CN114309603B - Method for preparing pure titanium by directly hot extruding titanium sponge 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 performs blank making, rapid heating sintering and thermo-mechanical consolidation forming to obtain a pure titanium product; wherein the total time of rapid heating sintering and thermo-mechanical consolidation forming is less than or equal to 30min, the grain diameter of the adopted titanium sponge particles is 0.1-20 mm, and the mass percentage of oxygen contained in the titanium sponge is less than or equal to 0.3wt.%. The method has low energy consumption, simple production process and lower production cost, solves 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 current process of preparing the pure titanium by powder metallurgy, and realizes the rapid preparation and forming of the powder metallurgy pure titanium product with low cost and low oxygen content.
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 titanium sponge particles.
Background
The pure titanium has low density (equivalent to 60 percent of stainless steel), medium strength (equivalent to the strength of stainless steel), good plasticity and high corrosion resistance, and is an ideal nonferrous 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 (below 1 wt.%) to titanium, along with grain refinement (ref: mimoto T, umeda J, kondoh K. Strengthening behaviour and mechanisms of extruded powder metallurgy pure Ti materials reinforced with ubiquitous light elements [ J ]. Powder Metallurgy,2016,59 (3): 223-228), the tensile strength of titanium can be greatly increased to above 800MPa while maintaining good tensile plasticity (elongation > 20%). The strength of titanium is obviously higher than that of stainless steel, so that the titanium is an ideal material for manufacturing parts of sports machinery such as automobiles, bicycles, scooters and the like, and has great application potential.
However, due to the high chemical activity of titanium, conventional titanium products are generally manufactured by two types of preparation methods:
first: ingot metallurgy method: specifically, a vacuum consumable furnace is adopted to smelt and cast the titanium sponge for 2-3 times to manufacture ingot metallurgy ingots, and then titanium products such as plates, bars, section bars, forgings and the like are manufactured through further thermo-mechanical processing. The number of remelting times can be reduced to one by using an electron beam melting furnace or a plasma melting furnace, but a large heat energy supply is still required. 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, and a large amount of energy is consumed for manufacturing titanium products, and meanwhile, the material loss is also 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.
Second,: powder metallurgy method: the method specifically comprises the following steps: the method comprises the steps of taking titanium powder or titanium hydride powder as a raw material, carrying out mechanical ball milling or mechanical mixing homogenization on the titanium powder or the titanium hydride powder and alloy element powder, then compacting or nearly net forming the powder mixture, and finally completing alloying and densification of titanium in a thermo-mechanical consolidation mode under the vacuum/protective atmosphere condition. This conventional titanium alloy powder metallurgy technique, while capable of significantly reducing energy consumption and cost, still suffers from the following typical shortcomings:
(1) The process of pulverizing is complex. The titanium powder or the titanium hydride powder is prepared by taking titanium sponge as a raw material, carrying out mechanical grinding and crushing after hydrogenation, and 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 procedure is repeated.
(2) The cost is still high. Such as: the price of the hydrogenated and dehydrogenated titanium powder of 200 meshes is more than 250 yuan/kg, the price of the low-cost titanium hydride powder manufactured by hydrogenating sponge titanium and mechanical grinding and the price of the intensified dehydrogenated titanium powder manufactured by dehydrogenating the titanium hydride powder are more than 30 percent higher than that of sponge titanium, so that the price of titanium products manufactured by using the hydrogenated and dehydrogenated titanium powder or the titanium hydride powder is more than 40 percent higher than that of sponge titanium, and the high price is a main obstacle for the wide application of commercial pure titanium compared with stainless steel.
(3) The oxygen content is high. Compared with the raw material titanium sponge particles, the particle size of the hydrogenated and dehydrogenated titanium powder or the hydrogenated titanium powder is in the micron level, and the particle size of the raw material titanium sponge particles is in the millimeter or even centimeter level, because the hydrogenated and dehydrogenated titanium powder or the hydrogenated titanium powder is smaller in size and larger in specific surface, the area of an oxide film is increased, and at the temperature of more than 700 ℃, the oxide film begins to dissolve, and oxygen can dissolve into a titanium matrix. At the same time, oxygen is very soluble in the titanium matrix at high temperature, which causes 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 a titanium matrix along with the dissolution of a powder oxide film, and because interstitial oxygen and nitrogen can produce solid solution strengthening on titanium and titanium alloy, the strength is improved, the molding is obviously reduced, the material failure can be caused by the excessively high oxygen and nitrogen content, meanwhile, the powder is more beneficial to the solid solution of oxygen and nitrogen in the titanium matrix because of the larger specific surface area of the powder, and the preparation of titanium products is mostly carried out in vacuum or protective atmosphere.
(5) The production period is long. Mainly embodied in powder sieving and powder mixing.
It is therefore of great importance to find a new process for the preparation of pure titanium articles.
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 procedures and lower production cost, and can specifically solve the problems of repeated powder preparation procedures, higher oxygen content, need of protective atmosphere, higher production cost, overlong production period and the like in the current powder metallurgy preparation process of pure titanium, thereby realizing the rapid preparation and forming of the powder metallurgy pure titanium product with low cost and low oxygen content.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the invention discloses a method for preparing pure titanium by directly hot extruding titanium sponge 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) Particle blank making
Pressing the dried titanium sponge particles into a titanium sponge pressed compact;
(3) Rapid heating sintering
Rapidly heating and sintering the titanium sponge pressed compact, wherein the sintering temperature is 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 temperature rising rate of 50-150 ℃/min, and then the temperature is continuously raised to the sintering temperature at the temperature rising 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
And cooling the titanium product to room temperature to obtain the pure titanium product.
In the step (1), the particle size of the titanium sponge particles is 0.1-20 mm, and the mass percentage 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 placed at 100-150 ℃ for drying 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 compact is 80-95%.
In the step (3), the sintering is heated and sintered rapidly, and the sintering is performed under a protective atmosphere or in air.
In the step (3), the sponge titanium compact is heated and sintered rapidly, preferably by an induction heating coil.
In the step (3), the protective atmosphere is preferably argon, and the mass percentage of oxygen contained in the argon is less than or equal to 200ppm.
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 shape and the size requirements of the cross section of the titanium product.
In the step (4), the extrusion die with the inner cavity can be bars, pipes and extruded long thick plates according to different dies used in densification and forming, and can also be a part die formed by forging.
In the step (5), air cooling is performed 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 thermo-mechanical consolidation forming in the step (4) is less than or equal to 30min, the total time is controlled by the heating rate, the temperature is increased to 1000 ℃ by adopting 50-150 ℃/min, and 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 thermo-mechanical consolidation forming in the step (4) can be performed 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 extrusion of the sponge titanium particles is different from the conventional ingot metallurgy multi-smelting and conventional powder metallurgy mechanical grinding and crushing, and aims at solving the problems of high oxygen content, complex and repeated preparation procedures, high cost and overlong production period of the prepared pure titanium, and the method for preparing the pure titanium by directly hot extrusion and consolidation of the sponge titanium particles serving as raw materials is realized, so that 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, low-cost titanium sponge particles are used as raw materials, and high-performance pure titanium is prepared by hot extrusion, solidification and rapid induction heating of sintered titanium sponge pressed compact in an 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 procedures 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 still has no influence on the performance of the titanium alloy, because the process of heating the sponge titanium blank by the medium-frequency induction heating device is a short-time sintering process, an oxide film is arranged on the front surface of the sponge titanium blank after being heated to 700 ℃ to prevent oxygen absorption, meanwhile, the compact forms closed pores in the short-time sintering process, and the oxide film is heated to more than 700 ℃ to be dissolved, but because the closed pores prevent oxygen absorption and internal oxidation, and the adverse influence on the performance of the titanium alloy caused by excessive oxygen absorption is avoided. The method has the advantages that the preparation of the pure titanium is different from the traditional powder metallurgy, the ball milling, the powder milling and other processes are omitted, the production process is simplified, and the cost for preparing the pure titanium is further reduced. Meanwhile, in order to meet more application requirements, sponge titanium with the oxygen content less than 0.3wt.% 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 combination of better strength and shaping, so that the application range of pure titanium is expanded, and meanwhile, the cost is reduced.
Drawings
Fig. 1 is a particle-bound gold phase diagram of example 1 sponge titanium particles to make pure titanium: (a) A metallographic phase of a sintered blank after rapid induction heating sintering, and (b) a metallographic phase of a pure titanium product after thermo-mechanical consolidation forming;
FIG. 2 is a microstructure of example 1 for preparing pure titanium by directly hot extruding titanium sponge particles;
FIG. 3 is a broken surface of a tensile test piece of pure titanium prepared by directly hot extruding titanium sponge particles in example 1;
FIG. 4 is a microstructure of example 3 for preparing pure titanium by directly hot extruding titanium sponge particles;
FIG. 5 is a microstructure of example 4 for preparing pure titanium by directly hot extruding titanium sponge particles;
FIG. 6 is a fracture surface of a tensile test piece of pure titanium prepared by directly hot extruding titanium sponge particles in example 4;
FIG. 7 is a microstructure of comparative example 2 in which titanium sponge particles were directly hot extruded to produce pure titanium;
FIG. 8 is a microstructure of comparative example 3 in which titanium sponge particles were directly hot extruded to produce pure titanium;
FIG. 9 is a process flow diagram of a method for preparing pure titanium by directly hot extruding titanium sponge particles according to the present invention.
Detailed Description
The present invention will be described in further detail with reference to examples.
In the examples below, titanium sponge particles having an oxygen content of less than 0.3wt.% are used, and titanium sponge particles having an excessively high oxygen content cause brittle failure of the titanium article.
Example 1
The embodiment provides a method for preparing pure titanium by directly hot extruding titanium sponge particles, the process flow chart of which is shown in fig. 9, comprising the following steps:
step one, weighing 400g, placing 0-level titanium sponge particles (with the oxygen content of 0.04 wt%) with the diameter of 2-12.7 mm in a tray, and then placing the tray in a drying box at 100-120 ℃ for drying for 120min to remove the moisture in the titanium sponge;
pouring the dried titanium sponge particles into a cylindrical briquette barrel coated with graphite lubricant and having a diameter of 53mm, using a 200t press to press under 850MPa for 5min, and reversely demoulding the pressed briquette by adopting a lower die ejection mode to obtain a titanium sponge briquette having a diameter of 53mm and a height of 46 mm; the relative density of the titanium sponge compact is 87.4%;
step three, carrying out vacuumizing treatment on a closed atmosphere box which is provided with an operable hydraulic press, wherein the vacuum degree is lower than 0.01MPa, and then introducing high-purity argon gas to ensure that the oxygen content is lower than 200ppm;
step four, rapidly heating the sponge titanium pressed compact by using an intermediate frequency induction heating device, heating the pressed compact to 1000 ℃ at 70 ℃/min, then heating the pressed compact from 1000 ℃ to 1200 ℃ at 50 ℃/min, and preserving heat for 5min to obtain a sintered compact;
and fifthly, rapidly transferring the sintered blank heated to 1200 ℃ to an extrusion cylinder die with the diameter of 57mm and the temperature of 400-450 ℃, adopting a round extrusion nozzle with the extrusion ratio of 16:1, adopting a 200t press, adopting 950MPa for hot extrusion forming, obtaining a pure titanium product, and air-cooling to room temperature.
Implementation results: under the protection of argon, the yield strength of the pure titanium bar prepared by hot extrusion reaches 196MPa, the tensile strength reaches 299MPa, the elongation is 63.2 percent, 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 percent), the invention relates to a method for preparing pure titanium by extrusion of sponge titanium particle pressed billets, the preparation process does not need complex procedures such as smelting, the energy consumption is reduced, the production procedure is simplified, and the production cost is reduced.
The metallographic phase of the sintered compact after rapid induction sintering in this example 1 is shown in fig. 1 (a), and the gold phase of the pure titanium product after thermo-mechanical consolidation molding is shown in fig. 1 (b); the method shows that the sponge titanium particles can be directly hot extruded to prepare nearly fully compact pure titanium products, and holes and cracks can be eliminated through hot extrusion deformation, so that better metallurgical bonding is achieved;
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 by the example is shown in fig. 3, and it can be seen from the graph that at the thermo-mechanical consolidation temperature of 1200 ℃, a large number of ductile pits exist on the fracture surface and holes exist in the ductile pits, which belongs to typical ductile fracture, and the fracture surface does not have weak bonding surfaces, so that the consolidation quality is better.
Example 2
A method for preparing pure titanium by directly hot extruding sponge titanium particles comprises the following steps:
firstly, 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 titanium sponge particles in a tray, and then putting the titanium sponge particles in a 100-120 ℃ drying box for drying for 120min to remove the moisture in the titanium sponge;
pouring the dried titanium sponge particles into a cylindrical compact cylinder coated with graphite lubricant and having a diameter of 53mm, pressing under 950MPa for 5min by using a 200t press, and reversely demolding the pressed compact by adopting a lower die ejection mode to obtain a compact with a diameter of 53mm and a height of 50 mm; the relative density of the titanium sponge compact is 90.4%;
and thirdly, rapidly heating the sponge titanium pressed compact by using an intermediate frequency induction heating device under the air condition, heating the pressed compact to 1000 ℃ at 70 ℃/min, heating the pressed compact to 1200 ℃ at 40 ℃/min, and preserving heat for 5min to obtain a sintered compact.
And fourthly, rapidly transferring the sintered blank with the temperature of 1200 ℃ to an extrusion cylinder die with the diameter of 57mm at the temperature of 400-450 ℃ under the air condition, adopting a square extrusion nozzle with the extrusion ratio of 9:1, adopting a 200t press, adopting 950MPa for hot extrusion forming, obtaining a pure titanium product, and air-cooling to room temperature.
Implementation results: the pure titanium bar prepared by hot extrusion rapid induction heating sintering of the sponge titanium particle pressed compact in air has the yield strength of 188MPa, the tensile strength of 298MPa and the elongation of 50 percent, and has the mechanical property 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), and the sponge titanium particles have smaller specific surface compared with powder because the size of the sponge titanium particles is larger, and the sponge titanium particles have fewer oxide films, and meanwhile, the temperature can promote the dissolution of the oxide films and the creep deformation of materials at two sides of the particles in the rapid induction heating sintering process, so that part of weak bonding surfaces further achieve better metallurgical bonding, and the creep deformation of the materials at two sides of the particles can eliminate micropores, so that densification is increased, and though larger holes are not eliminated, the larger holes can form internally-sealed holes in the rapid induction heating sintering process, so that titanium oxygen absorption and internal oxidation are prevented. The invention relates to a method for preparing pure titanium by using low-cost titanium sponge particles as raw materials, and by adopting a sponge titanium compact which is sintered by hot extrusion consolidation and rapid induction heating under the air condition, the performance of the method is equivalent to the mechanical performance of pure titanium prepared in a protective atmosphere, and the preparation process does not need complex procedures such as smelting, thereby reducing the energy consumption, simplifying the production procedures and reducing the production cost.
Room temperature mechanical property of sample prepared by hot extrusion of sponge titanium compact in argon protective atmosphere and air
H, O, N test results of the samples prepared by hot extrusion of titanium sponge compacts in an argon 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 1-grade titanium sponge particles with diameters of 2-12.7 mm (the oxygen content is 0.1 wt.%) and placing the titanium sponge particles in a tray, and then placing the titanium sponge particles in a 100-120 ℃ drying box for drying for 120min to remove the moisture in the titanium sponge;
pouring the dried titanium sponge particles into a cylindrical briquette barrel coated with graphite lubricant and having a diameter of 53mm, using a 200t press to press under 750MPa for 5min, and then reversely demoulding the pressed briquette by adopting a lower die ejection mode to obtain a titanium sponge briquette with a diameter of 53mm and a height of 47mm, wherein the relative density of the titanium sponge briquette is 85.5%;
step three, carrying out vacuumizing treatment on a closed atmosphere box which is provided with an operable hydraulic press, wherein the vacuum degree is lower than 0.01MPa, and then introducing high-purity argon gas to ensure that the oxygen content is lower than 200ppm;
step four, rapidly heating the sponge titanium pressed compact by using an intermediate frequency induction heating device, heating the pressed compact to 1000 ℃ at 70 ℃/min, then heating the pressed compact from 1000 ℃ to 1200 ℃ at 50 ℃/min, and preserving heat for 5min to obtain a sintered compact;
and fifthly, rapidly transferring the sintered blank heated to 1200 ℃ to an extrusion cylinder die with the temperature of 400-450 ℃ and the diameter of 57mm, adopting a round extrusion nozzle with the extrusion ratio of 16:1, adopting a 200t press, adopting 950MPa for hot extrusion forming, obtaining a pure titanium product, and air-cooling to room temperature.
Implementation results: under the protection of argon, the yield strength of the pure titanium bar prepared by hot extrusion is 240MPa, the tensile strength reaches 362MPa, the elongation is 37.3 percent, 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 percent), 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 the proper oxygen content. The invention relates to a method for preparing pure titanium by using sponge titanium particle pressed compact extrusion, which does not need complex procedures such as smelting and the like in the preparation process, reduces energy consumption, simplifies production procedures and reduces 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, placing 0-level titanium sponge particles (with the oxygen content of 0.04 wt%) with the diameter of 2-12.7 mm in a tray, and then placing the tray in a drying box at 100-120 ℃ for drying for 120min to remove the moisture in the titanium sponge;
pouring the dried titanium sponge particles into a cylindrical briquette barrel coated with graphite lubricant and having a diameter of 53mm, pressing under 750MPa for 5min by using a 200t press, and reversely demolding the pressed briquette by adopting a lower die ejection mode to obtain a titanium sponge briquette having a diameter of 53mm and a height of 47 mm; the relative density of the titanium sponge compact is 85.5%;
step three, carrying out vacuumizing treatment on a closed atmosphere box which is provided with an operable hydraulic press, wherein the vacuum degree is lower than 0.01MPa, and then introducing high-purity argon gas to ensure that the oxygen content is lower than 200ppm;
step four, rapidly heating the titanium sponge pressed compact by using an intermediate frequency induction heating device, heating the pressed compact to 1000 ℃ at 70 ℃/min, and preserving heat for 5min to obtain a sintered compact;
and fifthly, rapidly transferring the sintered blank heated to 1000 ℃ to an extrusion cylinder die with the diameter of 57mm and the temperature of 400-450 ℃, adopting a round extrusion nozzle with the extrusion ratio of 16:1, adopting a 200t press, adopting 950MPa for hot extrusion forming, obtaining a pure titanium product, and air-cooling to room temperature.
Implementation results: under the protection of argon, the yield strength of the pure titanium bar prepared by hot extrusion reaches 192MPa, the tensile strength reaches 292MPa, the elongation is 46.3 percent, 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, the elongation at break is more than or equal to 30 percent), the mechanical property of the pure titanium bar is equivalent to that of example 1, the tensile strength is equivalent, the elongation at break is reduced, the creep deformation of materials on two sides of particles is eliminated due to high temperature, the deformation of the particles is facilitated by high temperature, the densification degree of the materials is increased in the thermomechanical consolidation process, the particles and the particles are better metallurgically bonded, the temperature is lower, more weak bonding surfaces exist, the weak bonding surfaces become the root sources and the extension ways of cracks in the deformation process of the materials, and the elongation at break is reduced. The invention relates to a method for preparing pure titanium by extrusion of sponge titanium particle pressed compact, which does not need complex procedures such as smelting and the like in the preparation process, reduces energy consumption, simplifies production procedures and reduces production cost.
The microstructure diagram of the pure titanium prepared by directly hot-extruding the sponge titanium particles is shown in fig. 5;
in this example 4, the fracture surface of the pure titanium product prepared is shown in fig. 6, from which it can be seen that there are still unbound particles with smaller size at lower thermo-mechanical consolidation temperature, and by comparison with example 1, it is demonstrated that increasing the temperature will be beneficial to eliminate holes and microcracks, promote inter-particle bonding, and improve the inter-particle consolidation quality.
Example 5
The embodiment provides a method for preparing pure titanium by directly hot extruding titanium sponge particles, which comprises the following steps:
step one, weighing 400g, placing 0-level titanium sponge particles (with the oxygen content of 0.04 wt%) with the diameter of 15-20 mm in a tray, and then placing the tray in a drying box at 130-150 ℃ for drying for 100min to remove the moisture in the titanium sponge;
pouring the dried titanium sponge particles into a cylindrical briquette barrel coated with graphite lubricant and having a diameter of 53mm, pressing under 500MPa for 6min by using a 200t press, and reversely demolding the pressed briquette by adopting a lower die ejection mode to obtain a titanium sponge briquette having a diameter of 53mm and a height of 50 mm; the relative density of the titanium sponge compact is 80.4%;
step three, carrying out vacuumizing treatment on a closed atmosphere box which is provided with an operable hydraulic press, wherein the vacuum degree is lower than 0.01MPa, and then introducing high-purity argon gas to ensure that the oxygen content is lower than 200ppm;
step four, rapidly heating the sponge titanium pressed compact by using an intermediate frequency induction heating device, heating the pressed compact to 1000 ℃ at 50 ℃/min, then heating the pressed compact from 1000 ℃ to 1100 ℃ at 30 ℃/min, and preserving heat for 5min to obtain a sintered compact;
and fifthly, rapidly transferring the sintered blank heated to 1100 ℃ to an extrusion cylinder die with the temperature of 500-550 ℃ and the diameter of 57mm, adopting a round extrusion nozzle with the extrusion ratio of 70:1, adopting a 200t press, adopting 750MPa for hot extrusion consolidation forming by using the pressure of 200t press, obtaining a pure titanium product, and cooling to the room temperature at the speed of 50-60 ℃/min.
Example 6
The embodiment provides a method for preparing pure titanium by directly hot extruding titanium sponge particles, which comprises the following steps:
step one, weighing 400g, placing 0-level titanium sponge particles (with the oxygen content of 0.04 wt%) with the diameter of 2-12.7 mm in a tray, and then placing the tray in a drying box at 100-120 ℃ for drying for 120min to remove the moisture in the titanium sponge;
pouring the dried titanium sponge particles into a cylindrical briquette barrel coated with graphite lubricant and having a diameter of 53mm, pressing under 950MPa for 4min by using a 200t press, and reversely demolding the pressed briquette by adopting a lower die ejection mode to obtain a titanium sponge briquette having a diameter of 53mm and a height of 44 mm; the relative density of the titanium sponge compact is 91.3%;
and thirdly, rapidly heating the sponge titanium pressed compact by using an intermediate frequency induction heating device under the air condition, heating the pressed compact to 1000 ℃ at 100 ℃/min, heating the pressed compact to 1200 ℃ at 50 ℃/min, and preserving heat for 5min to obtain a sintered compact.
And step four, rapidly transferring the sintered blank with the temperature of 1200 ℃ to an extrusion cylinder die with the diameter of 57mm and the temperature of 450-500 ℃ under the air condition, adopting a square extrusion nozzle with the extrusion ratio of 30:1, adopting a 200t press with the extrusion rate of 10mm/s, adopting 550MPa for hot extrusion forming, obtaining a pure titanium product, and air-cooling to room temperature.
Example 7
The embodiment provides a method for preparing pure titanium by directly hot extruding titanium sponge particles, which comprises the following steps:
step one, weighing 400g, placing 0-level titanium sponge particles (with the oxygen content of 0.04 wt%) with the diameter of 2-12.7 mm in a tray, and then placing the tray in a drying box at 100-120 ℃ for drying for 120min to remove the moisture in the titanium sponge;
pouring the dried titanium sponge particles into a cylindrical briquette barrel coated with graphite lubricant and having a diameter of 53mm, pressing under 650MPa for 5min by using a 200t press, and reversely demolding the pressed briquette by adopting a lower die ejection mode to obtain a titanium sponge briquette having a diameter of 53mm and a height of 48 mm; the relative density of the titanium sponge compact is 83.7%;
step three, carrying out vacuumizing treatment on a closed atmosphere box which is provided with an operable hydraulic press, wherein the vacuum degree is lower than 0.01MPa, and then introducing high-purity argon gas to ensure that the oxygen content is lower than 200ppm;
step four, rapidly heating the sponge titanium pressed compact by using an intermediate frequency induction heating device, heating the pressed compact to 1000 ℃ at 150 ℃/min, then heating the pressed compact from 1000 ℃ to 1150 ℃ at 70 ℃/min, and preserving heat for 5min to obtain a sintered compact;
and fifthly, rapidly transferring the sintered blank heated to 1150 ℃ to an extrusion cylinder die with the diameter of 57mm and the temperature of 400-450 ℃, adopting a round extrusion nozzle with the extrusion ratio of 20:1, adopting a 200t press, adopting 500MPa for hot extrusion consolidation forming at the extrusion rate of 30mm/s, obtaining a pure titanium product, and cooling to the room temperature at the cooling rate of 80 ℃/min.
Example 8
The embodiment provides a method for preparing pure titanium by directly hot extruding titanium sponge particles, which comprises the following steps:
step one, weighing 400g, placing 0-level titanium sponge particles (with the oxygen content of 0.04 wt%) with the diameter of 2-12.7 mm in a tray, and then placing the tray in a drying box at 100-120 ℃ for drying for 120min to remove the moisture in the titanium sponge;
pouring the dried titanium sponge particles into a cylindrical briquette barrel coated with graphite lubricant and having a diameter of 53mm, pressing under 750MPa for 5min by using a 200t press, and reversely demolding the pressed briquette by adopting a lower die ejection mode to obtain a titanium sponge briquette having a diameter of 53mm and a height of 47 mm; the relative density of the titanium sponge compact is 85.5%;
and thirdly, rapidly heating the sponge titanium pressed compact by using an intermediate frequency induction heating device under the air condition, heating the pressed compact to 1000 ℃ at 80 ℃/min, heating the pressed compact to 1200 ℃ at 40 ℃/min, and preserving heat for 5min to obtain a sintered compact.
And fourthly, rapidly transferring the sintered blank with the temperature of 1200 ℃ to an extrusion cylinder die with the diameter of 57mm at the temperature of 400-450 ℃ under the air condition, adopting a square extrusion nozzle with the extrusion ratio of 90:1, adopting a 200t press, adopting 950MPa for hot extrusion forming, obtaining 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:
firstly, weighing 400g of-200 mesh hydrogenated and dehydrogenated titanium powder (with the oxygen content of 0.11 wt.%) and placing in a tray, and then placing in a drying box at 100-120 ℃ for drying for 120min to remove the moisture in the hydrogenated and dehydrogenated titanium powder;
pouring the dried hydrogenated and dehydrogenated titanium powder particles into a cylindrical compact cylinder coated with graphite lubricant and having the diameter of 53mm, pressing under 750MPa for 5min by using a 200t press, and reversely demolding the pressed compact in a lower die ejection mode to obtain a titanium sponge compact with the diameter of 53mm and the height of 46.5mm, wherein the relative density of the titanium sponge compact is 86.4%;
step three, carrying out vacuumizing treatment on a closed atmosphere box which is provided with an operable hydraulic press, wherein the vacuum degree is lower than 0.01MPa, and then introducing high-purity argon gas to ensure that the oxygen content is lower than 200ppm;
step four, rapidly heating the sponge titanium pressed compact by using an intermediate frequency induction heating device, heating the pressed compact to 1000 ℃ at 70 ℃/min, then heating the pressed compact from 1000 ℃ to 1200 ℃ at 50 ℃/min, and preserving heat for 5min to obtain a sintered compact;
and fifthly, rapidly transferring the sintered blank heated to 1200 ℃ to an extrusion cylinder die with the temperature of 400-450 ℃ and the diameter of 57mm, adopting a round extrusion nozzle with the extrusion ratio of 16:1, adopting a 200t press, adopting 950MPa for hot extrusion forming, obtaining a pure titanium product, and air-cooling to room temperature.
Implementation results: under the protection of argon, the pure titanium bar prepared by hot extrusion has the tensile strength reaching 370MPa and the elongation being 41 percent, 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 percent), compared with the hot mechanical solidification bar forming of-200 meshes of hydrogenated dehydrogenated titanium powder, the hot mechanical solidification extrusion forming of the sponge titanium particles in the example 3 also achieves better metallurgical bonding, however, the cost is calculated, the price of-200 meshes of hydrogenated dehydrogenated titanium powder or hydrogenated titanium powder is more than 250 yuan/kg, the price of low-cost hydrogenated titanium powder prepared by hydrogenation sponge titanium and mechanical grinding and the price of the reinforced dehydrogenated titanium powder prepared by hydrogenation titanium powder are more than 30 percent of sponge titanium, the price of a titanium product prepared by hydrogenation dehydrogenated powder or hydrogenated titanium powder is more than 40 percent of sponge titanium, the cost of directly hot extruding sponge titanium particles is far lower than that of traditional powder metallurgy, and the solidification quality of sponge titanium particles is equivalent to the solidification quality of titanium powder. The invention relates to a method for preparing pure titanium by using sponge titanium particle pressed compact extrusion, which does not need the traditional powder metallurgy powder process in the preparation process, reduces energy consumption, simplifies production procedures and reduces production cost.
Comparative example 2
A method for preparing pure titanium by directly hot extruding sponge titanium particles comprises the following steps:
firstly, weighing 400g of titanium sponge particles with diameters of 2-12.7 mm (oxygen content is 0.44 wt.%) and placing the titanium sponge particles in a tray, and then placing the titanium sponge particles in a 100-120 ℃ drying box for drying for 120min to remove water in the titanium sponge;
pouring the dried titanium sponge particles into a cylindrical briquette barrel coated with graphite lubricant and having a diameter of 53mm, pressing under 750MPa for 5min by using a 200t press, and reversely demolding the pressed briquette by adopting a lower die ejection mode to obtain a titanium sponge briquette having a diameter of 53mm and a height of 47.5 mm; the relative density of the titanium sponge compact is 84.6%;
step three, carrying out vacuumizing treatment on a closed atmosphere box which is provided with an operable hydraulic press, wherein the vacuum degree is lower than 0.01MPa, and then introducing high-purity argon gas to ensure that the oxygen content is lower than 200ppm;
step four, rapidly heating the sponge titanium pressed compact by using an intermediate frequency induction heating device, heating the pressed compact to 1000 ℃ at 70 ℃/min, then heating the pressed compact from 1000 ℃ to 1200 ℃ at 50 ℃/min, and preserving heat for 5min to obtain a sintered compact;
and fifthly, rapidly transferring the sintered blank heated to 1200 ℃ to an extrusion cylinder die with the diameter of 57mm and the temperature of 400-450 ℃, adopting a round extrusion nozzle with the extrusion ratio of 16:1, adopting a 200t press, adopting 950MPa for hot extrusion forming, obtaining a pure titanium product, and air-cooling to room temperature.
The titanium sponge used in this comparative example was different in oxygen content from that used in example 1, and the results of the implementation of this comparative example: under the protection of argon, the pure titanium bar prepared by hot extrusion is brittle broken, oxygen is a central problem for manufacturing titanium and titanium alloy, strong short-range repulsive interaction between interstitial oxygen and screw dislocation cores enhances the strength of titanium, but reduces the tensile plasticity and toughness of titanium, and the brittle broken is easy to occur due to the fact that the oxygen content is too high. The microstructure of the pure titanium product prepared in this comparative example is shown in fig. 7, and by comparing with examples 1 and 3, it is demonstrated that as the oxygen content increases, pure titanium is transformed from equiaxed structure to lamellar structure, because interstitial oxygen is a crystal defect as interstitial atoms, and new phases tend to nucleate at the crystal defect. Oxygen is dissolved in the alpha-Ti, so that the c/a value of the alpha-Ti is improved, the c/a value is increased, the distance between the prismatic surfaces of the alpha-Ti crystal lattice is reduced, the stacking density on the stacking surface is reduced to a certain extent compared with a basal plane, the sliding on the prismatic surfaces is not facilitated, the sliding system is reduced, and the shaping is reduced. Meanwhile, the excessive oxygen content can lead the pure titanium to generate uneven solid solution of oxygen, so that the yield strength difference of the soft and hard areas of the pure titanium can be larger, the coordinated deformation capacity of the soft and hard areas can be obviously reduced, and the fracture is finally initiated. It has been demonstrated that the process for the preparation of pure titanium by extrusion from compacted titanium sponge particles requires the use of titanium sponge particles having an oxygen content of less than 0.3wt.%.
Comparative example 3
A method for preparing pure titanium by directly hot extruding sponge titanium particles comprises the following steps:
step one, weighing 400g, placing 0-level titanium sponge particles (with the oxygen content of 0.04 wt%) with the diameter of 2-12.7 mm in a tray, and then placing the tray in a drying box at 100-120 ℃ for drying for 120min to remove the moisture in the titanium sponge;
pouring the dried titanium sponge particles into a cylindrical briquette barrel coated with graphite lubricant and having a diameter of 53mm, using a 200t press to press under 850MPa for 5min, and reversely demoulding the pressed briquette by adopting a lower die ejection mode to obtain a titanium sponge briquette having a diameter of 53mm and a height of 46 mm; the relative density of the titanium sponge compact is 87.4%;
step three, carrying out vacuumizing treatment on a closed atmosphere box which is provided with an operable hydraulic press, wherein the vacuum degree is lower than 0.01MPa, and then introducing high-purity argon gas to ensure that the oxygen content is lower than 200ppm;
step four, rapidly heating the titanium sponge pressed compact by using an intermediate frequency induction heating device, heating the pressed compact to 1000 ℃ at 70 ℃/min, and preserving heat for 40min to obtain a sintered compact;
and fifthly, rapidly transferring the sintered blank heated to 1000 ℃ to an extrusion cylinder die with the temperature of 400-450 ℃ and the diameter of 57mm, adopting a round extrusion nozzle with the extrusion ratio of 16:1, adopting a 200t press, adopting 950MPa for hot extrusion forming, obtaining a pure titanium product, and air-cooling to room temperature.
Implementation results: under the protection of argon, the tensile strength is lower than 240MPa, because the tissue becomes coarser due to the overlong heat preservation time, the tensile strength is obviously reduced, and compared with example 4, the microstructure is obviously coarser as shown in fig. 8.
Comparative example 4
A method for preparing pure titanium by directly hot extruding sponge titanium particles comprises the following steps:
step one, weighing 400g, placing 0-level titanium sponge particles (with the oxygen content of 0.04 wt%) with the diameter of 2-12.7 mm in a tray, and then placing the tray in a drying box at 100-120 ℃ for drying for 120min to remove the moisture in the titanium sponge;
pouring the dried titanium sponge particles into a cylindrical briquette barrel coated with graphite lubricant and having a diameter of 53mm, using a 200t press to press under 850MPa for 5min, and reversely demoulding the pressed briquette by adopting a lower die ejection mode to obtain a titanium sponge briquette having a diameter of 53mm and a height of 46 mm; the relative density of the titanium sponge compact is 87.4%;
step three, under the air condition, rapidly heating the sponge titanium pressed compact by using an intermediate frequency induction heating device, heating the pressed compact to 1000 ℃ at 70 ℃/min, and preserving heat for 40min to obtain a sintered compact;
and fourthly, rapidly transferring the sintered blank heated to 1000 ℃ to an extrusion cylinder die with the diameter of 57mm and the temperature of 400-450 ℃ under the air condition, adopting a round extrusion nozzle with the extrusion ratio of 16:1, adopting a 200t press, adopting 950MPa for hot extrusion forming, obtaining a pure titanium product, and air-cooling to room temperature.
Implementation results: under the air condition, the heat preservation time is more than or equal to 30min to prepare a pure titanium sample, the mechanical property of the pure titanium sample is obviously improved compared with that of the 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 can be dissolved in a Ti matrix through the broken oxide film along with the dissolution and the fracture of the oxide film at high temperature, and more oxygen can be dissolved in the Ti matrix along with the longer heat preservation time, so that the mechanical property of the pure titanium sample is obviously reduced, and the fracture is finally 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, placing 0-level titanium sponge particles (with the oxygen content of 0.04 wt%) with the diameter of 2-12.7 mm in a tray, and then placing the tray in a drying box at 100-120 ℃ for drying for 120min to remove the moisture in the titanium sponge;
pouring the dried titanium sponge particles into a cylindrical briquette barrel coated with graphite lubricant and having a diameter of 53mm, using a 200t press to press under 850MPa for 5min, and reversely demoulding the pressed briquette by adopting a lower die ejection mode to obtain a titanium sponge briquette having a diameter of 53mm and a height of 46 mm; the relative density of the titanium sponge compact is 87.4%;
step three, carrying out vacuumizing treatment on a closed atmosphere box which is provided with an operable hydraulic press, wherein the vacuum degree is lower than 0.01MPa, and then introducing high-purity argon gas to ensure that the oxygen content is lower than 200ppm;
step four, rapidly heating the titanium sponge pressed compact by using an intermediate frequency induction heating device, heating the pressed compact to 900 ℃ at 70 ℃/min, and preserving heat for 5min to obtain a sintered compact;
and fifthly, rapidly transferring the sintered blank heated to 900 ℃ to an extrusion cylinder die with the temperature of 400-450 ℃ and the diameter of 57mm, adopting a round extrusion nozzle with the extrusion ratio of 16:1, adopting a 200t press, adopting 950MPa for hot extrusion forming, obtaining a pure titanium product, and air-cooling to room temperature.
Implementation results: compared with the example 1, the strength of the pure titanium bar prepared by hot extrusion at 900 ℃ is reduced, the fracture elongation is lower than 20%, the comprehensive mechanical property is lower than TA1 (the tensile strength is not less than 240MPa, and the fracture elongation is not less than 30%), because the lower the temperature is, the oxide film on the surface of the titanium sponge particles is not dissolved, the interface bonding among the particles is poor finally, more microcracks and micropores exist, the densification degree of the material is reduced, the strength of the material is reduced, and meanwhile, the microcracks and the micropores become the root and the path of crack expansion in the deformation process of the material, so that the material is broken in advance, and the original mechanical property of the material is lost.
Comparative example 5
A method for preparing pure titanium by directly hot extruding sponge titanium particles comprises the following steps:
step one, weighing 400g, placing 0-level titanium sponge particles (with the oxygen content of 0.04 wt%) with the diameter of 2-12.7 mm in a tray, and then placing the tray in a drying box at 100-120 ℃ for drying for 120min to remove the moisture in the titanium sponge;
pouring the dried titanium sponge particles into a cylindrical briquette barrel coated with graphite lubricant and having a diameter of 53mm, using a 200t press to press under 850MPa for 5min, and reversely demoulding the pressed briquette by adopting a lower die ejection mode to obtain a titanium sponge briquette having a diameter of 53mm and a height of 46 mm; the relative density of the titanium sponge compact is 87.4%;
step three, carrying out vacuumizing treatment on a closed atmosphere box which is provided with an operable hydraulic press, wherein the vacuum degree is lower than 0.01MPa, and then introducing high-purity argon gas to ensure that the oxygen content is lower than 200ppm;
step four, rapidly heating the sponge titanium pressed compact by using an intermediate frequency induction heating device, heating the pressed compact to 1000 ℃ at 70 ℃/min, then heating the pressed compact to 1500 ℃ at 50 ℃/min, and preserving heat for 5min to obtain a sintered compact;
and fifthly, rapidly transferring the sintered blank heated to 1500 ℃ to an extrusion cylinder die with the temperature of 400-450 ℃ and the diameter of 57mm, adopting a round extrusion nozzle with the extrusion ratio of 16:1, adopting a 200t press, adopting 950MPa for hot extrusion forming, obtaining a pure titanium product, and air-cooling to room temperature.
Implementation results: in the argon protection atmosphere, the mechanical properties of the pure titanium product prepared by hot extrusion heated to 1500 ℃ are far lower than those of the pure titanium product prepared by hot extrusion in example 1, and the tensile strength is far lower than TA1 (the tensile strength is more than or equal to 240 MPa), because the higher temperature can lead the material structure and the grains to be coarser under the condition of meeting the consolidation quality of the particles, and the comprehensive mechanical properties of the material can be reduced.
Claims (8)
1. The method for preparing pure titanium by directly hot extruding sponge titanium particles is characterized by comprising the following steps of:
(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) Particle blank making
Pressing the dried titanium sponge particles into a titanium sponge pressed compact;
(3) Rapid heating sintering
Rapidly heating and sintering the titanium sponge pressed compact, wherein the sintering temperature is 1100-1200 ℃, and preserving heat for 5-10 min to obtain a sintered compact with uniform temperature;
wherein, the temperature is raised to 1000 ℃ at the temperature rising rate of 50-150 ℃/min, and then the temperature is raised to the sintering temperature continuously at the temperature rising 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
Cooling the titanium product to room temperature to obtain a pure titanium product;
wherein the total time of rapid heating sintering and thermo-mechanical consolidation forming is less than or equal to 30min;
the tensile strength of the prepared pure titanium product is more than or equal to 240MPa, and the elongation at break is more than or equal to 30%.
2. The method for preparing pure titanium by directly hot extruding titanium sponge particles according to claim 1, wherein the particle size of the titanium sponge particles is 0.1-20 mm, and the mass percentage of oxygen contained in the titanium sponge is less than or equal to 0.3wt.%.
3. The method for preparing pure titanium by directly hot extrusion of titanium sponge particles according to claim 1, wherein in the step (1), the titanium sponge particles are dried at 100-150 ℃ for 100-120 min.
4. The method for preparing pure titanium by directly hot extruding titanium sponge particles according to claim 1, wherein the pressing pressure is 500-950 mpa and the dwell time is 4-6 min.
5. The method for preparing pure titanium by directly hot extruding titanium sponge particles according to claim 1, wherein in the step (2), the relative density of the titanium sponge compact is 80-95%.
6. The method for preparing pure titanium by directly hot extrusion of titanium sponge particles according to claim 1, wherein in the step (3), rapid heating sintering is performed under a protective atmosphere or in air;
wherein the protective atmosphere is argon, and the mass percentage of oxygen contained in the argon is less than or equal to 200ppm.
7. The method for preparing pure titanium by directly hot extrusion of titanium sponge particles according to claim 1, wherein in the step (4), the temperature of an extrusion die with an inner cavity is 450-550 ℃.
8. The method for preparing pure titanium by directly hot extrusion of titanium sponge particles according to claim 1, wherein in the step (4), the extrusion strength is 500-950 MPa, and the extrusion ratio is (5-100): 1; the extrusion rate is 5-50 mm/s.
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