CN113088847B - Preparation method of high-density high-toughness ultrafine-grained molybdenum - Google Patents
Preparation method of high-density high-toughness ultrafine-grained molybdenum Download PDFInfo
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Abstract
The invention discloses a preparation method of high-density high-toughness ultrafine-grained metal pure molybdenum, which is characterized in that a repeated radial-axial forging method is adopted to carry out large plastic deformation on the pure molybdenum, the total deformation is more than 300%, and repeated multidirectional forging has strong grain refining capability, so that various mechanical properties of a molybdenum material are improved; therefore, the pure molybdenum prepared by the method has fine crystal grains, the average grain size is 1-5 mu m, and the microstructure is uniform; the relative density is high, and the average density is more than or equal to 99.9 percent; the mechanical property is excellent, the tensile strength at room temperature is more than or equal to 680MPa, and the elongation is more than or equal to 51 percent. In the method, annealing at a temperature close to the recrystallization temperature is adopted after multidirectional forging, so that the anisotropy of the processing structure and the mechanical property is improved. The multidirectional forging process adopted by the invention is simple, low in cost and easy to realize industrial production.
Description
Technical Field
The invention belongs to the technical field of metal processing, and particularly relates to a preparation method of high-density high-toughness ultrafine-grained metal pure molybdenum.
Background
Pure molybdenum is a rare metal with important strategic significance, has the advantages of high melting point, high elastic modulus, high-temperature strength, low linear expansion coefficient, good electric and thermal conductivity and the like, and is widely applied to the fields of aerospace, power electronics, medical treatment, war industry and the like. However, molybdenum has intrinsic brittleness and poor plasticity, which results in difficult processing and low yield, and also limits its further scale application. With the development of modern technology, the market puts higher and higher requirements on the microstructure and the performance of molybdenum, for example, products such as electronic target material industry, military chemical type covers and the like have strict requirements on the purity, the grain size, the density, the uniformity and the like of molybdenum, and the traditional processing methods such as powder metallurgy, forging, rolling and the like cannot meet the technical requirements, so that the search for new preparation and processing technologies is necessary.
The influence of different die forging processes on the performance of the metal molybdenum rod is reported in a text of 'the influence of the forging process on the structure and the performance of the powder metallurgy molybdenum rod', the forging process is divided into 6 die times, the deformation of each die time is 10-20%, and the die forging molybdenum rod with the tensile strength of 667MPa and the elongation of only 26% and the average grain size of about 40 mu m is obtained by tempering at 1100 ℃ for 15min every two die times.
A powder metallurgy and rolling process is adopted in a production method of a fine-grain plane molybdenum target material (ZL201510902253) to prepare the fine-grain molybdenum target material, but the average grain size of the fine-grain plane molybdenum target material still reaches 40-80 mu m.
Wangcheng discloses a pure molybdenum forging process in 'a large-size fine-grain molybdenum rod and a preparation method thereof' (application number 201911034992). The molybdenum rod with fine and uniform grains is obtained, the room-temperature tensile strength reaches 550MPa, and the elongation after fracture reaches 25%.
The patent of rapid preparation technology of fine grain molybdenum plate (ZL2019102663670) applied by the subject group combines the high-purity molybdenum powder microwave sintering blank making and cross rolling technology to prepare a uniform fine grain molybdenum plate, but the technology is difficult to realize batch production.
Disclosure of Invention
The invention aims to provide a preparation method of high-density high-toughness ultrafine-grained pure molybdenum metal, and the pure molybdenum metal prepared by the method has the characteristics of good shaping, fine texture grain size and uniform crystal phase.
The preparation method of the high-density high-toughness ultrafine grain metal pure molybdenum comprises the following steps:
the method comprises the following steps: adopting a sintered molybdenum cylindrical rod as a raw material, and carrying out heat treatment on the sintered molybdenum cylindrical rod in a hydrogen atmosphere to obtain a treated molybdenum rod;
step two: placing the molybdenum rod treated in the step one on the preheated upper and lower arc-shaped drill plates to perform radial forging for 3 times; the radial forging process is sequentially performed in three different directions, namely after each radial forging, the molybdenum rods rotate 60 ℃ towards the same direction; obtaining a radially forged molybdenum rod;
step three: tempering the radially forged molybdenum rod in a hydrogen atmosphere; obtaining a molybdenum rod after tempering treatment;
step four: axially forging the molybdenum rod subjected to tempering treatment in the third step on the preheated upper and lower plane drill plates for 3-4 passes to obtain an axially forged molybdenum rod;
step five: tempering the molybdenum rod axially forged in the fourth step in a hydrogen atmosphere to obtain a molybdenum rod subjected to secondary tempering;
step six: repeating the steps from the second step to the fifth step for 1 to 6 times, repeating the radial forging and axial forging on the molybdenum rod, and finally finishing the forging process by the fifth step or the second step to obtain primary high-density high-toughness ultrafine-grained metal pure molybdenum;
step seven: and annealing the primary high-density high-toughness ultrafine grain metal pure molybdenum in the sixth step to obtain the high-density high-toughness ultrafine grain metal pure molybdenum.
In the first step, the sintered molybdenum cylindrical rod is a commonly used molybdenum rod in the current industrial production, the relative density of the sintered molybdenum cylindrical rod is 94-96%, and the average grain size is 50-80 μm; the heat treatment temperature is 1200-1300 ℃, and the treatment time is 30-60 min.
In the second step, the radian of the upper arc-shaped drilling plate and the lower arc-shaped drilling plate is 120-150 degrees, and the preheating temperature is 620-750 ℃; the forging rate of radial forging is 500-800 times/min, and the deformation of each forging is 10-25%.
In the third step, the tempering temperature is 1000-1200 ℃, and the tempering time is 5-10 min.
In the fourth step, the preheating temperature is 620-750 ℃; the downward pressing speed of the hammer head during axial forging is 10-100 mm/s, and the deformation rate of each pass is 15-30%.
In the fifth step, the tempering temperature is 1000-1200 ℃, and the tempering time is 5-10 min.
In the sixth step, when the second to fifth steps are repeated, the tempering temperature needs to be gradually reduced, that is, the tempering temperature in the fifth step is lower than the tempering temperature in the third step, and the tempering temperature in the third step in the second cycle is lower than the tempering temperature in the fifth step in the first cycle.
And seventhly, annealing is carried out in a hydrogen atmosphere, the annealing temperature is 600-1200 ℃, and the heat preservation time is 30-90 min.
The high-density high-toughness ultrafine-grained pure metal molybdenum is prepared by the method, the density of the pure metal molybdenum is more than or equal to 99.9%, the room-temperature tensile strength is more than or equal to 680MPa, the elongation is more than or equal to 51%, and the average grain size is 1-5 μm.
The principle of the invention is as follows: since molybdenum is a high-stacking fault energy material, slippage is the primary mode of plastic deformation. In the process of multidirectional forging (MDF), along with the change of the deformation direction and the violent increase of the deformation amount, original coarse grains are forced to change the orientation and are possibly crushed, the rotation of crystal lattices is intensified, the distortion degree of the grains is increased, and high-density dislocation which is continuously generated is accumulated, so that the recrystallization and the refinement of the grains are promoted, namely, the stress strain is generated to induce the grain refinement; meanwhile, dislocation cross slip generated by grain deformation causes intersection of geometrically necessary interfaces (GNBs), so that original grains are separated into dislocation cellular structures, and small-sized equiaxed structures are further formed, and the grains are further refined. In addition, due to the high dislocation energy of molybdenum, dynamic recovery can occur in the MDF process, the effect of reducing the dislocation density in a deformed substructure is generated, and discontinuous dynamic recrystallization is inhibited, so that the growth of crystal grains is inhibited. The fine and uniform crystal grains are obtained, so that the strength and the elongation of the molybdenum are obviously improved.
The invention has the beneficial effects that:
(1) in the invention, the pure molybdenum is subjected to large plastic deformation by adopting a repeated radial-axial forging method, the total deformation is more than 300%, and the repeated multidirectional forging has strong grain refining capability, so that various mechanical properties of the molybdenum material are improved; therefore, the pure molybdenum prepared by the method has fine crystal grains, the average grain size is 1-5 mu m, and the microstructure is uniform; the relative density is high, and the average density is more than or equal to 99.9 percent; the mechanical property is excellent, the tensile strength at room temperature is more than or equal to 680MPa, and the elongation is more than or equal to 51 percent. (2) In the method, annealing at a temperature close to the recrystallization temperature is adopted after multidirectional forging, so that the anisotropy of the processing structure and the mechanical property is improved. (3) The multidirectional forging process adopted by the invention is simple, low in cost and easy to realize industrial production
Drawings
FIG. 1 is a schematic view of a multi-directional forging process of the present invention.
FIG. 2 is a photograph of the metallographic structure of wrought pure molybdenum prepared in example 1.
FIG. 3 is an SEM image of a wrought pure molybdenum tensile fracture prepared in example 1.
Detailed Description
In order to express the technical scheme of the invention more clearly, the following examples are given for illustration of the invention and are not limitative. All other embodiments and combinations according to the specific embodiments which can be obtained by persons skilled in the art without inventive step are within the scope of the invention.
A schematic representation of radial forging and axial forging in accordance with embodiments of the present invention is shown in FIG. 1, with specific steps in accordance with embodiments.
Example 1
A preparation method of high-density high-strength high-toughness pure metal molybdenum comprises the following steps:
(1) sintering the blank: sintering industrial pure molybdenum powder at 1850 ℃ in a reducing atmosphere to obtain an industrial sintered pure molybdenum rod with the average grain size of 55 microns and the relative density of 96 percent;
(2) placing the sintered pure molybdenum rod in a hydrogen atmosphere, and heating at 1300 ℃ for 30min to obtain a molybdenum rod after heat treatment;
(3) placing the molybdenum rod after heat treatment on an upper arc-shaped drilling plate and a lower arc-shaped drilling plate which have the radian of 120 degrees and are preheated to 680 ℃ for radial forging, wherein the forging rate is 600 times/min, the forging is carried out for three times, the molybdenum rod rotates anticlockwise for 60 degrees after each forging, and the deformation rates of 1-3 times are respectively 20%, 20% and 18%, so that the radially forged molybdenum rod is obtained;
(4) tempering the radially forged molybdenum rod at 1200 ℃ for 10min in a hydrogen atmosphere, then performing three-time axial forging between flat drill plates preheated to about 680 ℃, wherein the deformation rates of 1-3 times are respectively 25%, 23% and 22%, and the hammer pressing rate is 30mm/s, so as to obtain the axially forged molybdenum rod;
(5) tempering the axially forged molybdenum rod at 1150 ℃ for 8min in a hydrogen atmosphere, and then performing second radial forging (the direction change is the same as the step (3)), wherein the deformation rates of 1-3 passes in each direction are respectively set to be 20%, 18% and 16%; obtaining a molybdenum rod after secondary radial forging;
(6) tempering the molybdenum rod subjected to the second radial forging at 1125 ℃ for 8min in a hydrogen atmosphere, and then performing three-pass axial forging, wherein the 1-3-pass deformation rates are respectively 25%, 23% and 22%, and the hammer pressing rate is 30 mm/s; obtaining a molybdenum rod after secondary axial forging;
(7) tempering the molybdenum rod after the second axial forging at 1100 ℃ for 8min in a hydrogen atmosphere, and then performing third radial forging (the direction change is the same as the step (3)), wherein the 1-3-pass deformation rates in each direction are respectively set to be 20%, 18% and 16%, so as to obtain a molybdenum rod after the third radial forging;
(8) and annealing the molybdenum rod obtained in the previous step in the atmosphere, wherein the annealing temperature is 900 ℃, and the heat preservation time is 60 min.
According to the process, the high-density high-strength and high-toughness ultrafine-grain pure molybdenum material with the density of 99.98 percent, the room-temperature tensile strength of 680MPa, the elongation of 51.25 percent and the average grain size of 2-4 mu m can be prepared.
The gold phase diagram of the pure molybdenum material prepared in this example is shown in fig. 2, and it can be seen that the crystal grains are fine and relatively uniform, and the average crystal grain size is about 2-4 μm.
The SEM image of tensile fracture of the pure molybdenum material prepared in this example is shown in fig. 3, and it can be seen that the fracture is a sharp transgranular ductile fracture, not a brittle fracture of the conventional method.
Example 2
A preparation method of high-density high-strength high-toughness pure metal molybdenum comprises the following steps:
(1) sintering the blank: sintering industrial pure molybdenum powder at 1850 ℃ in a reducing atmosphere to obtain an industrial sintered pure molybdenum rod with the average grain size of 55 microns and the relative density of 96 percent;
(2) placing the sintered pure molybdenum rod in a hydrogen atmosphere, and heating at 1300 ℃ for 30min to obtain a molybdenum rod after heat treatment;
(3) placing the molybdenum rod after heat treatment on an upper arc-shaped drilling plate and a lower arc-shaped drilling plate which have the radian of 150 degrees and are preheated to about 680 degrees, and forging at the forging rate of 750 times/min for three times, wherein the molybdenum rod is anticlockwise rotated by 60 degrees after each forging, and the deformation rates of 1-3 times are respectively 20%, 18% and 16%, so that the molybdenum rod after radial forging is obtained;
(4) tempering the radially forged molybdenum rod at 1200 ℃ for 8min under hydrogen, then carrying out three-time axial forging between flat drill plates preheated to about 680 ℃, wherein the deformation rates of 1-3 passes are respectively 25%, 22% and 20%, and the hammer pressing rate is 30mm/s, so as to obtain the axially forged molybdenum rod;
(5) tempering the axially forged molybdenum rod at 1150 ℃ for 8min under hydrogen, and then performing second radial forging (the direction change is the same as the step (3)), wherein the deformation rates of 1-3 passes in each direction are respectively set to be 22%, 20% and 18%, so as to obtain a twice radially forged molybdenum rod;
(6) tempering the molybdenum rod subjected to the secondary radial forging at 1125 ℃ for 8min under hydrogen, and then performing three-pass axial forging, wherein the 1-3-pass deformation rates are respectively 28%, 24% and 22%, and the hammer pressing rate is 30 mm/s; obtaining a molybdenum rod after secondary axial forging;
(7) tempering the molybdenum rod after the second axial forging at 1100 ℃ for 8min under hydrogen, and then carrying out third radial forging (the direction change is the same as the step (3)), wherein the deformation rates of 1-3 passes in each direction are respectively set to be 18%, 16% and 15%, so as to obtain a molybdenum rod after the third radial forging;
(8) tempering the molybdenum rod subjected to the three-time radial forging at 1080 ℃ for 7min under hydrogen, and then performing three-time axial forging, wherein the deformation rates of 1-3 times are respectively 24%, 20% and 18%, and the hammer pressing rate is 30mm/s, so as to obtain a molybdenum rod subjected to three-time axial forging;
(9) tempering the molybdenum rod axially forged for three times at 1050 ℃ for 8min under hydrogen, and then performing radial forging for the fourth time (the direction change is the same as the step (3)), wherein the deformation rates of 1-3 passes in each direction are respectively set to be 16%, 14% and 10%, so as to obtain the molybdenum rod radially forged for four times;
(10) and annealing the molybdenum rod obtained in the previous step in the atmosphere, wherein the annealing temperature is 900 ℃, and the heat preservation time is 60 min.
According to the process, the high-density high-strength and high-toughness ultrafine-grained pure molybdenum material with the density of 99.99 percent, the room-temperature tensile strength of 700MPa, the elongation of 52 percent and the average grain size of 2-3 mu m can be prepared.
Example 3
A preparation method of high-density high-strength high-toughness pure metal molybdenum comprises the following steps:
(1) sintering the blank: sintering industrial pure molybdenum powder at 1850 ℃ in a reducing atmosphere to obtain an industrial sintered pure molybdenum rod with the average grain size of 55 microns and the relative density of 96 percent;
(2) placing the sintered pure molybdenum rod in a hydrogen atmosphere, and heating at 1300 ℃ for 30min to obtain a molybdenum rod after heat treatment;
(3) radially forging the molybdenum rod after heat treatment on an upper arc-shaped drilling plate and a lower arc-shaped drilling plate which have the radian of 120 degrees and are preheated to about 650 ℃, wherein the forging rate is 750 times/min, the forging is carried out for three times, the molybdenum rod rotates anticlockwise for 60 degrees after each forging, the deformation rate of each pass is 18 percent, 16 percent and 14 percent in 1-3 steps, and the radially forged molybdenum rod is obtained;
(4) tempering the radially forged molybdenum rod at 1200 ℃ for 8min under hydrogen, then performing three-time axial forging between flat drill plates preheated to about 650 ℃, wherein the deformation rates of 1-3 passes are respectively 24%, 22% and 20%, and the hammer pressing rate is 30mm/s, so as to obtain the axially forged molybdenum rod;
(5) tempering the axially forged molybdenum rod at 1170 ℃ for 8min under hydrogen, and then performing second radial forging (the direction change is the same as the step (3)), wherein the deformation rates of 1-3 passes in each direction are respectively set to be 24%, 22% and 20%; obtaining a molybdenum rod after secondary radial forging;
(6) tempering the molybdenum rod subjected to the secondary radial forging at 1150 ℃ for 6min under hydrogen, and then performing secondary axial forging, wherein the deformation rates of 1-3 passes are respectively 28%, 26% and 24%, and the hammer pressing rate is 30mm/s, so as to obtain a secondary axially forged molybdenum rod;
(7) tempering the twice axially forged molybdenum rod at 1125 ℃ for 8min under hydrogen, and then carrying out third radial forging (the direction change is the same as the step (3)), wherein the deformation rates of 1-3 passes in each direction are respectively set to be 20%, 18% and 16%, so as to obtain a molybdenum rod after the third radial forging;
(8) radially forging the molybdenum rods for three times; tempering at 1100 ℃ for 6min under hydrogen, and then carrying out axial forging for the third time, wherein the deformation rates of 1-3 passes are respectively set to be 25%, 22% and 18%, and the hammer pressing rate is 30 mm/s; obtaining a molybdenum rod axially forged for three times;
(9) tempering the molybdenum rod axially forged in the third time at 1080 ℃ for 8min under hydrogen, and then performing radial forging in the fourth time (the direction change is the same as the step (3)), wherein the deformation rates of 1-3 times in each direction are respectively set to be 15%, 12% and 10%, so as to obtain the molybdenum rod radially forged in the fourth time;
(10) tempering the molybdenum rod subjected to the four-time radial forging at 1050 ℃ for 6min under hydrogen, and then performing the fourth-time axial forging, wherein the deformation rates of 1-3 passes are respectively 20%, 18% and 15%, and the hammer pressing rate is 30 mm/s; obtaining a molybdenum rod axially forged for four times;
(11) obtaining a molybdenum rod which is axially forged for four times; and annealing in a hydrogen atmosphere at 900 ℃ for 40min to obtain the pure molybdenum material.
According to the process, the high-density high-strength and high-toughness ultrafine-grain pure molybdenum material with the density of 99.99 percent, the room-temperature tensile strength of 710MPa, the elongation of 52.5 percent and the average grain size of 1-3 mu m can be prepared.
In the above embodiments, for a specific experimental mode of the present invention, any person skilled in the art can easily think of the replacement or variation of some condition parameters, which should be within the protection scope of the present invention, and the specific protection should be determined by the claims.
Claims (4)
1. A preparation method of high-density high-toughness ultrafine-grained metal pure molybdenum comprises the following steps:
the method comprises the following steps: adopting a sintered molybdenum cylindrical rod as a raw material, and carrying out heat treatment on the sintered molybdenum cylindrical rod in a hydrogen atmosphere to obtain a treated molybdenum rod;
step two: placing the molybdenum rod treated in the step one on the preheated upper and lower arc-shaped drill plates to perform radial forging for 3 times; the radial forging process is performed in three different directions in sequence, i.e. after each radial forging, the molybdenum rods are rotated 60 in the same directiono(ii) a Obtaining a radially forged molybdenum rod;
step three: tempering the radially forged molybdenum rod in a hydrogen atmosphere; obtaining a molybdenum rod after tempering treatment;
step four: axially forging the molybdenum rod subjected to tempering treatment in the third step on the preheated upper and lower plane drill plates for 3-4 times to obtain an axially forged molybdenum rod;
step five: tempering the molybdenum rod axially forged in the fourth step in a hydrogen atmosphere to obtain a molybdenum rod subjected to secondary tempering;
step six: repeating the steps from the second step to the fifth step for 1 to 6 times, repeating the radial forging and axial forging on the molybdenum rod, and finally finishing the forging process by the fifth step or the second step to obtain primary high-density high-toughness ultrafine-grained metal pure molybdenum;
step seven: annealing the primary high-density high-toughness ultrafine grain metal pure molybdenum in the sixth step to obtain high-density high-toughness ultrafine grain metal pure molybdenum;
in the second step, the radian of the upper and lower arc-shaped drilling plates is 120-150oPreheating at 620-750 ℃; the forging rate of radial forging is 500-800 times/min, and the deformation of each forging is 10-25%;
in the third step, the tempering temperature is 1000-1200 ℃, and the tempering time is 5-10 min;
in the fourth step, the preheating temperature is 620-750 ℃; the downward pressing speed of the hammer head during axial forging is 10-100 mm/s, and the deformation rate of each pass is 15-30%;
in the fifth step, the tempering temperature is 1000-1200 ℃, and the tempering time is 5-10 min;
and seventhly, annealing is carried out in a hydrogen atmosphere, the annealing temperature is 600-1200 ℃, and the heat preservation time is 30-90 min.
2. The preparation method of the high-density high-toughness ultrafine grained metal pure molybdenum according to claim 1, characterized in that in the first step, the sintered molybdenum cylindrical rod is a molybdenum rod commonly used in the current industrial production, the relative density is 94-96%, and the average grain size is 50-80 μm; the heat treatment temperature is 1200-1300 ℃, and the treatment time is 30-60 min.
3. The method for preparing the high-density high-toughness ultrafine grained metal pure molybdenum according to claim 1, wherein in the sixth step, when repeating the second to fifth steps, the tempering temperature is required to be gradually reduced, that is, the tempering temperature in the fifth step is lower than the tempering temperature in the third step, and the tempering temperature in the third step in the second cycle is lower than the tempering temperature in the fifth step in the first cycle.
4. The high-density high-toughness ultrafine-grained pure metal molybdenum prepared by the preparation method according to any one of claims 1 to 3 is characterized in that the density of the pure metal molybdenum is more than or equal to 99.9%, the room-temperature tensile strength is more than or equal to 680MPa, the elongation is more than or equal to 51%, and the average grain size is 1-5 μm.
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