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EP1563110A1 - Weldable steel building component and method for making same - Google Patents

Weldable steel building component and method for making same

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Publication number
EP1563110A1
EP1563110A1 EP03789465A EP03789465A EP1563110A1 EP 1563110 A1 EP1563110 A1 EP 1563110A1 EP 03789465 A EP03789465 A EP 03789465A EP 03789465 A EP03789465 A EP 03789465A EP 1563110 A1 EP1563110 A1 EP 1563110A1
Authority
EP
European Patent Office
Prior art keywords
less
steel
equal
contents
temperature
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.)
Granted
Application number
EP03789465A
Other languages
German (de)
French (fr)
Other versions
EP1563110B1 (en
Inventor
Jean Beguinot
Jean-Georges Brisson
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.)
Industeel Creusot
Original Assignee
Industeel Creusot
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Filing date
Publication date
Application filed by Industeel Creusot filed Critical Industeel Creusot
Priority to SI200330933T priority Critical patent/SI1563110T1/en
Publication of EP1563110A1 publication Critical patent/EP1563110A1/en
Application granted granted Critical
Publication of EP1563110B1 publication Critical patent/EP1563110B1/en
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
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/18—Hardening; Quenching with or without subsequent tempering
    • 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
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/54—Ferrous alloys, e.g. steel alloys containing chromium with nickel with boron
    • 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
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/46—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for sheet metals

Definitions

  • the present invention relates to weldable structural steel parts and their method of manufacture.
  • the structural steels must have a certain level of mechanical characteristics to be adapted to the use that one wishes to make, and they must in particular have a high hardness.
  • steels are used that can be quenched, that is to say for which one can obtain a martensitic or bainitic structure when cooled sufficiently quickly and efficiently.
  • a bainitic critical velocity is thus defined, beyond which a bainitic, martensitic or martensite-bainitic structure is obtained, as a function of the cooling rate reached.
  • the quenchability of these steels depends on their content of quenching elements. In general, the more these elements are present in large quantities, the lower the bainitic critical speed is low.
  • the welding zone also known as the Zone Affectée Thermiquement or ZAT
  • ZAT Zone Affectée Thermiquement
  • C eq (% C +% Mn / 6 + (% Cr + ( % Mo +% W / 2) +% V) / 5 +% Ni / 15)
  • the lower its equivalent carbon the more the steel is weldable. It is therefore understandable that the improvement of the quenchability, which goes through a higher content of quenching elements, is at the expense of weldability.
  • micro-alloyed boron grades were then developed, taking advantage of the fact that, in particular, the quenching efficiency of this element decreases when the austenitization temperature increases.
  • the ZAT is less soaking than it would be in a grade of the same quenchability without boron, and it can thus reduce hardenability and hardness of this ZAT.
  • the object of the present invention is to overcome this drawback by proposing a structural steel having improved quenchability without reducing its weldability.
  • the invention firstly relates to a piece of weldable structural steel whose chemical composition comprises, by weight:
  • N ⁇ 0.025% optionally at least one element selected from V, Nb, Ta, S and Ca, in contents of less than 0.3%, and / or among Ti and Zr in contents of less than or equal to 0.5%, the rest being iron and impurities resulting from the elaboration, the contents of aluminum, boron, titanium and nitrogen, expressed in thousandths of a%, of said composition further satisfying the following relationship:
  • the silicon and aluminum contents of the composition furthermore satisfying the following conditions: if C> 0.145, then Si + Al ⁇ 0.95 and whose structure is bainitic, martensitic or martensite-bainitic and furthermore comprises from 3 to 20 % residual austenite, preferably 5 to 20% residual austenite.
  • the chemical composition of the steel of the piece according to the invention also satisfies the relationship:
  • the chemical composition the steel of the piece according to the invention furthermore satisfies the relationship:% Cr + 3 (% Mo +% W / 2) ⁇ 1, 8, preferably> 2.0.
  • the subject of the invention is also a method for manufacturing a weldable steel part according to the invention, characterized in that:
  • the room is austenitized by heating at a temperature between Ac 3 and 1000 ° C., preferably between Ac 3 and 950 ° C., and then it cools to a temperature of 200 ° C or lower so that in the center of the room the cooling rate between 800 ° C and 500 ° C is greater than or equal to the bainitic critical speed, makes an income at a temperature less than or equal to Ac,
  • the cooling rate may be slowed down, in particular to promote a phenomenon of self-income and the retention of 3 % to 20% residual austenite.
  • the cooling rate between 500 ° C and a temperature less than or equal to 200 ° C will then be between 0.07 ° C / s and 5 ° C / s; more preferably between 0.15 ° C / s and 2.5 ° C / s.
  • an income is made at a temperature below 300 ° C for a time less than 10 hours, after cooling to a temperature of less than or equal to 200 ° C.
  • the process according to the invention does not comprise any income after the cooling of the part to a temperature of less than or equal to 200 ° C.
  • the part subjected to the process according to the invention is a sheet of thickness between 3 and 150 mm.
  • the third subject of the invention is a process for manufacturing a weldable steel sheet according to the invention, whose thickness is between 3 mm and 150 mm, and which is characterized in that a quenching of said sheet, the cooling rate V R at the core of the sheet between 800 ° C and
  • the improvement of the quenchability makes it possible to cool the pieces more slowly, while guaranteeing an essentially bainitic, martensitic or martensite-bainitic structure.
  • This slower cooling combined with a sufficient content of carburigenic elements then allows the precipitation of fine carbides of chromium, molybdenum and / or tungsten by a so-called self-tempering phenomenon.
  • This phenomenon of self-income is, moreover, greatly favored by the slowing down of the cooling rate below 500 ° C.
  • this slowdown also favors the retention of austenite, preferably in a proportion of between 3% and 20%.
  • the manufacturing process is thus simplified while improving the mechanical characteristics of the steel, which no longer undergoes significant softening due to high temperature tempering, as is customary. It remains however possible to make such an income at usual temperatures, that is to say less than or equal to A.
  • the steel of the piece according to the invention contains, by weight: - more than 0.10% o carbon, to allow to obtain sufficient hardness, but less than 0.22% to obtain excellent weldability, good cutability, good bendability and satisfactory toughness;
  • the sum% Cr + 3 (% Mo +% W / 2) is preferably greater than 1.8%, and particularly preferably greater than 2.0%, in order to possibly limit the income to 300 ° C, or even delete it;
  • V, Nb, Ta, S and Ca optionally at least one element selected from V, Nb, Ta, S and Ca, in contents of less than 0.3% ", and / or among Ti and Zr in contents of less than or equal to 0.5%" and / or or aluminum at less than 0.9%.
  • V, Nb, Ta, Ti, Zr makes it possible to obtain precipitation hardening without excessively deteriorating the weldability.
  • Titanium, zirconium and aluminum can be used to fix the nitrogen present in the steel which protects the boron, titanium can be replaced in whole or in part by a double weight of Zr. Sulfur and calcium improve the machinability of the grade.
  • Aluminum is limited to 0.9% to avoid any clogging of the pipes during casting.
  • a steel according to the invention is produced, it is cast in the form of a half product which is then shaped by hot plastic deformation, for example by rolling or forging.
  • the part thus obtained is then austenitized by heating at a temperature above Ac 3 but below 1000 ° C., and preferably below 950 ° C., and then cooled to room temperature so that, at the heart of the piece, the cooling rate between 800 ° C and 500 ° C is greater than the bainitic critical speed.
  • the austenitization temperature is limited to 1000 ° C., since beyond this, the quenching effect of the boron becomes too weak.
  • the part is then optionally subjected to a conventional feed at a temperature less than or equal to A ⁇ ,, but it is preferred to limit the temperature to 300 ° C, or even to eliminate this step.
  • the absence of income can be, possibly, compensated by a phenomenon of self-income.
  • This is particularly favored by allowing a cooling rate at low temperature (that is to say below about 500 ° C) preferably between 0.07 s and 5 s; more preferably between 0.15 ° C / s and 2.5 ° C / s.
  • a cooling rate at low temperature that is to say below about 500 ° C
  • V1 From this velocity V1 is deduced the maximum sheet thicknesses that can be obtained while maintaining a substantially martensitic core structure and also comprising at least 3% residual austenite. These thicknesses were determined in the case of air quenching (A), oil
  • the improvement of the quenchability thus makes it possible to manufacture parts having a core hardened structure under less stringent cooling conditions than those of the prior art and / or in greater maximum thicknesses.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Heat Treatment Of Steel (AREA)
  • Heat Treatment Of Articles (AREA)
  • Heat Treatment Of Sheet Steel (AREA)

Abstract

The invention concerns weldable steel building components whereof the chemical composition comprises, by weight: 0.10 % ≤ C ≤ 0,22 %, 0.50 % ≤ Si ≤ 1.50 %, AI ≤ 0.9 %, 0 % ≤ Mn ≤ 3 %, 0 % ≤ Ni ≤ 5 %, 0 % ≤ Cr ≤ 4 %, 0 % ≤ Cu ≤ 1 %, 0 % ≤ Mo + W/2 ≤ 1.5 %, 0.0005 % ≤ B < 0.010 %, N ≤ 0.025 %, optionally at least one element selected among V, Nb, Ta, S et Ca, in contents less than 0.3 %, and/or among Ti and Zr in contents not more than 0.5 %, the rest being iron and impurities resulting from preparation, the aluminium, boron, titanium and nitrogen contents, expressed in thousandths of %, of said composition further satisfying the following relationship: B ≤ 1/3 x K+ 0.5, (1) with K = Min (l*; J*), I* = Max (0; I) and J* = Max (0; J), I = Min(N; N-0.29(Ti-5)), J = Min {N; 0.5 (N 0.52 AI + ∑j(N 0.52 AI)2 + 283)}, the silicon and aluminium contents of the composition additionally verifying the following conditions: if C > 0.145, then Si + AI < 0.95 and whereof the structure is bainitic, martensitic or martensitic/bainitic and further comprises 3 to 20 % of residual austenite.

Description

PIECE D'ACIER DE CONSTRUCTION SOUDABLE ET PROCEDE DE SOLDERABLE CONSTRUCTION STEEL PIECE AND METHOD OF
FABRICATIONMANUFACTURING
La présente invention concerne des pièces d'acier de construction soudables et leur procédé de fabrication.The present invention relates to weldable structural steel parts and their method of manufacture.
Les aciers de construction doivent présenter un certain niveau de caractéristiques mécaniques pour être adaptés à l'usage que l'on souhaite en faire, et ils doivent en particulier présenter une dureté élevée. Pour cela, on utilise des aciers susceptibles d'être trempés, c'est à dire pour lesquels on peut obtenir une structure martensitique ou bainitique lorsqu'on les refroidit de façon suffisamment rapide et efficace. On définit ainsi une vitesse critique bainitique, au-delà de laquelle on obtient une structure bainitique, martensitique ou martensito-bainitique, en fonction de la vitesse de refroidissement atteinte.The structural steels must have a certain level of mechanical characteristics to be adapted to the use that one wishes to make, and they must in particular have a high hardness. For this, steels are used that can be quenched, that is to say for which one can obtain a martensitic or bainitic structure when cooled sufficiently quickly and efficiently. A bainitic critical velocity is thus defined, beyond which a bainitic, martensitic or martensite-bainitic structure is obtained, as a function of the cooling rate reached.
L'aptitude à la trempe de ces aciers dépend de leur teneur en éléments trempants. En règle générale, plus ces éléments sont présents en grande quantité, plus la vitesse critique bainitique est faible.The quenchability of these steels depends on their content of quenching elements. In general, the more these elements are present in large quantities, the lower the bainitic critical speed is low.
En dehors de leurs caractéristiques mécaniques, les aciers de construction doivent également présenter une bonne soudabilité. Or, lorsqu'on soude une pièce d'acier, la zone de soudage, encore appelée Zone Affectée Thermiquement ou ZAT, est soumise à une très haute température pendant un temps bref, puis à un refroidissement brutal qui vont conférer à cette zone une dureté élevée qui peut conduire à des fissurations et restreindre ainsi la soudabilité de l'acier.Apart from their mechanical characteristics, structural steels must also have good weldability. However, when welding a piece of steel, the welding zone, also known as the Zone Affectée Thermiquement or ZAT, is subjected to a very high temperature for a short time, then to a sudden cooling that will give this area a hardness which can lead to cracking and thus restrict the weldability of the steel.
D'une façon classique, la soudabilité d'un acier peut être estimée à l'aide du calcul de son "carbone équivalent" donné par la formule suivante : Céq = (%C + %Mn/6 + (%Cr + (%Mo + %W/2) + %V)/5 + %Ni/15) En première approximation, plus son carbone équivalent est faible plus l'acier est soudable. On comprend donc que l'amélioration de la trempabilité, qui passe par une plus grande teneur en éléments trempants, se fait au détriment de la soudabilité.In a conventional way, the weldability of a steel can be estimated by calculating its "equivalent carbon" given by the following formula: C eq = (% C +% Mn / 6 + (% Cr + ( % Mo +% W / 2) +% V) / 5 +% Ni / 15) As a first approximation, the lower its equivalent carbon, the more the steel is weldable. It is therefore understandable that the improvement of the quenchability, which goes through a higher content of quenching elements, is at the expense of weldability.
Pour améliorer la trempabilité de ces aciers sans dégrader leur soudabilité, on a alors développé des nuances micro-alliées au bore, en profitant de ce que, notamment, l'efficacité trempante de cet élément diminue lorsque la température d'austénitisation augmente. Ainsi, la ZAT est moins trempante qu'elle ne le serait dans une nuance de même trempabilité sans bore, et l'on peut ainsi diminuer trempabilité et dureté de cette ZAT.To improve the hardenability of these steels without degrading their weldability, micro-alloyed boron grades were then developed, taking advantage of the fact that, in particular, the quenching efficiency of this element decreases when the austenitization temperature increases. Thus, the ZAT is less soaking than it would be in a grade of the same quenchability without boron, and it can thus reduce hardenability and hardness of this ZAT.
Toutefois, comme l'effet trempant du bore dans la partie non soudée de l'acier tend à saturer pour des teneurs efficaces de 30 à 50 ppm, une amélioration supplémentaire de la trempabilité de l'acier ne peut alors se faire qu'en ajoutant des éléments trempants dont l'efficacité ne dépend pas de la température d'austénitisation, ce qui pénalise automatiquement la soudabilité de ces aciers. De même, l'amélioration de la soudabilité passe par la diminution des teneurs en éléments trempants, qui réduit automatiquement la trempabilité.However, since the quenching effect of boron in the unwelded part of the steel tends to saturate for effective levels of 30 to 50 ppm, a further improvement in the quenchability of the steel can then be achieved only by adding quenching elements whose effectiveness does not depend on the austenitization temperature, which automatically penalizes the weldability of these steels. In the same way, the improvement of the weldability goes through the reduction of the contents in elements quenching, which reduces automatically quenchability.
Le but de la présente invention est de remédier à cet inconvénient en proposant un acier de construction ayant une trempabilité améliorée sans diminution de sa soudabilité. A cet effet, l'invention a pour premier objet une pièce d'acier de construction soudable dont la composition chimique comprend, en poids :The object of the present invention is to overcome this drawback by proposing a structural steel having improved quenchability without reducing its weldability. For this purpose, the invention firstly relates to a piece of weldable structural steel whose chemical composition comprises, by weight:
0,10% < C < 0,22% 0,50% < Si < 1 ,50% •AI < 0,9% 0% < Mn < 3%0.10% <C <0.22% 0.50% <If <1, 50% • AI <0.9% 0% <Mn <3%
0% < Ni < 5%0% <Ni <5%
0% < Cr < 4%0% <Cr <4%
0% < Cu < 1 %0% <Cu <1%
0% < Mo + W/2 < 1 ,5% 0,0005% < B < 0,010%0% <Mo + W / 2 <1, 5% 0.0005% <B <0.010%
N < 0,025% éventuellement au moins un élément pris parmi V, Nb, Ta, S et Ca, en des teneurs inférieures à 0,3%, et/ou parmi Ti et Zr en des teneurs inférieures ou égales à 0,5%, le reste étant du fer et des impuretés résultant de l'élaboration, les teneurs en aluminium, en bore, en titane et en azote, exprimées en millièmes de %, de ladite composition satisfaisant en outre la relation suivante :N <0.025% optionally at least one element selected from V, Nb, Ta, S and Ca, in contents of less than 0.3%, and / or among Ti and Zr in contents of less than or equal to 0.5%, the rest being iron and impurities resulting from the elaboration, the contents of aluminum, boron, titanium and nitrogen, expressed in thousandths of a%, of said composition further satisfying the following relationship:
B > - χ K + 0,5 , (1 )B> - χ K + 0.5, (1)
avec K = Min (I* ; J*) I* = Max (0 ; I) et J* = Max (0 ; J)with K = Min (I *; J *) I * = Max (0; I) and J * = Max (0; J)
1 = Min(N ; N-0,29 (Ti-5))1 = Min (N, N-0.29 (Ti-5))
les teneurs en silicium et en aluminium de la composition vérifiant en outre les conditions suivantes : si C > 0,145, alors Si + AI < 0,95 et dont la structure est bainitique, martensitique ou martensito-bainitique et comprend en outre de 3 à 20% d'austénite résiduelle, de préférence de 5 à 20% d'austénite résiduelle. the silicon and aluminum contents of the composition furthermore satisfying the following conditions: if C> 0.145, then Si + Al <0.95 and whose structure is bainitic, martensitic or martensite-bainitic and furthermore comprises from 3 to 20 % residual austenite, preferably 5 to 20% residual austenite.
Dans un mode de réalisation préféré, la composition chimique de l'acier de la pièce selon l'invention satisfait en outre la relation :In a preferred embodiment, the chemical composition of the steel of the piece according to the invention also satisfies the relationship:
1 ,1 %Mn + 0,7%Ni+ 0,6%Cr + 1 ,5(%Mo + %W/2) > 1 , de préférence > 2 (2) Dans un autre mode de réalisation préféré, la composition chimique de l'acier de la pièce selon l'invention satisfait en outre la relation : %Cr + 3(%Mo + %W/2) ≥ 1 ,8, de préférence > 2,0. L'invention a également pour deuxième objet un procédé de fabrication d'une pièce en acier soudable selon l'invention, caractérisé en ce que :1, 1% Mn + 0.7% Ni + 0.6% Cr + 1.5 (% Mo +% W / 2)> 1, preferably> 2 (2) In another preferred embodiment, the chemical composition the steel of the piece according to the invention furthermore satisfies the relationship:% Cr + 3 (% Mo +% W / 2) ≥ 1, 8, preferably> 2.0. The subject of the invention is also a method for manufacturing a weldable steel part according to the invention, characterized in that:
- on austénitise la pièce par chauffage à une température comprise entre Ac3 et 1 000°C, de préférence comprise entre Ac3 et 950°C, puis on la refroidit jusqu'à une température inférieure ou égale à 200°C de telle sorte que, au cœur de la pièce, la vitesse de refroidissement entre 800°C et 500°C soit supérieure ou égale à la vitesse critique bainitique, - éventuellement, on effectue un revenu à une température inférieure ou égale à Ac,the room is austenitized by heating at a temperature between Ac 3 and 1000 ° C., preferably between Ac 3 and 950 ° C., and then it cools to a temperature of 200 ° C or lower so that in the center of the room the cooling rate between 800 ° C and 500 ° C is greater than or equal to the bainitic critical speed, makes an income at a temperature less than or equal to Ac,
Entre 500°C environ et l'ambiante et notamment entre 500°C et une température inférieure ou égale à 200°C, la vitesse de refroidissement peut être éventuellement ralentie, notamment pour favoriser un phénomène d'auto-revenu et la rétention de 3% à 20% d'austénite résiduelle. Préférentiellement, la vitesse de refroidissement entre 500°C et une température inférieure ou égale à 200°C sera alors comprise entre 0,07°C/s et 5°C/s ; plus préférentiellement entre 0,15°C/s et 2,5°C/s.Between about 500 ° C. and ambient temperature and in particular between 500 ° C. and a temperature of less than or equal to 200 ° C., the cooling rate may be slowed down, in particular to promote a phenomenon of self-income and the retention of 3 % to 20% residual austenite. Preferably, the cooling rate between 500 ° C and a temperature less than or equal to 200 ° C will then be between 0.07 ° C / s and 5 ° C / s; more preferably between 0.15 ° C / s and 2.5 ° C / s.
Dans un mode de réalisation préféré, on effectue un revenu à une température inférieure à 300°C pendant un temps inférieur à 10 heures, à l'issue du refroidissement jusqu'à une température inférieure ou égale à 200°C.In a preferred embodiment, an income is made at a temperature below 300 ° C for a time less than 10 hours, after cooling to a temperature of less than or equal to 200 ° C.
Dans un autre mode de réalisation préféré, le procédé selon l'invention ne comprend pas de revenu à l'issue du refroidissement de la pièce jusqu'à une température inférieure ou égale à 200°C. Dans un autre mode de réalisation préféré, la pièce soumise au procédé selon l'invention est une tôle d'épaisseur comprise entre 3 et 150 mm.In another preferred embodiment, the process according to the invention does not comprise any income after the cooling of the part to a temperature of less than or equal to 200 ° C. In another preferred embodiment, the part subjected to the process according to the invention is a sheet of thickness between 3 and 150 mm.
L'invention a pour troisième objet un procédé de fabrication d'une tôle en acier soudable selon l'invention, dont l'épaisseur est comprise entre 3 mm et 150 mm, et qui est caractérisé en ce qu'on réalise une trempe de ladite tôle, la vitesse de refroidissement VR au coeur de la tôle entre 800°C etThe third subject of the invention is a process for manufacturing a weldable steel sheet according to the invention, whose thickness is between 3 mm and 150 mm, and which is characterized in that a quenching of said sheet, the cooling rate V R at the core of the sheet between 800 ° C and
500°C, exprimée en °C/heure, et la composition de l'acier étant telles que :500 ° C, expressed in ° C / hour, and the composition of the steel being such that:
1 ,1 %Mn + 0,7%Ni+ 0,6%Cr + 1 ,5(%Mo + %W/2) + log VR > 5,5, et de préférence > 6, log étant le logarithme décimal. La présente invention est basée sur le constat nouveau que l'ajout de silicium dans les teneurs indiquées ci-dessus permet d'accroître l'effet trempant du bore de 30 à 50%. Cette synergie intervient sans augmentation de la quantité de bore ajoutée, alors que le silicium ne présente pas d'effet trempant notable en l'absence de bore.1, 1% Mn + 0.7% Ni + 0.6% Cr + 1, 5 (% Mo +% W / 2) + log V R > 5.5, and preferably> 6, log being the logarithmic decimal. The present invention is based on the new observation that the addition of silicon in the contents indicated above makes it possible to increase the effect boron quenching from 30 to 50%. This synergy occurs without increasing the amount of boron added, while the silicon does not have a significant soaking effect in the absence of boron.
D'autre part, l'ajout de silicium n'affecte pas la propriété du bore de voir sa trempabilité se réduire puis s'annuler avec des températures d'austénitisation croissantes, comme c'est le cas dans la ZAT.On the other hand, the addition of silicon does not affect the boron property to see its hardenability reduce and then cancel with increasing austenitization temperatures, as is the case in the ZAT.
On voit donc que l'utilisation de silicium en présence de bore permet d'augmenter encore la trempabilité de la pièce sans altérer sa soudabilité.It can therefore be seen that the use of silicon in the presence of boron makes it possible to further increase the quenchability of the part without impairing its weldability.
Par ailleurs, on a également découvert que, grâce à l'amélioration de la trempabilité de ces nuances d'aciers, et en garantissant une teneur minimale en éléments carburigènes que sont, notamment, le chrome, le molybdène et le tungstène, on pouvait fabriquer ces aciers en n'effectuant qu'un revenu à faible température, voire même en le supprimant.Furthermore, it has also been discovered that, by improving the hardenability of these grades of steel, and by guaranteeing a minimum content of carburizing elements that are, in particular, chromium, molybdenum and tungsten, it is possible to manufacture these steels by only making a low-temperature income, or even by suppressing it.
En effet, l'amélioration de la trempabilité permet de refroidir les pièces plus lentement, tout en garantissant une structure essentiellement bainitique, martensitique ou martensito-bainitique. Ce refroidissement plus lent combiné à une teneur suffisante en éléments carburigènes permet alors la précipitation de fins carbures de chrome, de molybdène et/ou de tungstène par un phénomène dit d'auto-revenu. Ce phénomène d'auto-revenu est , de plus, grandement favorisé par le ralentissement de la vitesse de refroidissement en dessous de 500°C. De même ce ralentissement favorise aussi la rétention d'austénite, préférentiellement dans une proportion comprise entre 3% et 20%. On simplifie donc le procédé de fabrication, tout en améliorant les caractéristiques mécaniques de l'acier, qui ne subit plus d'adoucissement important dû à un revenu à haute température, comme on le pratique habituellement. Il reste cependant possible d'effectuer un tel revenu aux températures usuelles, c'est à dire inférieures ou égales à A .Indeed, the improvement of the quenchability makes it possible to cool the pieces more slowly, while guaranteeing an essentially bainitic, martensitic or martensite-bainitic structure. This slower cooling combined with a sufficient content of carburigenic elements then allows the precipitation of fine carbides of chromium, molybdenum and / or tungsten by a so-called self-tempering phenomenon. This phenomenon of self-income is, moreover, greatly favored by the slowing down of the cooling rate below 500 ° C. Similarly, this slowdown also favors the retention of austenite, preferably in a proportion of between 3% and 20%. The manufacturing process is thus simplified while improving the mechanical characteristics of the steel, which no longer undergoes significant softening due to high temperature tempering, as is customary. It remains however possible to make such an income at usual temperatures, that is to say less than or equal to A.
L'invention va maintenant être décrite plus en détail mais de façon non limitative. L'acier de la pièce selon l'invention contient, en poids : - plus de 0,10%o de carbone, pour permettre d'obtenir une dureté suffisante, mais moins de 0,22% pour obtenir une excellente soudabilité, une bonne découpabilité, une bonne aptitude au pliage et une ténacité satisfaisante ;The invention will now be described in more detail but in a nonlimiting manner. The steel of the piece according to the invention contains, by weight: - more than 0.10% o carbon, to allow to obtain sufficient hardness, but less than 0.22% to obtain excellent weldability, good cutability, good bendability and satisfactory toughness;
- plus de 0,50%, de préférence plus de 0,75%, et de façon particulièrement préférée plus de 0,85% en poids, de silicium afin d'obtenir la synergie avec le bore, mais moins de 1 ,5% en poids pour ne pas fragiliser l'acier ;more than 0.50%, preferably more than 0.75%, and particularly preferably more than 0.85% by weight, of silicon in order to obtain the synergy with boron, but less than 1, 5% by weight so as not to weaken the steel;
- plus de 0,0005%, de préférence plus de 0,001% de bore pour ajuster la trempabilité, mais moins de 0,010% en poids pour éviter une trop grande teneur en nitrures de bore néfastes pour les caractéristiques mécaniques de l'acier ;- more than 0.0005%, preferably more than 0.001% boron to adjust the quenchability, but less than 0.010% by weight to avoid too much boron nitride content harmful to the mechanical characteristics of the steel;
- moins de 0,025%, et de préférence moins de 0,015% d'azote, la teneur obtenue étant fonction du procédé d'élaboration de l'acier,less than 0.025%, and preferably less than 0.015% of nitrogen, the content obtained being a function of the process for producing the steel,
- de 0% à 3% et, de préférence de 0,3% à 1 ,8% de manganèse, de 0% à 5% et, de préférence de 0% à 2% de nickel, de 0% à 4% de chrome, de 0 à 1 % de cuivre, la somme de la teneur en molybdène et de la moitié de la teneur en tungstène étant inférieure à 1 ,50% de façon à obtenir une structure principalement bainitique, martensitique ou martensito-bainitique, le chrome, le molybdène et le tungstène ayant, de plus, l'avantage de permettre la formation de carbures favorables à la résistance mécanique et à l'usure comme indiqué précédemment ; en outre, la somme %Cr + 3(%Mo + %W/2) est de préférence supérieure à 1 ,8 %, et de façon particulièrement préférée supérieure à 2,0%, afin de pouvoir éventuellement limiter le revenu à 300°C, voire de le supprimer ;from 0% to 3% and, preferably from 0.3% to 1.8% of manganese, from 0% to 5% and, preferably from 0% to 2% of nickel, from 0% to 4% of chromium, from 0 to 1% copper, the sum of the molybdenum content and half of the tungsten content being less than 1, 50% so as to obtain a predominantly bainitic, martensitic or martensite-bainitic structure, chromium , molybdenum and tungsten having the further advantage of allowing the formation of carbides favorable to the mechanical strength and wear as previously indicated; in addition, the sum% Cr + 3 (% Mo +% W / 2) is preferably greater than 1.8%, and particularly preferably greater than 2.0%, in order to possibly limit the income to 300 ° C, or even delete it;
- éventuellement au moins un élément pris parmi V, Nb, Ta, S et Ca, en des teneurs inférieures à 0,3%», et/ou parmi Ti et Zr en des teneurs inférieures ou égales à 0,5%» et/ou de l'aluminium à une teneur inférieure à 0,9%. L'ajout de V, Nb, Ta, Ti, Zr permet d'obtenir un durcissement par précipitation sans détériorer excessivement la soudabilité. Le titane, le zirconium et l'aluminium peuvent être utilisés pour fixer l'azote présent dans l'acier ce qui protège le bore, le titane pouvant être remplacé en tout ou partie par un poids double de Zr. Le soufre et le calcium permettent d'améliorer l'usinabilité de la nuance. L'aluminium est limité à 0,9% pour éviter tout problème de bouchage des conduits lors de la coulée.- optionally at least one element selected from V, Nb, Ta, S and Ca, in contents of less than 0.3% ", and / or among Ti and Zr in contents of less than or equal to 0.5%" and / or or aluminum at less than 0.9%. The addition of V, Nb, Ta, Ti, Zr makes it possible to obtain precipitation hardening without excessively deteriorating the weldability. Titanium, zirconium and aluminum can be used to fix the nitrogen present in the steel which protects the boron, titanium can be replaced in whole or in part by a double weight of Zr. Sulfur and calcium improve the machinability of the grade. Aluminum is limited to 0.9% to avoid any clogging of the pipes during casting.
- les teneurs en aluminium, en bore, en titane et en azote, exprimées en millièmes de %, de ladite composition satisfaisant en outre la relation suivantethe contents of aluminum, boron, titanium and nitrogen, expressed in thousandths of a%, of said composition further satisfying the following relationship
B > - χ K + 0,5 , (1 )B> - χ K + 0.5, (1)
avec K = Min (I* ; J*) I* = Max (0 ; I) et J* = Max (0 ; J)with K = Min (I *; J *) I * = Max (0; I) and J * = Max (0; J)
I = Min(N ; N-0,29(Ti-5))I = Min (N, N-0.29 (Ti-5))
J = avec la condition supplémentaire que :J = with the additional condition that:
- si C > 0, 145 (et de préférence > 0,140), alors Si + Al < 0,95, et de préférence < 0,90, afin de délimiter clairement l'invention par rapport à la demande antérieure EP 0 725 156, - le reste étant du fer et des impuretés résultant de l'élaboration.if C> O, 145 (and preferably> 0.140), then Si + Al <0.95, and preferably <0.90, in order to clearly delimit the invention with respect to the previous application EP 0 725 156, the remainder being iron and impurities resulting from the preparation.
Pour fabriquer une pièce soudable, on élabore un acier conforme à l'invention, on le coule sous forme d'un demi produit qui est alors mis en forme par déformation plastique à chaud, par exemple par laminage ou par forgeage. La pièce ainsi obtenue est alors austénitisée par chauffage à une température au dessus de Ac3 mais inférieure à 1 000°C, et de préférence inférieure à 950°C, puis refroidie jusqu'à la température ambiante de telle sorte que, au cœur de la pièce, la vitesse de refroidissement entre 800°C et 500°C soit supérieure à la vitesse critique bainitique. On limite la température d'austénitisation à 1 000°C, car au-delà l'effet trempant du bore devient trop faible.To manufacture a weldable part, a steel according to the invention is produced, it is cast in the form of a half product which is then shaped by hot plastic deformation, for example by rolling or forging. The part thus obtained is then austenitized by heating at a temperature above Ac 3 but below 1000 ° C., and preferably below 950 ° C., and then cooled to room temperature so that, at the heart of the piece, the cooling rate between 800 ° C and 500 ° C is greater than the bainitic critical speed. The austenitization temperature is limited to 1000 ° C., since beyond this, the quenching effect of the boron becomes too weak.
Toutefois, il est également possible d'obtenir la pièce par refroidissement direct dans la chaude de mise en forme (sans réausténitisation) et dans ce cas, même si le chauffage avant mise en forme dépasse 1000°C tout en restant inférieur à 1300°C, le bore conservant son effet dans ce cas.However, it is also possible to obtain the room by direct cooling in the hot shaping (without réaustrénitisation) and in this case, even if the heating before formatting exceeds 1000 ° C while remaining below 1300 ° C, boron retaining its effect in this case.
Pour refroidir la pièce jusqu'à la température ambiante, depuis la température d'austénitisation, on peut tremper utiliser tous les procédés de trempes connus (air, huile, eau) dès lors que la vitesse de refroidissement reste supérieure à la vitesse critique bainitique.To cool the room to room temperature, from the austenitization temperature, it is possible to use all the known quenching processes (air, oil, water) as long as the cooling rate remains above the bainitic critical speed.
On soumet ensuite éventuellement la pièce à un revenu classique à une température inférieure ou égale à Aα,, mais on préfère limiter la température à 300°C, voire même supprimer cette étape. En effet, l'absence de revenu peut être, éventuellement, compensée par un phénomène d'auto- revenu. Celui-ci est notamment favorisé en autorisant une vitesse de refroidissement à basse température (c'est à dire en dessous de 500°C environ) préférentiellement comprise entre 0,07 s et 5 s ; plus préférentiellement entre 0,15°C/s et 2,5°C/s. A cet effet, on pourra employer tous les moyens de trempe connus, à condition de les contrôler si nécessaire. Ainsi, on pourra par exemple utiliser une trempe à l'eau si on ralentit la vitesse de refroidissement lorsque la température de la pièce descend en dessous de 500°C, ce qui pourra notamment se faire en sortant la pièce de l'eau pour finir la trempe à l'air. On obtient ainsi une pièce, et notamment une tôle, soudable constituée d'acier ayant une structure bainitique, martensitique ou martensito-bainitique à cœur, comprenant de 3 à 20% d'austénite résiduelle.The part is then optionally subjected to a conventional feed at a temperature less than or equal to Aα ,, but it is preferred to limit the temperature to 300 ° C, or even to eliminate this step. Indeed, the absence of income can be, possibly, compensated by a phenomenon of self-income. This is particularly favored by allowing a cooling rate at low temperature (that is to say below about 500 ° C) preferably between 0.07 s and 5 s; more preferably between 0.15 ° C / s and 2.5 ° C / s. For this purpose, it will be possible to use all known quenching means, provided that they are controlled if necessary. Thus, it will be possible for example to use a quenching with water if the cooling rate is slowed down when the temperature of the room falls below 500 ° C, which can be done in particular by leaving the piece of water to finish quenching it in the air. A piece is thus obtained, and in particular a weldable sheet made of steel having a bainitic, martensitic or martensitic-bainitic core structure, comprising from 3 to 20% of residual austenite.
La présence d'austénite résiduelle offre un intérêt particulier en regard du comportement de l'acier au soudage. En effet, en vue de limiter le risque de fissuration au soudage, et complémentairement à la réduction susmentionnée de la trempabilité de la ZAT, la présence d'austénite résiduelle dans le métal de base, au voisinage de la ZAT, permet de fixer une partie de l'hydrogène dissous, éventuellement introduit par l'opération de soudage, hydrogène qui non ainsi fixé, viendrait accroître le risque de fissuration. A titre d'exemple, on a fabriqué des lingotins avec les aciers 1 et 2 conformes à l'invention, et avec les aciers A et B selon l'art antérieur, dont les compositions sont, en millièmes de % en poids, et à l'exception du fer :The presence of residual austenite is of particular interest with regard to the behavior of steel during welding. Indeed, in order to limit the risk of welding cracking, and in addition to the abovementioned reduction in the hardenability of the ZAT, the presence of residual austenite in the base metal, in the vicinity of the ZAT, makes it possible to fix a part of dissolved hydrogen, possibly introduced by the welding operation, hydrogen which not so fixed, would increase the risk of cracking. By way of example, ingotins have been manufactured with steels 1 and 2 in accordance with the invention, and with steels A and B according to the prior art, the compositions of which are, in thousandths of a% by weight, and the exception of iron:
Après forgeage des lingotins, la trempabilité des quatre aciers a été évaluée par dilatométrie. On s'est ici intéressé à titre d'exemple à la trempabilité martensitique et donc à la vitesse critique martensitique V1 après une austénitisation à 900°C pendant 15 minutes.After forging the ingots, the quenchability of the four steels was evaluated by dilatometry. As an example, martensitic quenchability and therefore martensitic critical velocity V1 were investigated after austenitization at 900 ° C. for 15 minutes.
On déduit de cette vitesse V1 les épaisseurs maximales des tôles que l'on peut obtenir en conservant une structure essentiellement martensitique à cœur et comprenant également au moins 3% d'austénite résiduelle. Ces épaisseurs ont été déterminées dans le cas d'une trempe à l'air (A), à l'huileFrom this velocity V1 is deduced the maximum sheet thicknesses that can be obtained while maintaining a substantially martensitic core structure and also comprising at least 3% residual austenite. These thicknesses were determined in the case of air quenching (A), oil
(H) et à l'eau (E).(H) and water (E).
Enfin, on a estimé la soudabilité des quatre aciers en calculant leur pourcentage de carbone équivalent selon la formule :Finally, the weldability of the four steels was estimated by calculating their equivalent carbon percentage according to the formula:
Céq = (%c + %Mn/6 + (%Cr + (%Mo + %W/2) + %V)/5 + %Ni/15) Les caractéristiques des lingotins L1 et L2, conformes à l'invention, et des lingotins LA et LB, données à titre de comparaison, sont :C eq = (% c +% Mn / 6 + (% Cr + (% Mo +% W / 2) +% V) / 5 +% Ni / 15) The characteristics of the ingots L1 and L2, according to the invention , and LA and LB pellets, given for comparison, are:
On constate que les vitesses critiques martensitiques des pièces selon l'invention sont nettement inférieures aux vitesses correspondantes des lingotins en acier de l'art antérieur, ce qui signifie que leur trempabilité a été sensiblement améliorée, alors que dans le même temps leur soudabilité est inchangée. It can be seen that the martensitic critical speeds of the parts according to the invention are significantly lower than the corresponding speeds of the prior art ingots of steel, which means that their quenchability has been substantially improved, while at the same time their weldability is unchanged. .
L'amélioration de la trempabilité permet ainsi de fabriquer des pièces à structure trempée à cœur dans des conditions de refroidissement moins drastiques que celles de l'art antérieur et/ou dans des épaisseurs maximum plus fortes. The improvement of the quenchability thus makes it possible to manufacture parts having a core hardened structure under less stringent cooling conditions than those of the prior art and / or in greater maximum thicknesses.

Claims

REVENDICATIONS
1. Pièce d'acier de construction soudable, caractérisée en ce que sa composition chimique comprend, en poids : 0,10%<C<0,22%1. weldable structural steel part, characterized in that its chemical composition comprises, by weight: 0.10% <C <0.22%
0,50% < Si < 1,50%0.50% <If <1.50%
Al < 0,9%Al <0.9%
0% < Mn < 3%0% <Mn <3%
0% < Ni < 5% 0%<Cr<4%0% <Ni <5% 0% <Cr <4%
0%<Cu<1% 0% < Mo + W/2 < 1 ,5% 0,0005% <B<0,010% N < 0,025% éventuellement au moins un élément pris parmi V, Nb, Ta, S et Ca, en des teneurs inférieures à 0,3%, et/ou parmi Ti et Zr en des teneurs inférieures ou égales à 0,5%, le reste étant du fer et des impuretés résultant de l'élaboration, les teneurs en aluminium, en bore, en titane et en azote, exprimées en millièmes de %, de ladite composition satisfaisant en outre la relation suivante :0% <Cu <1% 0% <Mo + W / 2 <1, 5% 0.0005% <B <0.010% N <0.025% optionally at least one element selected from V, Nb, Ta, S and Ca, in contents of less than 0.3%, and / or among Ti and Zr in contents of less than or equal to 0.5%, the remainder being iron and impurities resulting from the elaboration, the contents of aluminum, of boron , in titanium and in nitrogen, expressed in thousandths of a%, of said composition further satisfying the following relationship:
avec K = Min (I* ; J*) l*= Max(0;l) et J* = Max (0 ; J) with K = Min (I *; J *) l * = Max (0; l) and J * = Max (0; J)
I = Min(N ; N-0,29(Ti-5))I = Min (N, N-0.29 (Ti-5))
J = les teneurs en silicium et en aluminium de la composition vérifiant en outre les conditions suivantes : si C > 0,145, alors Si + Al < 0,95 et dont la structure est bainitique, martensitique ou martensito-bainitique et comprend en outre de 3 à 20% d'austénite résiduelle.J = the silicon and aluminum contents of the composition furthermore satisfying the following conditions: if C> 0.145, then Si + Al <0.95 and whose structure is bainitic, martensitic or martensite-bainitic and further comprises from 3 to 20% of residual austenite.
2. Pièce d'acier selon la revendication 1 , caractérisée en ce que sa composition chimique satisfait en outre la relation suivante : 1 ,1 %Mn + 0,7%Ni+ 0,6%Cr + 1 ,5(%Mo + %W/2) > 1 (2)2. Steel part according to claim 1, characterized in that its chemical composition also satisfies the following relationship: 1, 1% Mn + 0.7% Ni + 0.6% Cr + 1, 5 (% Mo +% W / 2)> 1 (2)
3. Pièce d'acier selon la revendication 2, caractérisée en outre en ce que sa composition chimique satisfait la relation suivante :Steel part according to claim 2, further characterized in that its chemical composition satisfies the following relationship:
1 ,1 %Mn + 0,7%Ni+ 0,6%Cr + 1 ,5(%Mo + %W/2) > 2 (2)1, 1% Mn + 0.7% Ni + 0.6% Cr + 1, 5 (% Mo +% W / 2)> 2 (2)
4. Pièce d'acier selon l'une quelconque des revendications 1 à 3, caractérisée en ce que sa composition chimique satisfait en outre la relation suivante :4. Steel part according to any one of claims 1 to 3, characterized in that its chemical composition furthermore satisfies the following relationship:
%Cr + 3(%Mo + %W/2) > 1 ,8.% Cr + 3 (% Mo +% W / 2)> 1, 8.
5. Pièce d'acier selon la revendication 4, caractérisée en ce que sa composition chimique satisfait en outre la relation suivante : %Cr + 3(%Mo + %W/2) > 2,0.5. Steel part according to claim 4, characterized in that its chemical composition also satisfies the following relationship:% Cr + 3 (% Mo +% W / 2)> 2.0.
6. Procédé de fabrication d'une pièce en acier soudable selon l'une quelconque des revendications 1 à 5, caractérisé en ce que,6. A method of manufacturing a weldable steel part according to any one of claims 1 to 5, characterized in that,
- on austénitise la pièce par chauffage à une température comprise entre Ac3 et 1 000°C, puis on la refroidit jusqu'à une température inférieure ou égale à 200°C, de telle sorte que, au cœur de la pièce, la vitesse de refroidissement entre 800°C et 500°C soit supérieure ou égale à la vitesse critique bainitique,the room is austenitized by heating at a temperature between Ac 3 and 1000 ° C., and is then cooled to a temperature of less than or equal to 200 ° C., so that, in the center of the room, the speed between 800 ° C and 500 ° C is greater than or equal to the bainitic critical speed,
- éventuellement, on effectue un revenu à une température inférieure ou égale à Ac, optionally, an income is made at a temperature less than or equal to Ac,
7. Procédé selon la revendication 6, caractérisé en ce que, au cœur de ladite pièce, la vitesse de refroidissement entre 500°C et une température inférieure ou égale à 200°C est comprise entre 0,07°C/s et 5°C/s .7. Method according to claim 6, characterized in that, in the heart of said room, the cooling rate between 500 ° C and a temperature less than or equal to 200 ° C is between 0.07 ° C / s and 5 ° C / s.
8. Procédé selon la revendication 6 ou 7, caractérisé en ce que l'on effectue un revenu à une température inférieure à 300°C pendant un temps inférieur à 10 heures, à l'issue du refroidissement jusqu'à une température inférieure ou égale à 200°C. 8. Method according to claim 6 or 7, characterized in that one makes a tempering at a temperature below 300 ° C for a time less than 10 hours, after cooling to a temperature less than or equal to at 200 ° C.
9. Procédé selon la revendication 6 ou 7, caractérisé en ce que l'on n'effectue pas de revenu à l'issue du refroidissement jusqu'à une température inférieure ou égale à 200°C.9. The method of claim 6 or 7, characterized in that one does not make revenue after cooling to a temperature less than or equal to 200 ° C.
10. Procédé de fabrication d'une tôle en acier soudable selon l'une quelconque des revendications 1 à 5, dont l'épaisseur est comprise entre10. A method of manufacturing a weldable steel sheet according to any one of claims 1 to 5, whose thickness is between
3 mm et 150 mm, caractérisé en ce qu'on réalise une trempe de ladite tôle, la vitesse de refroidissement VR au cœur de la pièce entre 800°C et 500°C et la composition de l'acier étant telles que :3 mm and 150 mm, characterized in that a quenching of said sheet is carried out, the cooling rate V R in the center of the part between 800 ° C. and 500 ° C. and the composition of the steel being such that:
1 ,1 %Mn + 0,7%Ni+ 0,6%Cr + 1 ,5(%Mo + %W/2) + log VR > 5,5. 1, 1% Mn + 0.7% Ni + 0.6% Cr + 1.5 (% Mo +% W / 2) + log V R > 5.5.
11. Procédé de fabrication d'une tôle en acier soudable selon la revendication 10, dont l'épaisseur est comprise entre 3 mm et 150 mm, caractérisé en outre en ce qu'on réalise une trempe de ladite tôle, la vitesse de refroidissement VR au cœur de la pièce entre 800°C et 500°C et la composition de l'acier étant telles que : 1 ,1 %Mn + 0,7%Ni+ 0,6%Cr + 1 ,5(%Mo + %W/2) + log VR > 6. 11. A method of manufacturing a weldable steel sheet according to claim 10, whose thickness is between 3 mm and 150 mm, further characterized in that a quenching of said sheet is carried out, the cooling rate V R in the center of the room between 800 ° C and 500 ° C and the composition of the steel being such that: 1, 1% Mn + 0.7% Ni + 0.6% Cr + 1, 5 (% Mo +% W / 2) + log V R > 6.
EP03789465A 2002-11-19 2003-11-13 Weldable structural steel component and method for making same Expired - Lifetime EP1563110B1 (en)

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ZA200504149B (en) 2005-12-28
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US20060162825A1 (en) 2006-07-27
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BR0315696B1 (en) 2013-07-09
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DK1563110T3 (en) 2007-10-01
ATE368134T1 (en) 2007-08-15

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