CN102994905A - Preparation method of micro/nano-structure ultrahigh-strength plastic stainless steel containing Nb - Google Patents
Preparation method of micro/nano-structure ultrahigh-strength plastic stainless steel containing Nb Download PDFInfo
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Abstract
The invention belongs to the field of production of ultrahigh-strength plastic alloy steel, and relates to a preparation method of micro/nano-structure ultrahigh-strength plastic stainless steel containing Nb. The preparation method comprises the steps of: firstly preparing materials according to a composition proportion, adding 0.05-0.15% of Nb element on the basis of 316L austenitic stainless steel, then carrying out vacuum induction furnace smelting, casting blank forging, forged piece hot rolling and solution treatment, carrying out cold deformation on the steel plate which undergoes the solution treatment with deformations of 40%, 60%, 80% and 90% and with single reduction in pass controlled within 3-10% to prepare steel plate with different cold deformations, annealing the steel plate which undergoes the cold deformation with heating rate controlled at 50-200 DEG C/s, with heating temperature within 750-950 DEG C and with heat preservation time within 5-100s, and cooling to the room temperature at a cooling rate of 50-400 DEG C/s to obtain a superfine austenite structure with micro-nano scale. The obdurability of the material is synchronously improved. The yield strength of the final product can be up to 750-800MPa, the strength of extension is up to 1100-1200MPa and the percentage of elongation is 35-45%.
Description
Technical field
The invention belongs to the strong plastic metal steel of superelevation production field, relate to the preparation method of the strong plastic stainless steel of micrometer/nanometer composite structure superelevation of a kind of Nb of containing.
Background technology
As biomedical bone material commonly used, although calcium phosphate and bioactivity glass can promote the generation of osseous tissue, because these strengths of materials are on the low side, bending strength is only in the 42-200MPa scope, and frangible, causes its application also to be restricted.And austenitic stainless steel is owing to nonmagnetic, corrosion-resistant, easy-formation have simultaneously good mechanical property and be widely used in the biomedical materials such as joint prosthesis.But blemish in an otherwise perfect thing is that its biocompatibility still obviously is inferior to calcium phosphate and bioactivity glass.In recent years, Louisiana, United States vertical professor Misra of university studies show that, if the organized processing of the medical austenitic stainless steel of commodity is become to have Ultra-fine Grained/nanometer-size die composite structure, can have good tissue consistency.Traditional commercial austenitic stainless steel 301LN organizes grain-size 10-30 mu m range, and it can obtain to have the tissue of micrometer/nanometer composite structure after annealing through significant cold deformation again.This histioid material has than better strong plasticity combination before processing.
After obtaining having the reverse change austenite structure of micrometer/nanometer structure, in order to realize the cost degradation of element manufacturing, should utilize as far as possible pressure processing method.Yet metastable reverse becomes austenite structure under external force the strain inducing martensitic transformation might occur again, its good biocompatibility will not exist, and yes must avoid for this.For this reason, must manage to improve this histioid mechanical stability.
Microstructure is one of greatest factor that determines the ferrous materials mechanical property.In the development course of conventional steel iron construction material, for improving mechanical performance index, developed multiple microstructure control technique.Can improve simultaneously the obdurability of ferrous materials by the structure refinement technology.The 90's ends of last century, the countries such as Japan, Korea S, European Union, Australia just carried out research for the ferrite refinement limit to the beginning of this century, and the same period, China has proposed " deformation induced ferrite transformation " theory (DIFT).The result shows, if ferrite grain size is refine to about 5 microns from traditional about 20 microns, the yield strength of structural carbon steel can be brought up to the 400MPa level from the 200MPa level; The grain-size of microalloyed steel is refine to about 2 microns from tens microns, and yield strength can be brought up to the 700MPa level by the 400MPa level.
And aspect structure stability control, former studies work shows that a small amount of microalloy element that adds in the steel has obvious inhibition to recrystallize and the microstructure evolution that produces in the deformed austenite.This gives us a strong enlightenment, and this measure also may be used for reversing the change metastable austenite in the structure stability control of deformation processing process.This work is intended by the Nb microalloying, and preparation contains the Nb austenitic steel in the laboratory.Explore and obtain the martensitic reverse transformation control of the strain inducing optimum technology parameter that the compound reverse of micrometer/nanometer becomes austenite structure.Simultaneously, by the tracking observation to the compound reverse change of acquired micrometer/nanometer austenite structure deformation process, understand this histioid deformation mechanism.In addition, the research microalloying provides the basis on the impact of distortion, phase conversion mechanism for further optimizing Composition Design.
The present invention adds an amount of Nb element on the 316L basis, then by strain inducing martensitic transformation and anneal crystal grain thinning subsequently, acquisition waits axle austenite crystal complex tissue, obtain the micrometer/nanometer composite structure austenitic stainless steel of intensity, toughness and excellent compatibility, the present invention can be exploitation and melts the biomedical metallic material of new generation that satisfactory stability, strong plasticity and biocompatibility be integrated and provide reason to instruct and technical support.
Summary of the invention
The object of the invention is for Composition Design, in conjunction with actual production, on the basis of 316L austenite stainless composition of steel, increases the Nb element, then by different cold deformations, and the steel plate of preparation different distortion amount; The cold deformation steel plate is carried out anneal, by control heating rate, Heating temperature, soaking time, rate of cooling, obtain to have the ultra-fine austenite structure of micro-nano-scale.The obdurability of material is improved synchronously.Its yield strength can reach 750-800MPa, and tensile strength reaches 1100-1200MPa, and unit elongation is 35-45%.The production method of the strong plastic stainless steel of micrometer/nanometer composite structure superelevation by the invention provides a kind of Nb of containing especially solves the austenitic stainless steel low strength that traditional industry is produced, and biocompatibility is poor, the problem that mechanical stability is poor.
For achieving the above object, the production that proposes of the present invention contain Nb little/method of the strong plastic stainless steel of micro-nano structure superelevation comprises the steps:
(1) its chemical ingredients mass percent is as follows:
C 0.015-0.018%; Si 0.3-0.6%; Mn 1.2-1.5%; Cr 17.3-17.7%; Mo 2.3-2.7%; Ni 11.8-12.2%; N 0.07-0.10%; Nb 0.05-0.15%. obtains the sample steel ingot by corresponding proportioning by the vacuum oven melting;
(2) will smelt good strand, and cut rising head, and be swaged into required blank, the forging scheme is: strand is heated to 1230-1260 ℃, be incubated the i.e. forging of coming out of the stove after 1.5-2.5 hour, and final forging temperature is not less than 1100 ℃, be swaged into 20mm thick * the wide steel ingot of 150mm;
(3) blank is carried out equal thermal treatment, the control blank is in 1150～1250 ℃ of temperature ranges, and insulation 120～240min makes the abundant Hui Rong of microalloy element in the steel;
(4) to the processing of scaling of the slab after coming out of the stove, remove the iron scale that slab produces in heat-processed;
(5) the wide blank of * 150mm thick through the 20mm of 4 technique gained is carried out hot rolling, hot-rolled temperature is set as 1130-1160 ℃ of insulation 1.5-2.5h, and is rolling through 3 passages, then cooling, and last hot-rolled finished product thickness is 3.5-4.0mm;
(6) hot-rolled finished product after 5 art breading is carried out solution treatment, processing scheme is: hot-rolled finished product is heated to 1100-1150 ℃, insulation 5-15min, then Forced water cooling;
(7) steel plate after the solution treatment is carried out cold deformation, deflection is 40%, 60%, 80% and 90% cold roller and deformed, and the single pass draught is controlled at the 3-10% scope, prepares the steel plate of different cold deformations;
(8) the cold deformation steel plate after technique 7 is processed is carried out anneal, processing scheme is: heating rate is controlled at 50-200 ℃/s scope, Heating temperature is 750-950 ℃ of scope, and soaking time is in the 5-100s scope, is cooled to room temperature with the rate of cooling of 50-400 ℃/s scope.Namely obtain the strong plastic stainless steel of superelevation of the superfine crystal particle austenite structure of micrometer/nanometer yardstick, its yield strength reaches 750-800MPa, and tensile strength reaches 1100-1200MPa, and unit elongation is 35-45%.
Advantage of the present invention:
(1) a small amount of microalloy element that adds in the steel has obvious inhibition to recrystallize and the microstructure evolution that produces in the deformed austenite.This gives us a strong enlightenment, and this measure also may be used for reversing the change metastable austenite in the structure stability control of deformation processing process.The present invention intends by the Nb microalloying, and preparation contains the Nb austenitic steel in the laboratory, improves structure stability.Nb can also produce significant grain refining and medium precipitation strength effect;
(2) hot-rolled finished product is heated to 1100 ℃, insulation 10min, then Forced water cooling.Austenitic stainless steel contains the austenite formers such as a large amount of Ni, Mn, in the course of hot rolling, and Carbide Precipitation in the steel, crystal grain produces distortion, and the hardness of steel is higher.In order to make stainless steel obtain best use properties or to create good condition for stainless steel user deep processing, must carry out solution treatment to hot-rolled finished product.Austenitic stainless steel softens by solution treatment, generally steel are heated to about 950～1150 ℃, insulation for some time, make carbide and various alloying element be dissolved in sufficiently uniformly in the austenite, then fast hardening cooling, carbon and other alloying element have little time to separate out, and obtain pure austenite structure;
(3) austenite stainless steel plate after the solution treatment is carried out cold deformation, 40%, 60%, 80% and 90% deflection, the strain inducing martensitic transformation, martensitic content can change along with the change of deflection.
(4) heating rate in anneal is controlled at 50-200 ℃/s scope, and high temperature rise rate can inhibiting grain growth, reduces separating out of carbide; Heating temperature is 750-950 ℃ of scope, and soaking time is in the 5-100s scope, and the martensite austenite structure that changes into as much as possible that strain inducing is produced also will be controlled grain fineness number simultaneously, and soaking time is shorter, and grain fineness number is larger; Simultaneously the rate of cooling with 50-400 ℃/s scope is cooled to room temperature, fast coldly also can suppress Austenite Grain Growth, reduces the formation of carbide and oxide compound.
Description of drawings
Fig. 1 is that embodiment 1 adds 0.05%Nb, the austenite structure metallograph after the hot-rolled finished product solution treatment;
Fig. 2 is that embodiment 2 adds 0.05%Nb, the strain inducing martensitic stucture metallograph after 60% cold deformation;
Fig. 3 is that embodiment 3 adds 0.05%Nb, the strain inducing martensitic stucture metallograph after 80% cold deformation;
Fig. 4 is that embodiment 1 adds 0.05%Nb, through 80% cold deformation, and the metallograph behind 800 ℃, 100s annealing;
Fig. 5 is that embodiment 2 adds 0.05%Nb, through 60% cold deformation, and the metallograph behind 850 ℃, 100s annealing;
Fig. 6 is that embodiment 3 adds 0.05%Nb, through 80% cold deformation, and the metallograph behind 900 ℃, 60s annealing;
Embodiment
Embodiment 1
With chemical ingredients percentage ratio meter by weight, C 0.017%; Si 0.5%; Mn 1.3%; Cr 17.5%; Mo 2.5%; Ni 12%; N 0.09%; Nb 0.05%.Suitably with addition of graphite, obtain the sample steel ingot by corresponding proportioning by the melting of 50kg vacuum oven according to decarburization situation in the smelting process.With smelting good strand, cut rising head, be swaged into required blank, the forging scheme is: strand is heated to 1250 ℃, be incubated came out of the stove after 2 hours namely forges, final forging temperature is not less than 1100 ℃, be swaged into 20mm thick * 150mm is wide * steel ingot that 200mm grows.Blank is carried out equal thermal treatment, and the control blank temperature is 1250 ℃, and insulation 200min makes the abundant Hui Rong of microalloy element in the steel.To the processing of scaling of the slab after coming out of the stove, remove the iron scale that slab produces in heat-processed.
Blank after processing is carried out hot rolling, and hot-rolled temperature is set as 1150 ℃ of insulation 2h, and is rolling through 3 passages, then cooling, and last hot-rolled finished product thickness is 3.7mm.Hot-rolled finished product after 5 art breading is carried out solution treatment, and processing scheme is: hot-rolled finished product is heated to 1100 ℃, insulation 10min, then Forced water cooling.What obtain organizes as shown in Figure 1, is pure austenite structure.
Steel plate after the solution treatment is carried out cold deformation, and deflection is 80% cold roller and deformed, and the single pass draught is controlled at the 3-10% scope, the metallographic structure after the cold deformation as shown in Figure 3, the strain inducing martensite content is about 85%.Steel plate after the cold deformation is carried out anneal, and processing scheme is: heating rate is controlled at 50 ℃/s scope, and Heating temperature is 800 ℃ of scopes, and soaking time is being 100s, is cooled to room temperature with the rate of cooling of 50 ℃/s scope.What obtain organizes as shown in Figure 4, and strain inducing martensite reverses and to become austenite, reverses to become not thorough, does not have perfect recrystallization, residual a certain amount of martensite also in the tissue, and austenite content is about 70%.Crystal grain less than 300nm accounts for 50%, grain-size be 0.3-2 μ m account for 50%, effectively refinement final tissue.Yield strength can reach 800MPa, and tensile strength reaches 1200MPa, and unit elongation is 35%.
Embodiment 2
With chemical ingredients percentage ratio meter by weight, C 0.017%; Si 0.5%; Mn 1.3%; Cr 17.5%; Mo 2.5%; Ni 12%; N 0.09%; Nb 0.05%.Suitably with addition of graphite, obtain the sample steel ingot by corresponding proportioning by the melting of 50kg vacuum oven according to decarburization situation in the smelting process.With smelting good strand, cut rising head, be swaged into required blank, the forging scheme is: strand is heated to 1250 ℃, be incubated came out of the stove after 2 hours namely forges, final forging temperature is not less than 1100 ℃, be swaged into 20mm thick * 150mm is wide * steel ingot that 200mm grows.Blank is carried out equal thermal treatment, and the control blank temperature is 1250 ℃, and insulation 200min makes the abundant Hui Rong of microalloy element in the steel.To the processing of scaling of the slab after coming out of the stove, remove the iron scale that slab produces in heat-processed.Blank after processing is carried out hot rolling, and hot-rolled temperature is set as 1150 ℃ of insulation 2h, and is rolling through 3 passages, then cooling, and last hot-rolled finished product thickness is 3.7mm.Hot-rolled finished product after 5 art breading is carried out solution treatment.
Steel plate after the solution treatment is carried out cold deformation, and deflection is 60% cold roller and deformed, and the single pass draught is controlled at the 3-10% scope, the metallographic structure after the cold deformation as shown in Figure 2, the strain inducing martensite content is about 65%.Steel plate after the cold deformation is carried out anneal, and processing scheme is: heating rate is controlled at 50 ℃/s scope, and Heating temperature is 850 ℃ of scopes, and soaking time is being 100s, is cooled to room temperature with the rate of cooling of 50 ℃/s scope.What obtain organizes as shown in Figure 5, and strain inducing martensite reverses and to become austenite, and austenite content is about 100%, accounts for 35% less than the crystal grain of 600nm, grain-size be 0.6-5 μ m account for 65%, obtain to have the ultra-fine austenite structure of micro-nano-scale.Yield strength can reach 750MPa, and tensile strength reaches 1100MPa, and unit elongation is 45%.
Embodiment 3
With chemical ingredients percentage ratio meter by weight, C 0.017%; Si 0.5%; Mn 1.3%; Cr 17.5%; Mo 2.5%; Ni 12%; N 0.09%; Nb 0.05%.Suitably with addition of graphite, obtain the sample steel ingot by corresponding proportioning by the melting of 50kg vacuum oven according to decarburization situation in the smelting process.With smelting good strand, cut rising head, be swaged into required blank, the forging scheme is: strand is heated to 1250 ℃, be incubated came out of the stove after 2 hours namely forges, final forging temperature is not less than 1100 ℃, be swaged into 20mm thick * 150mm is wide * steel ingot that 200mm grows.Blank is carried out equal thermal treatment, and the control blank temperature is 1250 ℃, and insulation 200min makes the abundant Hui Rong of microalloy element in the steel.To the processing of scaling of the slab after coming out of the stove, remove the iron scale that slab produces in heat-processed.Blank after processing is carried out hot rolling, and hot-rolled temperature is set as 1150 ℃ of insulation 2h, and is rolling through 3 passages, then cooling, and last hot-rolled finished product thickness is 3.7mm.Hot-rolled finished product after 5 art breading is carried out solution treatment.
Steel plate after the solution treatment is carried out cold deformation, and deflection is 80% cold roller and deformed, and the single pass draught is controlled at the 3-10% scope, the metallographic structure after the cold deformation as shown in Figure 3, the strain inducing martensite content is about 85%.Steel plate after the cold deformation is carried out anneal, and processing scheme is: heating rate is controlled at 50 ℃/s scope, and Heating temperature is 900 ℃ of scopes, and soaking time is being 60s, is cooled to room temperature with the rate of cooling of 50 ℃/s scope.What obtain organizes as shown in Figure 6, and strain inducing martensite reverses and to become austenite, and austenite content is about 100%, accounts for 40% less than the crystal grain of 450nm, grain-size be 0.45-3.5 μ m account for 60%, obtain to have the ultra-fine austenite structure of micro-nano-scale.The obdurability of material is improved synchronously.The yield strength of the finished product can reach 780MPa, and tensile strength reaches 1150MPa, and unit elongation is 42%.
Claims (1)
- One kind contain Nb little/preparation method of the strong plastic stainless steel of micro-nano structure superelevation, it is characterized in that its concrete steps are as follows:(1) its chemical ingredients mass percent is as follows:C 0.015-0.018%; Si 0.3-0.6%; Mn 1.2-1.5%; Cr 17.3-17.7%; Mo 2.3-2.7%; Ni 11.8-12.2%; N 0.07-0.10%; Nb 0.05-0.15%. obtains the sample steel ingot by corresponding proportioning by the vacuum oven melting;(2) will smelt good strand, and cut rising head, and be swaged into required blank, the forging scheme is: strand is heated to 1230-1260 ℃, be incubated the i.e. forging of coming out of the stove after 1.5-2.5 hour, and final forging temperature is not less than 1100 ℃, be swaged into 20mm thick * the wide steel ingot of 150mm;(3) blank is carried out equal thermal treatment, the control blank is in 1150～1250 ℃ of temperature ranges, and insulation 120～240min makes the abundant Hui Rong of microalloy element in the steel;(4) to the processing of scaling of the slab after coming out of the stove, remove the iron scale that slab produces in heat-processed;(5) * 150mm wide blank thick through the 20mm of step (4) gained carried out hot rolling, hot-rolled temperature is set as 1130-1160 ℃, and insulation 1.5-2.5h is rolling through 3 passages, then cooling, and last hot-rolled finished product thickness is 3.5-4.0mm;(6) hot-rolled finished product after step (5) is processed is carried out solution treatment, processing scheme is: hot-rolled finished product is heated to 1100-1150 ℃, insulation 5-15min, then Forced water cooling;(7) steel plate after the solution treatment is carried out cold deformation, deflection is 40%, 60%, 80% and 90% cold roller and deformed, and the single pass draught is controlled at the 3-10% scope, prepares the steel plate of different cold deformations;(8) the cold deformation steel plate after step (7) is processed is carried out anneal, processing scheme is: heating rate is controlled at 50-200 ℃/s scope, Heating temperature is 750-950 ℃ of scope, and soaking time is in the 5-100s scope, is cooled to room temperature with the rate of cooling of 50-400 ℃/s scope; Namely obtain the strong plastic stainless steel of superelevation of the superfine crystal particle austenite structure of micrometer/nanometer yardstick, its yield strength reaches 750-800MPa, and tensile strength reaches 1100-1200MPa, and unit elongation is 35-45%.
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