EP3274483A1 - Parts with a bainitic structure having high strength properties and manufacturing process - Google Patents

Abstract

The subject of the invention is a part, the composition of which comprises, the contents being expressed as percentages by weight, 0.10 < C < 0.30, 1.6 < Mn < 2.1, 0.5 < Cr ≤ 1.7, 0.5 < Si < 1.0, 0.065 < Nb < 0.15, 0.0010 < B < 0.0050, 0.0010 < N < 0.0130, 0 < Al < 0.060, 0 < Mo < 1.00, 0 < Ni < 1.0, 0.01 < Ti < 0.07, 0 < V < 0.3, 0 < P < 0.050, 0.01 < S < 0.1, 0 < Cu < 0.5, 0 < Sn < 0.1, the remainder of the composition consisting of iron and inevitable impurities resulting from the smelting, the microstructure consisting, in surface proportions, of 100% to 70% bainite, of less than 30% residual austenite and of less than 5% ferrite, and a process for the manufacture thereof.

Description

 PARTS WITH A BAINITIQUE STRUCTURE HAVING HIGH RESISTANCE PROPERTIES AND METHOD OF MANUFACTURE

^The present invention covers a parts manufacturing high strength properties while being machineable, obtained from steels simultaneously having good hot ductility for performing hot forming operations and such that n hardenability It is not useful to perform tempering and tempering operations to obtain the advertised properties.

 The invention relates more precisely to parts having, whatever the shape and complexity of the part, a mechanical strength greater than or equal to 1100 MPa, having a yield strength greater than or equal to 700 MPa, an elongation at break A greater than or equal to 12 and a necking with Z-breaking greater than 30%,

 In the context of the present invention, each part, bar, any form, wire or complex piece obtained by hot forming process is defined as, for example, rolling, or forging with or without subsequent partial or total reheating operations. , thermal or thermochemical treatment and / or shaping with or without removal of material, or even with addition of material as for welding.

 By hot forming of a steel is meant any process that modifies the primary form of a product by an operation which is carried out at a temperature of the material such that the crystalline structure of the steel is predominantly austenitic.

The strong demand for reduced greenhouse gas emissions, coupled with growing automotive safety requirements and fuel prices, has prompted manufacturers of motorized land vehicles to look for materials with high mechanical strength. This reduces the weight of these parts while maintaining or increasing the mechanical strength performance. To obtain very high mechanical characteristics, traditional steel solutions have existed for a very long time. They contain alloying elements of greater or lesser quantity associated with thermal treatments of the austenitization type at a temperature greater than AC1, followed by quenching in an oil, polymer or even water-type fluid and generally an income at a temperature lower than Ar3. Some disadvantages associated with these steels and the treatments necessary to obtain the properties required can be of an economic nature (cost of alloys, cost of heat treatments), environmental (energy spent on re-austenitization, dispersed by quenching, treatment of baths tempering), or geometric (deformation of complex parts). In this perspective, steels to obtain a relatively high strength, just after hot forming, take on increasing importance. It has thus been proposed, over time, several families of steels offering various levels of mechanical strength, such as micro-alloyed steels ferritic pearlitic structure with different levels of carbon to obtain several levels of resistance. These micro-alloyed ferritic pearlitic steels have become widespread in recent decades and are very often used for all kinds of mechanical parts to obtain complex parts without heat treatment directly after hot forming. Although very efficient, these steels now have their limits when designers claim mechanical properties exceeding 700 MPa yield strength and 1100 MPa mechanical strength, which often requires them to return to traditional solutions mentioned above.

 In addition, depending on the thickness and shape of the parts, it can be difficult to ensure satisfactory homogeneity of the properties, particularly because of the heterogeneity of the cooling rates which impacts the microstructure.

In order to meet this demand for increasingly light vehicles, while retaining the economic and environmental benefits of microalloyed pearlite ferritic steels, it is therefore necessary to have increasingly resistant steels obtained directly after the operations. from fitness to hot. However, it is known that in the field of carbon steels, an increase in mechanical strength is generally accompanied by a loss of ductility and a loss of machinability. In addition, manufacturers of motorized land vehicles define more complex parts that require steels with high levels of. mechanical strength, fatigue resistance, toughness, formability, and machinability.

 EP0787812 describes a process for the manufacture of forged parts whose chemical composition comprises, by weight: 0.1% ≤C≤0.4%; 1% <Mn <1, 8%; 1, 2% <Si <1, 7%; 0% <Ni <1%; 0% <Cr <1, 2%; 0% <Mo <0.3%; 0% <V <0.3%; Cu < 0.35% optionally from 0.005% to 0.06% aluminum, optionally boron in contents of between 0.0005% and 0.01%, optionally between 0.005% and 0.03% titanium, optionally between 0.005 % and 0.06% of niobium, optionally from 0.005% to 0.1% of sulfur, optionally up to 0.006% of calcium, optionally up to 0.03% of tellurium, optionally up to 0.05% of selenium, optionally up to 0.05% bismuth, optionally up to 0.1% lead, the balance being iron and impurities resulting from the preparation. This method involves subjecting the workpiece to a heat treatment having a cooling from a temperature at which the steel is fully austenitic to a temperature Tm of between Ms + 100 D ° C and Ms-20 ° C at a temperature of cooling rate Vr greater than 0.5 ° C / s, followed by holding the workpiece between Tm and Tf, with Tf> Tm-100 ° C, and preferably Tf> Tm-60 ° C, for at least 2 minutes to obtain a structure comprising at least 15%, and preferably at least 30% of bainite formed between Tm and Tf. This technique requires many process steps that are detrimental to productivity.

On the other hand, it is known from the application EP1201774 whose objective of the invention is to provide a forging process carried out so as to improve the machinability, by modifying the metallographic structure of the products subjected to the impact load in a fine ferrito-pearlitic structure without adopting the quenching and tempering method, in order to obtain a yield strength exceeding that obtained by the quenching and tempering process. The tensile strength (Rm) obtained is lower than that obtained by the tempering and tempering process. This method also has the disadvantage of requiring many process steps that complicate the manufacturing process. Furthermore the absence of specific elements of chemical composition may lead to the use of ^"inadequate chemical composition forgings applications as harmful to the weldability, machinability or toughness.

 The object of the present invention is to solve the problems mentioned above. It aims to provide a steel for hot formed parts with high strength properties, simultaneously having a mechanical strength and a deformation capacity to perform hot forming operations. The invention more specifically relates to steels having a mechanical strength greater than or equal to 1100 MPa (ie a hardness greater than or equal to 300 Hv), having a yield strength greater than or equal to 700 MPa, and a higher breaking elongation or equal to 12%, with a failure greater than 30%. The invention also aims to provide a steel with an ability to be produced in a robust manner that is to say without large variations in properties depending on the manufacturing parameters and machinable with commercially available tools without loss of strength. productivity during implementation.

 For this purpose, the subject of the invention is a part according to claims 1 to 12 and a part manufacturing method according to claim 13.

 Other features and advantages of the invention will become apparent from the description below, given by way of non-limiting example.

 In the context of the invention, the chemical composition, in percentage by weight, must be the following:

The carbon content is between 0.10 and 0.30%. If the carbon content is below 0.10% by weight, there is a risk of forming pro-eutectoid ferrite and insufficient mechanical strength. Beyond 0.30%, the weldability becomes more and more reduced because it is possible to form low-tenacity microstructures in the heat-affected zone (ZAT) or in the melted zone. Within this range, the weldability is satisfactory, and the mechanical properties are stable and consistent with the targets of the invention. According to a preferred embodiment, the carbon content is between 0.15 and 0.27% and preferably between 0.17 and 0.25%.

The manganese is between 1, 6 and 2.1% and preferably between 1.7% and 2.0%. It is a hardening element with solid solution of substitution, it stabilizes the austenite and lowers the transformation temperature Ac3. Manganese therefore contributes to an increase in mechanical strength. A minimum content of 1.6% by weight is necessary to obtain the desired mechanical properties. However, beyond 2.1%, its gammagenic character leads to a significant slowing down of the bainitic transformation kinetics occurring during final cooling and the bainite fraction would be insufficient to achieve a yield strength greater than or equal to 700 MPa. . This combines a satisfactory mechanical strength without increasing the risk of decreasing the bainite fraction and thus reducing the yield strength, nor increasing the quenchability in welded alloys, which would adversely affect the weldability of steel according to the invention.

 The chromium content should be between 0.5% and 1.7% and preferably between 1.0 and 1.5%. This element makes it possible to control the formation of ferrite on cooling from a completely austenitic structure, because this ferrite, in a large quantity, reduces the mechanical strength required for the steel according to the invention. This element also makes it possible to harden and refine the bainitic microstructure, which is why a minimum content of 0.5% is necessary. However, this element considerably slows down the kinetics of the bainitic transformation, so, for contents greater than 1.7%, the bainite fraction may be insufficient to reach a yield strength greater than or equal to 700 MPa. Preferably, a range of chromium content of between 1.0% and 1.5% is chosen to refine the bainitic microstructure.

The silicon must be between 0.5 and 1.0%. In this range, the residual austenite stabilization is made possible by the addition of silicon which considerably slows the precipitation of carbides during bainitic transformation. This has been corroborated by the inventors who have noted that the bainite of the invention is virtually free of carbides. This is because the solubility of silicon in cementite is very low and this element increases carbon activity in austenite. Any formation of cementite will therefore be preceded by a step of rejection of Si at the interface. The enrichment of the austenite carbon, therefore leads to its stabilization at room temperature on the steel according to this first embodiment. Subsequently, the application of an external stress at a temperature below 200 ° C, for example, shaping or mechanical stressing type work hardening or fatigue type, may lead to the transformation of part of this austenite in martensite. This transformation will result in increasing the yield point. The minimum silicon content should be set at 0.5% by weight to achieve the stabilizing effect on the austenite and retard carbide formation. In addition, it is observed that, if the. silicon is less than 0.5%, the yield strength does not reach the required minimum of 700 MPa. Moreover, an addition of silicon in an amount greater than 1.0% will induce an excess of residual austenite which will reduce the yield strength. Preferably, the silicon content will be between 0.75 and 0.9% in order to optimize the aforementioned effects.

 The niobium should be between 0.065% and 0.15%. It is a micro-alloy element that has. the particularity of forming hardeners precipitating with carbon and / or nitrogen. II. also makes it possible to delay the bainitic transformation, in synergy with the micro-alloy elements such as boron and molybdenum present in the invention. The niobium content must nevertheless be limited to 0.15% to avoid the formation of large precipitates which may be crack initiation sites and to avoid the problems of loss of hot ductility associated with a possible intergranular precipitation of nitrides. In addition, the niobium content must be greater than or equal to 0.065% which, combined with titanium, makes it possible to have a stabilizing effect on the final mechanical properties, ie a lower sensitivity to the speed of cooling. Indeed, it can form mixed carbonitrides with titanium and remain stable at relatively high temperatures, which makes it possible to avoid the abnormal magnification of the grains at high temperature, or even allowing sufficiently high refinement of the austenitic grain. Preferably the maximum content of Nb is in the range 0.065% and 0, 0% to optimize the aforementioned effects.

The titanium content should be such that 0.010 <Ti <0.1%. A content maximum of 0.1% is tolerated, above titanium will have the effect of increasing the price and generate harmful precipitates for fatigue resistance and machinability. A minimum of 0.010% is required to control the austenitic grain size and to protect the boron from nitrogen. As a preference, a titanium content range of between 0% and 0.20% and 0.03% is chosen.

The boron content should be between 10 ppm (0.0010%) and 50 ppm (0.0050%). This element makes it possible to control the formation of ferrite on cooling from a completely austenitic structure, because this ferrite, in a large quantity, would reduce the mechanical strength and the elastic limit targeted by the invention. This is a soaking element. A minimum content of 10 ppm is necessary to avoid the formation of ferrite during natural cooling, so generally below 2 ° C / s for the types of parts covered by the invention. However, above 50 ppm boron will have the effect of forming iron borides that may be harmful to ductility. Preferably, a range of boron content of between 20 ppm and 30 ppm is chosen to optimize the above-mentioned effects.

The nitrogen content should be between 10 ppm (0.0010%) and 130 ppm (0.0130%). A minimum content of 10 ppm is required to form the abovementioned carbonitrides. However, above 130 ppm, the nitrogen may cause the bainitic ferrite to become too hard to harden, with possible reduction in the resilience of the finished part. Preferably, a range of nitrogen content between 50 ppm and 120 ppm is chosen to optimize the aforementioned effects.

The aluminum content must be less than or equal to 0.050% and preferably less than or equal to 0.040%, or even less than or equal to 0.020%. As a preference, the Al content is such that 0.003% <Al 0,0 0.015%. This is a residual element whose content we wish to limit. High levels of aluminum are considered to increase erosion of refractories and the risk of clogging of the nozzles during steel casting. In addition aluminum segregates negatively and, it can lead to macro-segregations. In excessive amounts, aluminum can reduce hot ductility and increase the risk of defects in continuous casting. Without a strong control of the casting conditions, the defects of the micro and macro segregation type ultimately give rise to segregation on the forged part. This band structure consists of alternating bainitic strips with different hardnesses which can adversely affect the formability of the material. The molybdenum content must be less than or equal to 1.0%, preferably less than or equal to 0.5%. Preferably, a range of molybdenum content of between 0.03 and 0.15% is chosen. Its presence is favorable for the formation of bainite by synergistic effect with boron and niobium. It thus makes it possible to guarantee the absence of pro-eutectoid ferrite at the grain boundaries. Beyond a content of 1.0%, it promotes the appearance of martensite which is not sought.

The nickel content must be less than or equal to 1.0%. A maximum content of 1.0% is tolerated, above the nickel will have the effect of increasing the price of the proposed solution, which may reduce its viability from an economic point of view. Preferably, a range of nickel content between 0 and 0.55% is chosen.

The vanadium content must be less than or equal to 0.3%. A maximum content of 0.3% is tolerated, above vanadium will have the effect of increasing the price of the solution and affect the resilience. Preferably, in this invention, a vanadium content range of between 0 and 0.2% is selected. Sulfur can be at different levels depending on the desired machinability. There will always be a small quantity because it is a residual element whose value can not be reduced to an absolute zero, but it can also be added voluntarily. A lower S content will be aimed if the desired fatigue properties are very high. In general, we will target between 0.015 and 0.04%, knowing that it is possible to add up to 0.1% to improve machinability. Alternatively, it is also possible to add in combination with sulfur one or more elements selected from tellurium, selenium, lead and bismuth in amounts of less than or equal to 0.1% for each element.

The phosphorus must be less than or equal to 0.050% and preferably less than or equal to 0.025%. It is an element that hardens in solid solution but significantly reduces weldability and hot ductility, especially due to its ability to segregate at grain boundaries or its tendency to co-segregate with manganese. . For these reasons, its content should be limited to 0.025% in order to obtain good weldability.

"The copper content must be less than or equal to 0.5% A maximum content of 0.5% is tolerated because above the copper will have the effect of reducing the fitness of the product.

The remainder of the composition consists of iron and unavoidable impurities resulting from processing, such as for example arsenic or tin.

In preferred embodiments, the chemical compositions according to the invention may furthermore fulfill the following conditions, taken alone or in combination:

0, 1 <S1 <0.4 and

0.5 <S2 <1, 8 0.7 <S3 <1, 6

0.3 <S4 <1.5 with

S1 = Nb + V + Mo + Ti + AI

S2 = C + N + Cr / 2 + (S1) / 6 + (Si + Mn - 4 * S) / 10 + Ni / 20 S3 = S2 + 1/3 x Vr600

S4 = S3 - Vr400 in which the contents of the elements are expressed as a percentage by weight and the cooling rates Vr400 and Vr600 are expressed in ° C / s. Vr400 represents the cooling rate in the temperature range between 420 and 380 ° C. Vr600 represents the cooling rate in the temperature range between 620 and 580 ° C.

As will be seen in the tests described below, the criterion S1 is correlated with the robustness of the mechanical properties compared to the variations of cooling conditions in general and in the face of Vr600 variations in particular. The respect of the value ranges of this criterion thus makes it possible to guarantee a very low sensitivity of the grade to the manufacturing conditions. In a preferred embodiment, 0.200 <S1 <0.4, which further improves the robustness.

 On the other hand, the criteria S2 to S4 are correlated with obtaining a predominantly bainitic structure with more than 70% for the grades according to the invention, thus making it possible to guarantee the attainment of the intended mechanical properties.

 According to the invention, the microstructure of the steel may contain, in surface proportion after the final cooling:

 - bainite in a content between 70 and 100%. In the context of the present invention, bainite means a bainite comprising less than 5% carbide surface and whose inter-slab phase is austenite.

 - residual austenite in a content of not more than 30%

 ferrite at a content of less than 5%. In particular, if the ferrite content is greater than 5%, the steel according to the invention will have a lower mechanical strength than the 1100 MPa referred to.

The steel according to the invention may be manufactured by the method described below:

a steel of composition according to the invention is supplied in the form of a bloom, a billet of rectangular or round square section, or in the form of an ingot, then

 - This steel is rolled as a semi-finished product, in the form of a bar or wire and

- one carries the semi-finished product to a reheating temperature (T _rec h) of between 00 ° C and 1300 ° C to obtain a semi-finished product heated, then the heated half-product is shaped while hot, the hot-forming end temperature being greater than or equal to 850 ° C. in order to obtain a hot-formed part;

said hot formed part is cooled to a temperature of between 620 and 580 ° C. at a cooling rate Vr600 of between 0.10 ° C./s and 10 ° C./s.

said part is cooled down to a temperature between 420 and 380 ° C. at a cooling rate Vr 400 of less than 4 ° C./s, and then the part is cooled between 380 ° C. and 300 ° C. at a lower speed. or equal to 0.3 ° C / s, then

the part is cooled to ambient temperature at a speed of less than or equal to 4 ° C./s, then

the heat-formed part which is cooled down to ambient temperature is optionally subjected to heat treatment at a temperature of between 300 ° C. and 450 ° C. for a period of between 30 minutes and 120 minutes; then

- We perform the machining parts.

In a preferred embodiment, the heat treatment of income is carried out to ensure the obtaining of very good properties of the parts after cooling.

To better illustrate the invention, tests were performed on three shades. testing

The chemical compositions of the steels used in the tests were collated in Table 1. The reheating temperature of these grades was 1250 ° C. The end temperature of hot shaping was 1220 ° C.

Cooling rates Vr600 and Vr400 are shown in Table 2.

The parts were cooled between 380 and ambient temperature to 0, 15 ° C / s and then machined. The conditions for carrying out the tests and the results of the characterization measurements have been compiled in Table 2. Table 1

Table 2

The results of these tests have been graphically represented as 4 figures. FIG. 1 shows the variation of the mechanical resistance to rupture Rm as a function of the cooling rate Vr600 for the grades A and B. FIG. 2 shows the variation of the elastic limit Re as a function of the cooling speed Vr600 for the shades A and B.

 It is found that the grade according to the invention has a high stability of its mechanical properties when the cooling conditions vary. The grade is therefore much more robust to variations in process conditions than grades according to the prior art.

 Furthermore, FIG. 3 shows the delta of the mechanical strength at break Rm as a function of the criterion S1 for the grades A, B and C. Similarly, FIG. 4 shows the delta of the elastic limit Re as a function of the criterion S1. for grades A, B and C.

 It is found that the sensitivity to the cooling conditions is even lower than the value of S1 is high.

The invention will notably be used with advantage for the manufacture of hot formed parts and in particular, hot forged, for applications in land motor vehicles. It also finds applications in the manufacture of parts for boats or in the field of construction, in particular for the manufacture of screw bars for formwork.

 In general, the invention can be implemented for the manufacture of all types of parts requiring to achieve the properties referred to

Claims

 1- Part whose composition includes, the contents being expressed in

 percentage by weight,

 0.10 <C <0.30

 1.6 <Mn <2.1

 0.5 <Cr <1.7

 0.5 <If <1.0

 0.065 <Numbers <0.15

0.0010≤ ^' B≤ 0.0050

 0.0010≤N≤, 0.0.130

 0 <Al <0.060

 0 <Mo <1.00

 0 <Ni <1.0

 0.01 <Ti <0.07

 0 <V <0.3

 0 <P <0.050

 0.01 <S <0.1

 0 <Cu <0.5

 0 <Sn <0.1

the remainder of the composition consisting of iron and unavoidable impurities resulting from the preparation, the microstructure being constituted, in surface proportions, of 100 to 70% of bainite, of less than 30% of residual austenite and of less than 5% ferrite.

 2- part according to claim 1, the contents of niobium, vanadium, molybdenum, titanium and aluminum are such that:

 0.1 <S1 <0.4

 with S1 = Nb + V + Mo + Ti + Al

 3- part according to claim 2, the contents of carbon, nitrogen, chromium, silicon, manganese, sulfur and nickel are such that: 0.5 <S 2 <1.8

0.7 <S3 <1.6 0.3 <S4 <1, 5

with S2 = C + N + Cr / 2 + (S1) / 6 + (Si + Mn - 4 * S) / 10 + Ni / 20 S3 = S2 + 1/3 x Vr600 S4 = S3 - Vr400

Vr400 and Vr600 being expressed in ° C / s, Vr400 representing the cooling rate of the part in the temperature range between 420 and 380 ° C and Vr600 representing the cooling rate of the part in the temperature range between 620 and 620. and 580 ° C.

4. Part according to any one of the preceding claims, the composition of which comprises the content being expressed as a percentage by weight.

0, 15 <C <0.27

5. Part according to any one of the preceding claims, the composition of which comprises the content being expressed as a percentage by weight.

1, 7 <Mn <2.0

6. Part according to any one of the preceding claims, the composition of which comprises the content being expressed as a percentage by weight

1.0% <Cr <1, 5. Part according to any one of the preceding claims, the composition of which comprises the content being expressed as a percentage by weight:

0.75 <Si <0.9

8- part according to any one of the preceding claims whose composition comprises, the content being expressed as a percentage by weight: 0.065 <Nb <0, 1 10

9- part according to any one of the preceding claims whose composition comprises, the content being expressed as a percentage by weight:

0.0020 <B <0.0030 10- part according to any one of the preceding claims whose composition comprises, the content being expressed as a percentage by weight:

 1-piece according to any one of the preceding claims whose composition comprises, the content being expressed as a percentage by weight:

0.003≤ Al≤ 0.015

12- part according to any one of the preceding claims whose composition comprises, the content being expressed as a percentage by weight:

0 <Ni <0.55 13- Part according to any one of the preceding claims, the composition of which comprises the content being expressed as a percentage by weight:

0 <V <0.2

14- part according to any one of the preceding claims whose composition comprises, the content being expressed as a percentage by weight: 0.03 <Mo <0.15

15 - part according to any preceding claim whose structure comprises 0% ferrite.

16 - A method of manufacturing a steel part comprising the following successive steps: - supplying a steel composition according to any one of claims 1 to 14 in the form of a bloom, billet square section rectangle or round, or under ingot shape, then

this steel is rolled in the form of a semi- _finished product, in the form of a bar or wire, and then said semi- _finished product is heated to a reheating temperature (T _reC h) of between 1100 ° C. and 1300 ° C. in order to obtain half-product warmed up, then said heated half-product is hot-shaped, the hot-forming end temperature being greater than or equal to 850 ° C. to obtain a hot-formed part, and then,

 said hot-formed part is cooled to a temperature of between 620 and 580 ° C. at a cooling rate Vr600 of between 0.10 ° C./s and 10 ° C./s.

 said part is cooled to a temperature of between 420 and 380 ° C. at a cooling rate Vr400 of less than 4 ° C./s, and then

 the part is cooled between 380 ° C. and 300 ° C. at a speed less than or equal to 0.3 ° C./s, and then

 the part is cooled to ambient temperature at a speed of less than or equal to 4 ° C./s, then

 the heat-formed part which is cooled down to ambient temperature is optionally subjected to heat treatment at a temperature of between 300 ° C. and 450 ° C. for a period of between 30 minutes and 120 minutes; then

 - We perform the machining parts.