JP2015129328A - Subzero treatment method and device - Google Patents

Subzero treatment method and device Download PDF

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JP2015129328A
JP2015129328A JP2014001359A JP2014001359A JP2015129328A JP 2015129328 A JP2015129328 A JP 2015129328A JP 2014001359 A JP2014001359 A JP 2014001359A JP 2014001359 A JP2014001359 A JP 2014001359A JP 2015129328 A JP2015129328 A JP 2015129328A
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heat medium
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zero treatment
oily liquid
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JP6328937B2 (en
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太希 堀野
Taiki Horino
太希 堀野
和田　智宏
Tomohiro Wada
智宏 和田
公哉 森
Kimiya Mori
公哉 森
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Taiyo Nippon Sanso Corp
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Abstract

PROBLEM TO BE SOLVED: To provide a subzero treatment method and a device therefor capable of preventing temperature unevenness, thus uniformly performing cooling, and further, simultaneously performing the removal of quenching oil.SOLUTION: In the subzero treatment where a metallic material is cooled to 0°C or lower, and subzero treatment is performed, a temperature-controlled oily liquid heat medium is introduced-delivered inside a subzero treatment tank 11 charged with a metallic material to be subjected to subzero treatment, while performing circulation, subzero treatment is performed, and further, the metallic material is cleaned with the oily liquid heat medium.

Description

本発明は、サブゼロ処理方法及び装置に関し、詳しくは、金属材料を０℃以下に冷却して硬度や靱性などの性能の向上や寸法安定性の向上を図るサブゼロ処理方法及び装置に関する。   The present invention relates to a sub-zero processing method and apparatus, and more particularly to a sub-zero processing method and apparatus for cooling a metal material to 0 ° C. or less to improve performance such as hardness and toughness and improve dimensional stability.

金属材料、例えば、鋼をオーステナイト組織の状態まで加熱した後に急冷することで鋼の組織をマルテンサイトに変化させ、鋼の硬度を上げる焼入れ処理が様々な部材に対して適用されている。焼入れ後の金属組織は、全てがマルテンサイト組織に変化することはなく、一部は残留オーステナイトと呼ばれる組織となって存在している。この残留オーステナイトは、焼入れ硬度の低下や、時間とともに徐々にマルテンサイトへ変化することによる寸法変化という不具合を発生する原因となることがある。このため、焼入れにより生成した残留オーステナイトを強制的にマルテンサイトへ変化させ、硬度の向上や寸法の安定化を行うことを目的としてドライアイスや液体窒素などを用いて金属材料を低温に冷却するサブゼロ処理と呼ばれる熱処理が行われている（例えば、特許文献１，２参照。）。   A quenching process is applied to various members that changes the steel structure to martensite by heating the metal material, for example, steel to an austenitic structure and then rapidly cooling the steel, thereby increasing the hardness of the steel. The metal structure after quenching does not completely change to a martensite structure, and a part of the metal structure exists as a structure called retained austenite. This retained austenite may cause problems such as a decrease in quenching hardness and a dimensional change due to a gradual change to martensite with time. For this reason, sub-zero that cools metallic materials to low temperature using dry ice or liquid nitrogen for the purpose of forcibly changing the retained austenite generated by quenching to martensite and improving hardness and stabilizing dimensions. Heat treatment called processing is performed (for example, refer to Patent Documents 1 and 2).

特開平１０−６０５２４号公報Japanese Patent Laid-Open No. 10-60524 特開２００５−１１３１１６号公報JP-A-2005-113116

しかし、従来のサブゼロ処理で一般に寒冷源として用いられているドライアイスや液体窒素による冷却では、温度ムラが発生しやすく、シャフトや圧延用ロールなどの大型の焼入れ品では、変形の原因となることがある。また、鋼をオーステナイト組織の状態まで加熱した後に急冷する際に、一般的に油（焼入れ油）を用いて冷却を行うため、製品から焼入れ油を除去する洗浄工程が必要になる。   However, when cooling with dry ice or liquid nitrogen, which is generally used as a cold source in conventional sub-zero treatment, temperature unevenness is likely to occur, and large quenching products such as shafts and rolling rolls may cause deformation. There is. Further, when the steel is rapidly cooled after being heated to an austenite structure, cooling is generally performed using oil (quenched oil), and thus a cleaning step for removing the quenching oil from the product is required.

そこで本発明は、温度ムラを防止して均一に冷却できるとともに、焼入れ油の除去も同時に行うことができるサブゼロ処理方法及び装置を提供することを目的としている。   Accordingly, an object of the present invention is to provide a sub-zero treatment method and apparatus capable of uniformly cooling by preventing temperature unevenness and simultaneously removing quenching oil.

上記目的を達成するため、本発明のサブゼロ処理方法は、金属材料を０℃以下に冷却してサブゼロ処理を行うサブゼロ処理方法において、サブゼロ処理を行う金属材料を投入したサブゼロ処理槽内に、温度制御した油性の液状熱媒体を導入、導出して循環させながらサブゼロ処理を行うとともに、前記油性の液状熱媒体によって前記金属材料の洗浄を行うことを特徴としている。   In order to achieve the above object, the sub-zero treatment method of the present invention is a sub-zero treatment method in which a metal material is cooled to 0 ° C. or lower and subjected to sub-zero treatment. While the controlled oil-based liquid heat medium is introduced, led out and circulated, sub-zero treatment is performed, and the metal material is washed with the oil-based liquid heat medium.

さらに、本発明のサブゼロ処理方法は、前記油性の液状熱媒体は、融点が−８０℃以下、沸点が３０℃以上の不燃性の液体であり、特に、ハイドロフルオロエーテルであることを特徴としている。また、前記油性の液状熱媒体は、沸点が−１００℃以下の液化不活性ガスとの間接熱交換によりあらかじめ設定した温度に冷却して前記サブゼロ処理槽内に導入すること、間接熱交換によって気化した不活性ガスを貯留し、該貯留した不活性ガスを前記サブゼロ処理槽内のパージガスとして使用することを特徴としている。   Furthermore, the sub-zero treatment method of the present invention is characterized in that the oily liquid heat medium is a non-flammable liquid having a melting point of −80 ° C. or lower and a boiling point of 30 ° C. or higher, and particularly a hydrofluoroether. . The oily liquid heat medium is vaporized by indirect heat exchange after being cooled to a preset temperature by indirect heat exchange with a liquefied inert gas having a boiling point of −100 ° C. or less and introduced into the sub-zero treatment tank. The inert gas thus stored is stored, and the stored inert gas is used as a purge gas in the sub-zero treatment tank.

そして、本発明のサブゼロ処理装置は、金属材料を０℃以下に冷却してサブゼロ処理を行うサブゼロ処理装置において、サブゼロ処理を行う金属材料を投入したサブゼロ処理槽と、該サブゼロ処理槽内に温度制御した油性の液状熱媒体を導入する熱媒体導入部と、前記サブゼロ処理槽内から前記油性の液状熱媒体を導出する熱媒体導出部と、前記油性の液状熱媒体をあらかじめ設定した温度に冷却する冷却手段と、前記油性の液状熱媒体を、前記冷却手段と前記サブゼロ処理槽とに循環させる循環ポンプとを備えていることを特徴としている。   The sub-zero treatment apparatus of the present invention is a sub-zero treatment apparatus that performs sub-zero treatment by cooling a metal material to 0 ° C. or lower, a sub-zero treatment tank in which a metal material to be subjected to sub-zero treatment is charged, and a temperature in the sub-zero treatment tank A heat medium introducing section for introducing a controlled oily liquid heat medium, a heat medium deriving section for deriving the oil liquid heat medium from the sub-zero treatment tank, and cooling the oil liquid heat medium to a preset temperature. And a circulation pump that circulates the oily liquid heat medium to the cooling means and the sub-zero treatment tank.

さらに、本発明のサブゼロ処理装置は、前記油性の液状熱媒体は、融点が−８０℃以下、沸点が０℃以上の不燃性の液体であり、特に、ハイドロフルオロエーテルであることを特徴としている。また、前記冷却手段は、沸点が−１００℃以下の液化不活性ガスと前記油性の液状熱媒体とを間接熱交換させて油性の液状熱媒体を冷却する熱交換器であること、前記熱交換器での前記油性の液状熱媒体との間接熱交換によって気化した不活性ガスを貯留する不活性ガス貯留槽と、該不活性ガス貯留槽に貯留した不活性ガスを前記サブゼロ処理槽内にパージガスとして導入するパージガス導入経路とを備えていることを特徴としている。   Furthermore, the sub-zero treatment apparatus of the present invention is characterized in that the oily liquid heat medium is a nonflammable liquid having a melting point of −80 ° C. or lower and a boiling point of 0 ° C. or higher, and particularly a hydrofluoroether. . The cooling means is a heat exchanger that cools the oily liquid heat medium by indirectly heat-exchanging the liquefied inert gas having a boiling point of −100 ° C. or less and the oily liquid heat medium, and the heat exchange. An inert gas storage tank that stores an inert gas vaporized by indirect heat exchange with the oily liquid heat medium in a vessel, and an inert gas stored in the inert gas storage tank is purged into the sub-zero treatment tank And a purge gas introduction path to be introduced.

本発明によれば、あらかじめ設定された温度に冷却された油性の液状熱媒体をサブゼロ処理槽内に導入、導出して金属材料のサブゼロ処理を行うので、サブゼロ処理槽内で流動する油性の液状熱媒体によって金属材料の全体を均一に冷却することができるとともに、油性の液状熱媒体によって金属材料の表面に付着している焼入れ油を洗浄して除去することができる。さらに、油性の液状熱媒体を冷却するために使用して気化した不活性ガスを、サブゼロ処理槽内から空気成分をパージするためのパージガスとして使用することにより、油性の液状熱媒体を冷却するための液化不活性ガスの有効利用を図ることができる。   According to the present invention, the oily liquid heat medium cooled to a preset temperature is introduced into the subzero treatment tank, and the subzero treatment of the metal material is performed, so that the oily liquid flowing in the subzero treatment tank The entire metal material can be uniformly cooled by the heat medium, and the quenching oil adhering to the surface of the metal material can be washed and removed by the oily liquid heat medium. Further, the inert gas vaporized by cooling the oily liquid heat medium is used as a purge gas for purging air components from the sub-zero treatment tank, thereby cooling the oily liquid heat medium. The liquefied inert gas can be effectively used.

本発明のサブゼロ処理方法を実施可能なサブゼロ処理装置の一形態例を示す概略ブロック図である。It is a schematic block diagram which shows one example of the subzero processing apparatus which can implement the subzero processing method of this invention.

図１は、本発明のサブゼロ処理方法を実施可能なサブゼロ処理装置の一形態例を示している。このサブゼロ処理装置は、金属材料のサブゼロ処理を行うサブゼロ処理槽１１と、該サブゼロ処理槽１１にあらかじめ設定された０℃以下の温度に温度制御された油性の液状熱媒体（以下、単に熱媒体ということがある。）を導入する熱媒体導入部１２と、前記サブゼロ処理槽１１内から前記熱媒体を導出する熱媒体導出部１３と、前記熱媒体をあらかじめ設定した温度に冷却する冷却手段である熱交換器１４と、前記熱媒体を前記熱交換器１４と前記サブゼロ処理槽１１とに循環させる循環ポンプ１５と、非処理時に熱媒体をサブゼロ処理槽１１から引き抜くための真空ポンプ１６と、非処理時に熱媒体を貯留するための熱媒体貯留槽１７と、真空ポンプ１６で引き抜いた熱媒体を熱交換器１４を通さずに熱媒体貯留槽１７に導入するための熱交換器バイパス経路１８と、処理時に熱交換器１４で冷却した熱媒体を熱媒体貯留槽１７を通さずにサブゼロ処理槽１１に導入するための熱媒体貯留槽バイパス経路１９と、処理終了時にサブゼロ処理槽１１に導入する熱媒体を加熱するための熱媒体加熱器２０とを備えるとともに、熱交換器１４で熱媒体を冷却するための冷却源となる液化不活性ガスを貯留する液化不活性ガス貯槽２１と、熱媒体の冷却状態に応じて液化不活性ガスの熱交換器１４への導入量を調節するための流量調整器２２と、熱交換器１４で液化不活性ガスが気化した不活性ガスを常温に加熱するガス加熱器２３と、ガス加熱器２３で加熱されて常温となった不活性ガスを貯留する不活性ガス貯留槽２４と、該不活性ガス貯留槽２４に貯留した不活性ガスをサブゼロ処理槽１１にパージガスとして導入するためのパージガス導入経路２５とを備えている。   FIG. 1 shows an example of a sub-zero processing apparatus that can implement the sub-zero processing method of the present invention. This sub-zero treatment apparatus includes a sub-zero treatment tank 11 that performs a sub-zero treatment of a metal material, and an oil-based liquid heat medium (hereinafter simply referred to as a heat medium) that is temperature-controlled at a temperature of 0 ° C. or lower that is preset in the sub-zero treatment tank 11. A heat medium introducing section 12 for introducing the heat medium, a heat medium deriving section 13 for deriving the heat medium from the sub-zero treatment tank 11, and a cooling means for cooling the heat medium to a preset temperature. A heat exchanger 14, a circulation pump 15 that circulates the heat medium to the heat exchanger 14 and the sub-zero treatment tank 11, a vacuum pump 16 for extracting the heat medium from the sub-zero treatment tank 11 during non-treatment, In order to introduce the heat medium storage tank 17 for storing the heat medium during non-treatment and the heat medium extracted by the vacuum pump 16 into the heat medium storage tank 17 without passing through the heat exchanger 14. A heat exchanger bypass path 18, a heat medium storage tank bypass path 19 for introducing the heat medium cooled by the heat exchanger 14 during processing into the sub-zero treatment tank 11 without passing through the heat medium storage tank 17, and at the end of processing A heat medium heater 20 for heating the heat medium to be introduced into the sub-zero treatment tank 11 and storing a liquefied inert gas serving as a cooling source for cooling the heat medium by the heat exchanger 14 A gas storage tank 21; a flow rate regulator 22 for adjusting the amount of liquefied inert gas introduced into the heat exchanger 14 in accordance with the cooling state of the heat medium; and an inert gas in which the liquefied inert gas is vaporized in the heat exchanger 14. A gas heater 23 that heats the active gas to normal temperature, an inert gas storage tank 24 that stores the inert gas heated to the normal temperature by being heated by the gas heater 23, and an inert gas stored in the inert gas storage tank 24. Sabze the active gas And a purge gas introduction path 25 for introducing a purge gas into the processing vessel 11.

また、サブゼロ処理槽１１には、槽内の温度を検出して前記流量調整器２２や循環ポンプ１５などを制御するための温度指示調節計２６及びパージガス排気経路１１ａが設けられ、不活性ガス貯留槽２４には、不活性ガス貯留槽２４内の圧力をあらかじめ設定された圧力に保持するための圧力指示調節計２７が設けられ、パージガス導入経路２５からは、余剰の不活性ガスを排気したり、不活性ガスの一部を他の機器や装置に供給したりするための不活性ガス導出経路２８が分岐している。   In addition, the sub-zero treatment tank 11 is provided with a temperature indicating controller 26 and a purge gas exhaust path 11a for detecting the temperature in the tank and controlling the flow rate regulator 22, the circulation pump 15, and the like, and store an inert gas. The tank 24 is provided with a pressure indicating controller 27 for maintaining the pressure in the inert gas storage tank 24 at a preset pressure, and excess inert gas is exhausted from the purge gas introduction path 25. The inert gas lead-out path 28 for supplying a part of the inert gas to other devices and apparatuses is branched.

このように形成したサブゼロ処理装置を使用したサブゼロ処理は、まず、サブゼロ処理槽１１内に処理対象となる金属材料を投入して密閉状態とした後、不活性ガス貯留槽２４からパージガス導入経路２５を介してサブゼロ処理槽１１内に不活性ガスをパージガスとして導入し、パージガス排気経路１１ａから排気することにより、サブゼロ処理槽１１内から空気成分、すなわち、サブゼロ処理槽１１内を冷却状態としたときに固化する水分などを排出する。   In the sub-zero processing using the sub-zero processing apparatus formed in this way, first, a metal material to be processed is put into the sub-zero processing tank 11 to be in a sealed state, and then the purge gas introduction path 25 from the inert gas storage tank 24. When an inert gas is introduced as a purge gas into the sub-zero treatment tank 11 and exhausted from the purge gas exhaust passage 11a, the air component from the sub-zero treatment tank 11, that is, the sub-zero treatment tank 11 is cooled. Drains moisture that solidifies.

パージ処理終了後、サブゼロ処理槽１１内への不活性ガスの導入を停止し、熱媒体貯留槽１７からサブゼロ処理槽１１内に油性の液状熱媒体を導入するとともに、循環ポンプ１５を作動させ、熱媒体をサブゼロ処理槽１１と熱交換器１４とに循環させる。循環経路内が常温の熱媒体で満たされたら、熱媒体貯留槽１７を通さずに熱媒体貯留槽バイパス経路１９を通して熱媒体を循環させる。また、温度指示調節計２６からの指示により、流量調整器２２で液化不活性ガス貯槽２１からの液化不活性ガスの供給量を調整し、熱交換器１４で液化不活性ガスと間接熱交換することにより冷却される熱媒体の温度が、あらかじめ設定された冷却温度になるように制御する。   After completion of the purge process, the introduction of the inert gas into the sub-zero treatment tank 11 is stopped, an oily liquid heat medium is introduced into the sub-zero treatment tank 11 from the heat medium storage tank 17, and the circulation pump 15 is operated. The heat medium is circulated through the sub-zero treatment tank 11 and the heat exchanger 14. When the inside of the circulation path is filled with the heat medium at room temperature, the heat medium is circulated through the heat medium storage tank bypass path 19 without passing through the heat medium storage tank 17. Further, in accordance with an instruction from the temperature indicating controller 26, the supply amount of the liquefied inert gas from the liquefied inert gas storage tank 21 is adjusted by the flow rate regulator 22, and indirect heat exchange with the liquefied inert gas is performed by the heat exchanger 14. Thus, the temperature of the heat medium to be cooled is controlled to be a preset cooling temperature.

これにより、サブゼロ処理槽１１内の熱媒体温度があらかじめ設定された処理温度に制御され、金属材料のサブゼロ処理が行われる。このとき、循環ポンプ１５によってサブゼロ処理槽１１と熱交換器１４とに循環する熱媒体が、サブゼロ処理槽１１内で熱媒体導入部１２から熱媒体導出部１３に向かう流れを形成するので、熱媒体導入部１２及び熱媒体導出部１３の位置や状態を適宜設定して熱媒体を適当に流動させることにより、金属材料の全体に満遍なく熱媒体を接触させることができ、大型の金属材料でも均一に冷却することができる。   Thereby, the heat medium temperature in the subzero treatment tank 11 is controlled to a preset treatment temperature, and the subzero treatment of the metal material is performed. At this time, the heat medium circulated between the sub-zero treatment tank 11 and the heat exchanger 14 by the circulation pump 15 forms a flow from the heat medium introduction part 12 to the heat medium lead-out part 13 in the sub-zero treatment tank 11. By appropriately setting the positions and states of the medium introduction part 12 and the heat medium lead-out part 13 and appropriately flowing the heat medium, the heat medium can be uniformly contacted with the entire metal material, and even a large metal material is uniform. Can be cooled to.

また、常温の熱冷媒をサブゼロ処理槽１１内に満たした後に、循環させながら熱交換器１４で冷却していくので、金属材料が急激に冷却されることがなく、金属材料に割れや変形を生じることもない。このサブゼロ処理中に熱交換器１４で熱媒体を冷却することによって昇温し、液化不活性ガスが気化した不活性ガスは、ガス加熱器２３で常温に加熱されてから不活性ガス貯留槽２４に貯留される。   In addition, after filling the subzero treatment tank 11 with room temperature thermal refrigerant, it is cooled by the heat exchanger 14 while circulating, so that the metal material is not rapidly cooled, and the metal material is not cracked or deformed. It does not occur. During the sub-zero treatment, the temperature of the heat medium is increased by cooling the heat medium in the heat exchanger 14, and the inert gas obtained by vaporizing the liquefied inert gas is heated to room temperature by the gas heater 23 and then the inert gas storage tank 24. It is stored in.

所定のサブゼロ処理を終了したら、流量調整器２２で液化不活性ガス貯槽２１から熱交換器１４への液化不活性ガスの供給を停止し、熱交換器バイパス経路１８を通して熱媒体を循環させながら、熱媒体加熱器２０を作動させて熱媒体を加熱し、サブゼロ処理槽１１内を常温に戻す。次に、熱媒体加熱器２０を停止させた後、循環ポンプ１５によってサブゼロ処理槽１１から抜き出した熱媒体を、熱媒体貯留槽バイパス経路１９を通さずに熱媒体貯留槽１７に導入して貯留することにより、サブゼロ処理槽１１内から熱媒体を抜き出していく。   When the predetermined sub-zero treatment is completed, the supply of the liquefied inert gas from the liquefied inert gas storage tank 21 to the heat exchanger 14 is stopped by the flow rate regulator 22, and the heat medium is circulated through the heat exchanger bypass path 18. The heat medium heater 20 is operated to heat the heat medium, and the inside of the sub-zero treatment tank 11 is returned to room temperature. Next, after stopping the heat medium heater 20, the heat medium extracted from the sub-zero treatment tank 11 by the circulation pump 15 is introduced and stored in the heat medium storage tank 17 without passing through the heat medium storage tank bypass path 19. As a result, the heat medium is extracted from the sub-zero treatment tank 11.

さらに、循環ポンプ１５を停止させて真空ポンプ１６を作動させ、サブゼロ処理槽１１内を真空排気することにより、金属材料に付着した熱媒体を含めてサブゼロ処理槽１１の内部全体から熱媒体を気化させて吸引し、全量を熱媒体貯留槽１７に回収する。   Further, the circulation pump 15 is stopped and the vacuum pump 16 is operated to evacuate the sub-zero treatment tank 11 to vaporize the heat medium from the entire interior of the sub-zero treatment tank 11 including the heat medium attached to the metal material. The whole amount is collected in the heat medium storage tank 17.

このようにして金属材料のサブゼロ処理を行う際に、冷却用熱媒体として油性の液状熱媒体を使用することにより、金属材料に付着している焼入れ油を熱媒体中に溶解して金属材料の表面から除去する洗浄操作をサブゼロ処理と同時に行うことができる。   When performing the sub-zero treatment of the metal material in this way, by using an oily liquid heat medium as the cooling heat medium, the quenching oil adhering to the metal material is dissolved in the heat medium and the metal material The cleaning operation for removing from the surface can be performed simultaneously with the sub-zero treatment.

また、真空ポンプ１６で真空排気することにより、熱媒体及び焼入れ油を金属材料の表面から確実に除去することができる。このとき、熱媒体の蒸気圧と焼入れ油の蒸気圧との差を利用することによって両者を分離することが可能である。   Further, by evacuating with the vacuum pump 16, the heat medium and the quenching oil can be reliably removed from the surface of the metal material. At this time, it is possible to separate the two by utilizing the difference between the vapor pressure of the heat medium and the vapor pressure of the quenching oil.

さらに、不活性ガス貯留槽２４に貯留した不活性ガスは、サブゼロ処理槽１１のパージに必要な量以上の不活性ガスを、不活性ガスを使用する他の機器や装置に供給することにより、不活性ガスを有効に利用することができ、ガスコストの低減を図ることができる。   Furthermore, the inert gas stored in the inert gas storage tank 24 is supplied to the other equipment or device using the inert gas by supplying an inert gas more than the amount necessary for purging the sub-zero treatment tank 11, An inert gas can be used effectively, and the gas cost can be reduced.

前記油性の液状熱媒体は、サブゼロ処理を行う温度で固化することなく、常温で気化せず、かつ、安全性を考慮すると、不燃性の任意の液状流体を使用することが可能であり、例えば、融点が−８０℃以下、沸点が３０℃以上の不燃性の液体、具体的には、ハイドロフルオロエーテル（凝固点約−１３５℃、沸点６０〜８０℃）が最適である。   The oily liquid heat medium is not solidified at the temperature at which the sub-zero treatment is performed, does not evaporate at room temperature, and in consideration of safety, any nonflammable liquid fluid can be used. An incombustible liquid having a melting point of −80 ° C. or lower and a boiling point of 30 ° C. or higher, specifically, hydrofluoroether (freezing point of about −135 ° C., boiling point 60 to 80 ° C.) is optimal.

また、熱媒体の冷却源は、沸点が−１００℃以下で、熱媒体をあらかじめ設定されたサブゼロ処理温度に効率よく冷却でき、気化後にサブゼロ処理槽１１のパージガスとして使用可能な液化ガス、例えば、液体窒素、液体アルゴンなどを用いることが好ましい。   The cooling source of the heat medium has a boiling point of −100 ° C. or less, can efficiently cool the heat medium to a preset subzero treatment temperature, and can be used as a purge gas for the subzero treatment tank 11 after vaporization, for example, It is preferable to use liquid nitrogen, liquid argon or the like.

なお、サブゼロ処理槽内に熱媒体を流動させる撹拌機を設けてもよい。また、サブゼロ処理槽における熱媒体導入部及び熱媒体導出部の位置や設置数は、循環時の流動状態を考慮して適宜な状態で配置することができ、熱媒体の循環時と抜き取り時とで使い分けるようにしてもよい。   In addition, you may provide the stirrer which makes a heat medium flow in a subzero processing tank. In addition, the position and the number of the heat medium introduction part and heat medium lead-out part in the sub-zero treatment tank can be arranged in an appropriate state in consideration of the flow state at the time of circulation, and when the heat medium is circulated and extracted. You may make it use properly.

１１…サブゼロ処理槽、１１ａ…パージガス排気経路、１２…熱媒体導入部、１３…熱媒体導出部、１４…熱交換器、１５…循環ポンプ、１６…真空ポンプ、１７…熱媒体貯留槽、１８…熱交換器バイパス経路、１９…熱媒体貯留槽バイパス経路、２０…熱媒体加熱器、２１…液化不活性ガス貯槽、２２…流量調整器、２３…ガス加熱器、２４…不活性ガス貯留槽、２５…パージガス導入経路、２６…温度指示調節計、２７…圧力指示調節計、２８…不活性ガス導出経路 DESCRIPTION OF SYMBOLS 11 ... Sub zero processing tank, 11a ... Purge gas exhaust path, 12 ... Heat-medium introduction part, 13 ... Heat-medium derivation part, 14 ... Heat exchanger, 15 ... Circulation pump, 16 ... Vacuum pump, 17 ... Heat-medium storage tank, 18 DESCRIPTION OF SYMBOLS ... Heat exchanger bypass path, 19 ... Heat medium storage tank bypass path, 20 ... Heat medium heater, 21 ... Liquefied inert gas storage tank, 22 ... Flow regulator, 23 ... Gas heater, 24 ... Inert gas storage tank 25 ... Purge gas introduction path, 26 ... Temperature indicating controller, 27 ... Pressure indicating controller, 28 ... Inert gas lead-out path

Claims (10)

金属材料を０℃以下に冷却してサブゼロ処理を行うサブゼロ処理方法において、サブゼロ処理を行う金属材料を投入したサブゼロ処理槽内に、温度制御した油性の液状熱媒体を導入、導出して循環させながらサブゼロ処理を行うとともに、前記油性の液状熱媒体によって前記金属材料の洗浄を行うことを特徴とするサブゼロ処理方法。   In a sub-zero treatment method in which a metal material is cooled to 0 ° C. or lower and subjected to sub-zero treatment, an oil-based liquid heat medium whose temperature is controlled is introduced, led out, and circulated in a sub-zero treatment tank in which the metal material to be subjected to sub-zero treatment is charged. The sub-zero treatment method is characterized in that the sub-zero treatment is performed and the metal material is washed with the oily liquid heat medium. 前記油性の液状熱媒体は、融点が−８０℃以下、沸点が３０℃以上の不燃性の液体であることを特徴とする請求項１記載のサブゼロ処理方法。   2. The sub-zero treatment method according to claim 1, wherein the oily liquid heat medium is a nonflammable liquid having a melting point of −80 ° C. or lower and a boiling point of 30 ° C. or higher. 前記油性の液状熱媒体は、ハイドロフルオロエーテルであることを特徴とする請求項１又は２記載のサブゼロ処理方法。   3. The sub-zero treatment method according to claim 1, wherein the oily liquid heat medium is hydrofluoroether. 前記油性の液状熱媒体は、沸点が−１００℃以下の液化不活性ガスとの間接熱交換によりあらかじめ設定した温度に冷却して前記サブゼロ処理槽内に導入することを特徴とする請求項１乃至３のいずれか１項記載のサブゼロ処理方法。   The oily liquid heat medium is cooled to a preset temperature by indirect heat exchange with a liquefied inert gas having a boiling point of −100 ° C. or less and introduced into the sub-zero treatment tank. 4. The sub-zero processing method according to any one of 3 above. 前記油性の液状熱媒体との間接熱交換によって気化した不活性ガスを貯留し、該貯留した不活性ガスを前記サブゼロ処理槽内のパージガスとして使用することを特徴とする請求項４記載のサブゼロ処理方法。   The subzero treatment according to claim 4, wherein an inert gas vaporized by indirect heat exchange with the oily liquid heat medium is stored, and the stored inert gas is used as a purge gas in the subzero treatment tank. Method. 金属材料を０℃以下に冷却してサブゼロ処理を行うサブゼロ処理装置において、サブゼロ処理を行う金属材料を投入したサブゼロ処理槽と、該サブゼロ処理槽内に温度制御した油性の液状熱媒体を導入する熱媒体導入部と、前記サブゼロ処理槽内から前記油性の液状熱媒体を導出する熱媒体導出部と、前記油性の液状熱媒体をあらかじめ設定した温度に冷却する冷却手段と、前記油性の液状熱媒体を、前記冷却手段と前記サブゼロ処理槽とに循環させる循環ポンプとを備えていることを特徴とするサブゼロ処理装置。   In a sub-zero treatment apparatus that cools a metal material to 0 ° C. or less and performs sub-zero treatment, a sub-zero treatment tank into which the metal material to be subjected to sub-zero treatment is charged, and a temperature-controlled oily liquid heat medium are introduced into the sub-zero treatment tank A heat medium introducing unit, a heat medium deriving unit for deriving the oily liquid heat medium from the sub-zero treatment tank, a cooling means for cooling the oily liquid heat medium to a preset temperature, and the oily liquid heat A sub-zero treatment apparatus comprising a circulation pump for circulating a medium through the cooling means and the sub-zero treatment tank. 前記油性の液状熱媒体は、融点が−８０℃以下、沸点が０℃以上の不燃性の液体であることを特徴とする請求項６記載のサブゼロ処理装置。   The sub-zero processing apparatus according to claim 6, wherein the oily liquid heat medium is a nonflammable liquid having a melting point of −80 ° C. or lower and a boiling point of 0 ° C. or higher. 前記油性の液状熱媒体は、ハイドロフルオロエーテルであることを特徴とする請求項６又は７記載のサブゼロ処理装置。   The sub-zero processing apparatus according to claim 6 or 7, wherein the oily liquid heat medium is hydrofluoroether. 前記冷却手段は、沸点が−１００℃以下の液化不活性ガスと前記油性の液状熱媒体とを間接熱交換させて油性の液状熱媒体を冷却する熱交換器であることを特徴とする請求項６乃至８のいずれか１項記載のサブゼロ処理装置。   The cooling means is a heat exchanger that cools an oily liquid heat medium by indirect heat exchange between a liquefied inert gas having a boiling point of -100 ° C or less and the oily liquid heat medium. The sub-zero processing device according to any one of 6 to 8. 前記熱交換器での前記油性の液状熱媒体との間接熱交換によって気化した不活性ガスを貯留する不活性ガス貯留槽と、該不活性ガス貯留槽に貯留した不活性ガスを前記サブゼロ処理槽内にパージガスとして導入するパージガス導入経路とを備えていることを特徴とする請求項９記載のサブゼロ処理装置。   An inert gas storage tank for storing an inert gas vaporized by indirect heat exchange with the oily liquid heat medium in the heat exchanger; and the inert gas stored in the inert gas storage tank for the sub-zero treatment tank. The sub-zero processing apparatus according to claim 9, further comprising a purge gas introduction path for introducing a purge gas therein.
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CN111286586A (en) * 2020-03-27 2020-06-16 中国科学院理化技术研究所 Method for strengthening and toughening steel material

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CN111286586A (en) * 2020-03-27 2020-06-16 中国科学院理化技术研究所 Method for strengthening and toughening steel material
CN111286586B (en) * 2020-03-27 2021-10-26 中国科学院理化技术研究所 Method for strengthening and toughening steel material

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