EP0003367B1 - Procédé de fabrication d'un fil à haute résistance mécanique - Google Patents

Procédé de fabrication d'un fil à haute résistance mécanique Download PDF

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Publication number
EP0003367B1
EP0003367B1 EP19790100277 EP79100277A EP0003367B1 EP 0003367 B1 EP0003367 B1 EP 0003367B1 EP 19790100277 EP19790100277 EP 19790100277 EP 79100277 A EP79100277 A EP 79100277A EP 0003367 B1 EP0003367 B1 EP 0003367B1
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Prior art keywords
wire
percent
temperature
alloy
strain
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Expired
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EP19790100277
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German (de)
English (en)
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EP0003367A1 (fr
Inventor
Jaak S. Van Den Sype
Lanier Stambaugh
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Union Carbide Corp
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Union Carbide Corp
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Priority claimed from US05/902,567 external-priority patent/US4161415A/en
Application filed by Union Carbide Corp filed Critical Union Carbide Corp
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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
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/06—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of rods or wires
    • C21D8/065—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of rods or wires of ferrous alloys
    • 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

Definitions

  • This invention relates to a process for improving the strength of wire, and, more particularly, to improving the tensile strength and the torsional yield strength characteristics of certain wires.
  • the chemical compositions of the metal alloys to which this invention is directed are well known and include those alloys listed in the "Steel Products Manual: Stainless and Heat Resisting Steels" published by American Iron and Steel Institute (AISl) now of Washington, D.C. in 1974 and designated as austenitic with the further proviso that these alloys at least initially have an Md temperature of no higher than about 100°C (i.e., plus 100°C) and an Ms temperature no higher than minus 100°C. It will be apparent that the AISI Series Designation 200 and 300 are of interest here. Other alloys contemplated here, again, must be austenitic and have the stated Md and Ms temperatures.
  • alloys include certain manganese- substituted non-stainless alloys containing iron, manganese, chromium, and carbon exemplified by those designated by DIN (Deutsche Industrie Norme) specifications X40 Mn Cr 18 and X40 Mn Cr 22 and described on pages 655 and 656 of the Metallic Materials Specification Handbook published by E & FN Spon Ltd., London 1972.
  • austenitic involves the crystalline microstructure of the alloy, which is referred to as austenitic or austenite when at least about 95 percent by volume of the microstructure has a face-centered cubic structure.
  • Sueh alloys can be referred to as being essentially or substantially in the austenitic phase. It is understood that the alloys of concern here are essentially in the austenitic or austenite phase at the temperature at which the first deformation step is carried out regardless of the work or temperature previously applied, e.g., the metal or alloy subjected to the first deformation step may have been previously annealed yet it is essentially austenitic when the first step is applied.
  • the other microstructure with which we are concerned here is a body-centered cubic structure and is referred to as martensitic or martensite.
  • martensitic When at least about 95 percent by volume of the structure is martensitic, the alloy is considered to be essentially or substantially in the martensite phase.
  • the microstructure can, of course, contain both an austenite phase and a martensite phase and the processing to be discussed here both in terms of the prior art and the present invention is one of transformation of at least part of the austenite to martensite thus' changing the microstructure of the alloy treated.
  • the Md temperature is defined as the temperature above which no martensitic transformation will take place regardless of the amount of mechanical deformation which is applied to the metal or alloy and can be determined by a simple and conventional tensile test carried out at various temperatures.
  • the Ms temperature is defined as the temperature at which martensitic transformation begins to take place spontaneously, i.e., without the application of mechanical deformation.
  • the Ms temperature can also be determined by conventional tests.
  • Md temperatures are as follows:
  • the 301, 302, 304 and 304L steels have Ms temperatures below minus 196°C.
  • the deformation referred to is a mechanical deformation and takes place in the range of plastic deformation, which follows the range of elastic deformation. It is caused by subjecting the material to a stress beyond its elastic limit sufficient to change the shape of all or part of the workpiece.
  • the strength property can readily be determined from a simple uniaxial tensile test as described in ASTM standard method E-8. This method appears in part 10 of the 1975 Annual Book of ASTM Standards published by the American Society for Testing and Materials, Philadelphia, Pa. The results of this test on a material can be summarized by stating the yield strength, tensile strength, and total elongation of the material: (a) the yield strength is the stress at which the material exhibits a specified limiting deviation from the proportionality of stress to strain.
  • the limiting deviation is determined by the offset method with a specified 0.2 percent strain;
  • the tensile strength is the maximum tensile stress which the material is capable of sustaining (tensile strength is the ratio of the maximum load during a tension test'carried to fracture to the original cross sectional area of the specimen);
  • the total elongation is the increase in gauge length of a tension test specimen tested to fracture, expressed as a percentage of the original gauge length. It is generally observed that when the yield and tensile strengths of metallic materials are increased through metallurgical processes, the total elongation decreases.
  • the torsional yield strength of wire can be determined by twisting a finite length of wire over increasing angles and observing when a first permanent angular distortion occurs.
  • a two percent torsional yield strength is defined as the shear stress occurring at the surface of the wire when twisted over an angle sufficient to give rise to a two percent permanent angular offset.
  • Stretching is defined as a deformation of workpieces in which one dimension, called the longitudinal direction, is much larger than the two other dimensions, e.g. wire.
  • This deformation comprises applying forces in the longitudinal direction so that essentially the entire cross-section of the workpiece is under uniform uniaxial tensile stress- during the deformation.
  • The. tensile stresses. are of sufficient magnitude to induce permanent plastic deformation in the workpiece, the application of stress being described in terms of percent strain. Since the term “stretching” as used herein is in contradistinction to other deformation processes such as drawing which involves multiaxial states of stress, the term “stretching ...
  • the second step prescribed in a preferred embodiment of the prior art may be considered a non-drawing step to emphasize the importance of uniaxial stretching and exclude.
  • This deficiency in drawn wire leads to further problems in a specific application, i.e., that of coil springs, where formability is of special interest.
  • the skin portion has to be sufficiently ductile to withstand wrapping without fracture about an arbor with a diameter at least equal to the diameter of the wire, but, unfortunately the preferential work-hardening of the skin during drawing causes the skin to become more brittle and less ductile thus reducing formability.
  • the low temperature stretching process is shown to have improved tensile strength and formability as well as torsional and fatigue properties.
  • the prestrain step improves even further on the tensile strength and toughness of the wire thus further upgrading these materials for commercial use.
  • An object of this invention is to provide an improvement in known wire cryodeformation processes whereby high strength, toughness, and torsional yield strength are attained while minimizing fracture, optimizing uniform strain capability, producing constant diameter wires, and eliminating sizing.
  • strain applied in step (a) will on occasion be referred to in this specification as "prestrain”.
  • Final optimization of the strenth properties is achieved by subjecting the wire to conventional aging at a temperature in the range of about 350°C to about 450°C.
  • the sole figure of the drawing is a schematic diagram illustrating the side view of apparatus, which can be used to carry out the drawing step referred to above.
  • the alloys to which the process is applied are described above and, as noted, are conventional. The only prerequisites are that when the first deformation step is applied they meet the definition of austenitic, and their Md temperatures are no higher than about 100°C and their Ms temperatures are not higher than about minus 100°C.
  • AISI series 300 alloys are preferred, particularly AISI 302 containing C, Ni, Cr, and Mn.
  • 302 alloy be used and that certain components of the 302 alloy fall within the following ranges (in weight percent): nickel 8.0 to 9.0; chromium 17.5 to 19.0; carbon 0.085 to 0.115: manganese less than 1; silicon 0.2 to 0.5; nitrogen 0.02 to 0.08, molybdenum, less than 0.6; sulphur, less than 0.01; and phosphorous, less than 0.035. It is desirable to minimize inclusions.
  • the deformation is mechanical and takes place in that region known as the region of plastic deformation.
  • the deformations must, of course, be sufficient to provide the stated percentages of martensite and austenite, which are first determined by conventional analytical techniques such as X-ray diffraction or magnetic measurements and then on the basis of the experience of the operator with the various alloys on deformation in the noted temperature ranges.
  • step (a) it has been set forth in terms of strain.
  • the strain occurring during process deformation is usually more complex than those ocurring during a simple tension test, it is found that for the materials to which the invention applies, the strengthening effects that occur during complex deformations can be evaluated from the observed strengthening effects during a simple tension test using the ' principle of "equivalent uniaxial" strain or "effective” strain as set forth, e.g. in "Mechanical Metallurgy" by G. E: Dieter, Jr., published by McGraw-Hill Book Company (1961), on page 66.
  • the minimum strain in step (a) deformation is at least about 10 percent. There is no upper limit for percent strain except that of practicality in that at a certain point the change in microstructure and strength-toughness properties become minimal and, of course, there is a limit as to fracture of the material.
  • the suggested strain range in this first step is from about 10 to about 80 percent and preferably about 20 to about 60 percent
  • the initial alloy utilized in the process is at least about 95 percent by volume austenite, the balance being martensite.
  • the alloy Under deformation in step (a) (or prestrain), the alloy may be changed slightly from a mictrostructural point of view so that 0 to about 10 percent by volume is in the martensite phase and about 90 to about 100 percent by volume is in theauste- nite phase, and there is, preferably, 0 to about 5 percent by volume martensite and about 95 to about 100 percent by volume austenite.
  • the deformation only decreases the austenitic phase: If the initial austenitic phase-is at 100 percent, for example, the deformation can be used to reduce it up to 10 percent as far as 90 percent. If the austenitic phase is 95 percent, the deformation will only be used to reduce the austenitic phase up to 5 percent to 90 percent.
  • the prestrain step is conducted at a temperature in the range of about Md minus 50°C to about Md plus 50°C, preferably about Md minus 10°C to about Md plus 10°C, said Md temperature being that of the alloy undergoing deformation, e.g., where the Md temperature is 43°C, Md minus 50°C will equal minus 7°C and Md plus 50°C will equal 93°C.
  • the alloys under consideration here are considered stable, i.e., austenitically stable, at these first step temperatures even though they undergo the changes set forth above when subjected to deformation.
  • the strain is further adjusted to provide yield strengths in the range of about 896 Mpa to about 1,586 Mpa. These particular yield strengths are obtained first by testing samples of the wire and then through the experience of the operator with the particular wire undergoing treatment, the temperature at which the step (a) deformation is undertaken, and the amount of strain used, the latter amount of strain usually being adjusted to accommodate the particular wire and temperature. Preferred yield strengths obtained by the prestrain are in the range of about 896 Mpa to about 1,241 Mpa. It is suggested that prior processing such as annealing and prestrain be optimized to achieve a small grain size.
  • the wire is cooled to a temperature no higher than about minus 75°C and, preferably, less than about minus 100°C.
  • these temperatures can be achieved by immersing the wire in liquid nitrogen (B.P. minus 196°C); liquid oxygen (B.P. minus 183°C; liquid argon (B.P. minus 186°C) liquid neon (B.P. minus 246°C); liquid hydrogen (B.P. minus 252°C) or liquid helium (B.P. minus 269°C).
  • Liquid nitrogen is preferred.
  • a mixture of dry ice and methanol, ethanol, or acetone has a boiling point of about minus 79°C and can also be used; however, the lower temperatures are preferred sincg, as is well known, the lower the temperature, the lower the amount of strain needed for each percent of improvement in tensile strength.
  • the cooling step, step (b) must take place prior to drawing step (c) and that the wire must enter the die at substantially the temperature to which it has been cooled in step (b). This means that steps (b) and (c) should be so coordinated that the time interval between the two steps is short enough to substantially avoid any temperature rise above the cooling temperature of step (b).
  • Step (c) is similar to step (a) insofar as deformation or strain is concerned, however, the deformation is defined in different terms.
  • sufficient strain must be applied to provide the stated percentages of martensite and austenite; first determined by conventional analysis and then by reliance on operator experience.
  • the minimum strain applied in the second deformation is at least about 10 percent.
  • there is no upper limit for percent strain except the bounds of practicality in that change in microstructure and strength-toughness properties tend to become minimal and there is a limit due to fracture of the material.
  • the suggested strain range is about 10 to about 60 percent and is, preferably, about 20 to about 40 percent.
  • step (c) the required strain is provided by drawing the cooled wire through a die under back-tension (i) wherein the back-tension on said wire just prior to the entry of the wire into the die is at least about 517 Mpa and (ii) whereby the cross-sectional area of the wire is reduced by a percentage in the range of about 7 percent to about 20 percent.
  • back-tension i) wherein the back-tension on said wire just prior to the entry of the wire into the die is at least about 517 Mpa and (ii) whereby the cross-sectional area of the wire is reduced by a percentage in the range of about 7 percent to about 20 percent.
  • the dies which may be used in this step are conventional, e.g., tungsten carbide drawing dies.
  • the cone angle of the carbide nib is found to be optimally about 12 degrees. Larger die angles give rise to an excessive amount of redundant work of deformation resulting in less than optimum properties. Die angles smaller than 12 degrees have two large a bearing length and the increased friction between die and metal is also found to provide less than optimum properties particularly with respect to torsional yield.
  • the lubricants used for the wire and which are applied prior to drawing are also conventional.
  • the wire is precoated with lubricant. This precoat is applied by dipping the coils in standard precoat solutions. These solutions may contain lime or oxalate.
  • the wire Prior to entering the die in step (c), and after step (b), the wire passes through a box filled with a dry soap such as calcium stearate soap. To enhance, its passage through the die, the wire may also be copper-coated.
  • the drawing speed is fast enough to move the cooled wire through the lubricant and to the entrance of the die aperture before the temperature of the wire rises substantially above the cooling temperature of step (b).
  • the drawing speed is about 30 to about 244m per minute for wire diameters of about 1.0 mm to about 5.1 mm.
  • the stated drawing speeds refer to the outgoing wire diameter, i.e., the diameter of the wire as it leaves the die. The drawing speed will be slower for larger diameter wire and faster for wire of thinner diameter, the most desirable speed being determined by the experience of the operator with the particular wire.
  • back-tension is defined as the stress in the longitudinal direction on the wire prior to entering the die. Stated back-tensions refer to the incoming wire diameter, i.e., the diameter of the wire as it enters the die. It is also referred to as "back-pull.” Back-pull wire drawing is well-known and is discussed in the Journal of the Iron and Steel Institute, November, 1947, at pages 417 to 428 and in the Steel Wire Handbook, Volume 1, published by the Wire Association, Inc., Stamford, Connecticut, 1965, at pages 245 to 250. The preferred amount of back-tension is in the range of about 517 Mpa to about 1,034 Mpa. The smoothest operation occurs with higher back-tension.
  • the preferred reduction in cross-sectional area of the wire is in the range of about 15 to about 25 percent.
  • step (c) the microstructure of the metal or alloy is changed appreciably so that at least 50 percent by volume is in the martensite phase and at least 10 percent by volume is in the austenite phase.
  • the preferred range lies in the area of about 60 to about 90 percent by volume martensite and about 10 to about 40 percent by volume austenite. It is believed that the. high austenite content contributes to the toughness of the processed material.
  • microstructure of the initial alloy and of the products of the prestrain, cryodrawing, and aging is considered to consist essentially of austenite and/or martensite in the percentages previously stated. Any other phases present are not of interest here since such phases, if they are present at all, are less than about one percent by volume and have little or no effect on the properties of the alloy.
  • the ranges, in which the strain percentages for step (a) and step (c) lie overlap. Although the percentages can be the same, it is preferred that the ratio of prestrain to drawing strain is in the range of about 1:1 to about 3:1.
  • the alloy is preferably subjected to aging to optimize strength.
  • Aging is carried out in a conventional manner at a temperature in the range of about 350°C to about 450°C and, preferably, in the range of about 375°C to about 425°C.
  • Aging time can range from about 30 minutes to about 10 hours and is preferably in the range of about 30 minutes to about 2.0 hours. Conventional testing is used here to determine the temperature and time, which give the highest strength properties.
  • Ratios of torsional yield strength to tensile strength, after aging are found to be in the range of about 0.45 to about 0.49 when subject process is carried out in the preferred manner.
  • the wire in all examples contains at least 95 percent by volume austenite prior to the first deformation and at least 90 percent by volume austenite prior to the drawing step. After the drawing step, the wire contains at least 50 percent by volume martensite and at least 10 percent by volume austenite. Percent by volume martensite is determined by quantitative X-ray diffraction technique. The balance (to make up a total of 100 percent) is considered to be austenite. Other phases are not more than one percent by volume and are not considered here.
  • Annealed AISI type 302 stainless steel wire is used. The annealing is accomplished with conventional techniques by heating the wire between 980°C and 1 150°C followed by rapid cooling.
  • double capstan cooler 3 an insulated metal dewar
  • Each capstan contains twenty grooves and wire 1 is wrapped around both capstans twenty times, the wire, of course, being in the grooves.
  • This procedure cools wire 1 to minus 196°C.
  • Back-tension is applied by means of brake 6 connected to capstan 5 (back-tension is not applied to welds made after the first. deformation).
  • wire 1 passes from capstan 5 to single grooved roller 7 where back-tension is measured by means of a strain gauge (not shown) after which the wire exits cooler 3. Moisture build-up on the cooled wire is avoided by use of a nitrogen shroud.
  • wire 1 enters die box 8 (a pressure die is preferably used here to enhance tubrication) which is filled with soap (a conventional lubricant) and is drawn through die 9 having an approach angle of 12 degrees. The drawing force is generated by means of conventional bull-block 10. Die 9 and die-box 8 are not immersed in liquid nitrogen, but the travel time between cooler 3 and die 9 is sufficiently short that no appreciable heating occurs.
  • the tensile strength is determined after the drawing step and then the wire is aged in a conventional manner at 400°C for 1/2 hour in a Lindberg Model 59744 furnace in air.
  • the surface oxidation of the wire occurring during ageing is assumed not to affect the resulting mechanical properties.
  • the temperature along the length of all specimens does not vary more than + 10°C from the preset temperature.
  • the wire of all of the examples shows adequate formability in that it can be wrapped around an arbor equal to the final wire diameter without fracture.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Mechanical Engineering (AREA)
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  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
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  • Heat Treatment Of Steel (AREA)
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Claims (6)

1. Procédé pour améliorer les caractéristiques de résistance d'un fil composé d'un alliage métallique austénitique choisi dans le groupe comprenant des alliages d'acier inoxydable des séries AISI 200 et 300 et des alliages d'acier non inoxydables contenant du fer; du manganèse, du chrome et du carbone, ledit, alliage ayant une temperature Md ne dépassant pas environ 100°C et une' température Ms ne dépassant pas environ moins 100°C, dans lequel la température Md est la température au-dessus de laquelle aucune transformation martensitique n'a lieu, quelle que soit l'amplitude de la. déformation mécanique qui est appliquée à l'alliage, dans lequel la température Ms est la température à laquelle une transformation martensitique commence à avoir lieu spontanément sans application de déformation mécanique, et dans lequel l'alliage est qualifié d'austénitique lorsqu'au moins environ 95% en volume de la microstructure cristalline de l'alliage présente une structure cubique à faces centrées, ledit procédé comprenant les opèrations suivantes:
(a) une déformation du fil par un allongement d'au moins environ 10% et à une température dans la plage d'environ Md moins 50°C à environ Md plus 50°C, ladite température Md étant celle de l'alliage subissant une déformation, de manière que le fil contienne une phase de martensite ne dèpassant pas environ 10% en volume et une phase d'austénite d'au moins environ 90% en volume;
(b) un refroidissement du fil à une température ne dépassant pas environ moins 75°C; et
(c) une déformation du fil refroidi de manière que le fil comprenne une phase de martensite d'au moins environ 50% en volume et une phase d'austénite d'au moins environ 10% en volume,

caractérisé par un réglage de l'allongement dans l'opération (a) pour produire une limite d'élasticité dans la plage d'environ 896 MPa à environ 1586 MPa; et par exécution de l'opération (b) de déformation par tréfilage du fil refroidi dans une filière sous contre-traction (i) dans lequel la contre-traction, définie comme étant la contrainte appliquée audit fil dans la direction longitudinale, immédiatement avant l'entrée du fil dans la filière, est d'au moins environ 517 MPa; et (ii) de manière que la section du fil soit réduite d'un pourcentage compris dans la plage d'environ 7% à environ 25%.
2. Procédé selon la revendication 1 comprenant l'opération supplémentaire suivante:
(d) un vieillissement du matériau produit dans l'opération (c) à une température dans la plage d'environ 350°C à environ 450°C.
3. Procédé selon la revendication 2,. dans lequel, dans l'opération (a), l'allongement est d'environ 10 à environ 80% et la limite d'élasticité est dans la plage d'environ 896 MPa à environ 1241 MPa et, dans l'opération (c), la contre-traction est dans la plage d'environ 517 MPa à environ 1034 MPa et la section du fil est réduite d'un pourcentage dans la plage d'environ 15% à environ 25%.
4. Procédé selon la revendication 3, dans lequel l'allongement dans l'opération (a) est produit par étirage.
5. Procédé selon la revendication 3, dans lequel l'allongement dans l'opération (a) est produit par tréfilage.
6. Procédé selon l'une quelconque des revendications 2 à 5, dans lequel le matériau est un alliage d'acier inoxydable de la série AISI 300.
EP19790100277 1978-02-01 1979-01-31 Procédé de fabrication d'un fil à haute résistance mécanique Expired EP0003367B1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
US87432678A 1978-02-01 1978-02-01
US874326 1978-02-01
US05/902,567 US4161415A (en) 1978-02-01 1978-05-03 Method for providing strong wire
US902567 1978-05-03

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EP0003367A1 EP0003367A1 (fr) 1979-08-08
EP0003367B1 true EP0003367B1 (fr) 1981-08-26

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BR (1) BR7900583A (fr)
CA (1) CA1095856A (fr)
DE (1) DE2960665D1 (fr)

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Publication number Priority date Publication date Assignee Title
BE873620A (nl) * 1979-01-22 1979-07-23 Bekaert Sa Nv Werkwijze voor het vervormen van voorwerpen uit gelegeerd staal
US4204885A (en) * 1979-03-21 1980-05-27 Union Carbide Corporation Method for providing strong wire
US4296512A (en) * 1979-11-09 1981-10-27 Union Carbide Corporation Method for making fasteners
CN104128379A (zh) * 2014-07-07 2014-11-05 江苏欣宏泰机电有限公司 能提高工作效率的铝线反手拉丝系统
CN110205451A (zh) * 2017-07-05 2019-09-06 凌伯勇 一种弹簧合金钢工件调质方法

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JPS4916166B1 (fr) * 1970-12-07 1974-04-20
US4042421A (en) * 1975-12-03 1977-08-16 Union Carbide Corporation Method for providing strong tough metal alloys

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BR7900583A (pt) 1979-08-28
CA1095856A (fr) 1981-02-17
EP0003367A1 (fr) 1979-08-08

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