CN113652620B - Preparation method of beryllium material with high micro-yield strength and high elongation, product and application thereof - Google Patents
Preparation method of beryllium material with high micro-yield strength and high elongation, product and application thereof Download PDFInfo
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- CN113652620B CN113652620B CN202110939028.1A CN202110939028A CN113652620B CN 113652620 B CN113652620 B CN 113652620B CN 202110939028 A CN202110939028 A CN 202110939028A CN 113652620 B CN113652620 B CN 113652620B
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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
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21J—FORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
- B21J1/00—Preparing metal stock or similar ancillary operations prior, during or post forging, e.g. heating or cooling
- B21J1/02—Preliminary treatment of metal stock without particular shaping, e.g. salvaging segregated zones, forging or pressing in the rough
- B21J1/025—Preliminary treatment of metal stock without particular shaping, e.g. salvaging segregated zones, forging or pressing in the rough affecting grain orientation
Abstract
The invention discloses a preparation method of beryllium material with high micro-yield strength and high elongation, a product and application thereof, wherein the method comprises the following steps: and (3) sequentially carrying out high-temperature annealing before forging, four-stage dynamic recrystallization forging and post-forging stabilization treatment on the isostatic beryllium material to obtain the beryllium material with high micro yield strength and high elongation. The method of high-temperature annealing before forging, four-stage dynamic recrystallization forging and stabilization treatment after forging can obviously improve the tissue homogenization of the beryllium material, refine crystal grains, eliminate the residual stress of the material and improve the stability of the beryllium material. The micro yield strength of the beryllium material treated by the method is improved from 30-40MPa to more than 60MPa, the elongation is improved from 1% to more than 8%, and the dimensional change of the beryllium material after being placed at room temperature for six months is less than 0.01%. Compared with the hot isostatic pressing beryllium material, the beryllium material obtained by the method has higher density which reaches over 99.5 percent.
Description
Technical Field
The invention belongs to the field of powder metallurgy material processing, and particularly relates to a preparation method of a beryllium material with high micro yield strength and high elongation, and a product and application thereof.
Background
Beryllium is a strategic and critical material, has a plurality of unique and excellent properties, and is mainly represented as follows: the specific stiffness is the largest in all metals, the specific heat capacity is the largest, the heat conduction performance is the best, the thermal neutron cross section scattering is the largest, and the melting point is the highest in light metals. Due to the characteristics, beryllium materials are widely applied to high-end fields, such as reflection layers of nuclear reactors, reducers, inertial navigation systems of strategic weapons such as attack nuclear submarines and strategic bombers, scientific and technological equipment such as American new generation Weber space telescopes, and aerospace systems such as rocket control cabins, spacecraft outer cover plates and satellite mounting frames.
Although beryllium has many excellent properties, the low elongation limits the development of beryllium as a structural material. The beryllium material is of a close-packed hexagonal structure (HCP), has 4 slip systems at room temperature, is easy to cleave by a basal plane, has low elongation and shows brittle characteristics at room temperature; due to low plasticity, fracture and mechanical damage are easy to occur in the processing and forming processes, and the evolution rule of the processing residual stress is complex; the micro yield strength of the beryllium material is influenced by internal microstructure factors such as grain size, initial texture and the like, and the mechanical property of the beryllium material is obviously asymmetric between tension and compression. The characteristics of brittleness, low plasticity, difficult processing, low micro yield strength and the like of the beryllium material are difficult to ensure the stability and the service life of the beryllium material as an aerospace structural component.
Plastic deformation is an effective method for improving the mechanical properties of materials by improving the texture. A large number of researches show that the material grains can be obviously refined by the pressure processing methods such as extrusion, rolling, forging and the like, and the strength and the plasticity of the material are improved. For beryllium materials in powder metallurgy, the plastic deformation method has great development potential for improving the elongation and the micro yield strength of the beryllium materials. The multistage forging technology has strong capability of refining grains, the true strain acting on the material is very large in the process, the material is subjected to the action of a variable axial external load in the deformation process to generate severe plastic deformation, and the effects of refining the grains, improving low plasticity and improving the micro yield strength are achieved by matching with the recrystallization process under the temperature condition.
At present, stress relief annealing, solid solution aging treatment and cold and hot circulating treatment are traditional methods for beryllium material regulation and control. The material is heated to a certain temperature for a certain time to be kept warm for solid solution, aging and destressing, or is subjected to cold-heat circulation within a certain temperature range, so that residual stress can be eliminated to a certain extent, impurity elements and impurity phases are stabilized, but because beryllium does not have phase change below 1250 ℃ and the content of the impurity elements is low, the single or composite stress-relief annealing treatment, cold-heat circulation treatment, high-temperature solid solution, aging treatment and other methods cannot cause mechanisms such as precipitation phase strengthening, fine grain strengthening, deformation strengthening and the like, so that the micro yield strength is improved, and the low plasticity and low elongation rate determined by a close-packed hexagonal beryllium structure cannot be improved.
Therefore, it is highly desirable in the art to develop a method for improving the beryllium material yield strength and elongation.
Disclosure of Invention
The invention aims to provide a preparation method of beryllium with high micro yield strength and high elongation, a product and application thereof.
The preparation method of the beryllium material with high micro yield strength and high elongation comprises the following steps: and (3) sequentially carrying out high-temperature annealing before forging, four-stage dynamic recrystallization forging and post-forging stabilization treatment on the isostatic beryllium material to obtain the beryllium material with high micro yield strength and high elongation.
The specific steps of the high-temperature annealing before forging are as follows: pressing the beryllium material into a square blank through isostatic pressing, then heating to an annealing temperature, preserving heat, cooling to a first-stage forging temperature along with a furnace to obtain the beryllium material subjected to high-temperature annealing treatment, and preparing for forging.
The annealing temperature is 1000-1100 ℃, the heat preservation time is 30-60 min, and the first-stage forging temperature is 700-800 ℃.
The four-stage dynamic recrystallization forging method comprises the following specific steps: primary forging: cooling the beryllium material subjected to high-temperature annealing treatment to a first-stage forging temperature along with a furnace, and then forging the square billet in three directions; until the deformation in three directions is greater than or equal to 15%; secondary forging: forging the square billet in two directions at the second-stage forging temperature until the deformation in the two directions is greater than or equal to 20%; three-stage forging: forging the non-forged one direction of the secondary forging at the third forging temperature until the deformation is greater than or equal to 15%; four-stage forging: and forging the square billet in three directions in sequence at the fourth forging temperature until the deformation in the three directions is greater than or equal to 10%.
The first-stage forging temperature is 700-800 ℃, the second-stage forging temperature is 700-800 ℃, the third-stage forging temperature is 800-900 ℃, and the fourth-stage forging temperature is 900-1000 ℃.
The stabilizing treatment comprises the following specific steps: rapidly circulating the beryllium material at 0-196 ℃, namely preserving the heat of the beryllium material for 5-30 min at liquid nitrogen at-196 ℃, taking out the beryllium material, putting the beryllium material into an ice-water mixture at 0 ℃, preserving the heat for 5-30 min, and circulating for 3-10 weeks; and finally, heating to 200-300 ℃, preserving heat for 12-24 hours, and finally cooling to room temperature along with the furnace.
Beryllium materials with high micro yield strength and high elongation are prepared according to the preparation method.
The beryllium material with high micro yield strength and high elongation is applied to the preparation of structural components of aviation, marine installations and nuclear reactors.
Principles and advantages
The conventional stress relief annealing treatment and the cold-hot cycle treatment can only eliminate partial residual stress of the beryllium material, and the high-temperature solution treatment and the high-temperature aging treatment can stabilize impurity elements and impurity phases of the beryllium material, but coarsen crystal grains and superpose the residual stress in the cooling process. Therefore, the purpose of improving the micro yield strength and the elongation of the beryllium material cannot be achieved by singly adopting the methods of stress relief annealing, cold-hot circulation, high-temperature solid solution, high-temperature aging and the like.
The high-temperature annealing treatment before forging is very important, the softening effect of the beryllium material is not enough due to the removal of the high-temperature annealing step or the reduction of the annealing temperature and the heat preservation time, the sufficient forging deformation cannot be borne, and the cracking phenomenon occurs in the four-stage dynamic recrystallization forging process; the unreasonable high-temperature annealing causes the beryllium to be deformed unevenly in the forging process, further causes the tissue to be uneven, and cannot achieve the purpose of greatly improving the micro yield strength and the elongation of the beryllium. Heating the beryllium material to 1000-1100 ℃ and preserving heat for 30-60 min, so that on one hand, the temperature of the beryllium material is uniform, the compressive stress introduced in the isostatic pressing process is partially eliminated, the deformability is improved, and the forging processing is facilitated; on the other hand, the crystal grains grow up partially, the number of crystal boundaries is reduced, the obstruction to dislocation and the constraint capacity to deformation are reduced, so that the yield point of the beryllium material is reduced, and the forging deformation is improved.
On the whole, the four-stage dynamic recrystallization forging deformation realizes large-range crushing of thick original grains, further refines the grains through recrystallization, releases stress, improves macrosegregation to a certain extent, welds internal pores, obtains reasonable fiber direction distribution and improves material density. The beryllium material is deformed by adopting different times of forging amount, original crystal grains are compressed and crushed along the forging direction under the action of intragranular sliding, thicker and larger crystal grains are crushed again along with the increase of the forging deformation amount, more and smaller crushed crystal grains begin to appear, the size of the crystal grains is promoted to be more uniform, more and more dislocations are generated in the crystal grains and are wound, and the subcrystal boundary is obviously increased. Secondly, controlling the single forging deformation rate, balancing the deformation and recrystallization processes, avoiding the local forging condition of single forging and obtaining more uniform grain structure; the dynamic recovery and recrystallization are combined to release internal stress, the work hardening is reduced to a certain degree, and the cracking phenomenon after a certain deformation is avoided. Then, through forging three directions, confirm the orientation that is the easiest to warp and forge until its deflection satisfies the requirement, need forge the other two directions simultaneously and provide even atress for inside, guarantee that structural stress reduces. The problem of structural uniformity is solved by repeated forging for multiple times, and the problems of more deformation dead zones, layered structures and flaky coarse crystals are avoided. And finally, the forging temperature is increased along with the pass, on one hand, in the later stage of forging, the work hardening accumulation is serious, the softening degree of the beryllium material caused by dynamic recrystallization is slightly larger than the work hardening degree caused by deformation due to the increased temperature, the driving force of the recovery recrystallization is increased, the dislocation density is reduced, the plasticity is correspondingly improved, and the subsequent forging deformation is easy to perform. On the other hand, the filament texture in the beryllium < 1010 > direction is gradually enhanced, and after the filament texture is formed, the basal plane {0001} is parallel to the forging direction, and the material strength is improved and the plastic deformation is not facilitated due to the fact that the Schmid factor is small and is in hard orientation, and slippage is difficult to carry out. Compared with other plastic deformation technologies, the four-stage dynamic recrystallization forging deformation process has the characteristics of simple equipment, convenience in operation and low cost, and can be directly used for industrial production.
The stabilizing treatment after forging is an important means for eliminating the overhigh residual stress and improving the stability. The rapid circulation at 0-196 ℃ and the low-temperature aging process at 200-300 ℃ are processes of superposing external thermal stress and releasing stress so as to reduce residual stress, and the phenomena of phase change, recovery and recrystallization can not be generated to further initiate the evolution of a tissue structure. After forging, the stabilizing treatment can avoid the phenomena of unstable and unreliable structure caused by relaxation and release of residual stress of the beryllium material in the long-term storage and service processes. It is noted that the stabilizing treatment is carried out on the basis of not reducing the micro yield strength and the elongation percentage of the beryllium material, and the treated beryllium material still maintains good toughness.
The invention has the beneficial effects that: 1) the method of high-temperature annealing before forging, four-stage dynamic recrystallization forging and stabilization treatment after forging can obviously improve the tissue homogenization of the beryllium material, refine crystal grains, eliminate the residual stress of the material and improve the stability of the beryllium material. 2) The micro yield strength of the beryllium material treated by the method is improved from 30-40MPa to more than 60MPa, the elongation is improved from 1% to more than 8%, and the dimensional change of the beryllium material after being placed at room temperature for six months is less than 0.01%. 3) Compared with the beryllium material with hot isostatic pressing, the beryllium material obtained by the method has higher density which reaches over 99.5 percent.
In conclusion, the invention improves the micro yield strength and the elongation of the beryllium material. The method has a very positive effect on improving the precision and reliability and prolonging the service life of the beryllium material structure device.
Detailed Description
In order to further enhance the understanding of the present invention, the following detailed description of the present invention is provided in connection with examples, and it should be noted that the scope of the present invention is not limited by the following examples.
Example 1:
heating the isostatic beryllium material to 1050 ℃, preserving the heat for 45min, and cooling the material to 750 ℃ along with the furnace. Forging is carried out; first-stage forging, wherein the square billet is forged in three directions at 750 ℃ until the deformation in the three directions is 25%; secondary forging: forging the square billet in two directions at 780 ℃ until the deformation in the two directions is 30 percent; three-stage forging: forging the non-forged direction in the secondary forging at 850 ℃ until the deformation amount is 15%; four-stage forging: the billet was forged in three directions in sequence at 950 ℃ until the amount of deformation in the three directions was 20%. Rapidly circulating the beryllium material at 0-196 ℃, namely preserving the heat of the beryllium material for 20min at liquid nitrogen at-196 ℃, taking out the beryllium material, putting the beryllium material into an ice-water mixture at 0 ℃, preserving the heat for 20min, and circulating for 6 weeks; finally heating to 250 ℃, preserving heat for 18h, and finally cooling to room temperature along with the furnace. The beryllium material has the micro yield strength of 79MPa, the elongation of 11.0 percent and the dimensional change of 0.003 percent after being placed at room temperature for six months.
Comparative example 1:
compared with the example 1, only the high-temperature annealing treatment step is different, other steps are the same, and the annealing treatment of the comparative example is as follows: and (3) heating the isostatic beryllium material to 800 ℃, preserving heat for 45min, cooling to 750 ℃ along with the furnace, and forging (after forging, a blank can be seen to have fine cracks). The final beryllium material has a micro yield strength of 56MPa, an elongation of 4.1% and a dimensional change of 0.010% after being placed at room temperature for six months.
In this comparative example, the high-temperature annealing temperature before forging was lowered, the sample was insufficiently softened, and lost the ability to withstand sufficient deformation during the subsequent four-stage dynamic recrystallization forging process, as compared with example 1, forging according to the four-stage dynamic recrystallization forging parameters of example 1 resulted in the occurrence of a forging crack phenomenon, which also resulted in the reduction of the yield strength and elongation, and generally, the occurrence of cracks was substantially a waste product.
Comparative example 2:
compared with the example 1, only the high-temperature annealing treatment step is different, other steps are the same, and the annealing treatment of the comparative example is as follows: and (3) heating the isostatic beryllium material to 1050 ℃, preserving the heat for 10min, and cooling the material to 750 ℃ along with the furnace to forge the material (after forging, the same as the comparative example 1, the fine cracks also appear). The finally obtained beryllium material has the micro yield strength of 51MPa, the elongation of 4.3 percent and the dimensional change of 0.011 percent after being placed at room temperature for six months.
In the comparative example, compared with example 1, the high-temperature annealing holding time before forging is shortened, the sample piece is insufficient in softening degree and loses the capacity of bearing enough deformation in the subsequent four-stage dynamic recrystallization forging process, forging is carried out according to the four-stage dynamic recrystallization forging parameters of example 1, the phenomenon of forging cracking and the phenomenon of waste products occur, and the micro yield strength and the elongation rate are reduced.
Comparative example 3:
compared with the example 1, only the high-temperature annealing treatment step is different, other steps are the same, and the annealing treatment of the comparative example is as follows: and (3) heating the isostatic beryllium material to 1150 ℃, preserving heat for 70min, cooling to 750 ℃ along with the furnace, and forging. The final beryllium material obtained has the micro yield strength of 51MPa, the elongation of 6.2 percent and the dimensional change of 0.009 percent after being placed at room temperature for six months.
In this comparative example, increasing the high temperature annealing temperature before forging resulted in a significant decrease in the micro yield strength and elongation of the treated beryllium material compared to example 1, due to: due to the fact that the beryllium material has uneven local structures such as coarse crystals or mixed crystals and the like and even has the phenomenon of overburning and overheating due to excessively high temperature and excessively long heat preservation time, the beryllium material is deformed unevenly in the forging process due to the unreasonable high-temperature annealing, the structure is uneven, and the micro yield strength and the elongation of the beryllium material are greatly improved.
Comparative example 4:
compared with the embodiment 1, only the forging process steps are different, and other steps are the same; the forging process in the comparative example comprises the following steps: first-stage forging, wherein the square billet is forged in three directions at 750 ℃ until the deformation in the three directions is 25%; secondary forging: the billet was forged at 780 ℃ in both directions until the amount of deformation in both directions was 30%. The final beryllium material has a micro yield strength of 46MPa, an elongation of 4.8 percent and a size change of 0.012 percent after being placed at room temperature for six months.
In this comparative example, only the forging process step was different compared to example 1. The comparative example only carries out two-stage recrystallization forging, the total deformation amount of the forging is not large enough, part of coarse grains exist, and the mixed crystal phenomena of uneven grain size and the like occur; meanwhile, the dislocation and the sub-grain boundary in the crystal grains are not enough, and the fine crystal strengthening is not obvious; in the second-stage forging process, forging is carried out in only two directions, so that the stress inside the beryllium material is uneven, and the structural stress is increased. In conclusion, reducing the forging pass leads to the problem of non-uniformity of the structure, and the problems of more deformation dead zones, layered structures and flaky coarse crystals appear, thereby further influencing the effective improvement of the micro yield strength and the elongation percentage.
Comparative example 5:
compared with the embodiment 1, only the forging process steps are different, and other steps are the same; the forging process in the comparative example comprises the following steps: first-stage forging, wherein the square billet is forged in three directions at 750 ℃ until the deformation in the three directions is 25%; secondary forging: forging the square billet in two directions at 780 ℃ until the deformation in the two directions is 30 percent; three-stage forging: the secondary forging was forged in one direction, unforged, at 850 ℃ until the deformation was 15%. The final beryllium material has a micro yield strength of 59MPa, an elongation of 6.1% and a dimensional change of 0.010% after being placed at room temperature for six months.
In this comparative example, only the forging process step was different compared to example 1. The comparative example only carries out three-stage recrystallization forging, the total deformation amount of the forging is not large enough, part of coarse grains exist, and the mixed crystal phenomena of uneven grain size and the like occur; meanwhile, the dislocation and the subgrain boundary in the crystal grain are not enough, and the fine crystal strengthening is not obvious. In conclusion, reducing the forging pass leads to the problem of non-uniformity of the structure, and the problems of more deformation dead zones, layered structures and flaky coarse crystals appear, thereby further influencing the effective improvement of the micro yield strength and the elongation percentage.
Comparative example 6:
compared with the embodiment 1, only the forging process steps are different, and other steps are the same; the forging process in the comparative example comprises the following steps: first-stage forging, wherein the square billet is forged in three directions at 750 ℃ until the deformation in the three directions is 5%; secondary forging: forging the square billet in two directions at 780 ℃ until the deformation in the two directions is 10 percent; three-stage forging: the secondary forging was forged in one direction, not forged, at 850 ℃ until the deformation was 5%. Four-stage forging: the billet was forged in three directions in sequence at 950 ℃ until the amount of deformation in the three directions was 5%. The final beryllium material has a micro yield strength of 39MPa, an elongation of 3.1% and a dimensional change of 0.005% after being placed at room temperature for six months.
In this comparative example, only the forging process step was different compared to example 1. The four-stage recrystallization forging of the comparative example has the advantages that the forging deformation of each stage is reduced, the total deformation is not large enough, part of coarse grains exist, and the mixed crystal phenomena of uneven grain size and the like occur; the single forging deformation is too small, and the single forging has local forging condition to obtain uneven grain structure; dynamic recovery and recrystallization cannot be effectively initiated, the deformation and recrystallization processes cannot be balanced, the work hardening and softening processes are not coordinated, and the cracking phenomenon can occur after a certain amount of deformation is locally achieved. The above phenomena will ultimately affect the effective improvement of the micro yield strength and elongation.
Comparative example 7:
compared with the embodiment 1, only the forging process steps are different, and other steps are the same; the forging process in the comparative example comprises the following steps: first-stage forging, wherein the square billet is forged in three directions at 850 ℃ until the deformation in the three directions is 25%; secondary forging: forging the square billet in two directions at 880 ℃ until the deformation in the two directions is 30 percent; three-stage forging: forging the non-forged one direction in the secondary forging at 950 ℃ until the deformation amount is 15%; four-stage forging: the billet is forged in three directions in sequence at 1050 ℃ until the deformation in the three directions is 20%. The final beryllium material has a micro yield strength of 38MPa, an elongation of 7.2% and a dimensional change of 0.008% after being placed at room temperature for six months.
In this comparative example, only the forging process step was different compared to example 1. The forging temperature of each stage of the four-stage dynamic recrystallization forging is increased by 100 ℃. The temperature of each stage of forging is too high, so that the softening degree of the beryllium material caused by dynamic recrystallization is far greater than the work hardening degree generated by deformation, the dislocation density is reduced, and the work hardening effect is not obvious; the dynamic recrystallization degree is increased, the phenomenon of growing and coarsening crystal grains is serious, and the micro yield strength and the elongation of the beryllium material are not favorably improved.
Comparative example 8:
compared with the embodiment 1, only the forging process steps are different, and other steps are the same; the forging process in the comparative example comprises the following steps: first-stage forging, wherein the square billet is forged in three directions at 650 ℃ until the deformation in the three directions is 25 percent; secondary forging: forging the square billet in two directions at 680 ℃ until the deformation in the two directions is 30 percent; three-stage forging: forging the non-forged one direction in the secondary forging at 750 ℃ until the deformation is 15%; four-stage forging: the billet is forged in three directions in turn at 850 ℃ until the deformation in the three directions is 20%. The final beryllium material obtained has a micro yield strength of 49MPa, an elongation of 5.5 percent and a size change of 0.013 percent after being placed at room temperature for six months.
In this comparative example, only the forging process step was different compared to example 1. Each stage of the four-stage dynamic recrystallization forging is performed at a temperature reduced by 100 ℃. The temperature of each stage of forging is too low, so that the softening degree of the beryllium material caused by dynamic recrystallization is far smaller than the work hardening degree generated by deformation, and the dislocation density grows; the dynamic recrystallization degree is reduced, and the residual stress and the deformation energy storage release are small, so that the subsequent forging deformation is not facilitated, the forging cracking phenomenon is caused, and waste products are caused.
Comparative example 9:
compared with the embodiment 1, only the stabilizing treatment process is different, and other steps are the same; this comparative example was not subjected to stabilization treatment. The final beryllium material has 75MPa of micro yield strength, 10.8 percent of elongation and 0.095 percent of dimensional change after being placed at room temperature for six months.
In this comparative example, no stabilization treatment was performed as compared with example 1. After forging, the beryllium material has no stress release, and the process of reducing the residual stress can lead the beryllium material to have the phenomena of unstable and unreliable structure caused by the relaxation and release of the residual stress in the long-term storage and service process.
Comparative example 10:
compared with the embodiment 1, only the stabilizing treatment process is different, and other steps are the same; the stabilizing treatment process in this comparative example comprises the following steps: rapidly circulating the beryllium material at 0-196 ℃, namely preserving the heat of the beryllium material for 20min at liquid nitrogen of-196 ℃, taking out the beryllium material, putting the beryllium material into an ice-water mixture of 0 ℃, preserving the heat for 20min, and circulating for 6 weeks. The final beryllium material has a micro yield strength of 79MPa, an elongation of 11.0% and a dimensional change of 0.043% after being placed at room temperature for six months.
In this comparative example, the low temperature aging treatment after rapid cycling at 0 to-196 ℃ was reduced, compared to example 1, only by the stabilization treatment process. Rapid cycling at 0 to-196 ℃ is a process of adding thermal stress and neutralizing the original stress state after forging, thereby reducing the residual stress. The beryllium material is heated to 250 ℃, the low-temperature aging process of heat preservation for 18 hours does not generate tissue change, and the process is a process of slowly releasing stress. But only rapid circulation at 0-196 ℃ will lead the stress of the beryllium material to be released insufficiently, and the residual stress relaxation and release-induced structural instability and unreliability of the beryllium material during long-term storage and service can be caused.
Comparative example 11:
compared with the embodiment 1, only the stabilizing treatment process is different, and other steps are the same; the stabilizing treatment process in this comparative example comprises the following steps: heating the beryllium material to 250 ℃, preserving the heat for 18h, and finally cooling the beryllium material to room temperature along with the furnace. The final beryllium material obtained has the micro yield strength of 79MPa, the elongation of 11.0 percent and the size change of 0.035 percent after being placed at room temperature for six months.
The stabilization treatment after forging is an important means for eliminating the excessive residual stress and improving the stability. The rapid circulation at 0-196 ℃ and the low-temperature aging process at 200-300 ℃ are processes of superposing external thermal stress and releasing stress so as to reduce residual stress, and the phenomena of phase change, recovery and recrystallization can not be generated to further initiate the evolution of a tissue structure. After forging, the stabilizing treatment can avoid the phenomena of unstable and unreliable structure caused by relaxation and release of residual stress of the beryllium material in the long-term storage and service processes. It is noted that the stabilizing treatment is carried out on the basis of not reducing the micro yield strength and the elongation percentage of the beryllium material, and the treated beryllium material still maintains good toughness.
In this comparative example, the rapid cycle treatment at 0 to-196 ℃ was reduced compared to example 1, except that the stabilization treatment process was different. Rapid cycling at 0 to-196 ℃ is a process of adding thermal stress and neutralizing the original stress state after forging, thereby reducing the residual stress. The beryllium material is heated to 250 ℃, the low-temperature aging process of heat preservation for 18 hours does not generate the change of the structure, and the process is a process of slowly releasing the stress. But only 250 ℃ is carried out, the stress release of the beryllium material is insufficient after the low-temperature aging of 18h of heat preservation, and the phenomena of unstable and unreliable structure caused by the relaxation and release of residual stress of the beryllium material in the long-term storage and service process can be caused.
Example 2:
heating the isostatic beryllium material to 1000 ℃, preserving the heat for 60min, and cooling the material to 700 ℃ along with the furnace. Forging, namely forging the square billet in three directions at 700 ℃ until the deformation in the three directions is 15%; secondary forging: forging the square billet in two directions at 700 ℃ until the deformation in the two directions is 20 percent; three-stage forging: forging the non-forged direction in the secondary forging at 800 ℃ until the deformation is 15%; four-stage forging: the billet is forged in three directions in sequence at 900 ℃ until the deformation in the three directions is 10 percent. Rapidly circulating the beryllium material at 0-196 ℃, namely preserving the heat of the beryllium material for 5min at liquid nitrogen at-196 ℃, taking out the beryllium material, putting the beryllium material into an ice-water mixture at 0 ℃, preserving the heat for 5min, and circulating for 5 weeks; finally heating to 200 ℃, preserving heat for 12h, and finally cooling to room temperature along with the furnace. The beryllium material has the micro yield strength of 73MPa, the elongation of 9.2 percent and the dimensional change of 0.009 percent after being placed at room temperature for six months.
Example 3:
heating the isostatic beryllium material to 1020 ℃, preserving the heat for 55min, and cooling the material to 750 ℃ along with the furnace. Forging is carried out; first-stage forging, wherein the square billet is forged in three directions at 750 ℃ until the deformation in the three directions is 20%; secondary forging: forging the square billet in two directions at 800 ℃ until the deformation in the two directions is 25 percent; three-stage forging: forging the non-forged direction in the secondary forging at 800 ℃ until the deformation is 20%; four-stage forging: the billet is forged in three directions in sequence at 900 ℃ until the deformation in the three directions is 20 percent. Rapidly circulating the beryllium material at 0-196 ℃, namely preserving the heat of the beryllium material for 15min at liquid nitrogen at-196 ℃, taking out the beryllium material, putting the beryllium material into an ice-water mixture at 0 ℃, preserving the heat for 15min, and circulating for 10 weeks; finally heating to 300 ℃, preserving heat for 24h, and finally cooling to room temperature along with the furnace. The beryllium material has the micro yield strength of 81MPa, the elongation rate of 8.1 percent and the dimensional change of 0.006 percent after being placed at room temperature for six months.
Example 4:
heating the isostatic beryllium material to 1030 ℃, preserving the heat for 50min, and cooling the material to 750 ℃ along with the furnace. Forging is carried out; first-stage forging, wherein the square billet is forged in three directions at 750 ℃ until the deformation in the three directions is 20%; secondary forging: forging the square billet in two directions at 750 ℃ until the deformation in the two directions is 20 percent; three-stage forging: forging the non-forged direction in the secondary forging at 800 ℃ until the deformation is 20%; four-stage forging: the billet is forged in three directions in sequence at 900 ℃ until the deformation in the three directions is 10 percent. Rapidly circulating the beryllium material at 0-196 ℃, namely preserving the heat of the beryllium material for 20min at liquid nitrogen at-196 ℃, taking out the beryllium material, putting the beryllium material into an ice-water mixture at 0 ℃, preserving the heat for 20min, and circulating for 8 weeks; finally heating to 200 ℃, preserving heat for 12h, and finally cooling to room temperature along with the furnace. The beryllium material has the micro yield strength of 70MPa, the elongation of 9.6 percent and the dimensional change of 0.007 percent after being placed at room temperature for six months.
Example 5:
heating the isostatic beryllium material to 1040 ℃, preserving the heat for 45min, and cooling the material to 750 ℃ along with the furnace. Forging is carried out; first-stage forging, wherein the square billet is forged in three directions at 750 ℃ until the deformation in the three directions is 15%; secondary forging: forging the square billet in two directions at 800 ℃ until the deformation in the two directions is 30 percent; three-stage forging: forging the non-forged direction in the secondary forging at 850 ℃ until the deformation amount is 15%; four-stage forging: the billet was forged in three directions in sequence at 950 ℃ until the amount of deformation in the three directions was 10%. Rapidly circulating the beryllium material at 0-196 ℃, namely preserving the heat of the beryllium material for 30min at liquid nitrogen at-196 ℃, taking out the beryllium material, putting the beryllium material into an ice-water mixture at 0 ℃, preserving the heat for 30min, and circulating for 8 weeks; finally heating to 300 ℃, preserving heat for 12h, and finally cooling to room temperature along with the furnace. The beryllium material has the micro yield strength of 66MPa, the elongation of 10.9 percent and the dimensional change of 0.008 percent after being placed at room temperature for six months.
Example 6:
heating the isostatic beryllium material to 1060 ℃, preserving the heat for 40min, and cooling the material to 750 ℃ along with the furnace. Forging is carried out; first-stage forging, wherein the square billet is forged in three directions at 750 ℃ until the deformation in the three directions is 20%; secondary forging: forging the square billet in two directions at 800 ℃ until the deformation in the two directions is 25 percent; three-stage forging: forging the non-forged direction in the secondary forging at 900 ℃ until the deformation amount is 15%; four-stage forging: the billet was forged at 950 ℃ in three directions in sequence until the amount of deformation in the three directions was 15%. Rapidly circulating the beryllium material at 0-196 ℃, namely preserving the heat of the beryllium material for 10min at liquid nitrogen at-196 ℃, taking out the beryllium material, putting the beryllium material into an ice-water mixture at 0 ℃, preserving the heat for 10min, and circulating for 10 weeks; finally heating to 280 ℃, preserving the heat for 20 hours, and finally cooling to room temperature along with the furnace. The beryllium material has the micro yield strength of 72MPa, the elongation rate of 10.2 percent and the dimensional change of 0.006 percent after being placed at room temperature for six months.
Example 7:
heating isostatic beryllium material to 1080 ℃, preserving heat for 40min, and cooling to 750 ℃ along with the furnace. Forging is carried out; first-stage forging, wherein the square billet is forged in three directions at 750 ℃ until the deformation in the three directions is 20%; secondary forging: forging the square billet in two directions at 750 ℃ until the deformation in the two directions is 20%; three-stage forging: forging the non-forged direction in the secondary forging at 900 ℃ until the deformation is 15%; four-stage forging: the billet is forged in three directions in sequence at 1000 ℃ until the deformation in the three directions is 20%. Rapidly circulating the beryllium material at 0-196 ℃, namely preserving the heat of the beryllium material for 20min at liquid nitrogen at-196 ℃, taking out the beryllium material, putting the beryllium material into an ice-water mixture at 0 ℃, preserving the heat for 20min, and circulating for 3 weeks; finally heating to 280 ℃, preserving heat for 16h, and finally cooling to room temperature along with the furnace. The beryllium material has the micro yield strength of 71MPa, the elongation of 10.6 percent and the dimensional change of 0.005 percent after being placed at room temperature for six months.
Example 8:
heating isostatic pressing beryllium material to 1100 ℃, preserving heat for 30min, and cooling to 800 ℃ along with the furnace. Forging is carried out; first-stage forging, wherein the square billet is forged in three directions at 800 ℃ until the deformation in the three directions is 30%; secondary forging: forging the square billet in two directions at 800 ℃ until the deformation in the two directions is 30 percent; three-stage forging: forging the non-forged direction in the secondary forging at 900 ℃ until the deformation amount is 15%; four-stage forging: the billet is forged in three directions in sequence at 1000 ℃ until the deformation in the three directions is 30%. Rapidly circulating the beryllium material at 0-196 ℃, namely preserving the heat of the beryllium material for 20min at liquid nitrogen at-196 ℃, taking out the beryllium material, putting the beryllium material into an ice-water mixture at 0 ℃, preserving the heat for 20min, and circulating for 10 weeks; finally heating to 300 ℃, preserving heat for 24h, and finally cooling to room temperature along with the furnace. The beryllium material has the micro yield strength of 73MPa, the elongation of 10.1 percent and the dimensional change of 0.004 percent after being placed at room temperature for six months.
Example 9:
heating the isostatic beryllium material to 1100 ℃, preserving the heat for 60min, and cooling the material to 800 ℃ along with the furnace. Forging is carried out; first-stage forging, wherein the square billet is forged in three directions at 800 ℃ until the deformation in the three directions is 15%; secondary forging: forging the square billet in two directions at 800 ℃ until the deformation in the two directions is 20 percent; three-stage forging: forging the non-forged direction in the secondary forging at 900 ℃ until the deformation amount is 15%; four-stage forging: the billet is forged in three directions in sequence at 1000 ℃ until the deformation in the three directions is 10 percent. Rapidly circulating the beryllium material at 0-196 ℃, namely preserving the heat of the beryllium material for 10min at liquid nitrogen at-196 ℃, taking out the beryllium material, putting the beryllium material into an ice-water mixture at 0 ℃, preserving the heat for 10min, and circulating for 3 weeks; and finally, heating to 250 ℃, preserving the heat for 15 hours, and finally cooling to the room temperature along with the furnace. The beryllium material has the micro yield strength of 62MPa, the elongation of 11.4 percent and the dimensional change of 0.008 percent after being placed at room temperature for six months.
Claims (3)
1. A preparation method of beryllium material with high micro yield strength and high elongation comprises the following steps: sequentially carrying out high-temperature annealing before forging, four-stage dynamic recrystallization forging and stabilizing treatment after forging on the isostatic pressing beryllium material to obtain the beryllium material with high micro yield strength and high elongation;
the specific steps of the high-temperature annealing before forging are as follows: pressing the beryllium material into a square blank through isostatic pressing, then heating to an annealing temperature, preserving heat, cooling to a first-stage forging temperature along with a furnace to obtain the beryllium material subjected to high-temperature annealing treatment, and preparing for forging, wherein: the annealing temperature is 1000-1100 ℃, the heat preservation time is 30-60 min, and the first-stage forging temperature is 700-800 ℃;
the four-stage dynamic recrystallization forging method comprises the following specific steps: primary forging: cooling the beryllium material subjected to high-temperature annealing treatment to a first-stage forging temperature along with a furnace, and then forging the square billet in three directions; until the deformation in three directions is greater than or equal to 15%; secondary forging: forging the square billet in two directions at the second-stage forging temperature until the deformation in the two directions is greater than or equal to 20%; three-stage forging: forging the non-forged one direction of the secondary forging at the third forging temperature until the deformation is greater than or equal to 15%; four-stage forging: sequentially forging the square billet in three directions at a fourth forging temperature until the deformation in the three directions is more than or equal to 10%; wherein: the first-stage forging temperature is 700-800 ℃, the second-stage forging temperature is 700-800 ℃, the third-stage forging temperature is 800-900 ℃, and the fourth-stage forging temperature is 900-1000 ℃;
the stabilizing treatment comprises the following specific steps: rapidly circulating the beryllium material at 0-196 ℃, namely preserving the heat of the beryllium material for 5-30 min at liquid nitrogen at-196 ℃, taking out the beryllium material, putting the beryllium material into an ice-water mixture at 0 ℃, preserving the heat for 5-30 min, and circulating for 3-10 weeks; and finally, heating to 200-300 ℃, preserving heat for 12-24 hours, and finally cooling to room temperature along with the furnace.
2. Beryllium material with high micro yield strength and high elongation is prepared according to the preparation method of claim 1.
3. Use of high micro yield strength and high elongation beryllium material according to claim 2 for the preparation of structural components for aeronautics, maritime installations, nuclear reactors.
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| US3954514A (en) * | 1975-04-02 | 1976-05-04 | Lockheed Missiles & Space Company, Inc. | Textureless forging of beryllium |
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| GB919423A (en) * | 1960-10-04 | 1963-02-27 | Atomic Energy Authority Uk | Metallurgical process for working beryllium |
| US3774290A (en) * | 1972-02-09 | 1973-11-27 | Brush Wellman | Method of fabricating a beryllium-titanium composite |
| US3954514A (en) * | 1975-04-02 | 1976-05-04 | Lockheed Missiles & Space Company, Inc. | Textureless forging of beryllium |
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