Conseil de Surveillance pour lEtude et lExploitation des Procedes Georges Claude
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Application filed by Air Liquide SA, LAir Liquide SA a Directoire et Conseil de Surveillance pour lEtude et lExploitation des Procedes Georges Claude filed Critical Air Liquide SA
Publication of EP1476585A1 publication Critical patent/EP1476585A1/en
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/62—Quenching devices
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/56—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering characterised by the quenching agents
    • C21D1/613—Gases; Liquefied or solidified normally gaseous material
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D2241/00—Treatments in a special environment
    • C21D2241/01—Treatments in a special environment under pressure

Definitions

  • the present invention relates to a gas quenching installation, of the type comprising a quenching cell intended to receive objects to be quenched and adapted to withstand a determined quenching pressure of the quenching gas, and means for supplying quenching gas under pressure, connected to this cell.
  • Gas quenching installations for steel parts.
  • Gas quenching systems are known.
  • Such an installation comprises a quenching cell in which the objects to be quenched are arranged and means for supplying quenching gas under pressure, connected to this cell.
  • Such quenching installations generally include a buffer gas intermediate storage capacity located between the gas source and the quenching cell.
  • the gas supply means comprise a compressor permanently connected to the source of quenching gas.
  • the object of the invention is to overcome these drawbacks by means of an economical quenching installation.
  • the subject of the invention is an installation of the aforementioned type, characterized in that the gas supply means comprise:
  • Said second connecting means being devoid of any means for compressing the gas between the evaporator and the buffer tank. According to particular embodiments of the installation, it may include one or more of the following characteristics:
  • the first sealing means divide said first connecting means into a buffer part associated with the buffer tank and into a cell part associated with the quenching cell and in that the volume (V ta mpon) of the buffer tank and the volume ( V ct ) of the buffer part of the connecting means form an effective buffer volume (V ta mpon- ⁇ ft), while the volume (V C ⁇ ⁇ U ie) of the quenching cell and the volume (V cc ) of the part cell connecting means form an effective cell volume (V ce ⁇ iuie-eff), the effective buffer volume (Vtampon-eff) being greater than the effective cell volume (V C ⁇ nuie-eff) •
  • the effective buffer volume (Vtampon-eff) is greater than 1.2 times the effective cell volume (V ce ⁇ iuie-eff), and in particular between 1, 4 times and 5 times this volume.
  • the buffer pressure (Ptampon) is greater than or equal to 1.2 times the quenching pressure (Pempempe), and is preferably between 1.2 and 1.8 times this pressure.
  • the quenching pressure (Tempering) is between 5 and 25 bars, and preferably between 10 and 20 bars.
  • the storage pressure (Pstockage) is greater than the buffer pressure (Ptampon), and is in particular greater than 8 bars, and is preferably between 10 and 40 bars, or even more preferably between 15 and 40 bars.
  • the installation further comprises an auxiliary source of quenching gas connected to the buffer tank by auxiliary connecting means, adapted to supply the buffer tank with auxiliary quenching gas.
  • the auxiliary source of quenching gas comprises at least one of the gases of the group formed by hydrogen and helium.
  • - Said quenching gas is nitrogen.
  • the invention further relates to a method of operating an installation as defined above, characterized by the following successive steps:
  • the buffer tank is filled with quenching gas at the buffer pressure;
  • the object to be quenched is placed in the quenching cell;
  • the first controllable closure means are open, establishing a connection between the buffer tank and the quenching cell, until the quenching pressure is established in the quenching cell,
  • the object to be soaked is cooled to a determined temperature; and - the quenched object is removed from the quench cell.
  • the installation is intended for quenching an object 3 by heat treatment.
  • the object is for example a piece of steel.
  • the quenching installation 2 comprises a high-pressure storage tank 4 for a quenching gas 6 in the liquid state, an evaporator 8 for this gas, a buffer tank 10 as well as a quenching cell 12.
  • the storage tank 4 is a so-called “high pressure” storage tank.
  • the quenching gas 6 is stored there under a storage pressure P storage greater than 8 bars, in this case between 15 and 40 bars.
  • the quenching gas 6 is for example nitrogen.
  • the storage tank 4 is provided with an outlet 14, which is connected to an inlet 16 of the evaporator 8 by a first connecting pipe 18.
  • the evaporator 8 is preferably a so-called "high pressure” evaporator, which is suitable to generate a gas under high pressure, from the reservoir of storage 4. This pressure is located slightly below the storage pressure.
  • the evaporator 8 has an outlet 20 which is connected to an inlet 22 of the buffer tank 10 by a second connecting pipe 24 provided with a first shut-off valve 26.
  • the first shut-off valve 26 is arranged at the inlet of the buffer tank 10.
  • these connecting means are devoid of any means of compressing the gas between the evaporator and the buffer tank.
  • the buffer tank 10 is adapted to withstand a pressure of the gas during the operation of the installation, called the buffer pressure Ptamp o n- It is substantially identical to the pressure of the gas at the outlet of the evaporator 8.
  • An outlet 28 of the buffer tank 10 is connected to an inlet 30 of the quenching cell 12 by means of a third connection pipe 32 provided with a second shut-off valve 34.
  • the quenching cell 12 is suitable for resist a gas pressure during quenching, called quenching pressure Ptr e mp e -
  • the buffer tank 10 proper has a volume V a mpon-
  • the volume of the third line 32 consists of a first part V ct associated with the buffer tank 10, extending between the buffer tank 10 and the second stop valve 34, as well as a second part V cc , associated with the quenching cell 12 and extending between the second valve 34 and this cell 12.
  • the quenching cell has a volume V ce ⁇ iuie-
  • the two volumes V ta mpon and V ct taken together define an effective buffer volume V tamp on- ⁇ ff, while the two volumes V C ⁇ nuie and V cc taken together define an effective cell volume V C ⁇ iiui ⁇ - ⁇ ff-
  • the effective buffer volume V la mpon- ⁇ ff is greater than the effective cell volume V C ⁇ ⁇ iui ⁇ - ⁇ ff.
  • the effective buffer volume V ta mpon-eff is greater than 1.2 times the effective cell volume V C ⁇ ⁇ U i ⁇ - ⁇ ff. and is in particular between 1, 4 times and 5 times this volume.
  • the effective buffer volume V ta mpon- ⁇ ff advantageously satisfies the condition Vtam P on-eff ⁇ Vceuuk-eff pe -.
  • the buffer— r quenching effective buffer volume and the effective cell volume are related by the relationship , which minimizes the size of the tank 10.
  • the installation also includes means for evacuating the quenching cell 12. These evacuation means consist of a vacuum pump 36 connected to the quenching cell 12 by a fourth pipe 38.
  • the installation according to the invention works as follows. Initially, the buffer tank 10 comprises quenching gas at a residual pressure, and the quenching cell 12 comprises a residual atmosphere generally at a pressure below atmospheric pressure. In the quenching cell there is no object to be quenched.
  • the second stop valve 34 is closed and the first stop valve 26 is open.
  • the evaporator 8 is thus started and produces quenching gas, which has substantially the buffer pressure P tampo n, and a temperature Ttampon-
  • This pressure P ta m P on is here between 25 and 35 bars.
  • the evaporator 8 is stopped by closing the first valve 26.
  • the filling of the buffer tank 10 typically lasts between 5 and 20 minutes.
  • the object to be soaked 3 undergoes a heat treatment (not shown). Then the object 3 to be soaked hot is placed in the quenching cell 12 and the latter is closed.
  • the pressure prevailing in the quenching cell 12 is often the ambient pressure i.e. around 1000 hPa (but it could also be under vacuum initially), and the temperature is ambient temperature.
  • the quenching gas 6 contained in the buffer tank 10 flows rapidly through the third line 32 in the quenching cell 12, until the desired quenching pressure is reached.
  • This quenching pressure Ptr e mp e is between 5 and 25 bars, preferably between 10 and 20 bars.
  • the buffer pressure Ptampon it is advantageous for the buffer pressure Ptampon to be chosen between 1.2 and 1.8 times the quenching pressure in order to be able to use a buffer tank which is not very bulky.
  • the quenching cell 12 When the object to be quenched 3 has reached the desired temperature, the quenching cell 12 is depressurized, and the quenched object 3 is removed from the cell. Finally, the second stop valve 34 is closed and the first stop valve 26 is open.
  • the treatment cycle can start again.
  • the installation according to the invention has the following advantages. Since the effective buffer volume V ta mpon-eff is greater than the effective cell volume V C ⁇ ⁇ iuie- ⁇ ff. the gas pressure in the buffer tank Ptampon is relatively low, for a given quenching pressure Ptempe. As a result, the wall thickness of the buffer tank 10 can be relatively small. In addition, this installation does not have a compressor placed between the evaporator 8 and the buffer tank 10, which eliminates the consumption of electrical energy during the generation of pressurized gas Pt ampo n- The installation also has a high availability thanks to the low maintenance time required. In addition, the installation is compact and produces little noise.
  • the buffer tank 10 can be arranged adjacent to the quenching cell 12, so that the third line 32 can be omitted.
  • the volumes V ct and V cc are equal to 0, and the effective volumes V tam pon- ⁇ ff and V c ⁇ ⁇ iui ⁇ -eff are identical to the respective volumes of the buffer tank 10 and the quenching cell 12.
  • the buffer tank is supplied only from the high-pressure liquid storage / evaporator assembly
  • auxiliary quenching gas gas advantageously comprising at least one of the gases of the group formed by hydrogen and helium, for example in order to thus have mixtures of quenching nitrogen-helium, nitrogen-hydrogen, C ⁇ 2 -helium etc ...
  • high pressure storage tank for quenching gas in liquid state has been used in all of the above to mean that there is thus a high pressure reserve in liquid form of quenching gas.
  • This reservation advantageously will simply be in the form of high pressure storage but it is understood that it is also possible (for example for practical reasons related to the local site), and without in any way departing from the scope of the present invention, consider this “high pressure storage tank” in the form of a combination of a storage tank in low pressure liquid form, which supplies a system for pressurizing the quenching gas in the liquid state.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Filling Or Discharging Of Gas Storage Vessels (AREA)
  • Superconductors And Manufacturing Methods Therefor (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Auxiliary Devices For And Details Of Packaging Control (AREA)
  • Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
  • Electrical Discharge Machining, Electrochemical Machining, And Combined Machining (AREA)

Abstract

The invention relates to a gas quenching installation comprising a quenching cell ( 12 ), a buffer tank ( 10 ) which is intended to contain the quenching gas ( 6 ), gas connection means ( 32 ) which link the buffer tank ( 10 ) with the quenching cell ( 12 ) and gas supply means. Said gas supply means consist of an evaporator ( 8 ), the outlet ( 20 ) of which is connected to an inlet ( 22 ) in the buffer tank ( 10 ), and a high pressure storage tank ( 4 ) for the liquid-state quenching gas ( 6 ) which is connected to an inlet ( 16 ) in the evaporator ( 8 ), the connection means between the evaporator and the buffer tank having no gas compression means. The invention applies to installations used for the nitrogen quenching of steel parts.

Description

INSTALLATION DE TREMPE PAR GAZ ET PROCEDE DE TREMPE CORRESPONDANT GAS QUENCHING PLANT AND CORRESPONDING QUENCHING METHOD
La présente invention concerne une installation de trempe par gaz, du type comprenant une cellule de trempe destinée à recevoir des objets à tremper et adaptée pour résister à une pression de trempe déterminée du gaz de trempe, et des moyens de fourniture de gaz de trempe sous pression, raccordés à cette cellule.The present invention relates to a gas quenching installation, of the type comprising a quenching cell intended to receive objects to be quenched and adapted to withstand a determined quenching pressure of the quenching gas, and means for supplying quenching gas under pressure, connected to this cell.
Elle s'applique notamment aux installations de trempe par gaz de pièces en acier. On connaît des installations de trempe par gaz. Une telle installation comprend une cellule de trempe dans laquelle sont disposés les objets à tremper et des moyens de fourniture de gaz de trempe sous pression, raccordés à cette cellule. De telles installations de trempe comprennent généralement une capacité tampon de stockage intermédiaire du gaz située entre la source de gaz et la cellule de trempe.It applies in particular to gas quenching installations for steel parts. Gas quenching systems are known. Such an installation comprises a quenching cell in which the objects to be quenched are arranged and means for supplying quenching gas under pressure, connected to this cell. Such quenching installations generally include a buffer gas intermediate storage capacity located between the gas source and the quenching cell.
Dans le cas d'une installation de trempe à haute pression (par exemple 20 bars et plus), les moyens de fourniture de gaz comprennent un compresseur relié en permanence à la source de gaz de trempe.In the case of a high-pressure quenching installation (for example 20 bars or more), the gas supply means comprise a compressor permanently connected to the source of quenching gas.
L'utilisation d'un compresseur dans une telle installation présente notamment les inconvénients suivants : le coût de l'investissement du compresseur, l'indisponibilité de l'installation de trempe pour le temps d'entretien du compresseur, la consommation électrique du compresseur et les nuisances sonores dues au compresseur.The use of a compressor in such an installation has in particular the following drawbacks: the cost of the investment of the compressor, the unavailability of the quenching installation for the compressor maintenance time, the electrical consumption of the compressor and noise pollution due to the compressor.
L'invention a pour but de pallier ces inconvénients au moyen d'une installation de trempe qui soit économique.The object of the invention is to overcome these drawbacks by means of an economical quenching installation.
A cet effet, l'invention a pour objet une installation du type précité, caractérisé en ce que les moyens de fourniture de gaz comprennent:To this end, the subject of the invention is an installation of the aforementioned type, characterized in that the gas supply means comprise:
- un évaporateur dont la sortie est reliée à une entrée du réservoir tampon, par des deuxièmes moyens de liaison, et - un réservoir haute pression de stockage du gaz de trempe à l'état liquide, sous une pression de stockage (Pstockage), relié à une entrée de l'évaporateur (8) par des troisièmes moyens de liaison;- an evaporator, the outlet of which is connected to an inlet of the buffer tank, by second connecting means, and - a high pressure tank for storing the quenching gas in the liquid state, under a storage pressure (P s tockage) , connected to an inlet of the evaporator (8) by third connection means;
- lesdits deuxièmes moyens de liaison étant dépourvus de tout moyen de compression du gaz entre l'évaporateur et le réservoir tampon. Suivant des modes particuliers de réalisation de l'installation, celle-ci peut comporter l'une ou plusieurs des caractéristiques suivantes :- Said second connecting means being devoid of any means for compressing the gas between the evaporator and the buffer tank. According to particular embodiments of the installation, it may include one or more of the following characteristics:
- les premiers moyens d'obturation divisent lesdits premiers moyens de liaison en une partie tampon associée au réservoir tampon et en une partie cellule associée à la cellule de trempe et en ce que le volume (Vtampon) du réservoir tampon et le volume (Vct) de la partie tampon des moyens de liaison forment un volume tampon effectif (Vtampon-θft), tandis que le volume (VCθιιUie) de la cellule de trempe et le volume (Vcc) de la partie cellule des moyens de liaison forment un volume de cellule effectif (Vceιiuie-eff), le volume tampon effectif (Vtampon-eff) étant supérieur au volume de cellule effectif (VCθnuie-eff) •the first sealing means divide said first connecting means into a buffer part associated with the buffer tank and into a cell part associated with the quenching cell and in that the volume (V ta mpon) of the buffer tank and the volume ( V ct ) of the buffer part of the connecting means form an effective buffer volume (V ta mpon-θft), while the volume (V Cθ ιι U ie) of the quenching cell and the volume (V cc ) of the part cell connecting means form an effective cell volume (V ce ιiuie-eff), the effective buffer volume (Vtampon-eff) being greater than the effective cell volume (V Cθ nuie-eff) •
- le volume tampon effectif (Vtampon-eff) est supérieur à 1 ,2 fois le volume de cellule effectif (Vceιiuie-eff), et notamment compris entre 1 ,4 fois et 5 fois ce volume.- The effective buffer volume (Vtampon-eff) is greater than 1.2 times the effective cell volume (V ce ιiuie-eff), and in particular between 1, 4 times and 5 times this volume.
- la pression tampon (Ptampon) est supérieure à la pression de trempe (Ptrempe), et le volume tampon et le volume de cellule effectifs sont liés par la- the buffer pressure (Ptampon) is greater than the quenching pressure (Ptr e mp e ), and the effective buffer volume and cell volume are linked by the
relation Vtamp(m_eff ≥Vcellule_eff p empe . tampon-Ptrempe relation V buffer (m _ eff ≥V cell _ eff p emp . buffer-P quenching
- le volume tampon effectif et le volume de cellule effectif sont liés par la relation . - the effective buffer volume and the effective cell volume are linked by the relation.
- la pression tampon (Ptampon) est supérieure ou égale à 1 ,2 fois la pression de trempe (Ptrempe), et est de préférence comprise entre 1 ,2 et 1 ,8 fois cette pression.- The buffer pressure (Ptampon) is greater than or equal to 1.2 times the quenching pressure (Pempempe), and is preferably between 1.2 and 1.8 times this pressure.
- la pression tampon (Ptampon) est comprise entre 15 et 35 bars.- the buffer pressure (Ptampon) is between 15 and 35 bars.
- la pression de trempe (Ptrempe) est comprise entre 5 et 25 bars, et de préférence entre 10 et 20 bars. - la pression de stockage (Pstockage) est supérieure à la pression tampon (Ptampon), et est notamment supérieure à 8 bars, et est de préférence comprise entre 10 et 40 bars, voire encore plus préférentiellement entre 15 et 40 bars.- the quenching pressure (Tempering) is between 5 and 25 bars, and preferably between 10 and 20 bars. - The storage pressure (Pstockage) is greater than the buffer pressure (Ptampon), and is in particular greater than 8 bars, and is preferably between 10 and 40 bars, or even more preferably between 15 and 40 bars.
- l'installation comprend en outre une source auxiliaire de gaz de trempe reliée au réservoir tampon par des moyens auxiliaires de liaison, aptes à alimenter le réservoir tampon en gaz auxiliaire de trempe. - la source auxiliaire de gaz de trempe comprend au moins l'un des gaz du groupe formé par l'hydrogène et l'hélium.- The installation further comprises an auxiliary source of quenching gas connected to the buffer tank by auxiliary connecting means, adapted to supply the buffer tank with auxiliary quenching gas. - The auxiliary source of quenching gas comprises at least one of the gases of the group formed by hydrogen and helium.
- ledit gaz de trempe est de l'azote.- Said quenching gas is nitrogen.
- ledit gaz de trempe est du C02 ou comporte du C02. L'invention a en outre pour objet un procédé d'exploitation d'une installation telle que définie ci-dessus, caractérisé par les étapes successives suivantes :- said quenching gas is C0 2 or comprises C0 2 . The invention further relates to a method of operating an installation as defined above, characterized by the following successive steps:
- le réservoir tampon est empli de gaz de trempe à la pression tampon ; - l'objet à tremper est disposé dans la cellule de trempe;- the buffer tank is filled with quenching gas at the buffer pressure; - the object to be quenched is placed in the quenching cell;
- les premiers moyens d'obturation commandables sont ouverts, établissant une liaison entre le réservoir tampon et la cellule de trempe, jusqu'à l'établissement de la pression de trempe dans la cellule de trempe,the first controllable closure means are open, establishing a connection between the buffer tank and the quenching cell, until the quenching pressure is established in the quenching cell,
- l'objet à tremper est refroidi à une température déterminée ; et - l'objet trempé est retiré de la cellule de trempe.- The object to be soaked is cooled to a determined temperature; and - the quenched object is removed from the quench cell.
L'invention sera mieux comprise à la lecture de la description qui va suivre, donnée uniquement à titre d'exemple et faite en se référant au dessin annexé dont la Figure unique représente schématiquement une installation suivant l'invention. La Figure unique montre une installation de trempe par gaz selon l'invention, désignée par la référence générale 2.The invention will be better understood on reading the description which follows, given solely by way of example and made with reference to the appended drawing, the single figure of which schematically represents an installation according to the invention. The single figure shows a gas quenching installation according to the invention, designated by the general reference 2.
L'installation est destinée à la trempe d'un objet 3 par traitement thermique. L'objet est par exemple une pièce en acier.The installation is intended for quenching an object 3 by heat treatment. The object is for example a piece of steel.
L'installation de trempe 2 comprend un réservoir de stockage haute pression 4 d'un gaz de trempe 6 à l'état liquide, un évaporateur 8 de ce gaz, un réservoir tampon 10 ainsi qu'une cellule de trempe 12.The quenching installation 2 comprises a high-pressure storage tank 4 for a quenching gas 6 in the liquid state, an evaporator 8 for this gas, a buffer tank 10 as well as a quenching cell 12.
Le réservoir de stockage 4 est un réservoir de stockage dit « haute pression ». Le gaz de trempe 6 y est stocké sous une pression de stockage Pstockage supérieure à 8 bars, en l'occurrence comprise entre 15 et 40 bars. Le gaz de trempe 6 est par exemple de l'azote.The storage tank 4 is a so-called “high pressure” storage tank. The quenching gas 6 is stored there under a storage pressure P storage greater than 8 bars, in this case between 15 and 40 bars. The quenching gas 6 is for example nitrogen.
Le réservoir de stockage 4 est muni d'une sortie 14, qui est reliée à une entrée 16 de l'évaporateur 8 par une première conduite de liaison 18. L'évaporateur 8 est préférentiellement un évaporateur dit « haute pression », qui est adapté pour générer un gaz sous une haute pression, à partir du réservoir de stockage 4. Cette pression est située légèrement au-dessous de la pression de stockage.The storage tank 4 is provided with an outlet 14, which is connected to an inlet 16 of the evaporator 8 by a first connecting pipe 18. The evaporator 8 is preferably a so-called "high pressure" evaporator, which is suitable to generate a gas under high pressure, from the reservoir of storage 4. This pressure is located slightly below the storage pressure.
L'évaporateur 8 comporte une sortie 20 qui est reliée à une entrée 22 du réservoir tampon 10 par une deuxième conduite de liaison 24 munie d'une première vanne d'arrêt 26. La première vanne d'arrêt 26 est disposée à l'entrée du réservoir tampon 10.The evaporator 8 has an outlet 20 which is connected to an inlet 22 of the buffer tank 10 by a second connecting pipe 24 provided with a first shut-off valve 26. The first shut-off valve 26 is arranged at the inlet of the buffer tank 10.
Conformément à l'invention, ces moyens de liaison sont dépourvus de tout moyen de compression du gaz entre l'évaporateur et le réservoir tampon.According to the invention, these connecting means are devoid of any means of compressing the gas between the evaporator and the buffer tank.
Le réservoir tampon 10 est adapté pour résister à une pression du gaz pendant l'exploitation de l'installation, appelée pression tampon Ptampon- Elle est sensiblement identique à la pression du gaz à la sortie de l'évaporateur 8.The buffer tank 10 is adapted to withstand a pressure of the gas during the operation of the installation, called the buffer pressure Ptamp o n- It is substantially identical to the pressure of the gas at the outlet of the evaporator 8.
Une sortie 28 du réservoir tampon 10 est reliée à une entrée 30 de la cellule de trempe 12 par l'intermédiaire d'une troisième conduite de liaison 32 munie d'une seconde vanne d'arrêt 34. La cellule de trempe 12 est adaptée pour résister à une pression du gaz lors de la trempe, appelée pression de trempe Ptrempe-An outlet 28 of the buffer tank 10 is connected to an inlet 30 of the quenching cell 12 by means of a third connection pipe 32 provided with a second shut-off valve 34. The quenching cell 12 is suitable for resist a gas pressure during quenching, called quenching pressure Ptr e mp e -
Le réservoir tampon 10 proprement dit a un volume Vampon- Le volume de la troisième conduite 32 est constituée d'une première partie Vct associée au réservoir tampon 10, s'étendant entre le réservoir tampon 10 et la seconde vanne d'arrêt 34, ainsi que d'une seconde partie Vcc, associée à la cellule de trempe 12 et s'étendant entre la seconde vanne 34 et cette cellule 12. La cellule de trempe a un volume Vceιiuie-The buffer tank 10 proper has a volume V a mpon- The volume of the third line 32 consists of a first part V ct associated with the buffer tank 10, extending between the buffer tank 10 and the second stop valve 34, as well as a second part V cc , associated with the quenching cell 12 and extending between the second valve 34 and this cell 12. The quenching cell has a volume V ce ιiuie-
Les deux volumes Vtampon et Vct pris ensemble définissent un volume tampon effectif Vtampon-θff, tandis que les deux volumes VCθnuie et Vcc prises ensemble définissent un volume de cellule effectif VCβiiuiβ-θff-The two volumes V ta mpon and V ct taken together define an effective buffer volume V tamp on-θff, while the two volumes V Cθ nuie and V cc taken together define an effective cell volume V C βiiuiβ-θff-
Selon un mode avantageux de mise en œuvre de l'invention, le volume tampon effectif Vlampon-θff est supérieur au volume de cellule effectif VCθιiuiθ- θff. De préférence, le volume tampon effectif Vtampon-eff est supérieur à 1 ,2 fois le volume de cellule effectif VCθιιUiθ-βff. et est notamment compris entre 1 ,4 fois et 5 fois ce volume.According to an advantageous embodiment of the invention, the effective buffer volume V la mpon-θff is greater than the effective cell volume V Cθ ιiuiθ- θ ff. Preferably, the effective buffer volume V ta mpon-eff is greater than 1.2 times the effective cell volume V Cθ ιι U iθ-βff. and is in particular between 1, 4 times and 5 times this volume.
Le volume tampon effectif Vtampon-θff satisfait avantageusement la condition VtamPon-eff≥Vceuuk-eff pe — . Dans un mode de réalisation particulier, le tampon— rtrempe volume tampon effectif et le volume de cellule effectif sont liés par la relation , ce qui permet de minimiser l'encombrement du réservoir 10.The effective buffer volume V ta mpon- θ ff advantageously satisfies the condition Vtam P on-eff≥Vceuuk-eff pe -. In a particular embodiment, the buffer— r quenching effective buffer volume and the effective cell volume are related by the relationship , which minimizes the size of the tank 10.
L'installation comporte par ailleurs des moyens de mise sous vide de la cellule de trempe 12. Ces moyens de mise sous vide sont constitués par une pompe à vide 36 reliée à la cellule de trempe 12 par une quatrième conduite 38. L'installation selon l'invention fonctionne de la façon suivante. Initialement, le réservoir tampon 10 comprend du gaz de trempe à une pression résiduelle, et la cellule de trempe 12 comprend une atmosphère résiduelle généralement à un pression inférieure à la pression atmosphérique. Dans la cellule de trempe il n'y a pas d'objet à tremper.The installation also includes means for evacuating the quenching cell 12. These evacuation means consist of a vacuum pump 36 connected to the quenching cell 12 by a fourth pipe 38. The installation according to the invention works as follows. Initially, the buffer tank 10 comprises quenching gas at a residual pressure, and the quenching cell 12 comprises a residual atmosphere generally at a pressure below atmospheric pressure. In the quenching cell there is no object to be quenched.
La seconde vanne d'arrêt 34 est fermée et la première vanne 26 d'arrêt est ouverte. L'évaporateur 8 est ainsi mis en route et produit du gaz de trempe, qui a sensiblement la pression tampon Ptampon, et une température Ttampon- Cette pression PtamPon est comprise ici entre 25 et 35 bars. Lorsque la pression dans le réservoir tampon 10 atteint la pressionThe second stop valve 34 is closed and the first stop valve 26 is open. The evaporator 8 is thus started and produces quenching gas, which has substantially the buffer pressure P tampo n, and a temperature Ttampon- This pressure P ta m P on is here between 25 and 35 bars. When the pressure in the buffer tank 10 reaches the pressure
Ptampon, l'évaporateur 8 est arrêté par fermeture de la première vanne 26. L'emplissage du réservoir tampon 10 dure typiquement entre 5 et 20 minutes.P t ampon, the evaporator 8 is stopped by closing the first valve 26. The filling of the buffer tank 10 typically lasts between 5 and 20 minutes.
Pendant ce temps, l'objet à tremper 3 subit un traitement thermique (non représenté). Puis l'objet 3 à tremper chaud est disposé dans la cellule de trempe 12 et celle-ci est fermée. La pression régnant dans la cellule de trempe 12 est souvent la pression ambiante i.e. environ 1000 hPa (mais elle pourrait également être sous vide initialement), et la température est la température ambiante.During this time, the object to be soaked 3 undergoes a heat treatment (not shown). Then the object 3 to be soaked hot is placed in the quenching cell 12 and the latter is closed. The pressure prevailing in the quenching cell 12 is often the ambient pressure i.e. around 1000 hPa (but it could also be under vacuum initially), and the temperature is ambient temperature.
Ensuite, la seconde vanne d'arrêt 34 est ouverte. Le gaz de trempe 6 contenu dans le réservoir tampon 10 s'écoule rapidement par l'intermédiaire de la troisième conduite 32 dans la cellule de trempe 12, jusqu'à ce que la pression de trempe désirée soit atteinte. Cette pression de trempe Ptrempe est comprise entre 5 et 25 bars, de préférence entre 10 et 20 bars. Par ailleurs, il est avantageux que la pression tampon Ptampon soit choisie entre 1 ,2 et 1 ,8 fois la pression de trempe afin de pouvoir utiliser un réservoir tampon qui ne soit pas très encombrant.Then, the second stop valve 34 is opened. The quenching gas 6 contained in the buffer tank 10 flows rapidly through the third line 32 in the quenching cell 12, until the desired quenching pressure is reached. This quenching pressure Ptr e mp e is between 5 and 25 bars, preferably between 10 and 20 bars. Furthermore, it is advantageous for the buffer pressure Ptampon to be chosen between 1.2 and 1.8 times the quenching pressure in order to be able to use a buffer tank which is not very bulky.
Lorsque l'objet à tremper 3 a atteint la température souhaitée, la cellule de trempe 12 est dépressurisée, et l'objet trempé 3 est retiré de la cellule. Enfin, la seconde vanne d'arrêt 34 est fermée et la première vanne d'arrêt 26 est ouverte.When the object to be quenched 3 has reached the desired temperature, the quenching cell 12 is depressurized, and the quenched object 3 is removed from the cell. Finally, the second stop valve 34 is closed and the first stop valve 26 is open.
Le cycle de traitement peut recommencer. L'installation suivant l'invention présente les avantages suivants. Etant donné que le volume tampon effectif Vtampon-eff est supérieur au volume de cellule effectif VCΘιiuie-θff. la pression du gaz dans le réservoir tampon Ptampon est relativement faible, pour une pression de trempe Ptrempe donnée. En conséquence, l'épaisseur de paroi du réservoir tampon 10 peut être relativement faible. En outre, cette installation est dépourvue d'un compresseur disposé entre l'évaporateur 8 et le réservoir tampon 10, ce qui supprime la consommation d'énergie électrique pendant la génération de gaz sous pression Ptampon- L'installation présente également une haute disponibilité grâce au faible temps d'entretien nécessaire. De plus, l'installation est peu encombrante et produit peu de bruit.The treatment cycle can start again. The installation according to the invention has the following advantages. Since the effective buffer volume V ta mpon-eff is greater than the effective cell volume V CΘ ιiuie-θff. the gas pressure in the buffer tank Ptampon is relatively low, for a given quenching pressure Ptempe. As a result, the wall thickness of the buffer tank 10 can be relatively small. In addition, this installation does not have a compressor placed between the evaporator 8 and the buffer tank 10, which eliminates the consumption of electrical energy during the generation of pressurized gas Pt ampo n- The installation also has a high availability thanks to the low maintenance time required. In addition, the installation is compact and produces little noise.
En variante, le réservoir tampon 10 peut être disposé adjacent à la cellule de trempe 12, de telle sorte que la troisième conduite 32 peut être supprimée. Dans ce cas, les volumes Vct et Vcc sont égaux à 0, et les volumes effectifs Vtampon-θff et Vcθιiuiθ-eff sont identiques aux volumes respectifs du réservoir tampon 10 et de la cellule de trempe 12.Alternatively, the buffer tank 10 can be arranged adjacent to the quenching cell 12, so that the third line 32 can be omitted. In this case, the volumes V ct and V cc are equal to 0, and the effective volumes V tam pon-θff and V cθ ιiuiθ-eff are identical to the respective volumes of the buffer tank 10 and the quenching cell 12.
Si l'invention a été tout particulièrement illustrée dans ce qui précède par une structure où le réservoir tampon est alimenté uniquement à partir de l'ensemble stockage liquide haute pression/évaporateur, on conçoit qu'il est possible également et extrêmement avantageux de prévoir selon l'invention la possibilité d'alimenter le réservoir tampon également en un gaz auxiliaire de trempe, via une source auxiliaire de gaz de trempe reliée au réservoir tampon par des moyens auxiliaires de liaison, un tel gaz auxiliaire de gaz de trempe comprenant avantageusement au moins l'un des gaz du groupe formé par l'hydrogène et l'hélium, par exemple afin de disposer ainsi de mélanges de trempe azote-helium, azote-hydrogène, Cθ2-hélium etc....If the invention has been particularly illustrated in the foregoing by a structure where the buffer tank is supplied only from the high-pressure liquid storage / evaporator assembly, it will be understood that it is also possible and extremely advantageous to provide according to the invention the possibility of supplying the buffer tank also with an auxiliary quenching gas, via an auxiliary source of quenching gas connected to the buffer tank by auxiliary connection means, such an auxiliary quenching gas gas advantageously comprising at least one of the gases of the group formed by hydrogen and helium, for example in order to thus have mixtures of quenching nitrogen-helium, nitrogen-hydrogen, Cθ 2 -helium etc ...
De même comme il apparaîtra clairement à l'homme du métier, on a utilisé dans tout ce qui précède la terminologie « réservoir de stockage haute pression du gaz de trempe à l'état liquide » pour signifier que l'on dispose ainsi d'une réserve haute pression sous forme liquide du gaz de trempe. Cette réserve se présentera avantageusement tout simplement sous la forme d'un stockage haute pression mais on conçoit que l'on peut également (par exemple pour des raisons pratiques liées au site local), et sans sortir en aucune façon du cadre de la présente invention, envisager ce « réservoir de stockage haute pression » sous la forme de la combinaison d'un réservoir de stockage sous forme liquide à basse pression, qui alimente un système de pressurisation du gaz de trempe à l'état liquide. Ceci bien sur dans la mesure où la condition selon l'invention selon laquelle les deuxièmes moyens de liaison entre l'évaporateur et le réservoir tampon sont dépourvus de tout moyen de compression du gaz est bien respectée. Likewise, as will be clear to a person skilled in the art, the terminology “high pressure storage tank for quenching gas in liquid state” has been used in all of the above to mean that there is thus a high pressure reserve in liquid form of quenching gas. This reservation advantageously will simply be in the form of high pressure storage but it is understood that it is also possible (for example for practical reasons related to the local site), and without in any way departing from the scope of the present invention, consider this “high pressure storage tank” in the form of a combination of a storage tank in low pressure liquid form, which supplies a system for pressurizing the quenching gas in the liquid state. This of course insofar as the condition according to the invention according to which the second connection means between the evaporator and the buffer tank are devoid of any gas compression means is well respected.

Claims

REVENDICATIONS
1. Installation de trempe par gaz, du type comprenant :1. Gas quenching installation, of the type comprising:
- une cellule de trempe (12) destinée à recevoir des objets à tremper (3) et adaptée pour résister à une pression de trempe (Ptrempe) déterminée du gaz de trempe ; et- a quenching cell (12) intended to receive objects to be quenched (3) and adapted to resist a determined quenching pressure (quenching) of the quenching gas; and
- des moyens de fourniture de gaz de trempe sous pression, raccordés à cette cellule, les moyens de fourniture de gaz comprenant : i) un réservoir tampon (10) adapté pour contenir le gaz de trempe (6) et pour résister à une pression tampon (Pta pon) déterminée du gaz de trempe, j) des premiers moyens de liaison (32) de gaz reliant le réservoir tampon (10) à la cellule de trempe (12); k) des premiers moyens d'obturation (34) commandables desdits premiers moyens de liaison (32) ;- means for supplying pressurized quenching gas, connected to this cell, the means for supplying gas comprising: i) a buffer tank (10) adapted to contain the quenching gas (6) and to resist a buffer pressure (Pt a pon) determined the quenching gas, j) first gas connecting means (32) connecting the buffer tank (10) to the quenching cell (12); k) first shutter means (34) controllable from said first connecting means (32);
I) des moyens d'alimentation (4, 8, 18, 24, 26) en gaz de trempe du réservoir tampon (10) sous une pression supérieure à la pression atmosphérique ; caractérisée en ce que les moyens d'alimentation en gaz comprennent :I) means (4, 8, 18, 24, 26) for supplying quench gas to the buffer tank (10) at a pressure greater than atmospheric pressure; characterized in that the gas supply means comprise:
- un évaporateur (8) dont la sortie (20) est reliée à une entrée (22) du réservoir tampon (10), par des deuxièmes moyens de liaison (24), etan evaporator (8), the outlet (20) of which is connected to an inlet (22) of the buffer tank (10), by second connecting means (24), and
- un réservoir de stockage (4) haute pression du gaz de trempe (6) à l'état liquide, sous une pression de stockage (Pstockage), relié à une entrée (16) de l'évaporateur (8) par des troisièmes moyens de liaison (18) ;- a high pressure storage tank (4) for the quenching gas (6) in the liquid state, under a storage pressure (storage), connected to an inlet (16) of the evaporator (8) by third means link (18);
- lesdits deuxièmes moyens de liaison étant dépourvus de tout moyen de compression du gaz entre l'évaporateur et le réservoir tampon.- Said second connecting means being devoid of any means for compressing the gas between the evaporator and the buffer tank.
2. Installation suivant la revendication 1 , caractérisée en ce que les premiers moyens d'obturation (34) divisent lesdits premiers moyens de liaison (32) en une partie tampon associée au réservoir tampon (10) et en une partie cellule associée à la cellule de trempe (12), et en ce que le volume (Vtampon) du réservoir tampon (10) et le volume (Vct) de la partie tampon des moyens de liaison (32) forment un volume tampon effectif (Vtampon-eff), tandis que le volume (Vceiiuie) de la cellule de trempe (12) et le volume (Vcc) de la partie cellule des moyens de liaison (32) forment un volume de cellule effectif (Vceιιuie-eff), et en ce que le volume tampon effectif (Vtampon-eff) est supérieur au volume de cellule effectif (VCθiiule-eff)-2. Installation according to claim 1, characterized in that the first sealing means (34) divide said first connecting means (32) into a buffer part associated with the buffer tank (10) and into a cell part associated with the cell quenching (12), and in that the volume (Vt am pon) of the buffer tank (10) and the volume (V ct ) of the buffer part of the connecting means (32) form an effective buffer volume (V ta mpon -eff), while the volume (Vceiiuie) of the quenching cell (12) and the volume (V cc ) of the cell part of the connecting means (32) form an effective cell volume (V ce ιι u i e - eff ), and in this that the effective buffer volume (V tam pon-eff) is greater than the effective cell volume (V C θiiule-eff) -
3. Installation suivant la revendication 2, caractérisée en ce que le volume tampon effectif (Vtampon-eff) est supérieur à 1 ,2 fois le volume de cellule effectif (Vceiiuie-eff), et notamment compris entre 1 ,4 fois et 5 fois ce volume.3. Installation according to claim 2, characterized in that the effective buffer volume (V tam pon-eff) is greater than 1.2 times the effective cell volume (Vceiiuie-eff), and in particular between 1, 4 times and 5 times this volume.
4. Installation suivant l'une quelconque des revendications 2 ou 3, caractérisée en ce que la pression tampon (Ptampon) est supérieure à la pression de trempe (Ptrempe), et en ce que le volume tampon et le volume de cellule p effectifs sont liés par la relation Vlampon_eff ≥ Vcdlule_eff p tampon- f ptrempe 5. Installation suivant la revendication 4, caractérisée en ce que le volume tampon effectif et le volume de cellule effectif sont liés par la relation4. Installation according to any one of claims 2 or 3, characterized in that the buffer pressure (P ta mp o n) is greater than the quenching pressure (Ptrempe), and in that the buffer volume and the volume of cell p effective are linked by the relation V lampon _ eff ≥ V cdlule _ eff p buffer- fp quenching 5. Installation according to claim 4, characterized in that the effective buffer volume and the effective cell volume are linked by the relation
6. Installation suivant l'une quelconque des revendications précédentes, caractérisée en ce que la pression tampon (Ptampon) est supérieure ou égale à 1 ,2 fois la pression de trempe (Ptrempe), et est de préférence comprise entre 1 ,2 et 1 ,8 fois cette pression.6. Installation according to any one of the preceding claims, characterized in that the buffer pressure (Ptampon) is greater than or equal to 1.2 times the quenching pressure (Ptrempe), and is preferably between 1, 2 and 1 , 8 times this pressure.
7. Installation suivant l'une quelconque des revendications précédentes, caractérisée en ce que la pression tampon (Ptampon) est comprise entre 15 et 35 bars. 7. Installation according to any one of the preceding claims, characterized in that the buffer pressure (Pt ampo n) is between 15 and 35 bars.
8. Installation suivant l'une quelconque des revendications précédentes, caractérisée en ce que la pression de trempe (Ptrempe) est comprise entre 5 et 25 bars, et de préférence entre 10 et 20 bars.8. Installation according to any one of the preceding claims, characterized in that the quenching pressure (P t r e mp e ) is between 5 and 25 bars, and preferably between 10 and 20 bars.
9. Installation suivant la revendication 8, caractérisée en ce que la pression de stockage (Pstockage) est supérieure à la pression tampon (Ptampon), et est notamment supérieure à 8 bars, et est de préférence comprise entre 10 et 40 bars, voire encore plus préférentiellement entre 15 et 40 bars.9. Installation according to claim 8, characterized in that the storage pressure (Pstockage) is greater than the buffer pressure (P tam pon), and is in particular greater than 8 bars, and is preferably between 10 and 40 bars, or even more preferably between 15 and 40 bars.
10. Installation suivant l'une des revendications précédentes, caractérisée en ce qu'elle comprend une source auxiliaire de gaz de trempe reliée au réservoir tampon par des moyens auxiliaires de liaison, aptes à alimenter le réservoir tampon en gaz auxiliaire de trempe. 10. Installation according to one of the preceding claims, characterized in that it comprises an auxiliary source of quenching gas connected to the buffer tank by auxiliary connecting means, capable of supplying the buffer tank with auxiliary quenching gas.
11. Installation suivant la revendication 10, caractérisée en ce que ladite source auxiliaire de gaz de trempe comprend au moins l'un des gaz du groupe formé par l'hydrogène et l'hélium.11. Installation according to claim 10, characterized in that said auxiliary source of quenching gas comprises at least one of the gases of the group formed by hydrogen and helium.
12. Installation suivant l'une quelconque des revendications précédentes, caractérisé en ce que ledit gaz de trempe est de l'azote.12. Installation according to any one of the preceding claims, characterized in that said quenching gas is nitrogen.
13. Installation suivant l'une quelconque des revendications 1 à 11 , caractérisé en ce que ledit gaz de trempe est du C02 ou comporte du C02.13. Installation according to any one of claims 1 to 11, characterized in that said quenching gas is C0 2 or comprises C0 2 .
14. Procédé d'exploitation d'une installation suivant l'une quelconque des revendications précédentes, caractérisé par les étapes successives suivantes :14. Method for operating an installation according to any one of the preceding claims, characterized by the following successive steps:
- le réservoir tampon (10) est empli de gaz de trempe à la pression tampon (PtamPon) ;- The buffer tank (10) is filled with quenching gas at the buffer pressure (P ta m P on);
- l'objet à tremper (3) est disposé dans la cellule de trempe (12);- the object to be quenched (3) is arranged in the quenching cell (12);
- les premiers moyens d'obturation (34) commandables sont ouverts, établissant une liaison entre le réservoir tampon (10) et la cellule de trempe (12), jusqu'à l'établissement de la pression de trempe (Ptrempe)dans la cellule de trempe (12),- the first valve means (34) controllable are opened, establishing a connection between the buffer reservoir (10) and the quenching cell (12), until the establishment of the quenching pressure (P tempered e) the quenching cell (12),
- l'objet à tremper (30) est refroidi à une température déterminée ;etthe object to be soaked (30) is cooled to a determined temperature; and
- l'objet trempé (3) est retiré de la cellule de trempe (12). - the quenched object (3) is removed from the quenching cell (12).
EP03720608A 2002-02-12 2003-02-10 Gas quenching installation and the corresponding quenching method Revoked EP1476585B1 (en)

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FR0201701A FR2835907B1 (en) 2002-02-12 2002-02-12 GAS QUENCHING INSTALLATION AND CORRESPONDING QUENCHING METHOD
FR0201701 2002-02-12
PCT/FR2003/000412 WO2003068998A1 (en) 2002-02-12 2003-02-10 Gas quenching installation and the corresponding quenching method

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DE10251486A1 (en) * 2002-11-05 2004-05-19 Linde Ag Recovering gas for re-use, from process chamber operating under pressure, e.g. quenching, involves using one or more compression stages for extraction, in accordance with chamber internal pressure
FR2858983B1 (en) 2003-08-21 2005-09-23 Air Liquide GAS TREATMENT METHOD USING A RECYCLING FACILITY
FR2863628B1 (en) * 2003-12-11 2006-11-17 Etudes Const Mecaniques DEVICE FOR TEMPERING STEEL PARTS
US20050193743A1 (en) * 2004-03-05 2005-09-08 John Foss High-pressure cryogenic gas for treatment processes
FR2879474B1 (en) 2004-12-16 2008-06-13 Air Liquide PROCESS FOR CLEANING AN INCORPORATING MIXTURE COMPRISING CARBON DIOXIDE (CO2) AND CARBON MONOXIDE (CO) FOR THE REMOVAL OF THE CARBON MONOXIDE (CO) CONTAINED IN THIS MIXTURE
US8820098B2 (en) 2011-05-17 2014-09-02 Air Products And Chemicals, Inc. Method and apparatus for quenching of materials in vacuum furnace
CN106498136B (en) * 2016-12-30 2018-04-03 上海颐柏热处理设备有限公司 A kind of device of high-pressure liquid or above-critical state quenching

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FR2835907A1 (en) 2003-08-15
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EP1476585B1 (en) 2005-10-12
ATE306565T1 (en) 2005-10-15
FR2835907B1 (en) 2004-09-17
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ES2250887T3 (en) 2006-04-16
DE60301860D1 (en) 2006-02-23

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