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WO2007006669A1 - Outil de soudage par friction-malaxage, et procede et dispositif pour commander un processus de soudage par friction-malaxage en temps reel, par detection des forces acceleratrices et/ou des oscillations au niveau du corps de l'outil - Google Patents

Outil de soudage par friction-malaxage, et procede et dispositif pour commander un processus de soudage par friction-malaxage en temps reel, par detection des forces acceleratrices et/ou des oscillations au niveau du corps de l'outil Download PDF

Info

Publication number
WO2007006669A1
WO2007006669A1 PCT/EP2006/063758 EP2006063758W WO2007006669A1 WO 2007006669 A1 WO2007006669 A1 WO 2007006669A1 EP 2006063758 W EP2006063758 W EP 2006063758W WO 2007006669 A1 WO2007006669 A1 WO 2007006669A1
Authority
WO
WIPO (PCT)
Prior art keywords
friction stir
stir welding
welding tool
tool
friction
Prior art date
Application number
PCT/EP2006/063758
Other languages
German (de)
English (en)
Inventor
Jean Pierre Bergmann
Johannes Wilden
Frank BARTHELMÄ
Bernd Aschenbach
Original Assignee
Technische Universität Ilmenau
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Technische Universität Ilmenau filed Critical Technische Universität Ilmenau
Priority to EP06764007A priority Critical patent/EP1901875A1/fr
Publication of WO2007006669A1 publication Critical patent/WO2007006669A1/fr

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
    • B23K20/12—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating the heat being generated by friction; Friction welding
    • B23K20/122—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating the heat being generated by friction; Friction welding using a non-consumable tool, e.g. friction stir welding
    • B23K20/1245—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating the heat being generated by friction; Friction welding using a non-consumable tool, e.g. friction stir welding characterised by the apparatus
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
    • B23K20/12—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating the heat being generated by friction; Friction welding
    • B23K20/122—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating the heat being generated by friction; Friction welding using a non-consumable tool, e.g. friction stir welding
    • B23K20/123—Controlling or monitoring the welding process
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
    • B23K20/12—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating the heat being generated by friction; Friction welding
    • B23K20/122—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating the heat being generated by friction; Friction welding using a non-consumable tool, e.g. friction stir welding
    • B23K20/1245—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating the heat being generated by friction; Friction welding using a non-consumable tool, e.g. friction stir welding characterised by the apparatus
    • B23K20/1255—Tools therefor, e.g. characterised by the shape of the probe

Definitions

  • the invention relates to a friction stir welding tool and a method and an arrangement for real-time control of a friction stir welding process.
  • Friction welding has been used industrially for a number of decades for a variety of joining tasks in which rotationally symmetric or flat workpieces are joined.
  • the heat is generated by friction of the joining surfaces, which is generated by the relative movement of the joining partners to each other.
  • Friction Stir Welding is a further development of friction welding technology and was patented in the early 1990s (GB 2 270 864). This method is due to the low joining ⁇ temperatures and the excellent property profile of the compounds of.
  • both the frictional heat and the pressure are generated by wear-resistant tool stir bolts. These consist of a shoulder and a pin and are pressed in rotation in the joining area in the workpiece material until the shoulder is in contact with the workpiece surface ⁇ piece. The friction between the workpiece material and the shoulder produces the required heat for plasticizing the workpiece material.
  • the plasticized material is stirred by the pin inside the seam and transported to its rear side.
  • It is therefore an object of the present invention to provide a compact, universally applicable friction stir welding tool as well as a method and an arrangement for real-time control provide a Rillonreibsch resumereas with which it is possible the joining process mieren easy and inexpensive to opti ⁇ so that in its result, the quality requirements ⁇ stakes corresponding joint seam without the need for post-processing occurs and the load on the friction stir welding mini ⁇ mized is.
  • Fig. 1 - representation of the velocity field during a friction stir welding process
  • FIG. 2 - schematic representation of a friction stir welding tool according to the invention
  • FIG. 3 schematic representation of a control loop for the friction stir welding process
  • Fig. 1 illustrates the components of a speed ⁇ field, as occurs in an ordinary Rhakreibsch resume polish.
  • FIG. 2 schematically shows a friction stir welding tool according to the invention, which is attached to a non-illustrated
  • Known friction stir welding Tools consist essentially of a tool body 2 made of tempered tool steel and a horrendbolzen 3, the latter being composed of a shoulder and a pin, which are firmly connected together.
  • the attachment of the istrandbolzens 3 on the tool base body 2 ⁇ takes place in a tool holder, for example a collet or chuck for parallel according to DIN 1835 part 1 and 2.
  • FIG. 1 A tool holder, for example a collet or chuck for parallel according to DIN 1835 part 1 and 2.
  • the heat generated in the friction stir welding process is dissipated via a closed cooling system 4.
  • the coolant is supplied to the tool via the inner coolant supply (IKZ) 5 of the machine spindle and via a radially rotatably mounted on the outer circumference of the tool coolant ring 6 derived.
  • IKZ inner coolant supply
  • the supply and discharge can be carried out via a modified coolant ring.
  • a correspondingly designed sensor arrangement 7 enables the detection of selected, process-related irregularities which are essentially due to changes in the material flow or in the friction behavior at the interface pin / substrate surface.
  • This Unre ⁇ larities, which originally result from a change in the rotational speed, the acceleration occurring in the tool can be determined by the measurement.
  • the acceleration can be multiaxial, for example, by means of a commercially available triaxial acceleration sensor based on piezos be measured. After further processing and evaluation of these measured values, it is then possible to make a statement about the vibrations occurring and loads on the machine.
  • the solution presented here offers the unique possibility of actively gaining information about the self-adjusting material flow in the case of non-similar material pairings (eg steel / aluminum, titanium / aluminum, etc.).
  • the different flow properties of the materials used lead to an untypical velocity field, which can only be defined by measuring the resulting velocity changes (accelerations).
  • the compact design according to the invention and the intelligent arrangement of the sensors in the friction stir welding head represent an essential feature of the invention, since thus the user can be offered a holistic, real-time process control "in one hand”.
  • the energy for the tool-internal electronics is inductively fed via a coupling point 9.
  • a stator 10 has the shape of a ⁇ preferably Kreisringaus section.
  • Fig. 3 the control circuit of a fiction, ⁇ friction stir welding system is shown schematically.
  • the respective sensor signals via a data pre-processing and a bidirectional telemetry unit are transmitted ⁇ unit to an evaluation .
  • the data is prepared and commands for controlling the action logic in the welding system are generated.
  • the generated commands for system control are transmitted via suitable interfaces, which in turn transmit the relevant process parameters, such as processing speed. speed, processing power and working temperature. This ensures that the process parameters are adapted to the changing process conditions during the welding process and that the welding process can be carried out in a quality-oriented manner.
  • the compact design of the friction stir welding tool according to the invention which is compatible with various welding systems or machining centers, proves to be very advantageous since it can be used universally and, in particular, offers small companies the possibility of reacting very flexibly to corresponding market requirements.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Pressure Welding/Diffusion-Bonding (AREA)

Abstract

L'invention concerne un outil de soudage par friction-malaxage, ainsi qu'un procédé et un dispositif pour commander un processus de soudage par friction-malaxage en temps réel. L'objectif de cette invention est de concevoir un outil de soudage par friction-malaxage qui soit compact et utilisable de manière universelle, ainsi qu'un procédé et un dispositif pour commander un processus de soudage par friction-malaxage en temps réel, de manière à obtenir un cordon de soudure de qualité, sans nécessairement effectuer un traitement ultérieur, et de façon à réduire au maximum les sollicitations exercées sur l'installation de soudage par friction-malaxage. A cet effet, le procédé selon l'invention consiste à détecter les oscillations d'un outil de soudage par friction-malaxage dans la direction des x, des y, et des z, les forces de traitement appliquées par l'outil de soudage par friction-malaxage, ainsi que les températures de travail générées directement au niveau du point de soudure, pendant le processus de soudage par friction-malaxage, au moyen de capteurs adaptés (7) dans le corps de base de l'outil (1) ; à transmettre télémétriquement les données détectées, par l'intermédiaire d'une unité (8), à une unité d'évaluation qui prépare ces données de manière assistée par ordinateur, et ; à réguler les paramètres de processus vitesse de traitement, force de traitement, et température de travail, par l'intermédiaire d'une unité de commande.
PCT/EP2006/063758 2005-07-09 2006-06-30 Outil de soudage par friction-malaxage, et procede et dispositif pour commander un processus de soudage par friction-malaxage en temps reel, par detection des forces acceleratrices et/ou des oscillations au niveau du corps de l'outil WO2007006669A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP06764007A EP1901875A1 (fr) 2005-07-09 2006-06-30 Outil de soudage par friction-malaxage, et procede et dispositif pour commander un processus de soudage par friction-malaxage en temps reel, par detection des forces acceleratrices et/ou des oscillations au niveau du corps de l'outil

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE200510032170 DE102005032170A1 (de) 2005-07-09 2005-07-09 Rührreibschweißwerkzeug und Verfahren und Anordnung zur online-Kontrolle eines Rührreibschweißprozesses
DE102005032170.4 2005-07-09

Publications (1)

Publication Number Publication Date
WO2007006669A1 true WO2007006669A1 (fr) 2007-01-18

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PCT/EP2006/063758 WO2007006669A1 (fr) 2005-07-09 2006-06-30 Outil de soudage par friction-malaxage, et procede et dispositif pour commander un processus de soudage par friction-malaxage en temps reel, par detection des forces acceleratrices et/ou des oscillations au niveau du corps de l'outil

Country Status (3)

Country Link
EP (1) EP1901875A1 (fr)
DE (1) DE102005032170A1 (fr)
WO (1) WO2007006669A1 (fr)

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US7992761B2 (en) * 2006-10-05 2011-08-09 The Boeing Company Process control system for friction stir welding
EP2268446A4 (fr) * 2008-04-15 2012-05-02 Lockheed Corp Systèmes de commande pour soudage par friction-malaxage d'alliages au titane et d'autres matières à point de fusion élevé
DE202012005397U1 (de) 2012-05-31 2012-06-21 Grenzebach Maschinenbau Gmbh Vorrichtung zur Verbesserung der Qualität der Schweißnaht beim Rührreibschweißen
US8342382B2 (en) 2010-02-18 2013-01-01 Rolls-Royce Plc Determining the quality of a friction weld using a double differential
DE102012010836B3 (de) * 2012-05-31 2013-06-20 Grenzebach Maschinenbau Gmbh Verfahren und Vorrichtung zur Verbesserung der Qualität der Schweißnaht beim Rührreibschweißen, Computerprogramm sowie maschinenlesbarer Träger
US8556156B1 (en) * 2012-08-30 2013-10-15 Apple Inc. Dynamic adjustment of friction stir welding process parameters based on weld temperature
DE202012103219U1 (de) 2012-08-24 2013-12-02 Kuka Systems Gmbh Pressschweißvorrichtung
DE202014000747U1 (de) 2014-01-28 2014-02-18 Grenzebach Maschinenbau Gmbh Vorrichtung zum Rührreibschweißen bei Materialien unterschiedlicher Dicke und bei Kehlnähten
US8657179B1 (en) 2012-03-26 2014-02-25 The United States Of America As Represented By The Administrator Of The National Aeronautics And Space Administration Weld nugget temperature control in thermal stir welding
DE202014002642U1 (de) 2014-03-26 2014-04-10 Grenzebach Maschinenbau Gmbh Vorrichtung zur Erhöhung der Festigkeit der Schweißnaht beim Rührreibschweißen
CN104259650A (zh) * 2014-07-31 2015-01-07 上海拓璞数控科技有限公司 一种搅拌摩擦焊接压力控制系统
DE102014004331B3 (de) * 2014-03-26 2015-06-11 Grenzebach Maschinenbau Gmbh Verfahren und Vorrichtung zur Erhöhung der Qualität der Schweißnaht beim Rührreibschweißen sowie Computerprogramm und maschinenlesbarer Träger mit einem Programmcode zur Durchführung des Verfahrens
DE102014001050A1 (de) 2014-01-28 2015-07-30 Grenzebach Maschinenbau Gmbh Verfahren und Vorrichtung zum Rührreibschweißen bei Materialien unterschiedlicher Dicke und bei Kehlnähten
CN102149506B (zh) * 2008-08-11 2015-10-07 梅加斯特尔技术公司 用于通过多轴环组件在高温下夹紧工具材料的旋转保持装置
CN106891089A (zh) * 2017-03-27 2017-06-27 宁波海天精工股份有限公司 一种多用主轴结构
US20180021882A1 (en) * 2015-01-07 2018-01-25 Yamamoto Metal Technos Co., Ltd. Friction stir welding device, and rotary tool used for friction stir welding
CN111250862A (zh) * 2020-03-23 2020-06-09 吉林大学 一种搅拌摩擦焊夹具及温度场反馈控制方法
CN111375885A (zh) * 2020-04-29 2020-07-07 桂林航天工业学院 一种2219铝合金板材用的摩擦搅拌焊接装置
CN112345726A (zh) * 2020-10-23 2021-02-09 安阳工学院 一种对搅拌摩擦焊焊缝质量的评价方法
WO2021155419A2 (fr) 2020-02-06 2021-08-12 Fill Gesellschaft M.B.H. Porte-outil de soudage par friction-malaxage
CN113369810A (zh) * 2021-05-31 2021-09-10 张家港沙钢金洲管道有限公司 一种基于搅拌摩擦焊的铝基复合材料管的制备方法
US11325203B2 (en) 2018-03-06 2022-05-10 Grenzebach Maschinenbau Gmbh Device and method for avoiding an interruption in the welding process during friction stir welding, in particular breakage of the friction pin
US12151301B2 (en) * 2023-03-24 2024-11-26 National Chung Cheng University Friction stir welding tool holder with thermal sensor

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DE102009060138B4 (de) 2009-12-23 2013-08-29 Hochschule Magdeburg-Stendal (Fh) Anordnung zum Reibschweißen kleiner Querschnittsflächen
EP2965851A1 (fr) 2014-07-11 2016-01-13 NELA Razvojni center d.o.o. Podruznica Vincarje Procédé de soudage par friction-malaxage avec détection de rupture d'outil hors ligne
EP2965858A1 (fr) 2014-07-11 2016-01-13 NELA Razvojni center d.o.o. Podruznica Vincarje Détection de rupture d'outil en temps réel pendant le processus de soudage par friction-malaxage
DE102015010638A1 (de) * 2015-08-13 2017-02-16 Grenzebach Maschinenbau Gmbh Vorrichtung und Verfahren zum homogenen Verschweißen flächig gebogener Strukturen durch Rührreibschweißen
JP6329707B2 (ja) 2015-10-21 2018-05-23 川崎重工業株式会社 摩擦撹拌点接合装置及び摩擦撹拌点接合方法
JP6143915B1 (ja) * 2016-04-28 2017-06-07 株式会社日立パワーソリューションズ 摩擦攪拌接合装置
DE102016217025A1 (de) 2016-09-07 2018-03-08 Airbus Defence and Space GmbH Verfahren zum betrieb einer rührreibschweiss-vorrichtung, rührreibschweiss-vorrichtung und rührreibschweiss-system
DE102016221112B4 (de) 2016-10-26 2018-12-20 Airbus Defence and Space GmbH Schweißwerkzeug und Rührreibschweißverfahren zum Verbinden wenigstens zweier Werkstücke mit einem Schweißwerkzeug
DE102016221110B4 (de) 2016-10-26 2018-10-25 Airbus Defence and Space GmbH Schweißwerkzeug und Rührreibschweißverfahren zum Verbinden wenigstens zweier Werkstücke mittels eines Schweißwerkzeugs
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CN112238289A (zh) * 2019-07-16 2021-01-19 中国科学院沈阳自动化研究所 一种搅拌摩擦焊机器人温度无线采集系统
CN113245687B (zh) * 2021-06-21 2021-11-02 宁波齐云新材料技术有限公司 一种转速智能控制的摩擦搅拌焊接系统

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Cited By (36)

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Publication number Priority date Publication date Assignee Title
US7992761B2 (en) * 2006-10-05 2011-08-09 The Boeing Company Process control system for friction stir welding
EP2268446A4 (fr) * 2008-04-15 2012-05-02 Lockheed Corp Systèmes de commande pour soudage par friction-malaxage d'alliages au titane et d'autres matières à point de fusion élevé
CN102149506B (zh) * 2008-08-11 2015-10-07 梅加斯特尔技术公司 用于通过多轴环组件在高温下夹紧工具材料的旋转保持装置
US8342382B2 (en) 2010-02-18 2013-01-01 Rolls-Royce Plc Determining the quality of a friction weld using a double differential
US8657179B1 (en) 2012-03-26 2014-02-25 The United States Of America As Represented By The Administrator Of The National Aeronautics And Space Administration Weld nugget temperature control in thermal stir welding
DE102012010836B3 (de) * 2012-05-31 2013-06-20 Grenzebach Maschinenbau Gmbh Verfahren und Vorrichtung zur Verbesserung der Qualität der Schweißnaht beim Rührreibschweißen, Computerprogramm sowie maschinenlesbarer Träger
WO2013178215A1 (fr) 2012-05-31 2013-12-05 Grenzebach Maschinenbau Gmbh Procédé et dispositif pour améliorer la qualité du cordon de soudure lors du soudage par friction-malaxage
US9956644B2 (en) 2012-05-31 2018-05-01 Grenzenbach Maschinenbau Gmbh Method and device for improving the quality of the weld seam in friction stir welding
DE202012005397U1 (de) 2012-05-31 2012-06-21 Grenzebach Maschinenbau Gmbh Vorrichtung zur Verbesserung der Qualität der Schweißnaht beim Rührreibschweißen
DE202012103219U1 (de) 2012-08-24 2013-12-02 Kuka Systems Gmbh Pressschweißvorrichtung
US10029329B2 (en) 2012-08-24 2018-07-24 Kuka Systems Gmbh Pressure welding device with a measuring device, measuring in a contactless manner, for detecting the surface quality, the true running and/or the axial runout in a front welding area
US8556156B1 (en) * 2012-08-30 2013-10-15 Apple Inc. Dynamic adjustment of friction stir welding process parameters based on weld temperature
DE202014000747U1 (de) 2014-01-28 2014-02-18 Grenzebach Maschinenbau Gmbh Vorrichtung zum Rührreibschweißen bei Materialien unterschiedlicher Dicke und bei Kehlnähten
US9937586B2 (en) 2014-01-28 2018-04-10 Grenzebach Maschinenbau Gmbh Method and device for friction stir welding materials of different thicknesses and having fillet welds
DE102014001050A1 (de) 2014-01-28 2015-07-30 Grenzebach Maschinenbau Gmbh Verfahren und Vorrichtung zum Rührreibschweißen bei Materialien unterschiedlicher Dicke und bei Kehlnähten
WO2015113542A1 (fr) 2014-01-28 2015-08-06 Grenzebach Maschinenbau Gmbh Procédé et dispositif de soudage par friction-malaxage de matériaux d'épaisseur différente et en cas de soudures d'angle
DE202014002642U1 (de) 2014-03-26 2014-04-10 Grenzebach Maschinenbau Gmbh Vorrichtung zur Erhöhung der Festigkeit der Schweißnaht beim Rührreibschweißen
WO2015144115A1 (fr) 2014-03-26 2015-10-01 Grenzebach Maschinenbau Gmbh Procédé et dispositif permettant d'améliorer la qualité d'un joint soudé produit par soudage par friction-malaxage
DE102014004331B3 (de) * 2014-03-26 2015-06-11 Grenzebach Maschinenbau Gmbh Verfahren und Vorrichtung zur Erhöhung der Qualität der Schweißnaht beim Rührreibschweißen sowie Computerprogramm und maschinenlesbarer Träger mit einem Programmcode zur Durchführung des Verfahrens
US10195696B2 (en) 2014-03-26 2019-02-05 Grenzebach Maschinenbau Gmbh Method and apparatus for increasing the quality of the weld seam in friction stir welding
CN104259650B (zh) * 2014-07-31 2017-07-04 上海拓璞数控科技股份有限公司 一种搅拌摩擦焊接压力控制系统
CN104259650A (zh) * 2014-07-31 2015-01-07 上海拓璞数控科技有限公司 一种搅拌摩擦焊接压力控制系统
US20180021882A1 (en) * 2015-01-07 2018-01-25 Yamamoto Metal Technos Co., Ltd. Friction stir welding device, and rotary tool used for friction stir welding
US10525549B2 (en) * 2015-01-07 2020-01-07 Yamamoto Metal Technos Co., Ltd. Friction stir welding device, and rotary tool used for friction stir welding
CN106891089A (zh) * 2017-03-27 2017-06-27 宁波海天精工股份有限公司 一种多用主轴结构
CN106891089B (zh) * 2017-03-27 2022-06-03 宁波海天精工股份有限公司 一种多用主轴结构
US11325203B2 (en) 2018-03-06 2022-05-10 Grenzebach Maschinenbau Gmbh Device and method for avoiding an interruption in the welding process during friction stir welding, in particular breakage of the friction pin
WO2021155419A2 (fr) 2020-02-06 2021-08-12 Fill Gesellschaft M.B.H. Porte-outil de soudage par friction-malaxage
CN111250862A (zh) * 2020-03-23 2020-06-09 吉林大学 一种搅拌摩擦焊夹具及温度场反馈控制方法
CN111250862B (zh) * 2020-03-23 2023-11-17 吉林大学 一种搅拌摩擦焊夹具及温度场反馈控制方法
CN111375885B (zh) * 2020-04-29 2021-11-05 桂林航天工业学院 一种2219铝合金板材用的摩擦搅拌焊接装置
CN111375885A (zh) * 2020-04-29 2020-07-07 桂林航天工业学院 一种2219铝合金板材用的摩擦搅拌焊接装置
CN112345726A (zh) * 2020-10-23 2021-02-09 安阳工学院 一种对搅拌摩擦焊焊缝质量的评价方法
CN112345726B (zh) * 2020-10-23 2022-11-18 安阳工学院 一种对搅拌摩擦焊焊缝质量的评价方法
CN113369810A (zh) * 2021-05-31 2021-09-10 张家港沙钢金洲管道有限公司 一种基于搅拌摩擦焊的铝基复合材料管的制备方法
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