CN114309603A - Method for preparing pure titanium by directly hot extruding sponge titanium particles - Google Patents
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Abstract
A method for preparing pure titanium by directly hot-extruding sponge titanium particles belongs to the technical field of titanium preparation. The method adopts titanium sponge particles as raw materials, and directly carries out blank making, rapid heating sintering and thermomechanical consolidation forming to obtain a pure titanium product; wherein the total time of the rapid heating sintering and the thermal mechanical consolidation forming is less than or equal to 30min, the particle size of the adopted titanium sponge particles is 0.1-20 mm, and the mass percent of oxygen contained in the titanium sponge is less than or equal to 0.3 wt.%. The method has low energy consumption, simple production process and lower production cost, solves the problems of repeated powder preparation process, higher oxygen content, protective atmosphere requirement, higher production cost, overlong production period and the like in the current process of preparing the pure titanium by powder metallurgy, and realizes the rapid preparation and forming of low-cost and low-oxygen-content powder metallurgy pure titanium products.
Description
Technical Field
The invention relates to the technical field of titanium preparation, in particular to a method for preparing pure titanium by directly hot-extruding sponge titanium particles.
Background
The pure titanium has low density (equivalent to 60 percent of stainless steel), moderate strength (equivalent to the strength of the stainless steel), good plasticity and high corrosion resistance, and is an ideal non-ferrous metal material applied to the aspects of heat exchangers, chemical equipment manufacturing, ship and ocean engineering facility construction, building outer surfaces and the like. It has also been found that by adding a certain amount of low cost oxygen (less than 1 wt.%) to titanium, together with grain refinement (ref: Mimoto T, Umeda J, Kondoh k. strenggthening modify and mechanism of extruded hole meter devices with below half light devices [ J ]. Powder meter devices, 2016,59(3):223-228), the tensile strength of titanium can be increased substantially above 800MPa while maintaining good tensile plasticity (elongation > 20%). The strength of the titanium is obviously higher than that of the stainless steel, so that the titanium becomes an ideal material for manufacturing parts of moving machinery, such as automobiles, bicycles, scooters and the like, and has great application potential.
However, because of the high chemical activity of titanium, the following two preparation methods are generally used for the manufacture of conventional titanium products:
firstly, the method comprises the following steps: ingot metallurgy: specifically, sponge titanium is smelted and cast for 2-3 times by using a vacuum consumable electrode furnace to manufacture ingot casting metallurgical ingots, and then titanium products such as plates, bars, sections, forgings and the like are manufactured through further thermal mechanical processing. The remelting times can be reduced to one time by using an electron beam melting furnace or a plasma melting furnace, but larger heat energy is still required for providing. Because the melting point of titanium is high (1670 ℃), the melting heat per unit mass is large, the working temperature of a melting furnace is high, the thermal efficiency is low, a large amount of energy is consumed for manufacturing titanium products, and meanwhile, the material loss is caused, so that the manufacturing cost of the titanium products is increased by more than 50% on the basis of the price of the raw material titanium sponge.
Secondly, the method comprises the following steps: powder metallurgy: the method comprises the following steps: titanium powder or titanium hydride powder is used as a raw material, the titanium powder or the titanium hydride powder and alloy element powder are subjected to mechanical ball milling or mechanical mixing homogenization, then a powder mixture is subjected to green pressing or near net forming green pressing, and finally alloying and densification of titanium are completed in a thermal mechanical consolidation mode under the vacuum/protective atmosphere condition. Although the conventional titanium alloy powder metallurgy technology can obviously reduce energy consumption and cost, the following typical defects still exist:
(1) the milling process is complicated. Titanium powder or titanium hydride powder is prepared by taking titanium sponge as a raw material, and preparing hydrogenated powder by mechanical grinding and crushing after hydrogenation, wherein the hydrogenated and dehydrogenated titanium powder is prepared by carrying out vacuum dehydrogenation treatment on the hydrogenated titanium powder, so that the energy consumption is increased, and the working procedures are repeated.
(2) The cost is still high. Such as: the price of 200-mesh hydrogenated dehydrogenated titanium powder or titanium hydride powder is more than 250 yuan/kg, the price of low-cost hydrogenated titanium powder produced by hydrogenated sponge titanium and mechanical grinding and reinforced dehydrogenated titanium powder produced by dehydrogenating titanium powder is more than 30% higher than that of sponge titanium, so that the price of titanium products produced by the hydrogenated dehydrogenated powder or titanium hydride powder is more than 40% higher than that of the sponge titanium, and the high price is a main obstacle to the wide application of commercial pure titanium compared with stainless steel.
(3) The oxygen content is higher. Compared with the raw material titanium sponge particles, the size of the hydrogenated dehydrotitanium powder or titanium hydride powder is in the micron level, while the size of the raw material titanium sponge particles is in the millimeter or even centimeter level, because the hydrogenated dehydrotitanium powder or titanium hydride powder has smaller size and larger specific surface, the area of an oxide film is increased, and the oxide film begins to dissolve at the temperature of over 700 ℃, and oxygen can dissolve into a titanium matrix. At the same time, at high temperatures, oxygen is very soluble in the titanium matrix, causing embrittlement of the titanium matrix.
(4) A protective atmosphere is required. When the temperature is more than or equal to 700 ℃, oxygen begins to dissolve in the titanium matrix along with the dissolution of the powder oxide film, the strength is improved to some extent because interstitial atom oxygen and nitrogen can generate solid solution strengthening on titanium and titanium alloy, the shaping is obviously reduced, the material failure can be caused by excessively high oxygen and nitrogen content, meanwhile, the specific surface of the powder is larger, the oxygen and the nitrogen are more favorably dissolved in the titanium matrix, and the preparation of the titanium product is mostly carried out in vacuum or protective atmosphere.
(5) The production cycle is long. Mainly embodied in powder screening and powder mixing.
Therefore, the method for preparing the new pure titanium product is significant.
Disclosure of Invention
The invention aims to provide a method for preparing pure titanium by directly hot-extruding sponge titanium particles, which can reduce energy consumption, has simple production process and lower production cost, and aims to solve the problems of repeated powder preparation process, higher oxygen content, need of protective atmosphere, higher production cost, overlong production period and the like in the conventional process for preparing pure titanium by powder metallurgy, and realize the rapid preparation and forming of low-cost low-oxygen-content powder metallurgy pure titanium products.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention discloses a method for preparing pure titanium by directly hot extruding sponge titanium particles, which comprises the following steps:
(1) drying the titanium sponge particles
Placing the titanium sponge particles into a vacuum drying box for drying to obtain dried titanium sponge particles;
(2) preparing a blank from the granules
Pressing the dried titanium sponge particles into a titanium sponge green compact;
(3) rapid heating sintering
Rapidly heating and sintering the titanium sponge green compact at the sintering temperature of 1000-1200 ℃, and preserving heat for 5-10 min to obtain a sintered compact with uniform temperature;
wherein, the temperature is raised to 1000 ℃ at the rate of 50-150 ℃/min, and then the temperature is raised to the sintering temperature at the rate of 30-70 ℃/min;
(4) thermo-mechanical consolidation forming
Placing the sintered blank in an extrusion die, extruding the extrusion die with an inner cavity, and solidifying and forming in the inner cavity of the extrusion die to obtain a titanium product;
(5) cooling down
And cooling the titanium product to room temperature to obtain a pure titanium product.
In the step (1), the particle size of the titanium sponge particles is 0.1-20 mm, and the mass percent of oxygen contained in the titanium sponge is less than or equal to 0.3 wt.%.
In the step (1), the titanium sponge particles are dried at 100-150 ℃ for 100-120 min.
In the step (2), the pressing pressure is 500-950 MPa, and the pressure maintaining time is 4-6 min.
In the step (2), the relative density of the titanium sponge green compact is 80-95%.
And (3) rapidly heating and sintering in a protective atmosphere or in air.
In the step (3), the titanium sponge green compact is rapidly heated and sintered, preferably by using an induction heating coil.
In the step (3), the protective atmosphere is preferably argon, and the mass percent of oxygen contained in the argon is less than or equal to 200 ppm.
In the step (4), the temperature of the extrusion die with the inner cavity is 450-550 ℃.
In the step (4), the extrusion strength is 500-950 MPa, and the extrusion ratio is (5-100): 1.
In the step (4), the extrusion rate is 5-50 mm/s.
In the step (4), the shape and the size of the extrusion die with the inner cavity are determined according to the requirements of the shape and the size of the cross section of the titanium product.
In the step (4), the extrusion die with the inner cavity can be a bar, a pipe and an extruded long thick plate or a forging die according to different dies used during densification and forming.
And (5) air-cooling to room temperature.
In the method for preparing pure titanium by directly hot-extruding the sponge titanium particles, the total time of the rapid heating sintering in the step (3) and the thermal mechanical consolidation forming in the step (4) is less than or equal to 30min, the total time is controlled by a heating rate, the temperature is increased to 1000 ℃ by adopting 50-150 ℃/min, and then the temperature is increased to the sintering temperature by adopting 30-70 ℃/min.
In the method for preparing pure titanium by directly hot extruding the titanium sponge particles, the rapid heating sintering in the step (3) and the thermomechanical consolidation forming in the step (4) can be carried out in a protective atmosphere or in air.
In the method for preparing pure titanium by directly hot-extruding the sponge titanium particles, the cost is far lower than that of a titanium product prepared by an ingot metallurgy method and a traditional powder metallurgy method, and the comprehensive mechanical property of the method is equivalent to that of TA1 (the tensile strength is more than or equal to 240MPa, and the elongation at break is more than or equal to 30%).
Compared with the prior art, the method for preparing pure titanium by directly hot extruding the titanium sponge particles has the beneficial effects that:
the method for preparing pure titanium by directly hot extruding the titanium sponge particles is different from the traditional ingot metallurgy multi-time smelting and traditional powder metallurgy mechanical grinding and crushing, the problems of high oxygen content, complex and repeated preparation procedures, high cost and overlong production period of the prepared pure titanium are solved in a targeted manner, the pure titanium is prepared by directly hot extruding and solidifying the titanium sponge particles serving as raw materials, the production procedures are simplified, the energy consumption is reduced, the preparation period is shortened, and the production cost is reduced.
According to the invention, the high-performance pure titanium is prepared by taking the low-cost titanium sponge particles as raw materials, hot extruding, consolidating, rapidly induction heating and sintering the titanium sponge pressed compact in the argon protective atmosphere or air, so that the preparation process of the pure titanium is simplified, the energy consumption and the preparation cost of the pure titanium are reduced, and meanwhile, excellent mechanical properties are obtained. The method for preparing the pure titanium is different from the traditional preparation method, and has the advantages that firstly, the sponge titanium does not undergo a series of complex processes of ingot metallurgy, so that the energy consumption is reduced; the method for preparing pure titanium can be completely carried out in the air, and the performance of the titanium and the titanium alloy can not be influenced because the process of heating the titanium sponge blank by the medium-frequency induction heating device is a short-time sintering process, and an oxidation film is arranged on the surface before heating to 700 ℃ to prevent oxygen absorption, and meanwhile, the pressed blank forms closed air holes in the short-time sintering process, and the oxidation film is dissolved when the pressed blank is heated to above 700 ℃, but the oxygen absorption and internal oxidation are prevented due to the closed air holes, so that the adverse influence of excessive oxygen content on the performance of the titanium alloy is avoided. The method for preparing pure titanium is different from the traditional powder metallurgy, and does not have the processes of ball milling, powder making and the like, so that the production process is simplified, and the cost for preparing pure titanium is reduced. Meanwhile, in order to meet more application requirements, sponge titanium with the oxygen content of less than 0.3 wt.% can be selected for hot extrusion, oxygen has a solid solution strengthening effect on the titanium alloy, and a proper oxygen content can obtain a good combination of strength and shaping, so that the application range of pure titanium is expanded, and the cost is reduced.
Drawings
FIG. 1 is a particle-bound gold phase diagram of titanium sponge particles of example 1 for producing pure titanium: (a) the metallographic phase of the sintered blank after rapid induction heating sintering, (b) the metallographic phase of the pure titanium product after thermomechanical consolidation forming;
FIG. 2 is a microstructure of pure titanium prepared by direct hot extrusion of titanium sponge particles according to example 1;
FIG. 3 is a fracture surface of a pure titanium tensile specimen prepared by directly hot-pressing titanium sponge particles according to example 1;
FIG. 4 is a microstructure of example 3 in which titanium sponge particles were directly hot-pressed to prepare pure titanium;
FIG. 5 is a microstructure of pure titanium prepared by direct hot extrusion of titanium sponge particles according to example 4;
FIG. 6 is a fracture surface of a pure titanium tensile specimen prepared by directly hot-pressing titanium sponge particles according to example 4;
FIG. 7 is a microstructure diagram of pure titanium prepared by directly hot-extruding titanium sponge particles according to comparative example 2;
FIG. 8 is a microstructure of comparative example 3 in which pure titanium was prepared by directly hot-extruding titanium sponge particles;
FIG. 9 is a process flow chart of a method for preparing pure titanium by directly hot-extruding sponge titanium particles according to the present invention.
Detailed Description
The present invention will be described in further detail with reference to examples.
In the following examples, titanium sponge particles with oxygen content below 0.3 wt.% are used, and titanium products are brittle with too high an oxygen content.
Example 1
The embodiment provides a method for preparing pure titanium by directly hot-extruding titanium sponge particles, and the process flow chart is shown in figure 9, and the method comprises the following steps:
step one, weighing 400g of 0-grade titanium sponge particles (with the oxygen content of 0.04 wt.%) with the diameter of 2-12.7 mm, placing the particles in a tray, and then placing the tray in a drying oven at 100-120 ℃ for drying for 120min to remove moisture in the titanium sponge;
step two, pouring the dried titanium sponge particles into a cylindrical green compact cylinder coated with a graphite lubricant and having a diameter of 53mm, pressing the titanium sponge particles at 850MPa by using a 200t press for 5min, and then reversely demoulding the pressed green compact by adopting a mode of ejecting out of a lower die to obtain a titanium sponge green compact with a diameter of 53mm and a height of 46 mm; the relative density of the titanium sponge compact was 87.4%;
step three, an operable closed atmosphere box is arranged on the hydraulic machine for vacuumizing treatment, the vacuum degree is lower than 0.01MPa, and then high-purity argon is introduced to ensure that the oxygen content is less than 200 ppm;
step four, rapidly heating the titanium sponge pressed blank by using a medium-frequency induction heating device, heating the pressed blank to 1000 ℃ at a speed of 70 ℃/min, then heating the pressed blank from 1000 ℃ to 1200 ℃ at a speed of 50 ℃/min, and preserving heat for 5min to obtain a sintered blank;
and step five, quickly transferring the sintering blank heated to 1200 ℃ to an extrusion cylinder mold with the temperature of 400-450 ℃ and the diameter of 57mm, performing hot extrusion forming by adopting a circular extrusion nozzle with the extrusion ratio of 16:1 and a 200t press under the pressure of 950MPa to obtain a pure titanium product, and air-cooling to room temperature.
The implementation results are as follows: under the argon protective atmosphere, the yield strength of a pure titanium bar prepared by hot extrusion reaches 196MPa, the tensile strength reaches 299MPa, the elongation is 63.2%, and the comprehensive mechanical property of the pure titanium bar is equivalent to that of TA1 industrial pure titanium (the tensile strength is more than or equal to 240MPa, and the elongation at break is more than or equal to 30%).
In the example 1, the metallographic phase of the sintered compact after the rapid induction heating sintering is shown in fig. 1(a), and the metallographic phase of the pure titanium product after the thermomechanical consolidation forming is shown in fig. 1 (b); the direct hot extrusion of the titanium sponge particles can prepare nearly fully dense pure titanium products, and the hot extrusion deformation can eliminate holes and cracks to achieve better metallurgical bonding;
the microstructure of the pure titanium article prepared in this example is shown in FIG. 2.
The fracture surface of the pure titanium product prepared in the example is shown in fig. 3, and it can be seen from the graph that when the thermomechanical consolidation temperature is 1200 ℃, a large number of dimples exist in the fracture surface, and holes exist in the dimples, which are typical ductile fractures, and the fracture surface does not have a weak bonding surface, and the consolidation quality is good.
Example 2
A method for preparing pure titanium by directly hot-extruding sponge titanium particles comprises the following steps:
weighing 450g of 0-grade titanium sponge particles (with the oxygen content of 0.04 wt.%) with the diameter of 2-12.7 mm, putting the particles into a tray, and then drying the particles in a drying oven at 100-120 ℃ for 120min to remove water in the titanium sponge;
step two, pouring the dried titanium sponge particles into a cylindrical green compact cylinder coated with a graphite lubricant and having a diameter of 53mm, pressing the titanium sponge particles at 950MPa by using a 200t press for 5min, and then reversely demoulding the pressed green compact by adopting a mode of ejecting out of a lower die to obtain a green compact with a diameter of 53mm and a height of 50 mm; the relative density of the titanium sponge green compact is 90.4%;
and step three, rapidly heating the titanium sponge pressed blank by using a medium-frequency induction heating device under the air condition, heating the pressed blank to 1000 ℃ at a speed of 70 ℃/min, then heating the pressed blank to 1200 ℃ at a speed of 40 ℃/min, and preserving heat for 5min to obtain a sintered blank.
And step four, rapidly transferring the sintering blank with the temperature of 1200 ℃ to an extrusion cylinder mould with the temperature of 400-450 ℃ and the diameter of 57mm under the air condition, performing hot extrusion forming by adopting a square extrusion nozzle with the extrusion ratio of 9:1 and a 200t press under the pressure of 950MPa to obtain a pure titanium product, and performing air cooling to room temperature.
The implementation results are as follows: the pure titanium bar prepared by hot extruding the sponge titanium particle pressed compact which is rapidly heated and sintered by induction heating in the air has the yield strength of 188MPa, the tensile strength of 298MPa and the elongation of 50 percent, the mechanical property of the titanium sponge is equivalent to that of TA1 industrial pure titanium (the tensile strength is more than or equal to 240MPa, the elongation at break is more than or equal to 30 percent), because the titanium sponge has larger particle size and smaller specific surface, compared with powder, the titanium sponge has less oxide film, meanwhile, in the rapid induction heating sintering process, the temperature can promote the dissolution of an oxide film and the creep deformation of materials at two sides of the particles, so that part of weak bonding surface can achieve better metallurgical bonding, and simultaneously, the creep deformation of the materials at two sides of the particles can eliminate micropores, increase the densification, although the larger holes are not eliminated, the larger holes can form internally closed holes in the rapid induction heating sintering process, so that the titanium is prevented from being oxidized by oxygen and being oxidized internally. The invention relates to a method for preparing pure titanium by using sponge titanium particles with low cost as raw materials, under the air condition, the properties of the pure titanium are equivalent to the mechanical properties of pure titanium prepared in protective atmosphere by hot extrusion consolidation and rapid induction heating sintering of the sponge titanium green compact, the preparation process does not need complicated procedures such as smelting and the like, the energy consumption is reduced, the production procedures are simplified, and the production cost is reduced.
Room temperature mechanical property of sample prepared by hot extruding sponge titanium pressed compact in argon protective atmosphere and air
H, O, N detection result of sample prepared by hot-extruding titanium sponge pressed compact in argon protective atmosphere and air
Example 3
A method for preparing pure titanium by directly hot-extruding sponge titanium particles comprises the following steps:
step one, weighing 400g of grade-1 titanium sponge particles (with the oxygen content of 0.1 wt.%) with the diameter of 2-12.7 mm, placing the titanium sponge particles in a tray, and then placing the tray in a drying oven at 100-120 ℃ for drying for 120min to remove moisture in the titanium sponge;
pouring the dried titanium sponge particles into a cylindrical green compact cylinder coated with a graphite lubricant and having a diameter of 53mm, pressing the titanium sponge particles at a pressing pressure of 750MPa by using a 200t press for 5min, and then reversely demoulding the pressed green compact by using a lower die ejection mode to obtain a titanium sponge green compact with a diameter of 53mm and a height of 47mm, wherein the relative density of the titanium sponge green compact is 85.5%;
step three, an operable closed atmosphere box is arranged on the hydraulic machine for vacuumizing treatment, the vacuum degree is lower than 0.01MPa, and then high-purity argon is introduced to ensure that the oxygen content is less than 200 ppm;
step four, rapidly heating the titanium sponge pressed blank by using a medium-frequency induction heating device, heating the pressed blank to 1000 ℃ at a speed of 70 ℃/min, then heating the pressed blank from 1000 ℃ to 1200 ℃ at a speed of 50 ℃/min, and preserving heat for 5min to obtain a sintered blank;
and step five, quickly transferring the sintering blank heated to 1200 ℃ to an extrusion cylinder mold with the temperature of 400-450 ℃ and the diameter of 57mm, performing hot extrusion forming by adopting a circular extrusion nozzle with the extrusion ratio of 16:1 and a 200t press under the pressure of 950MPa to obtain a pure titanium product, and air-cooling to room temperature.
The implementation results are as follows: under the protection of argon, the yield strength of a pure titanium bar prepared by hot extrusion is 240MPa, the tensile strength reaches 362MPa, the elongation is 37.3%, the comprehensive mechanical property of the pure titanium bar is equivalent to that of TA1 industrial pure titanium (the tensile strength is more than or equal to 240MPa, the elongation at break is more than or equal to 30%), the strength of the pure titanium bar is increased by solid solution strengthening of oxygen, the shaping is reduced, and a titanium product with better comprehensive mechanical property can be obtained by increasing proper oxygen content. The invention relates to a method for preparing pure titanium by extruding sponge titanium particle pressed compact, which does not need complex procedures such as smelting and the like in the preparation process, reduces the energy consumption, simplifies the production procedures and reduces the production cost; the microstructure of the pure titanium article prepared in this example is shown in FIG. 4.
Example 4
A method for preparing pure titanium by directly hot-extruding sponge titanium particles comprises the following steps:
step one, weighing 400g of 0-grade titanium sponge particles (with the oxygen content of 0.04 wt.%) with the diameter of 2-12.7 mm, placing the particles in a tray, and then placing the tray in a drying oven at 100-120 ℃ for drying for 120min to remove moisture in the titanium sponge;
step two, pouring the dried titanium sponge particles into a cylindrical green compact cylinder coated with a graphite lubricant and having a diameter of 53mm, pressing the titanium sponge particles at a pressing pressure of 750MPa by using a 200t press for 5min, and then reversely demoulding the pressed green compact by adopting a mode of ejecting out of a lower die to obtain a titanium sponge green compact with a diameter of 53mm and a height of 47 mm; the relative density of the titanium sponge green compact is 85.5%;
step three, an operable closed atmosphere box is arranged on the hydraulic machine for vacuumizing treatment, the vacuum degree is lower than 0.01MPa, and then high-purity argon is introduced to ensure that the oxygen content is less than 200 ppm;
step four, rapidly heating the titanium sponge pressed blank by using a medium-frequency induction heating device, heating the pressed blank to 1000 ℃ at a speed of 70 ℃/min, and preserving heat for 5min to obtain a sintered blank;
and step five, quickly transferring the sintering blank heated to 1000 ℃ to an extrusion cylinder mold with the temperature of 400-450 ℃ and the diameter of 57mm, performing hot extrusion forming by adopting a circular extrusion nozzle with the extrusion ratio of 16:1 and a 200t press under the pressure of 950MPa to obtain a pure titanium product, and air-cooling to room temperature.
The implementation results are as follows: under the protection of argon, the yield strength of a pure titanium bar prepared by hot extrusion reaches 192MPa, the tensile strength reaches 292MPa, the elongation is 46.3%, the mechanical property of the pure titanium bar is equivalent to that of TA1 industrial pure titanium (the tensile strength is more than or equal to 240MPa, and the elongation at break is more than or equal to 30%), compared with example 1, the mechanical property of the pure titanium bar is equivalent to that of TA1 industrial pure titanium, the elongation is reduced, the high temperature is favorable for creep deformation of materials at two sides of particles so as to eliminate micropores, the temperature is simultaneously increased so as to be favorable for particle deformation, the densification degree of the material is increased in the process of thermo-mechanical solidification, so that the particles and the particles achieve better metallurgical bonding, the temperature is lower, more weak bonding surfaces exist, the weak bonding surfaces become a root source for crack initiation and an expansion way in the deformation process of the material, and the elongation at break is reduced. The invention relates to a method for preparing pure titanium by extruding sponge titanium particle pressed compact, which does not need complex procedures such as smelting and the like in the preparation process, reduces the energy consumption, simplifies the production procedures and reduces the production cost.
The microstructure of pure titanium prepared by direct hot extrusion of titanium sponge particles is shown in FIG. 5;
in this example 4, the fracture surface of the prepared pure titanium product is shown in fig. 6, from which it can be seen that at a lower thermo-mechanical consolidation temperature, there are still unbonded particles with smaller size, and by comparison with example 1, it is demonstrated that increasing the temperature will be beneficial to eliminate holes and microcracks, promote bonding between particles, and improve the quality of consolidation between particles.
Example 5
The embodiment provides a method for preparing pure titanium by directly hot-extruding sponge titanium particles, which comprises the following steps:
step one, weighing 400g of 0-grade titanium sponge particles (with the oxygen content of 0.04 wt.%) with the diameter of 15-20 mm, placing the particles in a tray, and then placing the tray in a drying box at 130-150 ℃ for drying for 100min to remove water in the titanium sponge;
step two, pouring the dried titanium sponge particles into a cylindrical green compact cylinder coated with a graphite lubricant and having a diameter of 53mm, pressing the titanium sponge particles at 500MPa by using a 200t press for 6min, and then reversely demoulding the pressed green compact by adopting a mode of ejecting out of a lower die to obtain a titanium sponge green compact with a diameter of 53mm and a height of 50 mm; the relative density of the titanium sponge compact is 80.4%;
step three, an operable closed atmosphere box is arranged on the hydraulic machine for vacuumizing treatment, the vacuum degree is lower than 0.01MPa, and then high-purity argon is introduced to ensure that the oxygen content is less than 200 ppm;
step four, rapidly heating the titanium sponge pressed blank by using a medium-frequency induction heating device, heating the pressed blank to 1000 ℃ at a speed of 50 ℃/min, then heating the pressed blank from 1000 ℃ to 1100 ℃ at a speed of 30 ℃/min, and preserving heat for 5min to obtain a sintered blank;
and step five, rapidly transferring the sintering blank heated to 1100 ℃ to an extrusion cylinder mold with the temperature of 500-550 ℃ and the diameter of 57mm, adopting a circular extrusion nozzle with the extrusion ratio of 70:1, the extrusion speed of 5mm/s, utilizing a 200t press and the pressure of 750MPa to perform hot extrusion consolidation forming to obtain a pure titanium product, and cooling to the room temperature at 50-60 ℃/min.
Example 6
The embodiment provides a method for preparing pure titanium by directly hot-extruding sponge titanium particles, which comprises the following steps:
step one, weighing 400g of 0-grade titanium sponge particles (with the oxygen content of 0.04 wt.%) with the diameter of 2-12.7 mm, placing the particles in a tray, and then placing the tray in a drying oven at 100-120 ℃ for drying for 120min to remove moisture in the titanium sponge;
step two, pouring the dried titanium sponge particles into a cylindrical green compact cylinder coated with a graphite lubricant and having a diameter of 53mm, pressing the titanium sponge particles at a pressing pressure of 950MPa by using a 200t press for 4min, and then reversely demoulding the pressed green compact by using a lower die ejection mode to obtain a titanium sponge green compact with a diameter of 53mm and a height of 44 mm; the relative density of the titanium sponge compact was 91.3%;
and step three, rapidly heating the titanium sponge pressed blank by using a medium-frequency induction heating device under the air condition, heating the pressed blank to 1000 ℃ at a speed of 100 ℃/min, then heating the pressed blank to 1200 ℃ at a speed of 50 ℃/min, and preserving heat for 5min to obtain a sintered blank.
And step four, rapidly transferring the sintering blank with the temperature of 1200 ℃ to an extrusion cylinder mold with the temperature of 450-500 ℃ and the diameter of 57mm under the air condition, adopting a square extrusion nozzle with the extrusion ratio of 30:1, performing hot extrusion forming at the extrusion rate of 10mm/s and the pressure of 550MPa by using a 200t press to obtain a pure titanium product, and performing air cooling to the room temperature.
Example 7
The embodiment provides a method for preparing pure titanium by directly hot-extruding sponge titanium particles, which comprises the following steps:
step one, weighing 400g of 0-grade titanium sponge particles (with the oxygen content of 0.04 wt.%) with the diameter of 2-12.7 mm, placing the particles in a tray, and then placing the tray in a drying oven at 100-120 ℃ for drying for 120min to remove moisture in the titanium sponge;
step two, pouring the dried titanium sponge particles into a cylindrical green compact cylinder coated with a graphite lubricant and having a diameter of 53mm, pressing the titanium sponge particles at a pressure of 650MPa by using a 200t press for 5min, and then reversely demoulding the pressed green compact by using a lower die ejection mode to obtain a titanium sponge green compact with a diameter of 53mm and a height of 48 mm; the relative density of the titanium sponge green compact was 83.7%;
step three, an operable closed atmosphere box is arranged on the hydraulic machine for vacuumizing treatment, the vacuum degree is lower than 0.01MPa, and then high-purity argon is introduced to ensure that the oxygen content is less than 200 ppm;
step four, rapidly heating the titanium sponge pressed blank by using a medium-frequency induction heating device, heating the pressed blank to 1000 ℃ at a speed of 150 ℃/min, then heating the pressed blank from 1000 ℃ to 1150 ℃ at a speed of 70 ℃/min, and preserving heat for 5min to obtain a sintered blank;
and step five, quickly transferring the sintering blank heated to 1150 ℃ to an extrusion cylinder mold with the temperature of 400-450 ℃ and the diameter of 57mm, carrying out hot extrusion consolidation forming by adopting a circular extrusion nozzle with the extrusion ratio of 20:1 and a 200t press at the extrusion rate of 30mm/s and the pressure of 500MPa to obtain a pure titanium product, and cooling to room temperature at the cooling rate of 80 ℃/min.
Example 8
The embodiment provides a method for preparing pure titanium by directly hot-extruding sponge titanium particles, which comprises the following steps:
step one, weighing 400g of 0-grade titanium sponge particles (with the oxygen content of 0.04 wt.%) with the diameter of 2-12.7 mm, placing the particles in a tray, and then placing the tray in a drying oven at 100-120 ℃ for drying for 120min to remove moisture in the titanium sponge;
step two, pouring the dried titanium sponge particles into a cylindrical green compact cylinder coated with a graphite lubricant and having a diameter of 53mm, pressing the titanium sponge particles at a pressing pressure of 750MPa by using a 200t press for 5min, and then reversely demoulding the pressed green compact by adopting a mode of ejecting out of a lower die to obtain a titanium sponge green compact with a diameter of 53mm and a height of 47 mm; the relative density of the titanium sponge green compact is 85.5%;
and step three, rapidly heating the titanium sponge pressed blank by using a medium-frequency induction heating device under the air condition, heating the pressed blank to 1000 ℃ at a speed of 80 ℃/min, then heating the pressed blank to 1200 ℃ at a speed of 40 ℃/min, and preserving heat for 5min to obtain a sintered blank.
And step four, rapidly transferring the sintering blank with the temperature of 1200 ℃ to an extrusion cylinder mold with the temperature of 400-450 ℃ and the diameter of 57mm under the air condition, performing hot extrusion forming by adopting a square extrusion nozzle with the extrusion ratio of 90:1 and a 200t press under the pressure of 950MPa to obtain a pure titanium product, and cooling to the room temperature at the cooling rate of 10 ℃/min.
Comparative example 1
A method for preparing pure titanium by directly hot-extruding sponge titanium particles comprises the following steps:
step one, weighing 400g of-200-mesh hydrogenated and dehydrogenated titanium powder (with oxygen content of 0.11 wt.%) and placing the powder in a tray, then placing the tray in a drying box at 100-120 ℃ for drying for 120min, and removing water in the hydrogenated and dehydrogenated titanium powder;
step two, pouring the dried hydrogenated titanium powder particles into a cylindrical pressed blank cylinder coated with a graphite lubricant and having a diameter of 53mm, pressing the particles at a pressing pressure of 750MPa for 5min by using a 200t press, and then reversely demoulding the pressed blank by adopting a mode of ejecting out of a lower die to obtain a titanium sponge pressed blank with a diameter of 53mm and a height of 46.5mm, wherein the relative density of the titanium sponge pressed blank is 86.4%;
step three, an operable closed atmosphere box is arranged on the hydraulic machine for vacuumizing treatment, the vacuum degree is lower than 0.01MPa, and then high-purity argon is introduced to ensure that the oxygen content is less than 200 ppm;
step four, rapidly heating the titanium sponge pressed blank by using a medium-frequency induction heating device, heating the pressed blank to 1000 ℃ at a speed of 70 ℃/min, then heating the pressed blank from 1000 ℃ to 1200 ℃ at a speed of 50 ℃/min, and preserving heat for 5min to obtain a sintered blank;
and step five, quickly transferring the sintering blank heated to 1200 ℃ to an extrusion cylinder mold with the temperature of 400-450 ℃ and the diameter of 57mm, performing hot extrusion forming by adopting a circular extrusion nozzle with the extrusion ratio of 16:1 and a 200t press under the pressure of 950MPa to obtain a pure titanium product, and air-cooling to room temperature.
The implementation results are as follows: in the argon protective atmosphere, the tensile strength of a pure titanium bar prepared by hot extrusion reaches 370MPa, the elongation is 41%, the mechanical property of the pure titanium bar is equivalent to that of TA1 industrial pure titanium (the tensile strength is more than or equal to 240MPa, and the elongation at break is more than or equal to 30%), compared with the forming of a-200-mesh hydrogenated and dehydrogenated titanium powder thermo-mechanical consolidation bar, the forming of the sponge titanium particle thermo-mechanical consolidation extrusion also achieves better metallurgical bonding in example 3, however, the cost is calculated, the price of-200-mesh hydrogenated and dehydrogenated titanium powder or titanium powder is more than 250 yuan/kg, the price of low-cost hydrogenated titanium powder prepared by hydrogenated sponge titanium and mechanical grinding and the price of strengthened dehydrogenated titanium powder prepared by hydrogenated titanium powder dehydrogenation are more than 30% higher than that of the sponge titanium, and the price of a titanium product prepared by hydrogenated and dehydrogenated titanium powder is more than 40%, the cost for preparing pure titanium by directly hot-extruding the titanium sponge particles is far lower than that of the traditional powder metallurgy, and the consolidation quality of the titanium sponge particles is equivalent to that of titanium powder. The invention relates to a method for preparing pure titanium by extruding sponge titanium particle pressed compact, which does not pass through the traditional powder metallurgy powder preparation process, reduces the energy consumption, simplifies the production process and reduces the production cost.
Comparative example 2
A method for preparing pure titanium by directly hot-extruding sponge titanium particles comprises the following steps:
step one, weighing 400g of titanium sponge particles (with the oxygen content of 0.44 wt.%) with the diameter of 2-12.7 mm, placing the titanium sponge particles in a tray, and then placing the tray in a drying box at 100-120 ℃ for drying for 120min to remove water in the titanium sponge;
step two, pouring the dried titanium sponge particles into a cylindrical green compact cylinder coated with a graphite lubricant and having a diameter of 53mm, pressing the titanium sponge particles at a pressing pressure of 750MPa by using a 200t press for 5min, and then reversely demoulding the pressed green compact by adopting a mode of ejecting out of a lower die to obtain a titanium sponge green compact with a diameter of 53mm and a height of 47.5 mm; the relative density of the titanium sponge compact was 84.6%;
step three, an operable closed atmosphere box is arranged on the hydraulic machine for vacuumizing treatment, the vacuum degree is lower than 0.01MPa, and then high-purity argon is introduced to ensure that the oxygen content is less than 200 ppm;
step four, rapidly heating the titanium sponge pressed blank by using a medium-frequency induction heating device, heating the pressed blank to 1000 ℃ at a speed of 70 ℃/min, then heating the pressed blank from 1000 ℃ to 1200 ℃ at a speed of 50 ℃/min, and preserving heat for 5min to obtain a sintered blank;
and step five, quickly transferring the sintering blank heated to 1200 ℃ to an extrusion cylinder mold with the temperature of 400-450 ℃ and the diameter of 57mm, performing hot extrusion forming by adopting a circular extrusion nozzle with the extrusion ratio of 16:1 and a 200t press under the pressure of 950MPa to obtain a pure titanium product, and air-cooling to room temperature.
The comparative example, which has a different titanium dioxide content than example 1, shows the following results: in the protective atmosphere of argon, the pure titanium bar prepared by hot extrusion is brittle-broken, oxygen is the central problem for manufacturing titanium and titanium alloy, the strong and short-distance repulsion action between interstitial oxygen and screw dislocation nucleus enhances the strength of titanium but reduces the tensile plasticity and toughness of titanium, and the brittle-breaking is easy to occur due to the excessively high oxygen content. The microstructure of the pure titanium article prepared in this comparative example is shown in fig. 7, which is compared with examples 1 and 3 to illustrate that pure titanium is transformed from an equiaxed structure to a lamellar structure as the oxygen content increases, because interstitial oxygen is a crystal defect as an interstitial atom and a new phase tends to nucleate at the crystal defect. Oxygen is dissolved in alpha-Ti, the c/a value of the alpha-Ti is improved, the c/a value is increased, the distance of an alpha-Ti crystal lattice prism surface is reduced, the stacking density on a stacking surface is reduced to a certain extent compared with a basal surface, the sliding on the prism surface is not facilitated, the sliding system is reduced, and the shaping is reduced. Meanwhile, the excessive oxygen content can cause the pure titanium to generate uneven solid solution of oxygen, so that the yield strength difference of the soft and hard regions of the pure titanium is larger, the coordinated deformation capability of the soft and hard regions is also obviously reduced, and finally, the fracture is caused. It was demonstrated that the process for producing pure titanium by extrusion of a pressed compact of titanium sponge particles requires the use of titanium sponge particles having an oxygen content of less than 0.3 wt.%.
Comparative example 3
A method for preparing pure titanium by directly hot-extruding sponge titanium particles comprises the following steps:
step one, weighing 400g of 0-grade titanium sponge particles (with the oxygen content of 0.04 wt.%) with the diameter of 2-12.7 mm, placing the particles in a tray, and then placing the tray in a drying oven at 100-120 ℃ for drying for 120min to remove moisture in the titanium sponge;
step two, pouring the dried titanium sponge particles into a cylindrical green compact cylinder coated with a graphite lubricant and having a diameter of 53mm, pressing the titanium sponge particles at 850MPa by using a 200t press for 5min, and then reversely demoulding the pressed green compact by adopting a mode of ejecting out of a lower die to obtain a titanium sponge green compact with a diameter of 53mm and a height of 46 mm; the relative density of the titanium sponge compact was 87.4%;
step three, an operable closed atmosphere box is arranged on the hydraulic machine for vacuumizing treatment, the vacuum degree is lower than 0.01MPa, and then high-purity argon is introduced to ensure that the oxygen content is less than 200 ppm;
step four, rapidly heating the titanium sponge pressed blank by using a medium-frequency induction heating device, heating the pressed blank to 1000 ℃ at a speed of 70 ℃/min, and preserving heat for 40min to obtain a sintered blank;
and step five, quickly transferring the sintering blank heated to 1000 ℃ to an extrusion cylinder mold with the temperature of 400-450 ℃ and the diameter of 57mm, performing hot extrusion forming by adopting a circular extrusion nozzle with the extrusion ratio of 16:1 and a 200t press under the pressure of 950MPa to obtain a pure titanium product, and air-cooling to room temperature.
The implementation results are as follows: the tensile strength was lower than 240MPa in an argon atmosphere, because the structure became coarser and the tensile strength was significantly reduced due to the too long holding time, as shown in FIG. 8, the microstructure was significantly coarser compared to example 4.
Comparative example 4
A method for preparing pure titanium by directly hot-extruding sponge titanium particles comprises the following steps:
step one, weighing 400g of 0-grade titanium sponge particles (with the oxygen content of 0.04 wt.%) with the diameter of 2-12.7 mm, placing the particles in a tray, and then placing the tray in a drying oven at 100-120 ℃ for drying for 120min to remove moisture in the titanium sponge;
step two, pouring the dried titanium sponge particles into a cylindrical green compact cylinder coated with a graphite lubricant and having a diameter of 53mm, pressing the titanium sponge particles at 850MPa by using a 200t press for 5min, and then reversely demoulding the pressed green compact by adopting a mode of ejecting out of a lower die to obtain a titanium sponge green compact with a diameter of 53mm and a height of 46 mm; the relative density of the titanium sponge compact was 87.4%;
rapidly heating the titanium sponge pressed blank by using a medium-frequency induction heating device under the air condition, heating the pressed blank to 1000 ℃ at a speed of 70 ℃/min, and preserving heat for 40min to obtain a sintered blank;
and step four, rapidly transferring the sintering blank heated to 1000 ℃ to an extrusion cylinder mould with the temperature of 400-450 ℃ and the diameter of 57mm under the air condition, performing hot extrusion forming by adopting a circular extrusion nozzle with the extrusion ratio of 16:1 and a 200t press under the pressure of 950MPa to obtain a pure titanium product, and air-cooling to room temperature.
The implementation results are as follows: under the air condition, the heat preservation time is more than or equal to 30min, a pure titanium sample is prepared, the mechanical property of the pure titanium sample is obviously improved compared with that of example 4, but the fracture elongation is lower than 10%, and the fracture elongation is far lower than TA1 (the fracture elongation is more than or equal to 30%), because oxygen in the air is dissolved and dissolved in the Ti matrix through the fractured oxide film along with the dissolution and fracture of the oxide film at high temperature, more oxygen is dissolved in the Ti matrix along with the longer heat preservation time, and the mechanical property of the pure titanium sample is obviously reduced, and finally fracture is initiated.
Comparative example 5
A method for preparing pure titanium by directly hot-extruding sponge titanium particles comprises the following steps:
step one, weighing 400g of 0-grade titanium sponge particles (with the oxygen content of 0.04 wt.%) with the diameter of 2-12.7 mm, placing the particles in a tray, and then placing the tray in a drying oven at 100-120 ℃ for drying for 120min to remove moisture in the titanium sponge;
step two, pouring the dried titanium sponge particles into a cylindrical green compact cylinder coated with a graphite lubricant and having a diameter of 53mm, pressing the titanium sponge particles at 850MPa by using a 200t press for 5min, and then reversely demoulding the pressed green compact by adopting a mode of ejecting out of a lower die to obtain a titanium sponge green compact with a diameter of 53mm and a height of 46 mm; the relative density of the titanium sponge compact was 87.4%;
step three, an operable closed atmosphere box is arranged on the hydraulic machine for vacuumizing treatment, the vacuum degree is lower than 0.01MPa, and then high-purity argon is introduced to ensure that the oxygen content is less than 200 ppm;
step four, rapidly heating the titanium sponge pressed blank by using a medium-frequency induction heating device, heating the pressed blank to 900 ℃ at a speed of 70 ℃/min, and preserving heat for 5min to obtain a sintered blank;
and step five, quickly transferring the sintering blank heated to 900 ℃ to an extrusion cylinder mold with the temperature of 400-450 ℃ and the diameter of 57mm, performing hot extrusion forming by adopting a circular extrusion nozzle with the extrusion ratio of 16:1 and a 200t press under the pressure of 950MPa to obtain a pure titanium product, and air-cooling to room temperature.
The implementation results are as follows: in the argon protective atmosphere, the pure titanium bar prepared by hot extrusion at 900 ℃ has the advantages that compared with the pure titanium bar prepared in the embodiment 1, the strength is reduced, the fracture elongation is lower than 20%, and the comprehensive mechanical property is lower than TA1 (the tensile strength is more than or equal to 240MPa, and the fracture elongation is more than or equal to 30%), because the lower the temperature is, the oxide film on the surface of the titanium sponge particles is not dissolved in time, finally, the interface bonding among the particles is poor, more micro cracks and micropores exist, the densification degree of the material is reduced, the strength is reduced, and meanwhile, the micro cracks and the micropores can become the root source and the path of crack expansion in the deformation process of the material, so that the material is broken in advance, and the material loses the original mechanical property.
Comparative example 5
A method for preparing pure titanium by directly hot-extruding sponge titanium particles comprises the following steps:
step one, weighing 400g of 0-grade titanium sponge particles (with the oxygen content of 0.04 wt.%) with the diameter of 2-12.7 mm, placing the particles in a tray, and then placing the tray in a drying oven at 100-120 ℃ for drying for 120min to remove moisture in the titanium sponge;
step two, pouring the dried titanium sponge particles into a cylindrical green compact cylinder coated with a graphite lubricant and having a diameter of 53mm, pressing the titanium sponge particles at 850MPa by using a 200t press for 5min, and then reversely demoulding the pressed green compact by adopting a mode of ejecting out of a lower die to obtain a titanium sponge green compact with a diameter of 53mm and a height of 46 mm; the relative density of the titanium sponge compact was 87.4%;
step three, an operable closed atmosphere box is arranged on the hydraulic machine for vacuumizing treatment, the vacuum degree is lower than 0.01MPa, and then high-purity argon is introduced to ensure that the oxygen content is less than 200 ppm;
step four, rapidly heating the titanium sponge pressed blank by using a medium-frequency induction heating device, heating the pressed blank to 1000 ℃ at a speed of 70 ℃/min, then heating the pressed blank to 1500 ℃ at a speed of 50 ℃/min, and preserving heat for 5min to obtain a sintered blank;
and step five, rapidly transferring the sintering blank heated to 1500 ℃ to an extrusion cylinder mold with the temperature of 400-450 ℃ and the diameter of 57mm, performing hot extrusion forming by adopting a circular extrusion nozzle with the extrusion ratio of 16:1 and a 200t press under the pressure of 950MPa to obtain a pure titanium product, and air-cooling to room temperature.
The implementation results are as follows: compared with example 1, the tensile strength of the pure titanium product prepared by hot extrusion in the argon protective atmosphere and heated to 1500 ℃ is much lower than that of TA1 (the tensile strength is more than or equal to 240MPa), because the higher temperature makes the material structure and crystal grains coarser under the condition of meeting the consolidation quality of the particles, which leads to the reduction of the comprehensive mechanical properties of the material.
Claims (10)
1. A method for preparing pure titanium by directly hot-extruding sponge titanium particles is characterized in that the sponge titanium particles are used as raw materials, and blank preparation, rapid heating sintering and thermal mechanical consolidation forming are directly carried out to obtain a pure titanium product; wherein the total time of the rapid heating sintering and the thermomechanical consolidation forming is less than or equal to 30 min.
2. A method for preparing pure titanium by directly hot-extruding sponge titanium particles is characterized by comprising the following steps:
(1) drying the titanium sponge particles
Placing the titanium sponge particles into a vacuum drying box for drying to obtain dried titanium sponge particles;
(2) preparing a blank from the granules
Pressing the dried titanium sponge particles into a titanium sponge green compact;
(3) rapid heating sintering
Rapidly heating and sintering the titanium sponge green compact at the sintering temperature of 1000-1200 ℃, and preserving heat for 5-10 min to obtain a sintered compact with uniform temperature;
wherein, the temperature is raised to 1000 ℃ at the rate of 50-150 ℃/min, and then the temperature is raised to the sintering temperature at the rate of 30-70 ℃/min;
(4) thermo-mechanical consolidation forming
Placing the sintered blank in an extrusion die, extruding the extrusion die with an inner cavity, and solidifying and forming in the inner cavity of the extrusion die to obtain a titanium product;
(5) cooling down
And cooling the titanium product to room temperature to obtain a pure titanium product.
3. The method for preparing pure titanium by directly hot extruding the titanium sponge particles according to claim 1 or 2, wherein the particle size of the titanium sponge particles is 0.1-20 mm, and the mass percent of oxygen contained in the titanium sponge is less than or equal to 0.3 wt.%.
4. The method for preparing pure titanium by directly hot extruding the titanium sponge particles according to claim 2, wherein in the step (1), the titanium sponge particles are dried at 100-150 ℃ for 100-120 min.
5. The method for preparing pure titanium by directly hot extruding the titanium sponge particles according to claim 2, wherein the pressing pressure is 500-950 MPa, and the pressure maintaining time is 4-6 min.
6. The method for preparing pure titanium by directly hot-extruding the titanium sponge particles as claimed in claim 2, wherein in the step (2), the relative density of the titanium sponge green compact is 80-95%.
7. The method for preparing pure titanium by directly and thermally extruding the titanium sponge particles as claimed in claim 2, wherein in the step (3), the titanium sponge particles are rapidly heated and sintered under a protective atmosphere or in air;
wherein the protective atmosphere is argon, and the mass percent of oxygen contained in the argon is less than or equal to 200 ppm.
8. The method for preparing pure titanium by directly hot extruding the titanium sponge particles according to claim 2, wherein the temperature of the extrusion die with the inner cavity in the step (4) is 450-550 ℃.
9. The method for preparing pure titanium by directly hot extruding the titanium sponge particles according to claim 2, wherein in the step (4), the extrusion strength is 500-950 MPa, and the extrusion ratio is (5-100): 1; the extrusion rate is 5 to 50 mm/s.
10. The method for preparing pure titanium by directly and thermally extruding the titanium sponge particles as claimed in claim 2, wherein in the method for preparing pure titanium by directly and thermally extruding the titanium sponge particles, the total time of the step (3) of rapid heating sintering and the step (4) of thermomechanical consolidation forming is less than or equal to 30 min.
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