EP0451050B1 - Verfahren und Einrichtung zur Wärmebehandlung mit Gasabschreckung - Google Patents

Verfahren und Einrichtung zur Wärmebehandlung mit Gasabschreckung Download PDF

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Publication number
EP0451050B1
EP0451050B1 EP91400900A EP91400900A EP0451050B1 EP 0451050 B1 EP0451050 B1 EP 0451050B1 EP 91400900 A EP91400900 A EP 91400900A EP 91400900 A EP91400900 A EP 91400900A EP 0451050 B1 EP0451050 B1 EP 0451050B1
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EP
European Patent Office
Prior art keywords
helium
pressure
heat treatment
gas
buffer tank
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Revoked
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EP91400900A
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English (en)
French (fr)
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EP0451050A1 (de
Inventor
Benoît Lhote
Philippe Queille
Jean-Pierre Zumbrunn
Eric Duchateau
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Air Liquide SA
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Original Assignee
Air Liquide SA
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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    • 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
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
    • C21D1/767—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material with forced gas circulation; Reheating thereof
    • 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
    • C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
    • C21D1/773—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material under reduced pressure or vacuum

Definitions

  • the present invention relates to the heat treatment of objects with quenching in a gaseous medium.
  • the quenching gas is caused to recirculate in contact with said treated objects with cooling of the quenching gas by means of an external heat exchanger.
  • vacuum ovens suitable for gas quenching are equipped with a powerful recirculation blower and the gas injected under pressure into the oven enclosure is successively moved through the charge during treatment. There is therefore convection cooling while the gas thus heated then passes through a heat exchanger, water for example, which cools it before it is returned to the load of objects being treated.
  • the rate of cooling of the parts in an atmosphere depends, among other factors, on the pressure, the rate of recirculation and the nature of the gas.
  • the gas speed is imposed by the recirculation blower.
  • the pressure is controlled by the amount of gas injected into the oven; it is limited by the characteristics of the oven which define a maximum pressure admissible by the enclosure.
  • the gases commonly used for quenching are nitrogen and argon.
  • gases having a better heat conductivity hydrogen or helium (see for example EP-A-313 888)
  • EP-A-313 888 This promotes heat exchange by convection between the treated part and the cooling flow.
  • the gain obtained on the cooling speed makes it possible to quench under gas a wider range of materials; for a given treatment, it is also possible to reduce the pressure of the gas in the furnace, lowering the stresses to which the material is subjected, or else to increase the mass of material which can be treated during a cycle.
  • the technical problem underlying the present invention is the use of helium, or a mixture based on helium, in gas quenching treatments, while remaining economically competitive with conventional treatments under argon or nitrogen and this objective is achieved in that at the end of a quenching operation, the helium charge is extracted from the treatment enclosure, in the final phase by pump until a primary vacuum is obtained, the helium extracted at a purification pressure is brought by compressor associated with a mechanical filter, and the said helium is passed at purification pressure through a purifier for removing impurities, for transfer, if necessary, after recompression, in the buffer capacity.
  • the end of quenching helium which is polluted by impurities, in particular oxygen and water, present on the charge or in the furnace, by possible air leaks and by the recovery or recompression equipment, is recovered. after careful purification.
  • the helium at the purification pressure is collected in an intermediate capacity, after which it is sent to a permeation membrane separator delivering the purified helium under lower pressure, which is then dried and then discharged under pressure by the same compressor to the buffer capacity of the oven.
  • the helium extracted, recompressed to a pressure higher than the waiting pressure of the buffer capacity and mechanically filtered is brought to transfer into a device for purifying residual oxygen of the type to controlled addition of hydrogen for catalytic formation of water vapor, after which the gas is optionally cooled and dried, then transferred to said holding capacity.
  • the helium extracted, recompressed at a pressure higher than the waiting pressure of the buffer capacity and mechanically filtered is brought to transfer into a purification device of the catalytic type with oxygen scavenging. residual and regenerating the catalyst with a stream of hydrogen, after which the gas is optionally cooled and dried, then transferred to said holding capacity.
  • the helium extracted, recompressed to a pressure higher than the waiting pressure of the buffer capacity and mechanically filtered is brought to transfer into an oxygen purifying device and possibly residual water vapor, of the molecular sieve type allowing the adsorption of oxygen and possibly water vapor, the regeneration of which is ensured by depressurization or by increasing the temperature, after which the gas is if necessary cooled and dried, then transferred to said buffer capacity.
  • the helium extracted, brought to a purification pressure passes directly and substantially in its entirety through a purifier for removing impurities, if necessary after being collected in an intermediate capacity. It is also possible, in particular when the content of impurities in the extracted helium, to purify only a fraction of said extracted helium or to purify it only after it has been used for at least two successive quenching operations.
  • the invention also relates to an installation for the thermal treatment of objects with quenching in a gaseous medium incorporating at least substantially helium, of the type comprising a gas recirculation blower oven, connected on the one hand with valve lines to a capacity -buffer, on the other hand to a primary vacuum pump bypassed by a valve and expansion valve line, which is characterized in that it comprises, at the pump outlet, an equalization capacity, a compressor, a filter mechanical, a helium purifier, and if necessary, a dryer preferably trapped in water vapor by molecular sieve.
  • the installation may, if necessary, also include a valve line bypassing the helium purifier.
  • the invention provides for the interposition of an intermediate reservoir upstream of the purifier which is of the membrane separator type, the outlet of the purified gas of which is connected to a dryer and then by valve upstream of said compressor, the outlet of which is also directly connected by valve to the buffer tank.
  • the helium purifier is of the type with controlled addition of hydrogen for catalytic formation of water vapor.
  • the purification of helium is of the type with catalytic elimination of residual oxygen and regeneration of the catalyst by a stream of hydrogen.
  • the purification of helium can also be of the type with elimination by passage and adsorption on molecular sieve of oxygen and possibly of water vapor, the regeneration of said molecular sieves being done by depressurization or increase in temperature, possibly accompanied by passing a stream of pure gas.
  • a vacuum quenching furnace 1 is normally connected on the one hand to a buffer tank 2 by a pipe 3 with valve 4, on the other hand, to a vacuum pump 5 by a pipe of emptying 6 with valve 7.
  • the gas quenching is carried out, at the end of the temperature rise of the objects in the oven put under vacuum by the pump 5 (valve 7 open), by sudden discharge of the buffer capacity 2 in oven 1 by opening valve 4 (valves 7 and 27 closed).
  • a recirculation blower 8 ensures the homogenization of the atmosphere of the oven.
  • the buffer capacity 2 is recharged to a maximum pressure via a charging line 9.
  • the installation described above receives a helium recovery equipment at the end of quenching, which comprises, at the outlet of the emptying pump 5, a connecting pipe. 11 towards a waiting capacity 12, which successively incorporates a valve 10 on the discharge of the pump 5, a small equalizing capacity 29, a three-way valve 13, a compressor 14, an oil separator filter 15, a three-way valve 16.
  • the holding capacity 12 is connected by a pipe 17 with a valve 18 to the upstream high pressure compartment 19 of a permeator 20 with permeation membrane 21 for separation from a downstream low pressure compartment 22.
  • the high pressure compartment 19 is connected to an evacuation pipe 23 for impurities, while the purified helium arriving in the downstream compartment under low pressure 22 is dried at 35 and necessarily maintained under intermediate pressure via the compressor 14.
  • the three-way valve 16 is connected by a line 25 to the buffer capacity 2.
  • the vacuum pump 5 is by-passed through a line 26 with valve 27 and pressure regulator 28.
  • a helium charge is initially introduced via line 9 into the buffer capacity 2. Quenching is carried out in the usual manner by opening the valve 4 with unloading, for example, until a substantial equilibrium of part of the helium stored in the buffer capacity 2 and the quenching operation is carried out with recirculation of the helium by the blower 8 to an exchanger-cooler (not shown).
  • the polluted helium is first transferred from the furnace 1 to the holding capacity 12 (valve 27 open, valves 7 and 10 closed, pump 5 stopped), valve three tracks 13, the compressor 14, the oil separator filter 15, the three-way valve 16 open towards the holding tank 12, where the partially purified helium gas is stored under pressure thanks to the compressor 14 in operation (valve 18 closed).
  • the vacuum pump 5 is put into operation (valves 27 closed, valves 7 and 10 open) with delivery to the compressor 14 which acts as previously.
  • the pump 5 is stopped (valves 7 and 10 closed) and the three-way valves 13 and 16 switched to their second positions, where they respectively connect the downstream compartment 22 of the permeator 20 with the inlet of compressor 14 (through valve 13), the outlet of the oil separator filter with buffer capacity 2 (via valve 16).
  • the gaseous purification of the helium stored in the holding tank 12 can then be carried out by opening the valve 18, at the same time as the helium purified under low pressure collected and transported by the line 24 is recompressed by the compressor 14 to be stored in the buffer capacity 2. Once this operation is complete, the valve 18 is closed and the three-way valves 13 and 16 switched to their initial positions for free passage from the oven 1 to the waiting capacity 12.
  • Buffer capacity 2 having collected only a portion, which is however very substantial, of the helium used during quenching, additional filling is carried out via line 9 to reach normal operating pressure and a new operation helium quenching can then take place.
  • the slightly polluted helium is transferred from the furnace 1 to the open valve 16 towards the buffer tank 2, this after passage of the helium in the pump 5, the compressor 14 and the oil separator filter 15 as indicated above; the helium stored in buffer capacity 2 can then be reused for a new quenching operation.
  • the valve 16 is switched so as to allow the installation to operate according to the embodiment described above, and allowing its purification.
  • the recycling equipment is installed on a vacuum furnace with an internal volume of 10 m3 in which treatments of nickel-based alloy parts are carried out. After a plateau at a temperature of 1300 ° C., quenching is carried out under pure helium at a pressure of 2.5 bar absolute.
  • the helium is cold in the oven, at a pressure of 2.5 bar absolute.
  • the valve 27 is then opened and the gas is expanded at 28 in a circuit bypassing the primary vacuum pump of the oven; the gas is then recompressed 14, filtered and de-oiled at 15 and stored in a holding capacity 12 at a pressure higher than the buffer capacity 2 of the oven.
  • the valve 27 is closed, the valves 7 and 10 are open; the primary pump 5 is put into operation and sucks the gas to return it to the inlet of the compressor 14.
  • the oven 1 is then put into the air, then opened and ready for unloading-recharging.
  • the helium in the holding capacity 12 is already filtered and de-oiled beforehand; it is then purified in the membrane separator 20, recompressed at 14 and returned to the buffer tank 2 of the oven. You just need to fill in 9 the amount of helium lost during recovery, before starting another treatment cycle.
  • a cooler 34 followed by a dryer 35 of the type with water vapor trapping by molecular sieve and purged by a stream of nitrogen 36-36 ′, before reinjection. in buffer capacity 2 under waiting pressure.
  • a cooler 34 may optionally also be available.
  • at least two molecular sieves arranged in parallel are used, one being in operation and the other in regeneration by depressurization or increase in temperature, possibly accompanied by the passage of a stream of pure gas.

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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)
  • Separation Using Semi-Permeable Membranes (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Separation Of Gases By Adsorption (AREA)
  • Waste-Gas Treatment And Other Accessory Devices For Furnaces (AREA)
  • Drying Of Gases (AREA)

Claims (12)

  1. Verfahren zur thermischen Behandlung von Gegenständen mittels Abschreckung in einem umgewälzten (8) gasförmigen Medium im Kontakt mit den behandelten Gegenständen und mittels Kühlung des Abschreckungsgases mit Hilfe eines Wärmetauschers, wobei man Helium als Abschreckungsgas verwendet, das bei Bereitschaftsdruck in einem Zwischenspeicher (2) gespeichert wird, dadurch gekennzeichnet, daß man am Ende eines Abschreckungsvorgangs die Heliumfüllung aus der Behandlungskammer abzieht (27-28), und zwar in der Endphase mittels einer Pumpe (5) bis zur Erzielung eines primären Vakuums, daß man mittels eines einem mechanischen Filter (15) zugeordneten Kompressors (14) das abgezogene Helium auf einen Reinigungsdruck bringt, und daß man das Helium bei Reinigungsdruck in eine Reinigungsvorrichtung zur Entfernung der Verunreinigungen (20-35) (31-35) eintreten läßt, um es bei Bedarf nach einer erneuten Verdichtung in den Zwischenspeicher (2) zu überführen.
  2. Verfahren zur thermischen Behandlung von Gegenständen nach Anspruch 1, dadurch gekennzeichnet, daß das Helium bei dem Reinigungsdruck in einem Zwischenbehälter (12) gesammelt wird, woraufhin man es in eine Trennvorrichtung (20) mit Permeationsmembran (21) schickt, die gereinigtes Helium mit niedrigerem Druck abgibt, welches daraufhin getrocknet (25) und unter Druck durch denselben Kompressor (14) zu dem Zwischenspeicher (2) des Ofens gefördert wird.
  3. Verfahren zur thermischen Behandlung von Gegenständen nach Anspruch 1, dadurch gekennzeichnet, daß das auf einen Druck über dem Bereitschaftsdruck des Zwischenspeichers (2) erneut verdichtete (14) und mechanisch gefilterte (15) abgezogene Helium einer Vorrichtung zur Entfernung von Restsauerstoff (31) zugeführt wird, wobei Wasserstoff (32) zur katalytischen Bildung von Wasserdampf kontrolliert hinzugefügt wird, worauf-hin das Gas bei Bedarf gekühlt (34) und getrocknet (35) und daraufhin in den Zwischenspeicher(2) überführt wird.
  4. Verfahren zur thermischen Behandlung von Gegenständen nach Anspruch 1, dadurch gekennzeichnet, daß das auf einen Druck oberhalb des Bereitschaftsdrucks des Zwischenspeichers (2) erneut verdichtete (14) und mechanisch gefilterte (15) abgezogene Helium einer Vorrichtung zur katalytischen Reinigung (31) zugeführt wird, wobei der Restsauerstoff in einer Falle abgeschieden und der Katalysator durch einen Wasserstoffstrom regeneriert wird (33-33'), woraufhin das Gas bei Bedarf gekühlt (34) und getrocknet (35) und daraufhin in den Zwischenspeicher (2) überführt wird.
  5. Verfahren zur thermischen Behandlung von Gegenständen nach Anspruch 1, dadurch gekennzeichnet, daß das auf einen Druck oberhalb des Bereitschaftsdrucks des Zwischenspeichers (2) erneut verdichtete und mechanisch gefilterte (15) abgezogene Helium einer Vorrichtung zur Entfernung von Sauerstoff und eventuell von Restwasserdämpfen zugeführt wird, wobei ein Molekularsieb zur Adsorption von Sauerstoff und eventuell Wasserdampf mit einer Regenerierung durch Druckabsenkung oder Temperaturerhöhung eingesetzt wird, möglicherweise von einem hindurchgeleiteten Strom reinen Gases begleitet, woraufhin das Gas bei Bedarf gekühlt (34) und getrocknet (35) und daraufhin zu dem Zwischenspeicher (2) überführt wird.
  6. Verfahren zur thermischen Behandlung von Gegenständen nach einem der Ansprüche 1 bis 5, dadurch gekennzeichnet, daß nur ein Bruchteil des abgezogenen Heliums in die Reinigungsvorrichtung zur Entfernung der Verunreinigungen überführt wird.
  7. Verfahren zur thermischen Behandlung nach einem der Ansprüche 1 bis 5, dadurch gekennzeichnet, daß das abgezogene Helium in die Reinigungsvorrichtung zur Entfernung der Verunreinigungen geführt wird, nachdem es für mindestens zwei aufeinanderfolgende Abschreckungsvorgänge benutzt wurde.
  8. Anlage zur thermischen Behandlung von Gegenständen mittels Abschreckung in einem gasförmigen Medium, das zumindest im wesentlichen Helium enthält, wobei die Anlage einen Ofen (1) mit Turbine zur Gasumwälzung (8) aufweist, der über mit Ventilen ausgestatteten Leitungen einerseits mit einem Zwischenspeicher (2) und andererseits mit einer Primär-Vakuumpumpe (5) verbunden ist, die eine Umgehungsleitung mit einem Ventil (27) und einem Druckminderer (28) hat, dadurch gekennzeichnet, daß sie am Ausgang der Pumpe (5) einen Ausgleichsbehälter (29), einen Kompressor (14), einen mechanischen Filter (15), eine Heliumreinigungsvorrichtung (20-31) und bei Bedarf einen Trockner (35), vorzugsweise mit einer Wasserdampffalle mittels Molekularfilter, aufweist.
  9. Anlage zur thermischen Behandlung von Gegenständen nach Anspruch 8, gekennzeichnet durch Zwischenschaltung eines Zwischenbehälters (12) stromauf von der Reinigungsvorrichtung (20), die sich einer Membrantrennvorrichtung (21) bedient, wobei der Austritt des gereinigten und getrockneten (35) Gases mit einem Ventil (13) stromauf von dem Kompressor (14) verbunden ist, dessen Ausgang ebenfalls mittels eines Ventils (16) mit dem Pufferbehälter (2) verbunden ist.
  10. Anlage zur thermischen Behandlung von Gegenständen nach Anspruch 8, dadurch gekennzeichnet, daß bei der Heliumreinigungsvorrichtung (31) Wasserstoff (32) zur katalytischen Bildung von Wasserdampf kontrolliert hinzugefügt wird.
  11. Anlage zur thermischen Behandlung von Gegenständen nach Anspruch 8, dadurch gekennzeichnet, daß bei der Heliumreinigungsvorrichtung (31) der Restsauerstoff katalytisch entfernt und der Katalysator durch einen Wasserstoffstrom (33) (33') regeneriert wird.
  12. Anlage zur thermischen Behandlung von Gegenständen nach Anspruch 8, dadurch gekennzeichnet, daß man sich bei der Heliumreinigungsvorrichtung (31) eines Molekularsiebs zur Adsorption des Sauerstoffs und möglicherweise des Wasserdampfs mit Regenerierung mittels Druckabsenkung oder Temperaturerhöhung, möglicherweise von einem hindurchgeleiteten Strom reinen Gases begleitet, bedient.
EP91400900A 1990-04-04 1991-04-03 Verfahren und Einrichtung zur Wärmebehandlung mit Gasabschreckung Revoked EP0451050B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR9004309A FR2660669B1 (fr) 1990-04-04 1990-04-04 Procede et installation de traitement thermique d'objets avec trempe en milieux gazeux.
FR9004309 1990-04-04

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EP0451050A1 EP0451050A1 (de) 1991-10-09
EP0451050B1 true EP0451050B1 (de) 1995-03-01

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US (1) US5158625A (de)
EP (1) EP0451050B1 (de)
JP (1) JPH06207214A (de)
CA (1) CA2039515A1 (de)
DE (1) DE69107651T2 (de)
ES (1) ES2069234T3 (de)
FR (1) FR2660669B1 (de)

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CN110499409A (zh) * 2019-09-25 2019-11-26 上海颐柏科技股份有限公司 一种热处理淬火过程中二氧化碳循环利用装置及其方法
CN111850256A (zh) * 2020-08-04 2020-10-30 赣州市合安科技有限公司 一种下落冲洗清理的热处理淬火池
CN112747253A (zh) * 2020-12-09 2021-05-04 格瑞拓动力股份有限公司 一种氦气压缩装置
KR102902672B1 (ko) * 2022-12-29 2025-12-22 동우에이치에스티 주식회사 열처리용 냉각장치
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JPH03296820A (ja) * 1990-04-16 1991-12-27 Matsushita Electric Ind Co Ltd アセンブル処理方法及びアセンブル処理装置

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DE102005015450B3 (de) * 2005-04-04 2006-08-17 Ipsen International Gmbh Verfahren sowie Vorrichtung zur Gasabschreckung

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JPH06207214A (ja) 1994-07-26
ES2069234T3 (es) 1995-05-01
DE69107651T2 (de) 1995-07-06
CA2039515A1 (fr) 1991-10-05
US5158625A (en) 1992-10-27
FR2660669B1 (fr) 1992-06-19
FR2660669A1 (fr) 1991-10-11
DE69107651D1 (de) 1995-04-06
EP0451050A1 (de) 1991-10-09

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