CN115055532B - Preparation method of cobalt-chromium-based alloy seamless tube with high strength and high plasticity - Google Patents
Preparation method of cobalt-chromium-based alloy seamless tube with high strength and high plasticityInfo
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- CN115055532B CN115055532B CN202210603873.6A CN202210603873A CN115055532B CN 115055532 B CN115055532 B CN 115055532B CN 202210603873 A CN202210603873 A CN 202210603873A CN 115055532 B CN115055532 B CN 115055532B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES, PROFILES OR LIKE SEMI-MANUFACTURED PRODUCTS OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C37/00—Manufacture of metal sheets, rods, wire, tubes, profiles or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape
- B21C37/06—Manufacture of metal sheets, rods, wire, tubes, profiles or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape of tubes or metal hoses; Combined procedures for making tubes, e.g. for making multi-wall tubes
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/08—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for tubular bodies or pipes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
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- Y02P10/00—Technologies related to metal processing
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Abstract
提供一种兼具高强度和高塑性的钴铬基合金无缝管制备方法，属于钴铬基合金管材加工技术领域，本发明采用两步法，首先通过大变形的三辊行星温轧制对管坯粗大晶粒进行有效破碎，然后通过部分再结晶热处理形成大晶粒+小晶粒的双峰组织。根据受力时大晶粒优先变形的机制，再通过小变形的冷轧或冷拉拔进一步对大晶粒进行变形，然后通过高温短时热处理形成更小的晶粒，通过合理控制道次变形量和热处理温度匹配，得到兼具高强度、高延伸率的钴铬基合金管材，有效解决了常规加工的钴基合金管材强度高、塑性低的问题。
A method for preparing a cobalt-chromium-based alloy seamless tube with both high strength and high plasticity is provided, belonging to the technical field of cobalt-chromium-based alloy tube processing. The present invention employs a two-step process: first, coarse grains in the tube billet are effectively crushed through large-deformation three-roll planetary warm rolling, followed by a partial recrystallization heat treatment to form a bimodal structure with large and small grains. Based on the mechanism by which large grains deform preferentially under stress, the large grains are further deformed through small-deformation cold rolling or cold drawing, followed by a high-temperature, short-time heat treatment to form smaller grains. By rationally controlling the deformation amount per pass and matching the heat treatment temperature, a cobalt-chromium-based alloy tube with both high strength and high elongation is obtained, effectively solving the problem of high strength and low plasticity in conventionally processed cobalt-based alloy tubes.
Description
Technical Field
The invention belongs to the technical field of cobalt-chromium-based alloy pipe processing, and particularly relates to a preparation method of a cobalt-chromium-based alloy seamless pipe with high strength and high plasticity.
Background
Cobalt-chromium-based alloys have been widely used in the fields of gas turbines, dentistry, orthopedics, cardiovascular and the like due to their excellent mechanical properties, corrosion resistance and good biocompatibility. Particularly in the cardiovascular field, the high-strength cobalt-based alloy stent can reduce the width of a stay (the width of the current thinnest connecting rib is 50 mu m) to the greatest extent on the premise of ensuring the radial supporting strength and the ray visibility, thereby reducing the stimulation of the vascular stent to the vascular wall, further reducing the potential cause of stent restenosis and improving the success rate of implantation of the vascular stent. Meanwhile, in the process of stent expansion, the stent can generate plastic deformation, stress concentration can occur at the stent node, and fracture can occur. According to ISO and ASTM standards, L605 alloy in the working state Rp >1GPa, rm >1.2GPa, A >5%, annealed state Rp >500MPa, rm >900MPa, A >30%, therefore, the raw material for the stent-seamless pipe must have both high strength and high ductility.
But the strength-elongation of metallic materials tends to be an "inverted" relationship. According to the Hall-Petch relationship, the fine-grain structure (several tens of nanometers to several tens of micrometers) has higher strength but lower ductility, while the coarse-grain structure has higher elongation but lower strength. Reasonable control of grain size and distribution of metallic materials is an effective approach to solving the high strength-high elongation balance.
At present, a tube blank for preparing the cobalt-chromium-based alloy tube is generally prepared by centrifugal casting or hot extrusion, and further adopts a rotary forging/rolling/cold drawing process. For example, chinese patent No. CN113680985B discloses a preparation method of a low-cost short-flow high-temperature alloy seamless pipe, which adopts a centrifugal casting pipe blank and a rolling method to prepare the seamless pipe, the core process is a vacuum centrifugal casting technology, and Chinese patent No. CN 105331913B discloses a method for preparing a high-temperature alloy Inconel 625 pipe by short-flow hot extrusion and cold drawing, and the core process is a hot extrusion technology. The two patents are mainly focused on the short-process preparation of the tube blank, the single-pass deformation amount of the subsequent common rolling/drawing is smaller, the casting or hot extrusion coarse tissues are difficult to effectively crush, the cobalt-chromium alloy is fast in work hardening, the grain size is larger due to frequent heat treatment, and the high strength and the high plasticity are difficult to simultaneously achieve. In summary, aiming at the field of cobalt-chromium-based alloy seamless pipe preparation, a method for simultaneously improving the high strength and the elongation of a pipe is not related at present. There is therefore a need for improvements.
Disclosure of Invention
Aiming at the defects of the prior art, the invention adopts a two-step method, firstly, coarse grains of a tube blank are effectively crushed through three-roller planetary warm rolling with large deformation, then a double-peak structure of large grains and small grains is formed through partial recrystallization heat treatment, the large grains are further deformed through cold rolling or cold drawing with small deformation according to a mechanism of preferential deformation of the large grains when being stressed, then smaller grains are formed through high-temperature short-time heat treatment, and the cobalt-chromium-based alloy tube with high strength and high elongation is obtained through reasonably controlling the pass deformation and heat treatment temperature matching, thereby effectively solving the problems of high strength and low plasticity of the conventionally processed cobalt-based alloy tube.
The technical scheme adopted by the invention is that the preparation method of the cobalt-chromium-based alloy seamless pipe with high strength and high plasticity comprises the following steps:
Preparing a cobalt-chromium-based alloy tube blank by adopting a hot extrusion or vacuum centrifugal casting method, and then homogenizing and heat treating in a vacuum tube furnace, wherein the average grain size after homogenizing and heat treating is 200-300 um;
Preheating a cobalt-chromium-based alloy tube blank by adopting an induction heating device, and then carrying out three-roller planetary warm rolling, wherein the reduction of the section of the three-roller planetary warm rolling tube is 85% -90%, and the tube is naturally air-cooled after rolling;
Step three, partial recrystallization annealing, namely cleaning, alkali washing and acid washing and partial recrystallization annealing are carried out on the cobalt-chromium-based alloy pipe rolled by the three-roller planetary temperature in the step two to form a bimodal structure of large grains and small grains;
Cold rolling or cold drawing, namely cold rolling or cold drawing the cobalt-chromium-based alloy pipe annealed in the third step at room temperature, and then straightening and cleaning sequentially to obtain the required pipe, wherein the deformation of each cold rolling or cold drawing is 8% -12%, and high-temperature short-time heat treatment is carried out after each 1-2 times;
And fifthly, performing high-temperature short-time heat treatment, namely performing high-temperature short-time heat treatment on the cobalt-chromium-based alloy pipe in the fourth step in an environment of sealing a vacuum quartz pipe and filling argon with 0.1 MPa.
In the first step, the outer diameter of the cobalt-chromium-based alloy tube blank is 28-32 mm, the wall thickness is 4-5 mm, the temperature of homogenizing heat treatment is 1250-1300 ℃, and the heat preservation time is 2-3 h.
In the second step, the preheating temperature of the cobalt-chromium-based alloy tube blank is 300-400 ℃, and the heat is preserved for 30min.
In the third step, the partial recrystallization annealing temperature is 850-950 ℃, the temperature is kept for 30-60 min, and the furnace is cooled.
In the fifth step, the high-temperature short-time heat treatment temperature is 1150-1200 ℃, the heat preservation is carried out for 1-5 min, and the water cooling is carried out.
In the first step, the nominal composition of the cobalt-chromium-based alloy pipe blank is L605 or MP35N.
Compared with the prior art, the invention has the advantages that:
1. According to the scheme, the characteristics of oxidation resistance and high temperature resistance of the cobalt-based alloy are utilized, a two-step method is adopted, firstly, coarse grains of a pipe blank are effectively crushed through three-roller planetary warm rolling with large deformation, then a bimodal structure of large grains and small grains is formed through partial recrystallization heat treatment;
2. Although the recrystallization heat treatment in the scheme is a means for refining grains, as the local part is non-uniform deformation when the pipe is deformed, the deformation degree of the inner surface, the outer surface and the core part is different, the deformation degree of the outer surface is maximum when the recrystallization heat treatment is performed, the inner surface is secondary, the core part is minimum, the deformation energy of each part of the pipe is different, the growth driving force of the grains of the outer surface, the inner surface and the core part is different when the heat treatment is performed, and the grain sizes of each part are non-uniform;
3. In the scheme, the three-roller planetary warm rolling process of the cobalt-base alloy tube blank mainly comprises radial compression, and the cold rolling or cold drawing mainly comprises axial drawing, and the two are combined to act together, so that the uniform deformation of crystal grains in a structure in all directions is effectively ensured, the crystal grains are further refined, and the mechanical property of the cobalt-base alloy seamless tube is improved. Meanwhile, the three-roller planetary warm rolling process has large single-pass deformation, reduces the processing times compared with the common periodic rolling, and improves the efficiency.
Drawings
FIG. 1 is an as-cast structure diagram of a cobalt-chromium-based alloy L605 pipe blank in example 1 of the present invention;
FIG. 2 is a diagram showing the homogenization texture of a cobalt-chromium-based alloy L605 tube blank in example 1 of the present invention;
FIG. 3 is a cross-sectional view of a cobalt-chromium-based alloy L605 tube material Φ12X1.0 mm prepared in example 1 of the present invention;
FIG. 4 is a longitudinal cross-sectional view of a cobalt-chromium-based alloy L605 pipe material Φ12X1.0 mm prepared in example 1 of the present invention;
FIG. 5 is a graph showing the detection of the roughness of the inner and outer surfaces of a cobalt-chromium-based alloy L605 pipe prepared in example 1 of the present invention;
FIG. 6 is a graph showing the mechanical properties of the cobalt-chromium-based alloy L605 pipe prepared in example 1 of the present invention;
FIG. 7 is a longitudinal structure diagram of a cobalt-chromium-based alloy MP35N pipe material phi 11.95X1.0 mm prepared in example 2 of the present invention;
FIG. 8 is a transverse structure diagram of a cobalt-chromium-based alloy MP35N pipe material phi 11.95X1.0 mm prepared in example 2 of the present invention;
FIG. 9 is a graph showing the mechanical properties of the cobalt-chromium-based alloy MP35N pipe prepared in example 2 of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
It should be noted that, in this document, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising" does not exclude the presence of additional identical elements in a process, method, article, or apparatus that comprises the element.
Referring to fig. 1-6, embodiments of the present invention are described in detail.
Example 1:
The embodiment comprises the following steps:
Preparing a pipe blank, namely preparing a cobalt-chromium-based alloy L605 pipe blank by adopting a hot extrusion or vacuum centrifugal casting method, and homogenizing and heat-treating the pipe blank in a vacuum pipe furnace, wherein the outer diameter of the cobalt-chromium-based alloy L605 pipe blank is 28mm, the wall thickness is 4mm, the homogenizing and heat-treating temperature is 1250 ℃, the heat-preserving time is 3 hours, and the average grain size after heat treatment is 300 microns.
And step two, three-roller planetary temperature rolling, namely preheating the cobalt-chromium-based alloy L605 tube blank to 300 ℃ by adopting an induction heating device, and preserving heat for 30min. And then three-roller planetary warm rolling is carried out, wherein the reduction of the section of the three-roller planetary warm rolling pipe is 87%, and the pipe is naturally air-cooled after rolling. The concrete process is that an L605 cobalt-chromium base alloy pipe blank with the size of 28mm multiplied by 4.0mm (external diameter multiplied by wall thickness) is processed to 13mm multiplied by 1.0mm (external diameter multiplied by wall thickness).
And thirdly, performing partial recrystallization annealing, namely cleaning, alkali washing and acid washing and partial recrystallization annealing on the cobalt-chromium-based alloy L605 pipe rolled by the three-roller planetary temperature in the second step, wherein the annealing temperature is 950 ℃, preserving the heat for 30min, and cooling in a furnace to form a large-grain and small-grain bimodal structure.
And step four, cold rolling or cold drawing, namely cold drawing the cobalt-chromium-based alloy L605 pipe annealed in the step three at room temperature, and then straightening and cleaning sequentially to obtain the required pipe. The deformation amount of each cold drawing pass is 8.3%, and high-temperature short-time heat treatment is carried out after each 1-2 cold drawing passes. The concrete process is that an L605 cobalt-based alloy pipe blank with the size of 13mm multiplied by 1.0mm (external diameter multiplied by wall thickness) is processed to 12mm multiplied by 1.0mm (external diameter multiplied by wall thickness).
And fifthly, performing high-temperature short-time heat treatment, namely performing high-temperature short-time heat treatment on the cobalt-chromium-based alloy L605 pipe in the fourth step in an environment of sealing a vacuum quartz pipe and filling argon with 0.1MPa, wherein the high-temperature short-time heat treatment temperature is 1200 ℃, preserving heat for 1min, and performing water cooling.
The cobalt-chromium-based alloy L605 micro-pipe prepared in the embodiment has the dimensions of 12.0mm multiplied by 1.0mm (outer diameter multiplied by wall thickness), the length of 1700mm, the roughness of the inner surface and the outer surface of the pipe respectively of 0.255um and 0.225um, the average grain size of 11 grades and the room temperature stretchability of Rm=1185 MPa, rp 0.2=640 MPa and A=49.5 percent.
Example 2:
The embodiment comprises the following steps:
Preparing a pipe blank, namely preparing a cobalt-chromium-based alloy MP35N pipe blank by adopting a hot extrusion or vacuum centrifugal casting method, and carrying out homogenization heat treatment in a vacuum pipe furnace, wherein the outer diameter of the cobalt-chromium-based alloy MP35N pipe blank is 32mm, the wall thickness is 5mm, the temperature of the homogenization heat treatment is 1300 ℃, the heat preservation time is 2 hours, and the average grain size after the heat treatment is 200 microns.
And step two, three-roller planetary temperature rolling, namely preheating the cobalt-chromium-based alloy MP35N tube blank to 400 ℃ by adopting an induction heating device, and preserving heat for 30min. And then three-roller planetary warm rolling is carried out, wherein the three-roller planetary warm rolling tube has a reduction of section of 90 percent, and the tube is naturally air-cooled after rolling. The specific process is that cobalt-chromium base alloy MP35N pipe blank with the size of 32mm multiplied by 5.0mm (external diameter multiplied by wall thickness) is processed to 14.5mm multiplied by 1.0mm (external diameter multiplied by wall thickness).
And thirdly, performing partial recrystallization annealing, namely cleaning, alkali washing and acid washing and partial recrystallization annealing on the cobalt-chromium-based alloy MP35N pipe subjected to the three-roller planetary temperature rolling in the second step. The annealing temperature is 850 ℃, the temperature is kept for 30min, and the furnace is cooled to form a bimodal structure of large grains and small grains.
And step four, cold rolling or cold drawing, namely cold rolling the cobalt-chromium-based alloy MP35N pipe annealed in the step three at room temperature, and then straightening and cleaning sequentially to obtain the required pipe. The deformation amount of each cold rolling pass is 11.9 percent and 8.0 percent respectively, and high-temperature short-time heat treatment is carried out after 2 passes. The specific process is that the change of the dimension from 14.5mm multiplied by 1.0mm (external diameter multiplied by wall thickness) -12.9 mm multiplied by 1.0mm (external diameter multiplied by wall thickness) -11.95 mm multiplied by 1.0mm (external diameter multiplied by wall thickness) is cold rolled. .
And fifthly, performing high-temperature short-time heat treatment, namely performing high-temperature short-time heat treatment on the cobalt-chromium-based alloy MP35N pipe in the fourth step in an environment of sealing a vacuum quartz pipe and filling argon with 0.1MPa, wherein the heat treatment temperature is 1150 ℃, preserving heat for 5min, and performing water cooling.
The MP35N cobalt-based alloy small micro pipe prepared in the embodiment has the dimensions of 11.95mm multiplied by 1.0mm (outer diameter multiplied by wall thickness), the length of 1500mm, the roughness of the inner surface and the outer surface of the pipe is 0.255um, the average grain size is 9.5 grade, and the room temperature stretchability is Rm=1227MPa, rp0.2=632MPa and A=42.6 percent.
In summary, the invention adopts a two-step method, firstly, coarse grains of a tube blank are effectively crushed through three-roller planetary warm rolling with large deformation, then a bimodal structure of large grains and small grains is formed through partial recrystallization heat treatment, and according to a mechanism of preferential deformation of the large grains when stressed, the large grains are further deformed through cold rolling or cold drawing with small deformation, then smaller grains are formed through high-temperature short-time heat treatment, and the cobalt-chromium-based alloy tube with high strength-high elongation is obtained through reasonably controlling the pass deformation and heat treatment temperature matching, thereby effectively solving the problems of high strength and low plasticity of the conventionally processed cobalt-based alloy tube.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. Accordingly, the embodiments are to be considered in all respects as illustrative and not restrictive. The scope of the invention is indicated by the appended claims rather than by the foregoing description, and all changes that come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.
Claims (5)
1. The preparation method of the cobalt-chromium-based alloy seamless pipe with high strength and high plasticity is characterized by comprising the following steps of:
Preparing a cobalt-chromium-based alloy tube blank by adopting a hot extrusion or vacuum centrifugal casting method, and then homogenizing and heat treating in a vacuum tube furnace, wherein the average grain size after homogenizing and heat treating is 200-300 um;
Preheating a cobalt-chromium-based alloy tube blank by adopting an induction heating device, and then carrying out three-roller planetary warm rolling, wherein the reduction of the section of the three-roller planetary warm rolling tube is 85% -90%, and the tube is naturally air-cooled after rolling;
Step three, partial recrystallization annealing, namely cleaning, alkali washing and acid washing and partial recrystallization annealing are carried out on the cobalt-chromium-based alloy pipe rolled by the three-roller planetary temperature in the step two to form a bimodal structure of large grains and small grains;
Cold rolling or cold drawing, namely cold rolling or cold drawing the cobalt-chromium-based alloy pipe annealed in the third step at room temperature, and then straightening and cleaning sequentially to obtain the required pipe, wherein the deformation of each cold rolling or cold drawing is 8% -12%, and high-temperature short-time heat treatment is carried out after each 1-2 times;
Fifthly, performing high-temperature short-time heat treatment, namely performing high-temperature short-time heat treatment on the cobalt-chromium-based alloy pipe in the fourth step in an environment of sealing a vacuum quartz pipe and filling argon with 0.1 MPa;
And step five, the high-temperature short-time heat treatment temperature is 1150-1200 ℃, the heat preservation is carried out for 1-5 min, and the water cooling is carried out.
2. The method for preparing the cobalt-chromium-based alloy seamless pipe with high strength and high plasticity according to claim 1 is characterized in that in the first step, the outer diameter of the cobalt-chromium-based alloy pipe blank is 28-32 mm, the wall thickness is 4-5 mm, the temperature of the homogenizing heat treatment is 1250-1300 ℃, and the heat preservation time is 2-3 h.
3. The method for preparing the cobalt-chromium-based alloy seamless pipe with high strength and high plasticity according to claim 1, wherein in the second step, the preheating temperature of the cobalt-chromium-based alloy pipe blank is 300-400 ℃, and the heat is preserved for 30min.
4. The method for preparing the cobalt-chromium-based alloy seamless pipe with high strength and high plasticity according to claim 1, wherein in the third step, the partial recrystallization annealing temperature is 850-950 ℃, and the temperature is kept for 30-60 min, and the pipe is cooled in a furnace.
5. The method for producing a cobalt-chromium-based alloy seamless pipe having both high strength and high plasticity as claimed in any one of claims 1 to 4, wherein in the above step one, the nominal composition of the cobalt-chromium-based alloy pipe blank is L605 or MP35N.
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| CN112404163B (en) * | 2020-11-04 | 2023-02-28 | 太原科技大学 | A preparation method of high-performance difficult-to-deform metal precision seamless pipe |
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