CN117165759A - Heat treatment integrated furnace for high-activity titanium alloy high-flux components and preparation method - Google Patents
Heat treatment integrated furnace for high-activity titanium alloy high-flux components and preparation method Download PDFInfo
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- 238000010438 heat treatment Methods 0.000 title claims abstract description 100
- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 75
- 230000000694 effects Effects 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000001816 cooling Methods 0.000 claims abstract description 44
- 238000003723 Smelting Methods 0.000 claims abstract description 40
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000012546 transfer Methods 0.000 claims abstract description 20
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 16
- 239000010937 tungsten Substances 0.000 claims abstract description 16
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Abstract
A heat treatment integrated furnace for high-activity titanium alloy high-flux components and a preparation method thereof relate to a smelting and casting integrated device and a preparation method. The invention aims to solve the problems of complex process, high cost and difficult guarantee of mechanical properties of the traditional titanium alloy. The water-cooling crucible assembly and the heat treatment furnace are arranged in a furnace body, the turning transfer clamp is movably and hermetically inserted in the furnace body, the water-cooling system is arranged at the lower part of the furnace body, the electric arc gun transmission mechanism is vertically and hermetically inserted in the furnace body, the non-self-consumption tungsten electrode is arranged at the lower end of the electric arc gun transmission mechanism, and the non-self-consumption tungsten electrode is positioned right above the water-cooling crucible assembly; after smelting is completed by utilizing the water-cooled copper crucible, heat treatment can be directly carried out without re-opening the furnace, thereby ensuring the recycling of argon, reducing the cost, saving energy and improving the production efficiency. The method is used for preparing the titanium alloy.
Description
Technical Field
The invention relates to a heat treatment integrated furnace and a preparation method thereof, in particular to a device for preparing as-cast ultrahigh-strength and high-toughness titanium alloy by utilizing a high-flux component design and a heat treatment integrated furnace and a preparation method thereof, wherein solid solution aging heat treatment is carried out through the same furnace transfer, alpha phases with different forms are separated out from beta phases, the structure of the titanium alloy is improved, and the oxygen content in an ingot is lower than 300ppm, so that the strength and toughness of the ingot are improved, the ultrahigh-toughness titanium alloy is obtained in an as-cast state, a foundation is provided for the deformation rolling of a next-step titanium alloy plate and wire rod, and the device belongs to the technical field of the processing of the ingot with the low oxygen content of the high-activity titanium alloy.
Background
The ultra-high strength and toughness titanium alloy is an indispensable advanced structural material in the aerospace field, is focused, and has fast and remarkable progress. Along with the rapid development of various aircrafts and the continuous expansion of the application scene of the titanium alloy, the realization of the good matching of the strength, the plasticity and the toughness of the ultra-high strength and toughness titanium alloy is the hot spot and the front edge of the current international research. In order to fully mine the application potential of the high-strength titanium alloy, the alloy is applied more importantly in more key fields, and the deep understanding of the research and development status, processing technology, structure-performance relationship, deformation behavior, fracture mechanism, toughening mechanism and the like is very important, so that the innovation of alloying regulation and control and preparation methods, the adoption of different heat treatment means and the like are common research methods.
The structure of the titanium alloy can be regulated and controlled by a solid solution aging heat treatment processThereby significantly affecting the mechanical properties of the titanium alloy. Solution treatment is carried out below the transformation point of the titanium alloy, and the microstructure is a two-phase structure of alpha+beta, namely a matrix of beta grains is distributed with a large amount of unconverted primary alpha phase (alpha p ) The particles and beta grains are in a strip shape, and are beneficial to the plasticity and toughness of the alloy. A large amount of crisscrossed (alpha) are precipitated in the structure after aging of the beta-titanium alloy s ) The interface between the strips can prevent the sliding, make the deformation more difficult, alpha s The more the phase content, the finer the grains and the higher the strength of the material.
Most of the preparation of the ultra-high strength and toughness titanium alloy needs to regulate and control the structure by heat treatment. Aiming at the current titanium alloy research situation, the aerospace fine stock limited company (patent publication No. CN 204022922U) designs a novel titanium alloy solution heat treatment furnace, ensures that a product is not easy to oxidize in the water-cooling solution process, ensures the mechanical property of the product after solution, but the equipment can only perform solution heat treatment regulation and control, and has single process. The Jiangsu Henghong aerospace new material limited company (patent publication No. CN 214937739U) discloses a heat treatment device for processing a titanium alloy bar before rolling, which ensures the heating uniformity of the titanium alloy bar and prevents uneven heating, but the device is only suitable for the bar before rolling, and the alloy structure needs to be regulated and controlled in multiple steps, so that the steps are complex and the cost is higher. Therefore, the titanium alloy structure is regulated and controlled in a convenient mode, so that the cost and the time can be saved, and meanwhile, the required performance requirement can be met, and the method is one direction pursued by the current titanium alloy preparation. Although Beijing university of science and technology (patent publication No. CN 111705256A) also proposes a system and method for preparing a metal material in high throughput, unlike the above-mentioned method, induction melting is adopted in the apparatus, the equipment cost is high and special induction melting equipment is required. For titanium alloy materials, the arc melting can be satisfied and the melting speed is high, and the temperature and alloy components can be precisely controlled, so that highly customized metal materials can be produced, and the method is suitable for large-scale industrial production.
In addition, when the titanium alloy is subjected to heat treatment, a tube is usually sealed, or the titanium alloy is protected by argon atmosphere, or the titanium alloy is directly placed in air. The tube sealing treatment of the titanium alloy can avoid the influence of external oxygen on the alloy during heating, but the size of the cast ingot is limited due to the limitation of the tube sealing size. The heat treatment under the protection of argon atmosphere avoids the influence of external oxygen and has no size limitation, but the operation is complicated, and the process flow and the cost are increased. The titanium alloy is directly placed in the air for treatment, and although the alloy size is not limited, the titanium alloy is high in activity and easy to oxidize at high temperature, and an oxide layer can fall off layer by layer, so that the mechanical property of the titanium alloy can be adversely affected.
In conclusion, the existing titanium alloy has the problems of complex process, high cost and difficult guarantee of mechanical properties.
Disclosure of Invention
The invention aims to solve the problems of complex process, high cost and difficult guarantee of mechanical properties in the preparation of the traditional titanium alloy. Further provides a heat treatment integrated furnace with high-activity titanium alloy high-flux components and a preparation method thereof.
The technical scheme of the invention is as follows: the integrated furnace for heat treatment of high-activity titanium alloy high-flux components comprises a furnace body, a gas cylinder and a vacuumizing system, wherein an observation window is formed in the side end surface of the upper part of the furnace body, the gas cylinder and the vacuumizing system are arranged outside the furnace body and are communicated with the inside of the furnace body, the integrated furnace further comprises a water-cooling crucible assembly, an arc gun transmission mechanism, a non-consumable tungsten electrode, a water-cooling system, a turning transfer clamp and a heat treatment furnace, the water-cooling crucible assembly and the heat treatment furnace are arranged in the furnace body, the turning transfer clamp is movably and hermetically inserted in the furnace body, the water-cooling system is arranged at the lower part of the furnace body, the arc gun transmission mechanism is vertically and hermetically inserted in the furnace body, the non-consumable tungsten electrode is arranged at the lower end of the arc gun transmission mechanism, and the non-consumable tungsten electrode is positioned right above the water-cooling crucible assembly; the water-cooling crucible assembly comprises a water-cooling crucible and a water-cooling bracket, the water-cooling bracket is vertically arranged in the furnace body, and the water-cooling crucible is arranged on the upper end surface of the water-cooling bracket; the heat treatment furnace comprises a control cabinet, a motor, a heat treatment furnace cavity, a heat preservation layer, a screw rod, an objective table, a liftable support, a resistance wire and a thermocouple, wherein the motor is arranged on the outer side wall of the furnace body, an output shaft of the motor is connected with a nut through a coupler, the nut is arranged on the screw rod which is vertically arranged, the heat treatment furnace cavity is connected with the nut, the heat treatment furnace cavity is driven by a nut screw pair formed by the nut and the screw rod to lift, the heat preservation layer is embedded in the heat treatment furnace cavity, the liftable support is arranged in the heat preservation layer, the objective table is arranged on the liftable support, the resistance wire and the thermocouple are all arranged on the inner side wall of the heat preservation layer, and the control cabinet is respectively electrically connected with the motor, the resistance wire and the thermocouple.
Further, the material turning transfer clamp is movably and hermetically inserted in the middle position of the upper part of the furnace body.
Further, a plurality of ingot casting grooves are formed in the upper end face of the water-cooled crucible.
Preferably, the ingot groove is circular in shape.
Further, the water cooling system comprises a water inlet and a water outlet which are respectively arranged at the lower part of the outer side wall of the furnace body.
Still further, it still includes admission valve and air outlet valve, and admission valve and air outlet valve are installed in the lateral wall lower part of furnace body respectively.
The invention also provides a preparation method of the heat treatment integrated furnace adopting the high-flux component of the high-activity titanium alloy, which comprises the following steps:
step one: preparing raw materials;
designing and preparing button ingots with the diameter of 30-60 mm by using high-flux components as raw materials;
step two: placing raw materials;
step two,: placing the prepared raw materials in an ingot casting groove of a water-cooled copper crucible in sequence, placing small particles in the raw materials at the lower part of the groove so as to prevent blowing off when smelting is started, and stacking large-scale titanium sponge on the small particles;
step two: after the raw materials are placed, the furnace door of the furnace body is closed, the furnace body is vacuumized to a vacuum state by a vacuumizing system, and the vacuum degree in the furnace is 3-8 multiplied by 10 -3 In Pa;
step two, three: argon is filled into the furnace body to-0.05 MPa;
smelting raw materials by adjusting the current of a non-consumable tungsten electrode in an argon environment, and turning over a smelted button ingot by using a turning transfer clamp after each smelting is completed for four times, so that the components are uniform;
step four: performing heat treatment;
after the button ingot is smelted, waiting for 30 minutes until the temperature in the furnace body is reduced in an argon environment, opening a heat treatment furnace door, transferring the button ingot in the same furnace body in the second step by means of a turning transfer clamp, placing the button ingot into the heat treatment furnace, closing a furnace door of the heat treatment furnace, and setting the heating rate, the heating temperature and the heat preservation time required by heat treatment to perform heat treatment;
step five: performing performance detection on the ingot after heat treatment;
the titanium alloy components (element types and contents), the heat treatment temperature (700-900 ℃) and the time (10 min-24 h) are systematically adjusted to meet the performance requirements (1300 MPa,50 MPa.m) of the ultra-high strength and toughness titanium alloy 1/2 ) The structure change is researched, and the change of the performance is analyzed, so that the optimal preparation process is obtained.
Further, the raw material component in the first step is titanium alloy, wherein the main alloy elements are Ti (70-80 wt.%), mo (2-7 wt.%), al (1-5 wt.%), zr (1-5 wt.%), nb (0-4 wt.%), cr (0-3 wt.%) and Fe (0-2 wt.%) and the ingredients are proportioned according to the selected alloy element proportion.
In the third step, the current is slowly increased when the first smelting is carried out, so that the influence of blowing off of small particles on the final result is avoided, and the mode of reducing 50A for 10s is adopted when the last smelting is carried out, so that the cooling speed is ensured to be consistent. The glass is observed at any time in the smelting process, and if the glass stops accidentally and timely.
In the fifth step, the measurement of the titanium alloy components after the heat treatment is performed by means of the self-contained energy spectrum software of a Merlin Compact scanning electron microscope.
Compared with the prior art, the invention has the following effects:
1. the invention designs a heat treatment integrated furnace with high flux component design, which can be transferred with the furnace to carry out solid solution aging heat treatment after smelting is completed in argon atmosphere, does not need to further open the furnace to contact with external air, can eliminate negative influence caused by external oxygen in the heat treatment process (brittle oxide is formed to deteriorate the toughness of the brittle oxide due to overhigh oxygen content), also avoids size limitation caused by vacuum tube sealing (limited by the size of a sealing tube), shortens the technological flow of transferring the furnace, re-filling argon or increasing the sealing tube, saves argon resources, reduces the technological cost, obtains titanium alloy mother ingots with low oxygen content, thereby ensuring the alloy toughness, and is particularly important, thereby preparing for obtaining high-toughness deformed ingots subsequently.
2. The invention combines the high flux component design with the heat treatment device to form a whole set of short-flow smelting and heat treatment device, reduces the technological flow, shortens the time of casting in the subsequent production process, has low energy and can improve the productivity.
3. According to the invention, alloy components are prepared by utilizing high-flux component design, 19 alloy ingots with different components can be obtained simultaneously by one-time smelting, the influence of external environment is eliminated by smelting in the same batch and the same atmosphere, a plurality of alloys with different components are prepared at one time, a large amount of relational data between the components and the performances are obtained in a short time, so that component screening is realized rapidly, the development period is short, and the alloy preparation efficiency is improved.
4. The device can directly perform heat treatment after smelting by utilizing the water-cooled copper crucible without opening the furnace again, thereby ensuring the recycling of argon, reducing the cost, saving energy and improving the production efficiency.
5. The device is carried out under the protection of argon atmosphere no matter in the smelting process or the heat treatment process of the alloy, so that the low oxygen content of the alloy material is ensured, the subsequent strength and toughness performance reduction caused by the overhigh oxygen content of the alloy is avoided, and the equipment can be reused.
Drawings
FIG. 1 is an overall schematic diagram of an integrated furnace for heat treatment of high-flux components of a high-activity titanium alloy of the present invention;
FIG. 2 is a partially enlarged view of a heat treatment furnace;
FIG. 3 is a top view of the water-cooled crucible 14;
FIG. 4 is the oxygen content of the titanium alloy prepared in scheme one and scheme two (apparatus of the present invention);
FIG. 5 is a diagram showing the elemental distribution of a titanium alloy prepared in accordance with scheme one;
FIG. 6 is a diagram showing the elemental distribution of a titanium alloy prepared in scheme II (apparatus of the present invention);
FIG. 7 is a comparison of tensile properties of titanium alloys prepared in accordance with scheme one and scheme two (apparatus of the present invention);
FIG. 8 is a comparison of fracture toughness properties of titanium alloys prepared according to scheme one and scheme two (apparatus of the present invention).
Detailed Description
The first embodiment is as follows: the embodiment is described with reference to fig. 1 to 3, and comprises a furnace body 11, a gas cylinder 15 and a vacuumizing system 7, wherein an observation window 8 is formed in the upper side end surface of the furnace body 11, the gas cylinder 15 and the vacuumizing system 7 are arranged outside the furnace body 11 and are communicated with the inside of the furnace body 11, the embodiment further comprises a water-cooling crucible assembly, an arc gun transmission mechanism 10, a non-consumable tungsten electrode 12, a water-cooling system, a turning transfer clamp 9 and a heat treatment furnace, the water-cooling crucible assembly and the heat treatment furnace are arranged in the furnace body 11, the turning transfer clamp 9 is movably and hermetically inserted in the furnace body 11, the water-cooling system is arranged at the lower part of the furnace body 11, the arc gun transmission mechanism 10 is vertically and hermetically inserted in the furnace body 11, the non-consumable tungsten electrode 12 is arranged at the lower end of the arc gun transmission mechanism 10, and the non-consumable tungsten electrode 12 is positioned right above the water-cooling crucible assembly; the water-cooling crucible assembly comprises a water-cooling crucible 14 and a water-cooling bracket 16, the water-cooling bracket 16 is vertically arranged in the furnace body 11, and the water-cooling crucible 14 is arranged on the upper end surface of the water-cooling bracket 16; the heat treatment furnace comprises a control cabinet 6, a motor 4, a heat treatment furnace cavity 3, a heat preservation 19, a screw rod 20, an objective table 21, a liftable support 24, a resistance wire 23 and a thermocouple 22, wherein the motor 4 is arranged on the outer side wall of the furnace body 11, an output shaft of the motor 4 is connected with a nut through a coupler and a transmission shaft, the nut is arranged on the screw rod 20 which is arranged vertically, the heat treatment furnace cavity 3 is connected with the nut, the heat treatment furnace cavity 3 is driven by a nut screw rod pair formed by the nut and the screw rod 20 to realize lifting, the heat preservation 19 is embedded in the heat treatment furnace cavity 3, the liftable support 24 is arranged in the heat preservation 19, the objective table 21 is arranged on the liftable support 24, and the resistance wire 23 and the thermocouple 22 are all arranged on the inner side wall of the heat preservation 19, and the control cabinet 6 is respectively electrically connected with the motor 4, the resistance wire 23 and the thermocouple 22.
The non-consumable tungsten electrode 12 in this embodiment is vertically inserted into the cavity of the furnace 11, and the height and angle of the non-consumable tungsten electrode 12 can be adjusted to be directly above the material.
The height and angle of the turning transfer clamp 9 in the furnace body 11 in the embodiment can be adjusted at will.
The resistance wire 23 in the embodiment is close to the inner side of the furnace body, so that the heating is convenient. The liftable support 24 is located below the stage 21 and its height is adjustable.
19 alloy ingots can be simultaneously smelted in one water-cooled copper crucible in the embodiment, so that a plurality of alloy ingots with different components are obtained under one-time smelting condition, and the high-flux design of the alloy components is realized.
The second embodiment is as follows: the description of the present embodiment is made with reference to fig. 1, in which the turning transfer clip 9 of the present embodiment is movably inserted in a middle position of an upper portion of the furnace body 11 in a sealed manner. So set up, be convenient for simultaneously operate water-cooled crucible subassembly and heat treatment furnace, if: turn over, flexible in use. Other compositions and connection relationships are the same as those of the first embodiment.
And a third specific embodiment: the present embodiment will be described with reference to fig. 3, in which a plurality of ingot grooves are formed in the upper end surface of the water-cooled crucible 14. By the arrangement, the titanium alloy with different components is conveniently cast, and high-flux component analysis is performed. Other compositions and connection relationships are the same as those of the first or second embodiment.
The specific embodiment IV is as follows: the ingot groove of the present embodiment is circular in shape, as described with reference to fig. 3. So set up, simple structure is convenient for fuse casting. Other compositions and connection relationships are the same as those of the first, second or third embodiments.
Fifth embodiment: the water cooling system of the present embodiment includes a water inlet 17 and a water outlet 18, which are respectively provided at the lower portion of the outer sidewall of the furnace body 11, as described with reference to fig. 1. So set up, be convenient for cool off the water-cooled crucible. Other compositions and connection relationships are the same as those of the first, second, third or fourth embodiments.
Specific embodiment six: the present embodiment will be described with reference to fig. 1, and further includes an intake valve 1 and an exhaust valve 2, and the intake valve 1 and the exhaust valve 2 are respectively mounted on the lower portion of the outer side wall of the furnace body 11. So arranged, accurate control of the gas introduced into the furnace body 11 is facilitated. Other compositions and connection relationships are the same as those of the first, second, third, fourth or fifth embodiments.
Seventh embodiment: the method for producing the high-activity titanium alloy of the present embodiment, which is described with reference to fig. 1 to 3, includes the steps of:
step one: preparing raw materials;
designing and preparing button ingots with the diameter of 30-60 mm by using high-flux components as raw materials;
step two: placing raw materials;
step two,: placing the prepared raw materials in the ingot casting groove of the water-cooled copper crucible 14 in sequence, placing small particles in the raw materials at the lower part of the groove so as to prevent the raw materials from being blown off when smelting is started, and stacking large blocks of titanium sponge on the small particles;
step two: after the raw materials are placed, the furnace door of the furnace body 11 is closed, the vacuum state is pumped into the furnace body 11 through the vacuum pumping system 7, and the vacuum degree in the furnace is 3-8 multiplied by 10 -3 In Pa;
step two, three: argon is filled into the furnace body 11 to-0.05 MPa, so that the oxygen content in the furnace body is reduced, and the oxidation of materials in the smelting process is prevented, so that the performance is influenced;
smelting raw materials by adjusting the current of a non-consumable tungsten electrode 12 in an argon environment, and smelting for four times, wherein after each smelting is finished, a smelted button ingot is turned over by using a turning transfer clamp 9, so that the components are uniform;
step four: performing heat treatment;
after button ingot smelting is completed, waiting for 30 minutes until the temperature in the furnace body is reduced in an argon environment, opening a heat treatment furnace door, transferring the button ingot in the same furnace body 11 in the second step by means of a turning transfer clamp 9, placing the button ingot into the heat treatment furnace, closing a furnace door of the heat treatment furnace, and setting a heating rate (5-10 ℃/min), a heating temperature (700-900 ℃) and a heat preservation time (10 min-24 h) required by heat treatment to perform heat treatment;
step five: performing performance detection on the ingot after heat treatment;
the titanium alloy components (element types and contents), the heat treatment temperature (700-900 ℃) and the time (10 min-24 h) are systematically adjusted to meet the performance requirements (1300 MPa,55 MPa.m) of the ultra-high strength and toughness titanium alloy 1/2 ) The optimal preparation process is obtained, the basis is used for the subsequent deformation rolling of the wire rod, the plate and the like, and the structure is further applied to an aerospace system.
Other compositions and connection relationships are the same as those of the first, second, third, fourth, fifth or sixth embodiments.
Eighth embodiment: the present embodiment will be described with reference to fig. 1 to 3, in which the raw material composition in step one of the present embodiment is a titanium alloy in which the main alloying elements are Ti (70 to 80 wt.%) Mo (2 to 7 wt.%) Al (1 to 5 wt.%) Zr (1 to 5 wt.%) Nb (0 to 4 wt.%) Cr (0 to 3 wt.%) and Fe (0 to 2 wt.%) and the ingredients are dosed in accordance with the selected alloying element proportions. By the arrangement, the Ti-Mo-Al-Zr-Nb-Cr-Fe alloy system contains various beta stabilizing elements, has stronger solid solution strengthening capability, does not contain or contains a small amount of V, fe element which is easy to segregate, and is easy to obtain excellent strength and toughness matching. Other compositions and connection relationships are the same as those in any one of the first to seventh embodiments.
The alloy composition of the embodiment is a Ti-Mo-Al-Zr-Nb-Cr-Fe system, the beta stabilizing element has a plurality of types, has excellent solid solution strengthening effect, is not added with element (V) like easy segregation, and most of the ultra-high strength and toughness alloy systems at present contain V, and the Fe element is easy to segregate, but the Fe element only contains 1 percent. And also contains no higher elements. That is, the alloy of the present invention has a high content of β -stable elements, and therefore, the alloy has a high solid solution strengthening effect, is not likely to segregate, and has the potential to obtain ultra-high strength and toughness.
The alloy system belongs to a near beta-type titanium alloy system, the content of beta-stable elements in the alloy is higher, wherein Mo and Nb are beta-isomorphous elements, the lattice type of the Mo and Nb is the same as that of Ti, the Mo and Nb can be infinitely dissolved in beta phase to stabilize beta phase, and the generated lattice distortion is small due to small difference between the Mo and Nb and the radius of Ti atoms, so that the strength is improved, and meanwhile, the toughness is reduced. Cr and Fe belong to beta eutectoid elements, and the stability of beta phase can be maintained after alloy quenching. In addition, the alloy also contains a small amount of alpha stabilizing element (Al) and neutral element (Zr), so that the beta-phase content in the equilibrium state tissue exceeds 50%, and the alloy has stronger toughness matching.
In addition, the O element belongs to an impurity element in the titanium alloy, although researches show that a small amount of oxygen can improve the toughness of the alloy, the O element is a harmful element in most cases, tiO is easily formed by combining with Ti, the plasticity, the fracture toughness and the like are seriously reduced, so that the content of the oxygen element in the alloy is reduced in the preparation process of the alloy.
Detailed description nine: in the third step of the present embodiment, referring to fig. 1 to 3, the current is slowly increased during the first smelting to prevent the particles of the small block from being blown off and affecting the final result, and the cooling rate is ensured to be uniform by reducing the current by 50A for 10s during the last smelting. The glass is observed at any time in the smelting process, and if the glass stops accidentally and timely. By the arrangement, the accuracy of components is guaranteed, the difference caused by different cooling speeds is prevented, and meanwhile, furnace body damage caused by improper operation is avoided. Other compositions and connection relationships are the same as those in any one of the first to seventh embodiments.
Detailed description ten: in the fifth step of the present embodiment, measurement of the titanium alloy component after the heat treatment is performed by means of the spectral software of the Merlin Compact scanning electron microscope, which is described with reference to fig. 1 to 3. Through component measurement, it is confirmed that the device can obtain a plurality of ingots with different alloy components under one-time smelting condition, so that high-flux preparation of the alloy is realized. In addition, the component tests show that the oxygen content of the prepared alloy is lower than 300ppm, and the prepared alloy belongs to the low oxygen content range.
Examples:
embodiments of the present invention are illustrated in accordance with the heat treatment integrated furnace schematic diagrams of the high-flux components of the high-activity titanium alloy of fig. 1, 2 and 3.
Before the start of the experiment, the ingredients were dosed according to the following alloy composition: ti (81 wt.%), mo (6 wt.%), al (4 wt.%), zr (4 wt.%), nb (3 wt.%) and Cr (2 wt.%).
Table 1 shows nominal and actual compositions of the high-flux titanium alloys prepared by the apparatus.
Scheme one: the prepared alloy is placed in a water-cooled copper crucible 14, a furnace door is closed, and argon is introduced after the vacuum pumping system 7 is used for vacuumizing, so that smelting is performed. And after smelting, taking out the cast ingot, and putting the cast ingot into a heat treatment furnace for heat treatment to obtain a final cast ingot.
Scheme II: the prepared alloy is placed in a water-cooled copper crucible 14, a furnace door is closed, and argon is introduced after the vacuum pumping system 7 is used for vacuumizing, so that smelting is performed. After smelting, the ingot is moved into a heat treatment furnace by using a turning transfer clamp 9, a furnace door is closed, a program is set by a control cabinet 6, and heat treatment is carried out, so that a final ingot is obtained.
The ingots obtained in the first and second schemes were subjected to oxygen content measurement and comparison by using the self-contained energy spectrum software of the Merlin Compact scanning electron microscope, and the experimental results are shown in FIG. 4. According to the results of fig. 4, it can be seen that the oxygen content of the alloy ingot prepared by the device is less than 300ppm, which is obviously lower than that of the alloy ingot prepared by taking out the alloy ingot subjected to heat treatment in air after smelting, which indicates that the oxygen content in the alloy ingot prepared by the device is lower, thereby avoiding the formation of oxides such as TiO and the like and being beneficial to improving the toughness of the alloy.
The elemental distribution analysis is carried out on the cast ingots prepared in the first scheme and the second scheme by utilizing the self-contained energy spectrum analysis of a transmission electron microscope, and the experimental results are shown in fig. 5 and 6 respectively. The experimental results also show that compared with the alloy ingot prepared by the device provided by the invention, the alloy ingot has lower oxygen content (the oxygen content is less, and the oxygen is not detected when the detection is carried out, so the element distribution of the oxygen-free element in the element distribution diagram of fig. 6).
The alloy ingots prepared in the first and second modes were subjected to tensile and fracture toughness tests by using an electronic universal tester, and the results are shown in fig. 7 and 8. The result shows that the tensile strength and the fracture toughness of the alloy cast ingot prepared by the device are higher, the tensile strength is improved from 898 to 1321MPa, the fracture toughness is improved from 47 to 76MPa, the toughness is improved, the performance index requirements of the ultra-high strength and toughness titanium alloy are met, and the low-oxygen-content alloy cast ingot prepared by the device is favorable for improving the alloy toughness.
The preparation of high flux components can be realized by proportioning alloy cast ingots with different components to prevent the alloy cast ingots from being in the groove. In order to obtain the desired components as accurately as possible, the burn rate of the elements should be taken into account when dosing. The effect of the high flux component design is mainly to quickly screen out alloy components with optimal performance, and the influence of external environment is eliminated by smelting in the same atmosphere and batch.
The invention is kept under argon atmosphere during smelting and heat treatment, and is directly transferred with the furnace after smelting, thereby ensuring that oxygen is not contacted during the transfer process.
While the invention has been described with reference to the preferred embodiments, it is not intended to limit the invention, but rather to cover various modifications which may be made by those skilled in the art without departing from the spirit of the invention.
Claims (10)
1. The utility model provides a integrative stove of thermal treatment of high activity titanium alloy high flux composition, it includes furnace body (11), gas cylinder (15) and evacuating system (7), has seted up observation window (8) on furnace body (11) upper portion side terminal surface, and gas cylinder (15) and evacuating system (7) are installed in the outside of furnace body (11) and are communicate its characterized in that with the inside of furnace body (11): it also comprises a water-cooling crucible assembly, an electric arc gun transmission mechanism (10), a non-consumable tungsten electrode (12), a water-cooling system, a turning transfer clamp (9) and a heat treatment furnace,
the water-cooling crucible assembly and the heat treatment furnace are arranged in the furnace body (11), the turning transfer clamp (9) is movably and hermetically inserted in the furnace body (11), the water-cooling system is arranged at the lower part of the furnace body (11), the electric arc gun transmission mechanism (10) is vertically and hermetically inserted in the furnace body (11), the non-consumable tungsten electrode (12) is arranged at the lower end of the electric arc gun transmission mechanism (10), and the non-consumable tungsten electrode (12) is positioned right above the water-cooling crucible assembly;
the water-cooling crucible assembly comprises a water-cooling crucible (14) and a water-cooling bracket (16), the water-cooling bracket (16) is vertically arranged in the furnace body (11), and the water-cooling crucible (14) is arranged on the upper end surface of the water-cooling bracket (16);
the heat treatment furnace comprises a control cabinet (6), a motor (4), a heat treatment furnace cavity (3), a heat insulation layer (19), a screw rod (20), an objective table (21), a liftable bracket (24), a resistance wire (23) and a thermocouple (22),
the motor (4) is installed on the lateral wall of furnace body (11), the output shaft of motor (4) passes through shaft coupling and transmission shaft and nut connection, the nut is installed on lead screw (20) of vertical arrangement, heat treatment furnace cavity (3) are connected with the nut, and heat treatment furnace cavity (3) are realized going up and down under the drive of the nut screw pair that nut and lead screw (20) formed, heat preservation (19) are embedded in heat treatment furnace cavity (3), liftable support (24) are installed in heat preservation (19), objective table (21) are installed on liftable support (24), resistance wire (23) and thermocouple (22) are all installed on the inside wall of heat preservation (19), switch board (6) respectively with motor (4), resistance wire (23) and thermocouple (22) electric connection.
2. The integrated furnace for heat treatment of high-flux components of high-activity titanium alloy according to claim 1, wherein: the material turning transfer clamp (9) is movably and hermetically inserted in the middle position of the upper part of the furnace body (11).
3. The integrated furnace for heat treatment of high-flux components of high-activity titanium alloy according to claim 2, characterized in that: a plurality of ingot casting grooves are arranged on the upper end surface of the water-cooled crucible (14).
4. A high-activity titanium alloy high-flux component heat treatment integrated furnace as claimed in claim 3, wherein: the shape of the ingot casting groove is round.
5. The integrated furnace for heat treatment of high-flux components of high-activity titanium alloy according to claim 4, wherein: the water cooling system comprises a water inlet (17) and a water outlet (18), and the water inlet (17) and the water outlet (18) are respectively arranged at the lower part of the outer side wall of the furnace body (11).
6. The integrated furnace for heat treatment of high-flux components of high-activity titanium alloy according to claim 5, wherein: the furnace also comprises an air inlet valve (1) and an air outlet valve (2), wherein the air inlet valve (1) and the air outlet valve (2) are respectively arranged at the lower part of the outer side wall of the furnace body (11).
7. A method for producing a high-activity titanium alloy using the high-flux component heat treatment integrated furnace for a high-activity titanium alloy according to any one of claims 1 to 6, characterized by: it comprises the following steps:
step one: preparing raw materials;
designing and preparing button ingots with the diameter of 30-60 mm by using high-flux components as raw materials;
step two: placing raw materials;
step two,: placing the prepared raw materials in an ingot casting groove of a water-cooled copper crucible (14) in sequence, placing small particles in the raw materials at the lower part of the groove so as to prevent the raw materials from being blown off when smelting is started, and stacking large-scale titanium sponge on the small particles;
step two: after the raw materials are placed, the furnace door of the furnace body (11) is closed, the vacuum state in the furnace body (11) is pumped to be in a vacuum state through the vacuum pumping system (7), and the vacuum degree in the furnace is 3-8 multiplied by 10 -3 In Pa;
step two, three: argon is filled into the furnace body (11) to be minus 0.05MPa;
step three: smelting raw materials;
smelting raw materials by adjusting the current of a non-consumable tungsten electrode (12) in an argon environment, wherein smelting is performed four times, and after each smelting is completed, a smelted button ingot is turned over by using a turning transfer clamp (9), so that the components are uniform;
step four: performing heat treatment;
after the button ingot is smelted, waiting for 30 minutes until the temperature in the furnace body is reduced in an argon environment, opening a heat treatment furnace door, transferring the button ingot in the same furnace body (11) in the second step by means of a turning transfer clamp (9), placing the button ingot into the heat treatment furnace, closing a furnace door of the heat treatment furnace, and setting the heating rate, the heating temperature and the heat preservation time required by heat treatment to perform heat treatment;
step five: performing performance detection on the ingot after heat treatment;
by systematically adjusting the components, the heat treatment temperature and the time of the titanium alloy, the titanium alloy meets the performance requirement of the ultra-high strength and toughness titanium alloy, and the structural change is researched, so that the change of the performance is analyzed, and the optimal preparation process is obtained.
8. The method for producing a high-activity titanium alloy according to claim 7, wherein: the raw material components in the first step are titanium alloy, wherein the main alloy elements are Ti (70-80 wt.%), mo (2-7 wt.%), al (1-5 wt.%), zr (1-5 wt.%), nb (0-4 wt.%), cr (0-3 wt.%) and Fe (0-2 wt.%) and the ingredients are proportioned according to the selected alloy element proportion.
9. The method for producing a high-activity titanium alloy according to claim 8, wherein: in the third step, the current is slowly increased when the first smelting is carried out, so that the influence of blowing off of small particles on the final result is prevented, and the mode of reducing 50A for 10s is adopted when the last smelting is carried out, so that the cooling speed is ensured to be consistent.
10. The method for producing a high-activity titanium alloy according to claim 9, wherein: and fifthly, measuring the titanium alloy components after heat treatment by means of self-contained energy spectrum software of a scanning electron microscope.
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