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EP1438150B1 - Dispositif et procede de production de materiaux microcristallins - Google Patents

Dispositif et procede de production de materiaux microcristallins Download PDF

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Publication number
EP1438150B1
EP1438150B1 EP02799373A EP02799373A EP1438150B1 EP 1438150 B1 EP1438150 B1 EP 1438150B1 EP 02799373 A EP02799373 A EP 02799373A EP 02799373 A EP02799373 A EP 02799373A EP 1438150 B1 EP1438150 B1 EP 1438150B1
Authority
EP
European Patent Office
Prior art keywords
deformation
pressure
specimen
sample
steps
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.)
Expired - Lifetime
Application number
EP02799373A
Other languages
German (de)
English (en)
Other versions
EP1438150A1 (fr
Inventor
Reinhard Pippan
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.)
Innovationsagentur GmbH
Original Assignee
Innovationsagentur GmbH
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 Innovationsagentur GmbH filed Critical Innovationsagentur GmbH
Priority to AT02799373T priority Critical patent/ATE329707T1/de
Publication of EP1438150A1 publication Critical patent/EP1438150A1/fr
Application granted granted Critical
Publication of EP1438150B1 publication Critical patent/EP1438150B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D7/00—Modifying the physical properties of iron or steel by deformation
    • C21D7/02—Modifying the physical properties of iron or steel by deformation by cold working
    • C21D7/10—Modifying the physical properties of iron or steel by deformation by cold working of the whole cross-section, e.g. of concrete reinforcing bars
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES, PROFILES OR LIKE SEMI-MANUFACTURED PRODUCTS OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C23/00—Extruding metal; Impact extrusion
    • B21C23/001—Extruding metal; Impact extrusion to improve the material properties, e.g. lateral extrusion
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES, PROFILES OR LIKE SEMI-MANUFACTURED PRODUCTS OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C23/00—Extruding metal; Impact extrusion
    • B21C23/01—Extruding metal; Impact extrusion starting from material of particular form or shape, e.g. mechanically pre-treated
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21J—FORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
    • B21J1/00—Preparing metal stock or similar ancillary operations prior, during or post forging, e.g. heating or cooling
    • B21J1/02—Preliminary treatment of metal stock without particular shaping, e.g. salvaging segregated zones, forging or pressing in the rough
    • B21J1/025—Preliminary treatment of metal stock without particular shaping, e.g. salvaging segregated zones, forging or pressing in the rough affecting grain orientation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21J—FORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
    • B21J5/00—Methods for forging, hammering, or pressing; Special equipment or accessories therefor
    • 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
    • C21D2201/00—Treatment for obtaining particular effects
    • C21D2201/03—Amorphous or microcrystalline structure

Definitions

  • the invention relates to an apparatus and a method for producing submicron or nanocrystalline materials by multiple plastic deformation of a material sample, wherein the outer shape of the material sample after the first deformation essentially corresponds to that after the last deformation (see 2.B. US-A -4,721,537).
  • Submicron or nanocrystalline materials in particular of metals, alloys, or intermetallic compounds, are ideally suited for a wide range of applications and in particular have a very high strength. Such materials have been used since the 1980's, e.g. manufactured by powder metallurgical way. However, metallic materials produced in such a way unfortunately have a relatively low ductility.
  • the material sample 1 to be deformed is located in a cylindrical recess of a pressure-resistant mold 2 and is pressurized with a pressure piston 3 with a cylindrical cross-section.
  • an angled channel is formed in a pressure-resistant mold 2, through which the material sample 1 is pressed by means of a punch 3. After removal of the material sample from the angled channel this is again - as indicated by dashed lines - introduced on the side of the plunger 3 in the mold 2, which can be carried out to achieve the desired fine structure more similar deformation steps.
  • the material sample essentially retains its outer shape, that is, the outer shape of the material sample after the first deformation substantially corresponds to that after the last deformation, although many Such deformation steps are performed sequentially.
  • Fig. 3 the CEC method is sketched, in which the pressure-resistant mold 2 has a cylindrical channel with a taper.
  • the material sample 1 is pressed by means of a first plunger 3 through the cylindrical taper of the channel against the pressure of a second plunger 3, wherein the sample is subjected to a compression followed by extrusion. Thereafter, the direction of movement of the two plunger 3 is reversed and the sample of material 1 is again pressed through the cylindrical taper.
  • the outer shape of the material sample remains essentially unchanged and the cyclic deformation can be repeated until the desired fine structure is achieved.
  • a disadvantage of the two methods according to FIGS. 2 and 3 is the inhomogeneous deformation in the two end regions of the material sample 1, as well as the relatively large force required to overcome the frictional forces between the shape and the material sample.
  • the starting material in contrast to the present invention, is not a solid, homogeneous material sample, but a mass M of particulate material which is pressure sintered by applying first, second and third compressive forces in directions normal to each other to form a final product.
  • Means for heating the mass M suitable for supplying a sintering heat, e.g. an induction heating unit with a coil surrounding the mass M or an electric heating unit with opposite current-conducting electrodes.
  • a sintering heat e.g. an induction heating unit with a coil surrounding the mass M or an electric heating unit with opposite current-conducting electrodes.
  • JP 08-188838 A discloses a device with which a homogeneous particle distribution in particle-reinforced aluminum alloys is to be achieved.
  • a variant of the ECA method is described in a first embodiment, in which two angled channels are combined in the form of a cross channel, but here - as in all ECA method - the sample by more or less formed edges (change in direction by 90 °) must be pressed, whereby large frictional forces arise.
  • JP 08-188838 A two opposing plunger are used in each case, which are guided by their conical shape in the pairwise movement to each other sliding and change the volume and shape of the interior.
  • the high frictional forces of the pressure pistons guided against one another must be mentioned.
  • Object of the present invention is to propose a device or a method for producing finely crystalline, preferably submicron or nanocrystalline materials by multiple plastic deformation of a material sample, with homogeneous, submicron or nanocrystalline materials are to arise at relatively low energy consumption.
  • the device according to the invention has a pressure-resistant form with a substantially parallelepiped or cube-shaped interior, wherein at least one of the interior wall bounding surfaces is designed as movable in the direction of the interior plunger, after the pressurization, the material sample is substantially normal to Pressure direction in a free area of the pressure-resistant mold expands.
  • the strength of recrystallized pure copper from about 60 MPa can be increased to 500 MPa, without significant losses in the elongation at break.
  • Intermetallic Ni 3 Al materials are relatively brittle. Such treatment can give them considerable ductility.
  • Recrystallized pure chromium has a brittle-transition temperature of about 300 ° C. In a submicron crystalline pure chromium produced by multiple plastic deformation, the brittle transition temperature is below room temperature.
  • step b a compression deformation of the material sample along a third of three substantially normal mutually adjoining spatial directions, wherein after a free expansion of the sample in at least one of the other two spatial directions boundaries are set.
  • a deformation path of more than 30%, preferably 50 to 60%, of the thickness of the material sample in the direction of deformation is carried out.
  • 8 to 10 deformation steps are necessary. With increasing number of cycles, the grain size decreases further and the misorientation (tilting) of the neighboring grains increases.
  • At least one pressure stamp is used to deform the material sample, which alternately acts on different boundary surfaces of the material sample, which boundary surfaces enclose an angle of substantially 90 °.
  • FIGS. 4a to 4c The simplest embodiment of the device according to the invention is shown in FIGS. 4a to 4c.
  • the material sample 1 which essentially corresponds to a cuboid, has mutually parallel cover surfaces A, B and C, and is arranged in a substantially parallelepiped or cube-shaped interior of a pressure-resistant mold 2.
  • the individual wall surfaces of the pressure-resistant mold 2 are labeled 4 (bottom surface), 5 (top surface) and 6 (side surfaces).
  • one of the wall surfaces 4 to 6, namely the top surface 5 is designed as a pressure stamp 3 which is movable in the direction of the interior and has a rectangular or square cross-section.
  • the material sample 1 is first of all inserted into the pressure-resistant mold 2, as shown in FIG. 4 a, with the top surface A of the sample resting against the pressure ram 3. Thereafter, as shown in FIG. 4b, a compression deformation of the sample, wherein the plunger 3 in the example shown a Deformation path of about 50% of the thickness or height of the material sample travels in the deformation direction.
  • the sample expands normal to the printing direction into the free area 7 of the pressure-resistant mold 2 until the expansion is limited by the side surfaces 6. This results again in a material sample of the same or very similar outer shape as in Fig. 4a with the boundary surfaces A to C.
  • the sample is rotated and used for the next deformation of FIG. 4c in the mold 2.
  • two or three plungers 3 are used whose axes are normal to one another.
  • one of the two pressure pistons 3 can be held in each case, and thus form part of the pressure-resistant mold 2, while the other pressure piston 3 deforms the material sample 1.
  • the manipulation effort is thereby reduced since the material sample 1 does not have to be removed from the mold 2 after each deformation, rotated and replaced.
  • two or three mutually adjoining wall surfaces are designed as pressure stamps 3 which can be actuated alternately.
  • the guide elements for the three pressure pistons 3 are indicated only by dashed lines, the material sample is concealed by the cyclically actuable pressure pistons 3.
  • At least one of the wall surfaces bounding the interior space may be made removable or slidable.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Extrusion Of Metal (AREA)
  • Powder Metallurgy (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Casting Or Compression Moulding Of Plastics Or The Like (AREA)

Claims (6)

  1. Procédé de fabrication de matière submicrocristalline ou nanocristallines par une déformation plastique multiple d'un échantillon de matière selon lequel la forme extérieure de l'échantillon de matière correspond pratiquement, après la première déformation, chaque fois à la dernière déformation,
    caractérisé par les étapes suivantes :
    a) déformation sous pression de l'échantillon de matière suivant une première parmi trois directions de l'espace essentiellement perpendiculaires les unes aux autres et après expansion libre de l'échantillon dans au moins l'une des deux autres directions de l'espace, on fixe des limites,
    b) déformation sous pression de l'échantillon de matière suivant une seconde des trois directions de l'espace essentiellement perpendiculaires les unes aux autres, et après expansion libre de l'échantillon on fixe des limites au moins dans l'une des deux autres directions de l'espace,
    c) on poursuit par les étapes a, b jusqu'à obtenir une structure fine définie au préalable pour l'échantillon de matière et les différentes étapes de déformation sont exécutées à des températures Tv comprises entre la température ambiante et une température de 0,5 Ts, la température Ts étant la température de fusion de cette matière et on effectue entre 8 et 10 étapes de transformation.pour obtenir des limites de granulométrie d'angle grossier supérieur à 15°,
  2. Procédé selon la revendication 1,
    caractérisé en ce qu'
    après l'étape b) on effectue une déformation sous pression de l'échantillon de matière suivant une troisième des trois directions de l'espace essentiellement perpendiculaires les unes aux autres et après la libre expansion de l'échantillon, on fixe des limites au moins dans l'une des deux autres directions de l'espace.
  3. Procédé selon la revendication 1 ou 2,
    caractérisé en ce que
    par des étapes de déformation, on exécute une course de déformation supérieure à 30 %, de préférence comprise entre 50 % et 60 % de l'épaisseur de l'échantillon de matière dans le sens de la déformation.
  4. Procédé selon l'une des revendications 1 à 3,
    caractérisé en ce qu'
    on utilise deux ou trois poinçons de pression dont les axes sont perpendiculaires les uns aux autres.
  5. Dispositif pour la mise en oeuvre du procédé selon l'une des revendications 1 à 4 pour la déformation plastique d'un échantillon de matière (1) dans un moule (2) résistant à la pression, en utilisant au moins un poinçon de pression (3) agissant sur l'échantillon de matière (1), le moule résistant à la pression (2) ayant une cavité intérieure essentiellement parallélépipédique et au moins l'une des surfaces de paroi (4, 5, 6) qui délimite le volume intérieur est réalisée par un poinçon de pression (3) mobile en direction du volume intérieur et après la mise en pression, l'échantillon de matière (1) s'expanse pratiquement perpendiculairement à la direction d'exercice de la pression dans une zone libre (7) du moule (2) résistant à la pression,
    caractérisé en ce que
    chaque fois trois des surfaces de paroi directement adjacentes sont réalisées sous la forme de poinçons de pression (3) actionnés alternativement.
  6. Dispositif selon la revendication 5,
    caractérisé en ce que
    pour l'extraction de l'échantillon de matière (1), au moins l'une des surfaces de paroi (4), délimitant le volume intérieur, n'est pas réalisée comme poinçon de pression (3) mais peut être enlevée ou coulissée.
EP02799373A 2001-09-25 2002-09-19 Dispositif et procede de production de materiaux microcristallins Expired - Lifetime EP1438150B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT02799373T ATE329707T1 (de) 2001-09-25 2002-09-19 Vorrichtung und verfahren zur herstellung feinkristalliner werkstoffe

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
AT0151601A AT411027B (de) 2001-09-25 2001-09-25 Vorrichtung und verfahren zur herstellung feinkristalliner werkstoffe
AT15162001 2001-09-25
PCT/AT2002/000272 WO2003026815A1 (fr) 2001-09-25 2002-09-19 Dispositif et procede de production de materiaux microcristallins

Publications (2)

Publication Number Publication Date
EP1438150A1 EP1438150A1 (fr) 2004-07-21
EP1438150B1 true EP1438150B1 (fr) 2006-06-14

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EP02799373A Expired - Lifetime EP1438150B1 (fr) 2001-09-25 2002-09-19 Dispositif et procede de production de materiaux microcristallins

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Country Link
EP (1) EP1438150B1 (fr)
AT (2) AT411027B (fr)
DE (1) DE50207219D1 (fr)
WO (1) WO2003026815A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110508635A (zh) * 2019-08-27 2019-11-29 太原理工大学 一种具有分离式凸模的非对称往复挤压装置及加工方法

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GB0323541D0 (en) * 2003-10-08 2003-11-12 Univ Strathclyde A method of treating a metal billet
AT501546B1 (de) * 2005-03-08 2007-02-15 Austria Wirtschaftsservice Tec Verfahren zur herstellung metallischer verbundwerkstoffe
DE102009050543B3 (de) * 2009-10-23 2011-05-26 Peter Prof. Dr.-Ing. Dipl.-Wirtsch.-Ing. Groche Verfahren und Vorrichtung zur Herstellung von feinkörnigen, polykristallinen Werkstoffen oder Werkstücken aus länglichen oder rohrförmigen Halbzeugen
AT510770B1 (de) * 2010-11-29 2015-01-15 Ait Austrian Inst Technology Verfahren zur herstellung eines gegenstandes aus einem metall oder einer legierung, daraus hergestellter gegenstand sowie presswerkzeug hierfür
KR101278290B1 (ko) * 2011-10-20 2013-06-21 포항공과대학교 산학협력단 압축비틀림을 이용한 나선형 층상복합재료 제조 방법
CN103785844B (zh) * 2014-01-13 2017-08-08 上海交通大学 一种纳米结构块体镁材料及制备方法
CN104690205B (zh) * 2015-01-27 2016-08-17 浙江大学 制备三维大尺寸全致密纳米晶铁块体材料的模具和方法
DE102015107308B4 (de) * 2015-05-11 2017-10-19 Gottfried Wilhelm Leibniz Universität Hannover Verfahren zum Strangpressen, Strangpressvorrichtung sowie Strangpresswerkzeug
CN105107914A (zh) * 2015-08-17 2015-12-02 盐城工学院 一种高压扭转成形机
DE102015218408A1 (de) 2015-09-24 2017-03-30 Siemens Aktiengesellschaft Bauteil und/oder Oberfläche aus einem Refraktärmetall oder einer Refraktärmetalllegierung für thermozyklische Belastungen und Herstellungsverfahren dazu
CN106269971B (zh) * 2016-08-17 2018-06-19 中国兵器工业第五九研究所 一种多向压缩扭转复合挤压制备微纳米铜的方法
CN106381458A (zh) * 2016-10-13 2017-02-08 南京工程学院 一种基于限定型高压扭转的非晶合金强化方法
CN106825097B (zh) * 2017-04-01 2018-06-19 哈尔滨理工大学 一种等通道转角挤压与往复式挤扭复合成形装置及方法
CN108714631B (zh) * 2018-05-17 2020-12-01 北京科技大学 一种扭-挤复合强塑变成形方法及工艺装置
CN109759488B (zh) * 2018-12-29 2019-11-22 华中科技大学 一种高压扭转成形模具
CN111139346B (zh) * 2020-01-16 2021-07-27 暨南大学 一种塑性变形处理提高Fe基非晶合金电解水析氢催化活性的方法
CN113369328B (zh) * 2021-06-11 2023-04-25 中国兵器工业第五九研究所 一种开放型腔循环挤压模具
CN113774297B (zh) * 2021-09-08 2022-06-24 厦门理工学院 基于剧烈塑性变形的可提高铝合金耐腐蚀性和力学性能的方法及高性能耐腐蚀铝合金
CN116765756B (zh) * 2023-06-21 2025-08-29 江西保太有色金属集团有限公司 一种亚微晶磷铜球的加工方法

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Also Published As

Publication number Publication date
WO2003026815A1 (fr) 2003-04-03
DE50207219D1 (de) 2006-07-27
AT411027B (de) 2003-09-25
ATA15162001A (de) 2003-02-15
EP1438150A1 (fr) 2004-07-21
ATE329707T1 (de) 2006-07-15

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