EP0451050A1 - Verfahren und Einrichtung zur Wärmebehandlung mit Gasabschreckung - Google Patents

Verfahren und Einrichtung zur Wärmebehandlung mit Gasabschreckung Download PDF

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Publication number
EP0451050A1
EP0451050A1 EP91400900A EP91400900A EP0451050A1 EP 0451050 A1 EP0451050 A1 EP 0451050A1 EP 91400900 A EP91400900 A EP 91400900A EP 91400900 A EP91400900 A EP 91400900A EP 0451050 A1 EP0451050 A1 EP 0451050A1
Authority
EP
European Patent Office
Prior art keywords
helium
pressure
quenching
heat treatment
gas
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
EP91400900A
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English (en)
French (fr)
Other versions
EP0451050B1 (de
Inventor
Benoît Lhote
Philippe Queille
Jean-Pierre Zumbrunn
Eric Duchateau
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.)
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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Publication date
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First worldwide family litigation filed litigation Critical https://patents.darts-ip.com/?family=9395441&utm_source=google_patent&utm_medium=platform_link&utm_campaign=public_patent_search&patent=EP0451050(A1) "Global patent litigation dataset” by Darts-ip is licensed under a Creative Commons Attribution 4.0 International License.
Application filed by Air Liquide SA, LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude filed Critical Air Liquide SA
Publication of EP0451050A1 publication Critical patent/EP0451050A1/de
Application granted granted Critical
Publication of EP0451050B1 publication Critical patent/EP0451050B1/de
Anticipated expiration legal-status Critical
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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 recirculation speed 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 better heat conductivity hydrogen or helium. 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 decrease 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 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 purification 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 cleaning 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 by valve lines on the one hand 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, a small 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 tank 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, whose outlet is also and 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 furnace atmosphere.
  • 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 three-way valve 13, a compressor 14, an oil separator filter 15, a three-way valve 16.
  • the waiting 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.
  • the 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).
  • 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 to 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 (via 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 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 of free passage from the oven 1 to the waiting capacity 12.
  • 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 greater than the buffer capacity 2 of the furnace.
  • 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)
  • Separation Of Gases By Adsorption (AREA)
  • Waste-Gas Treatment And Other Accessory Devices For Furnaces (AREA)
  • Drying Of Gases (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
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
FR9004309 1990-04-04
FR9004309A FR2660669B1 (fr) 1990-04-04 1990-04-04 Procede et installation de traitement thermique d'objets avec trempe en milieux gazeux.

Publications (2)

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

Family

ID=9395441

Family Applications (1)

Application Number Title Priority Date Filing Date
EP91400900A Revoked EP0451050B1 (de) 1990-04-04 1991-04-03 Verfahren und Einrichtung zur Wärmebehandlung mit Gasabschreckung

Country Status (7)

Country Link
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)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0727557A1 (de) * 1995-02-17 1996-08-21 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Verfahren und Vorrichtung zum Füllen von einem Gehäuse mit Füllgas
WO1997000974A1 (en) * 1995-06-22 1997-01-09 Aga Aktiebolag (Publ) A method and an apparatus for the treatment of components by a gas mixture
FR2835907A1 (fr) * 2002-02-12 2003-08-15 Air Liquide Installation de trempe par gaz et procede de trempe correspondant
FR2858983A1 (fr) * 2003-08-21 2005-02-25 Air Liquide Procede de trempe par gaz mettant en oeuvre une installation de recyclage
WO2006058709A1 (de) * 2004-12-03 2006-06-08 Linde Aktiengesellschaft Verfahren zur gasabschreckung mit heliumhaltigen kühlgas
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

Families Citing this family (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4225982A1 (de) * 1992-08-06 1994-02-10 Linde Ag Verfahren zum kontinuierlichen Glühen von metallischem Gut unter wasserstoffreichem Schutzgas
US5364828A (en) * 1992-10-21 1994-11-15 Minerals Technologies Spheroidal aggregate of platy synthetic hydrotalcite
US5399246A (en) * 1993-08-26 1995-03-21 Ceramatec, Inc. Inert gas purification
US5704964A (en) * 1994-12-27 1998-01-06 Nippon Sanso Corporation Pressure swing adsorption process
US20020104589A1 (en) * 2000-12-04 2002-08-08 Van Den Sype Jaak Process and apparatus for high pressure gas quenching in an atmospheric furnace
US20020125591A1 (en) * 2000-12-04 2002-09-12 Jaynes Scot Eric Process and apparatus for producing atomized powder using recirculating atomizing gas
US6517791B1 (en) * 2000-12-04 2003-02-11 Praxair Technology, Inc. System and process for gas recovery
WO2003011431A1 (en) * 2001-07-31 2003-02-13 Praxair Technology, Inc. Helium recovery
DE10251486A1 (de) * 2002-11-05 2004-05-19 Linde Ag Verfahren und Vorrichtung zur Gaserückgewinnung
JP4285481B2 (ja) * 2003-07-23 2009-06-24 東亞合成株式会社 水性インク
DE102005015450B3 (de) * 2005-04-04 2006-08-17 Ipsen International Gmbh Verfahren sowie Vorrichtung zur Gasabschreckung
AT502238B1 (de) * 2005-05-12 2007-12-15 Ebner Ind Ofenbau Verfahren zur chargenweisen wärmebehandlung von glühgut
CN101684515B (zh) * 2008-09-28 2014-07-23 傅家仁 大型压力容器原位逐段热处理方法
US8444749B2 (en) * 2009-06-10 2013-05-21 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Method and system for membrane-based gas recovery
CN101893383B (zh) * 2010-07-23 2012-07-04 上海联川自动化科技有限公司 一种工业炉抽真空并充填惰性气体的方法及装置
JP5978816B2 (ja) * 2012-07-11 2016-08-24 新日鐵住金株式会社 熱処理後の不活性ガスの回収・再利用方法及び回収・再利用装置
PL228193B1 (pl) * 2014-10-06 2018-02-28 Seco/Warwick Społka Akcyjna Urzadzenie do jednostkowego hartowania czesci urzadzen technicznych
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
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

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2450081A (en) * 1945-04-05 1948-09-28 George R Burkhardt Noble gas metallurgy
EP0266745A2 (de) * 1986-11-03 1988-05-11 Air Products And Chemicals, Inc. Verfahren zur Trennung der Komponenten eines Gasstroms
EP0313888B1 (de) * 1987-10-28 1991-07-31 ALD Vacuum Technologies GmbH Verfahren zur Wärmebehandlung metallischer Werkstücke

Family Cites Families (3)

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Publication number Priority date Publication date Assignee Title
US3713271A (en) * 1970-10-09 1973-01-30 Texaco Inc Process and apparatus for recovering a gas constituent by membrane separation
GB8327143D0 (en) * 1983-10-11 1983-11-09 Petrocarbon Dev Ltd Purification of helium
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

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2450081A (en) * 1945-04-05 1948-09-28 George R Burkhardt Noble gas metallurgy
EP0266745A2 (de) * 1986-11-03 1988-05-11 Air Products And Chemicals, Inc. Verfahren zur Trennung der Komponenten eines Gasstroms
EP0313888B1 (de) * 1987-10-28 1991-07-31 ALD Vacuum Technologies GmbH Verfahren zur Wärmebehandlung metallischer Werkstücke

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0727557A1 (de) * 1995-02-17 1996-08-21 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Verfahren und Vorrichtung zum Füllen von einem Gehäuse mit Füllgas
FR2730790A1 (fr) * 1995-02-17 1996-08-23 Air Liquide Procede d'introduction d'un gaz de remplissage dans une enceinte et installation de mise en oeuvre
US5676736A (en) * 1995-02-17 1997-10-14 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Process for introducing a filling gas into an enclosure and installation for employing same
WO1997000974A1 (en) * 1995-06-22 1997-01-09 Aga Aktiebolag (Publ) A method and an apparatus for the treatment of components by a gas mixture
US5938866A (en) * 1995-06-22 1999-08-17 Aga Aktiebolag Method and an apparatus for the treatment of components by a gas mixture
FR2835907A1 (fr) * 2002-02-12 2003-08-15 Air Liquide Installation de trempe par gaz et procede de trempe correspondant
WO2003068998A1 (fr) * 2002-02-12 2003-08-21 L'air Liquide, Societe Anonyme A Directoire Et Conseil De Surveillance Pour L'etude Et L'exploitation Des Procedes Georges Claude Installation de trempe par gaz et procede de rempe correspondant
FR2858983A1 (fr) * 2003-08-21 2005-02-25 Air Liquide Procede de trempe par gaz mettant en oeuvre une installation de recyclage
WO2005021805A1 (fr) * 2003-08-21 2005-03-10 L'air Liquide Societe Anonyme A Directoire Et Conseil De Surveillance Pour L'etude Et L'exploitation Des Procedes Georges Claude Procede de trempe par gaz mettant en oeuvre une installation de recyclage
US7632453B2 (en) 2003-08-21 2009-12-15 L'air Liquide-Societe Anonyme A Directoire Et Conseil De Surveillance Pour L'etude Et L'exploitation Des Procedes Georges Claude Gas quenching method using a recycling facility
WO2006058709A1 (de) * 2004-12-03 2006-06-08 Linde Aktiengesellschaft Verfahren zur gasabschreckung mit heliumhaltigen kühlgas
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

Also Published As

Publication number Publication date
EP0451050B1 (de) 1995-03-01
FR2660669A1 (fr) 1991-10-11
JPH06207214A (ja) 1994-07-26
CA2039515A1 (fr) 1991-10-05
FR2660669B1 (fr) 1992-06-19
DE69107651D1 (de) 1995-04-06
ES2069234T3 (es) 1995-05-01
US5158625A (en) 1992-10-27
DE69107651T2 (de) 1995-07-06

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