EP0430754A1 - Rostfreie Formgedächtnislegierung und Verfahren zu ihrer Herstellung - Google Patents

Rostfreie Formgedächtnislegierung und Verfahren zu ihrer Herstellung Download PDF

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Publication number
EP0430754A1
EP0430754A1 EP90403251A EP90403251A EP0430754A1 EP 0430754 A1 EP0430754 A1 EP 0430754A1 EP 90403251 A EP90403251 A EP 90403251A EP 90403251 A EP90403251 A EP 90403251A EP 0430754 A1 EP0430754 A1 EP 0430754A1
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EP
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Prior art keywords
temperature
alloy
shape memory
stainless
annealing
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EP90403251A
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English (en)
French (fr)
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EP0430754B1 (de
Inventor
Marc Mantel
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Ugine SA
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Ugine Aciers SA
Ugine Aciers de Chatillon et Guegnon
Ugine SA
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Application filed by Ugine Aciers SA, Ugine Aciers de Chatillon et Guegnon, Ugine SA filed Critical Ugine Aciers SA
Priority to AT90403251T priority Critical patent/ATE101878T1/de
Publication of EP0430754A1 publication Critical patent/EP0430754A1/de
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/38—Ferrous alloys, e.g. steel alloys containing chromium with more than 1.5% by weight of manganese

Definitions

  • the present invention relates to a stainless iron-based alloy having a so-called shape memory effect consisting, after a mechanical deformation determined when cold, in recovering the initial shape by heating, said shape memory alloy being produced for the production products such as sheets, wires, profiles used in particular in industrial applications such as tube fittings, sleeves, clamping rings and collars.
  • the present invention also relates to a process for the preparation of such an alloy.
  • Shape memory metal alloys have been known for many years and have long been considered solely as laboratory products, their cost of development not making it possible to envisage industrial development.
  • the shape memory effect is a phenomenon linked to the modification, in the alloy, of an initial austenitic phase ⁇ into a martensitic phase ⁇ , modification generated in a temperature interval determined by a determined mechanical deformation.
  • the temperature range in which the phase ⁇ can be created is limited to a temperature interval [M s , M f ] in which M s is the start temperature of the trans martensitic formation and M f the temperature at the end of the martensitic transformation, the temperature range generally being between + 100 ° C and - 50 ° C.
  • the mechanical deformation can be partially or totally erased, after heating of the deformed alloy, to a temperature comprised in a temperature range in which the martensite phase ⁇ becomes again an austenitic phase ⁇ , temperature range limited to an interval [A s , A f ] in which A s is the temperature at the start of the martensite reversion and A f is the temperature at the end of the martensite reversion, temperature range between 50 ° C and 300 ° C.
  • the shape memory effect is obtained by promoting the formation of martensite ⁇ during mechanical deformations.
  • An intrinsic stacking fault in the face centered cubic structure of the ⁇ phase is considered to generate a hexagonal phase or ⁇ phase, the transition from a ⁇ phase to a ⁇ phase being obtained by the movement of a partial Schockley dislocation. both of them crystalline planes.
  • the alloy is composed of: - 20 to 40% manganese, - 3.5 to 8% silicon, - one or more components such as chromium, nickel, cobalt, in a content of less than 10%, - less than 2% molybdenum, - and less than 1% of carbon, aluminum and copper.
  • phase ⁇ generating the shape memory effect can only be induced with manganese contents greater than 20% and that beyond a content in manganese of 40%, a phase other than the ⁇ phase predominates with a loss of the memory effect, and, on the other hand, that silicon promotes the creation of the ⁇ phase, the values of the silicon contents greater than 8% resulting in difficulties in developing the alloy and a loss of the machinability qualities of said alloy.
  • chromium which improves the obtaining of the ⁇ phase also creates intermellic compounds with low melting point, which causes with contents greater than 10% a great difficulty in developing the 'alloy.
  • the chromium contents remain below 5%.
  • the quoted value range of the manganese contents is from 20 to 40%, it is noted that the average value of the manganese contents of the alloys studied and grouped in a table representing examples of composition, is of the order of 30 %. In addition, contrary to the teaching disclosed, it is also possible to obtain a phase ⁇ in an iron-based alloy when the manganese content is less than 20% by weight.
  • the alloy described in Japanese patent application No. 60.249957 is not a stainless alloy, and the arguments stated with regard to the contents given show that it is not possible to obtain a stainless alloy with such a composition .
  • Such an alloy contains a large proportion of nickel and cobalt which are strategic materials, whose prices, fluctuating, dominate the costs of developing this alloy.
  • nickel when added in a content greater than 5% by weight, increases the energy of stacking failure, while elements such as manganese in a proportion less than 14.8% and silicon reduce this energy, on the other hand, nitrogen is introduced only as an additional alloying element, in a proportion corresponding to an order of magnitude of residual impurity the.
  • Another shape memory alloy is described in Japanese patent application No. 63.216946.
  • one, which may be stainless contains chromium, silicon, 27.4% of manganese, and gives the alloy a recovery rate of 60%.
  • the subject of the invention is a stainless iron-based alloy having a so-called total shape memory effect consisting, after a mechanical deformation determined when cold, in recovering the initial shape by heating, characterized in that its weight composition is the next one : - 9 to 13% chromium, - 15 to 25% manganese, - 3 to 6% of silicon, - the remainder being iron and residual impurities resulting from the fusion of the materials necessary for the preparation, the proportions of the elements having to satisfy the relationship: 1.43 (% Si) + 1 (% Cr) ⁇ 17.
  • the alloy additionally contains, in its weight composition, a nitrogen content of between 0 and 0.3% by weight, the proportions of the elements having to satisfy the relationship: 1.43 (% Si) + 1 (% Cr) ⁇ 19.5 ⁇ 0.66 (% Mn) + 29 (% N).
  • the alloy additionally contains, in its weight composition, a nickel element content of between 0 and 5% by weight, the proportions of the elements must satisfy the relationship: 1.43 (% Si) + 1 (% Cr) ⁇ 19.5 ⁇ 0.66 (% Mn) +29 (% N) +2.1 (% Ni).
  • the range of chromium contents is determined to protect the alloy against corrosion, that is to make it stainless, and manganese is the main element favoring the creation of the martensitic phase ⁇ .
  • silicon reduces the energy of stacking fault in the austenitic phase ⁇ .
  • silicon in the presence of chromium improves the corrosion resistance of the alloy when its content is greater than or equal to 3%.
  • Nitrogen which it has been noted that the solubility limit in the alloy is approximately 0.3%, greatly increases the elastic limit of the alloy and thus promotes the appearance of the ⁇ phase.
  • the high solubility of nitrogen in the alloy is linked to the presence in said alloy of a relatively high manganese content.
  • Nitrogen also has the advantage of delaying the precipitation of intermetallic compounds such as the ⁇ phase, and of allowing the addition of chromium in sufficient content to give the alloy good resistance to corrosion.
  • nickel substituted for manganese in proportions of less than 5%, does not increase the stacking fault energy and improves the ductility of the alloy.
  • Nitrogen and nickel limit the creation of the weakening ⁇ phase and consequently reduce the brittleness of the alloy, while retaining its shape memory properties.
  • the invention contrary to the teaching given in Japanese patent application No. 60.249957, allows an alloy to be obtained whose chromium content is greater than 6%, the chromium content between 9 and 13% giving to the alloy a stainless character.
  • the present invention also relates to a process for the preparation of such an iron-based stainless alloy having a shape memory effect, from ingots produced by casting, characterized in that said ingots are subjected to different physical and mechanical transformation stages including: - forging dishes at a temperature between 1150 and 1250 ° C, - a correction for the elimination of surface defects, - at least one hot rolling at a temperature between 1000 and 1200 ° C with a reduction rate greater than 70%, - at least one annealing at a temperature above 900 ° C for a time between 1 and 30 minutes, after each hot rolling, - at least one cold rolling with a reduction rate of more than 50%, - And at least one annealing at a temperature between 900 and 1100 ° C for a time between 1 and 30 minutes.
  • - hot rolling is carried out at a temperature equal to 1100 ° C
  • the annealing, after each hot rolling is carried out at a temperature equal to 1000 ° C. for 20 minutes
  • - Annealing after each cold rolling is carried out at a temperature equal to 1000 ° C for 20 minutes.
  • the alloy according to the invention is a stainless iron-based alloy, called shape memory.
  • This alloy has a shape memory effect, that is to say that after mechanical deformation at room temperature, the alloy fully or partially recovers its initial shape after heating to a temperature within a determined temperature range, favoring the formation of the austenitic phase ⁇ , with a face-centered cubic crystal structure.
  • the alloy according to the invention is produced from cast ingots whose weight composition is as follows: - 22% manganese, - 12% chromium, - 5% silicon.
  • the ingots undergo according to the process of the invention, forging at 1200 ° C. into dishes of 15mm x 100mm x length.
  • the dishes are then ground to a thickness of 14mm to eliminate surface defects.
  • the plates are subjected after forging, to a hot rolling at 1100 ° C in four stages so as to obtain sheets 1.5 mm thick, then to an annealing at 1000 ° C for 20 minutes and finally to one or several cold rolling, respectively followed by annealing at 1000 ° C for 20 minutes.
  • Knowing the temperature of the embrittling phases has made it possible to determine a suitable casting treatment cycle so as to obtain a malleable alloy.
  • the alloy according to the invention does not contain phase ⁇ .
  • Phase ⁇ is generated in the alloy by mechanical deformation of it at room temperature.
  • the ambient temperature is included in the temperature range in which the phase ⁇ can be created.
  • FIG. 1 represents a reversion curve for the phase ⁇ .
  • the reversion of the phase ⁇ is carried out in the interval [A s , A f ] in which A s is the temperature of the beginning of the martensite reversion and A f is the temperature of the end of the martensite reversion.
  • This interval is little different from 100 ° C with A s very little different from 100 ° C and A f very little different from 200 ° C.
  • M s the temperature at the start of the martensitic transformation, M s, is very little different from 90 ° C, and the temperature at the end of the martensitic transformation M f is below ambient temperature. After a few cycles, M s decreases (M s very little different from 50 ° C).
  • test specimens produced for highlighting deformations due to the shape memory effect have the following dimensions: 1.5mm x 8mm x 95mm
  • Deformation in bending by bending on a cylinder or in tension is carried out on each test piece, and the test piece after deformation is placed in ovens whose temperature varies from 50 ° C to 50 ° C between room temperature and 500 ° C .
  • the deformation is calculated after returning to ambient temperature, and it is found that the recovery of the form is carried out between 50 and 250 ° C.
  • test piece is subjected to a series of deformation-rise cycles in temperature.
  • the test piece is deformed at room temperature with a constant deformation temperature, then heated to 1000 ° C and cooled in air.
  • FIG. 2 represents a curve of the rates of deformation and shape recovery over several successive cycles (R) and a curve of the rates of deformation and shape recovery accumulated over several cycles (RC).
  • the two recovery rates are close to 70%.
  • the form recovery rate remains constant and equal to approximately 95%, while the cumulative form recovery rate decreases.
  • the recovery rate of the test piece being 94%, we can consider that the memory effect is total.
  • the recovery rate of 94% is obtained with initial deformation rates of between 0.7% and 3.6%, and the recovery of the initial shape takes place essentially between room temperature and 300 ° C.
  • the ingots 10, 11 and 12 are given as an indication and show that the memory effect is improved when the point M s is located just below ambient temperature.
  • the limit value of the manganese content ie 25% by weight in the weight composition is defined by the fact that above this value, with at least 9% chromium and / or nickel, it is difficult to obtain a shape memory effect, large enough to be industrially exploitable.
  • the ingot 13 also given as an indication shows that an improvement in the effect of memory is obtained by the addition of silicon. This effect is materialized both on the recovery rate, after three cycles of form recovery (R), and after a recovery of cumulative form over ten cycles (RC).
  • Ingots 3 and 4 show that nickel can be added in small quantities, 2 and 4% to improve the ductility of the alloy without degrading the properties of the memory effect.
  • Ingot 5 shows the positive effect of nitrogen on shape recovery in the case of a shape recovery cycle (96%) and in the case of several cumulative shape recovery cycles (45%).
  • the production process according to the invention makes it possible to obtain a malleable alloy which has a total shape memory effect for a deformation of approximately 3% per cycle, as indicated in the column Def. of Table II and which can be used industrially.
  • the shape memory alloy thus produced can be produced for the production of products such as sheets, wires or profiles used in particular in industrial applications such as tube fittings, sleeves, clamping rings or collars .

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Heat Treatment Of Steel (AREA)
  • Metal Extraction Processes (AREA)
  • Forging (AREA)
  • Materials For Medical Uses (AREA)
  • Coating With Molten Metal (AREA)
  • Resistance Heating (AREA)
  • Conductive Materials (AREA)
EP90403251A 1989-11-22 1990-11-16 Rostfreie Formgedächtnislegierung und Verfahren zu ihrer Herstellung Expired - Lifetime EP0430754B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT90403251T ATE101878T1 (de) 1989-11-22 1990-11-16 Rostfreie formgedaechtnislegierung und verfahren zu ihrer herstellung.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8915341 1989-11-22
FR8915341A FR2654748B1 (fr) 1989-11-22 1989-11-22 Alliage inoxydable a memoire de forme et procede d'elaboration d'un tel alliage.

Publications (2)

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EP0430754A1 true EP0430754A1 (de) 1991-06-05
EP0430754B1 EP0430754B1 (de) 1994-02-23

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Country Status (8)

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US (1) US5173131A (de)
EP (1) EP0430754B1 (de)
AT (1) ATE101878T1 (de)
CA (1) CA2030501C (de)
DE (1) DE69006830T2 (de)
DK (1) DK0430754T3 (de)
ES (1) ES2051487T3 (de)
FR (1) FR2654748B1 (de)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2194154A1 (de) * 2008-12-04 2010-06-09 Daido Tokushuko Kabushiki Kaisha Zweiwege Formwiederherstellungslegierung
CN110983152A (zh) * 2019-12-27 2020-04-10 燕山大学 一种Fe-Mn-Si-Cr-Ni基形状记忆合金及其制备方法

Families Citing this family (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1997003215A1 (en) * 1995-07-11 1997-01-30 Kari Martti Ullakko Iron-based shape memory and vibration damping alloys containing nitrogen
FI982407A0 (fi) 1998-03-03 1998-11-06 Adaptamat Tech Oy Toimielimet ja laitteet
US6149742A (en) * 1998-05-26 2000-11-21 Lockheed Martin Corporation Process for conditioning shape memory alloys
RU2169205C1 (ru) * 2000-03-27 2001-06-20 Открытое акционерное общество "КАМАЗ" Нержавеющая сталь
CN1128244C (zh) * 2000-10-26 2003-11-19 艾默生电气（中国）投资有限公司 含Cr和N铁锰硅基形状记忆合金及其训练方法
JP3950963B2 (ja) * 2002-12-18 2007-08-01 独立行政法人物質・材料研究機構 ＮｂＣ添加Ｆｅ−Ｍｎ−Ｓｉ系形状記憶合金の加工熱処理法
DE602006017881D1 (de) * 2005-11-09 2010-12-09 Japan Science & Tech Agency Auf eisen basierende legierung mit formgedächtniseigenschaft und superelastizität und herstellungsverfahren dafür
US20080235920A1 (en) * 2007-03-29 2008-10-02 Dimart, Llc Beach clamp
CN108486488A (zh) * 2018-03-22 2018-09-04 南京工业大学 一种低Mn含量的Fe基形状记忆合金及制备方法
DE102019109719A1 (de) * 2019-04-12 2020-10-15 Thyssenkrupp Steel Europe Ag Verfahren zur Herstellung eines Formgedächtnis-Bauteils mit Umwandlungsfunktionalität

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB439045A (en) * 1934-05-28 1935-11-28 Deutsche Edelstahlwerke Ag An improved chromium manganese steel alloy
DE692327C (de) * 1934-05-24 1940-06-17 Edelstahlwerke Akt Ges Deutsch Chrom-Mangan-Silizium-Stahl
DE692732C (de) * 1934-05-24 1940-06-26 Edelstahlwerke Akt Ges Deutsch Stahllegierung fuer Gegenstaende, die eine hohe Zunderbestaendigkeit besitzen muessen
DE864405C (de) * 1935-04-09 1953-01-26 Stahlwerke Roechling Buderus A Eisenlegierung fuer Zwecke, fuer welche bislang Silber oder Neusilber verwendet wird
EP0176272A1 (de) * 1984-09-07 1986-04-02 Nippon Steel Corporation Formgedächtnislegierung und Verfahren zu ihrer Herstellung
JPS63216946A (ja) * 1987-03-04 1988-09-09 Sumitomo Metal Ind Ltd 形状記憶合金
EP0336157A1 (de) * 1988-04-05 1989-10-11 Nkk Corporation Formgedächtnislegierung auf Eisenbasis mit vortrefflichen Formgedächtniseigenschaften und sehr guter Korrosionsbeständigkeit

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5032195A (en) * 1989-03-02 1991-07-16 Korea Institute Of Science And Technology FE-base shape memory alloy

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE692327C (de) * 1934-05-24 1940-06-17 Edelstahlwerke Akt Ges Deutsch Chrom-Mangan-Silizium-Stahl
DE692732C (de) * 1934-05-24 1940-06-26 Edelstahlwerke Akt Ges Deutsch Stahllegierung fuer Gegenstaende, die eine hohe Zunderbestaendigkeit besitzen muessen
GB439045A (en) * 1934-05-28 1935-11-28 Deutsche Edelstahlwerke Ag An improved chromium manganese steel alloy
DE864405C (de) * 1935-04-09 1953-01-26 Stahlwerke Roechling Buderus A Eisenlegierung fuer Zwecke, fuer welche bislang Silber oder Neusilber verwendet wird
EP0176272A1 (de) * 1984-09-07 1986-04-02 Nippon Steel Corporation Formgedächtnislegierung und Verfahren zu ihrer Herstellung
JPS63216946A (ja) * 1987-03-04 1988-09-09 Sumitomo Metal Ind Ltd 形状記憶合金
EP0336157A1 (de) * 1988-04-05 1989-10-11 Nkk Corporation Formgedächtnislegierung auf Eisenbasis mit vortrefflichen Formgedächtniseigenschaften und sehr guter Korrosionsbeständigkeit

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2194154A1 (de) * 2008-12-04 2010-06-09 Daido Tokushuko Kabushiki Kaisha Zweiwege Formwiederherstellungslegierung
CN110983152A (zh) * 2019-12-27 2020-04-10 燕山大学 一种Fe-Mn-Si-Cr-Ni基形状记忆合金及其制备方法

Also Published As

Publication number Publication date
ES2051487T3 (es) 1994-06-16
DE69006830T2 (de) 1994-09-29
FR2654748B1 (fr) 1992-03-20
FR2654748A1 (fr) 1991-05-24
DK0430754T3 (da) 1994-03-28
DE69006830D1 (de) 1994-03-31
ATE101878T1 (de) 1994-03-15
CA2030501C (fr) 1999-12-28
CA2030501A1 (fr) 1991-05-23
EP0430754B1 (de) 1994-02-23
US5173131A (en) 1992-12-22

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