CN113322388A - Preparation method of high-Mo titanium alloy ingot - Google Patents
Preparation method of high-Mo titanium alloy ingot Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21J—FORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
- B21J5/00—Methods for forging, hammering, or pressing; Special equipment or accessories therefor
- B21J5/002—Hybrid process, e.g. forging following casting
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- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/17—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by forging
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- B22—CASTING; POWDER METALLURGY
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Abstract
A preparation method of a high Mo titanium alloy ingot comprises the following steps: mixing Mo powder and Ti powder in proportion, molding, vacuum sintering and fine forging to obtain a Ti-Mo intermediate alloy core rod; assembling and welding a Ti-Mo intermediate alloy core rod and a prepared electrode block to form a consumable electrode; the content of each component of the consumable electrode is consistent with that of each component of the titanium alloy to be prepared; mo element in the consumable electrode is introduced by a Ti-Mo intermediate alloy core rod; the Ti element part and other elements are all introduced from the electrode block; and carrying out vacuum consumable arc melting on the consumable electrode to obtain the high-Mo titanium alloy ingot with the Mo element content of 10-40%. The titanium alloy ingot has no Mo infusible block, and the components meet the national standard requirements.
Description
Technical Field
The invention belongs to the technical field of nonferrous metal processing, and particularly relates to a preparation method of a high-Mo titanium alloy ingot with Mo content of 10-40% by mass.
Background
The titanium alloy has excellent specific strength, specific rigidity, corrosion resistance and other properties, and is widely applied to the fields of aerospace and biomedical science. Wherein, a part of titanium alloys such as Ti15Mo, TB3, TB7, TB8 and the like are added with more high-melting-point element Mo. The melting point of Ti element is 1668 ℃, and the density is 4.5g/cm3The melting point of Mo element is 2617 deg.C, the density is 10.28g/cm3The difference of melting points and densities of the two elements is great, and the alloying and homogenization control difficulty of the Mo element is great. The improper adding mode and the improper smelting process of the Mo element can cause Mo-rich areas in the ingot to form Mo-poor blocks, and the application and popularization of the alloy are always restricted by the problem.
Disclosure of Invention
The invention aims to provide an adding mode for introducing Mo element by an alloy mode, and a high Mo titanium alloy ingot with the diameter of 440-640 mm, no high-density inclusion and meeting the national standard requirement can be obtained by a reasonable smelting process.
In order to achieve the purpose, the technical scheme adopted by the invention is a preparation method of a high Mo titanium alloy ingot, which comprises the following steps:
preparing a Ti-Mo intermediate alloy core rod: mixing Mo powder and Ti powder in proportion, molding, vacuum sintering and fine forging to obtain a Ti-Mo intermediate alloy core rod;
preparing a Mo-free electrode block: preparing a corresponding electrode block without Mo element according to the content of each component of the prepared titanium alloy containing Mo element;
preparing a consumable electrode: assembling and welding the electrode block without Mo element and the prepared Ti-Mo intermediate alloy core rod to form a consumable electrode, wherein the content of each element component in the consumable electrode is consistent with that of the titanium alloy corresponding to the electrode block without Mo element; in the consumable electrode, Mo element is introduced by a Ti-Mo intermediate alloy core rod, Ti element is introduced by an electrode block and the Ti-Mo intermediate alloy core rod together, and other elements are introduced by the electrode block;
vacuum consumable arc melting: and carrying out vacuum consumable arc melting on the prepared consumable electrode to obtain a high-Mo titanium alloy ingot with the Mo content of 10-40% by mass percent.
Preferably, in the step of preparing the Ti-Mo intermediate alloy core rod, the ratio of Mo powder to Ti powder is 3: 7-4: 6 by mass ratio.
Preferably, in the step of preparing the Ti-Mo master alloy core rod, the sintered blank is heated and then subjected to finish forging; the single-pass deformation is not more than 15mm, and the single-pass forging is carried out for 2-5 passes; and (3) machining the forged bar, and then requiring 100% of light to obtain the Ti-Mo intermediate alloy core rod.
Preferably, the heating temperature before finish forging is 500 ℃ to 1200 ℃.
Preferably, the asbestos is wrapped in the forging process for slow cooling.
Preferably, in the step of preparing the Mo-free electrode block, when the electrode block is prepared, Ti element is mainly introduced by sponge titanium, and other elements are introduced by binary alloy; when a certain element is introduced from a binary alloy and cannot meet the matching amount, the deficiency is introduced from the simple substance metal of the element.
Preferably, in the step of preparing the consumable electrode, the consumable electrode has a structure that the Ti-Mo intermediate alloy core rod is centered, and the electrode block wraps the outer peripheral surface of the Ti-Mo intermediate alloy core rod.
Preferably, in the vacuum consumable arc melting step, the vacuum consumable arc melting parameters are: controlling the leakage rate to be below 1.2Pa/min, controlling the vacuum degree to be below 5.0Pa, controlling the smelting current to be 6-40 kA, controlling the smelting voltage to be 25-45V, controlling the cooling time to be not less than 6 hours after smelting, entering a feeding stage at the later stage of smelting, reducing the smelting current step by step, and finally ensuring that the molten powder is completely reserved.
Preferably, the vacuum consumable arc melting is carried out three times: the first time and the second time of vacuum consumable arc melting respectively adopt crucibles with the diameters of 360 mm-440 mm and 440 mm-560 mm, the leakage rate is controlled to be below 1.2Pa/min, the vacuum degree is controlled to be below 20.0Pa, the melting current is controlled to be 6-40 kA, the melting voltage is controlled to be 25-40V, and the cooling time after melting is not less than 6.0 hours;
and a crucible with the diameter of 520-640 mm is adopted for the third vacuum consumable arc melting, the leakage rate is controlled to be below 0.8Pa/min, the vacuum degree is controlled to be below 5.0Pa, the melting current is 6-40 kA, the melting voltage is 25-45V, feeding is carried out when the consumable electrode melting residual mass is 100-1000 kg, the melting current is reduced step by step, the complete reservation of the molten tail is finally ensured, and the cooling time after melting is not less than 6.0 hours.
The invention also provides a preparation method of the Ti-Mo titanium alloy ingot, which comprises the following steps:
preparing a consumable electrode: mixing Mo powder and Ti powder according to the proportion of the components of the titanium-molybdenum-titanium alloy, uniformly mixing, forming, vacuum sintering and precisely forging to obtain a Ti-Mo consumable electrode;
and (3) carrying out vacuum consumable arc melting on the Ti-Mo consumable electrode obtained in the step to obtain a titanium alloy ingot with the Mo content of 10-40% by mass.
When preparing a TB7 titanium alloy ingot, the Ti-Mo intermediate alloy core rod can be used as a consumable electrode to carry out vacuum consumable arc melting.
The invention has the beneficial effects that: mixing, pressing and sintering Ti powder and Mo powder to obtain a Ti-Mo intermediate alloy blank with a lower melting point and high uniformity, wherein the Mo content of the Ti-Mo intermediate alloy is 30-40% by mass; the blank is forged and machined to prepare the Ti-Mo intermediate alloy core rod. In the consumable electrode, Mo element is introduced through a Ti-Mo intermediate alloy core rod, other components are also introduced through an intermediate alloy mode during the preparation of an electrode block, and a high-Mo titanium alloy ingot with the Mo content of 10-40% by mass is prepared through an intermediate alloy introduction mode and vacuum consumable arc melting; the problem that the risk of Mo clinker is high when the existing high-Mo titanium alloy ingot is produced is solved, and the high-Mo titanium alloy ingot which is free of Mo clinker impurities and has the components meeting the national standard requirements is obtained.
Detailed Description
The preparation method of the high-Mo titanium alloy ingot specifically comprises the following steps:
preparing a Ti-Mo intermediate alloy core rod: the method comprises the following steps of mixing Mo powder and Ti powder in a mass ratio of 3: 7-4: 6, uniformly mixing, forming, vacuum sintering, and performing precision forging to obtain a Ti-Mo intermediate alloy core rod, wherein the precision forging process comprises the following steps: the heating temperature before finish forging is 500-1200 ℃, the single-pass deformation is not more than 15mm, and the single-fire forging is carried out for 2-5 passes; after machining, the forged bar requires 100% of light;
preparing a Mo-free electrode block: preparing a corresponding electrode block without Mo element according to the content of each component of the prepared titanium alloy containing Mo element; when the electrode block is prepared, Ti element is mainly introduced by sponge titanium, and other elements are introduced by binary alloy; when a certain element is introduced from a binary alloy and cannot meet the matching amount, the deficiency is introduced from the simple substance metal of the element.
Preparing a consumable electrode: assembling and welding the electrode block without Mo element and the prepared Ti-Mo intermediate alloy core rod to form a consumable electrode, wherein the content of each element component in the consumable electrode is consistent with that of the titanium alloy corresponding to the electrode block without Mo element; in the consumable electrode, Mo element is introduced by a Ti-Mo intermediate alloy core rod, Ti element is introduced by an electrode block and the Ti-Mo intermediate alloy core rod together, and other elements are introduced by the electrode block.
When the titanium alloy needing to be prepared only contains two elements of titanium and molybdenum, the prepared Ti-Mo intermediate alloy core rod can be directly used as a consumable electrode to carry out vacuum consumable arc melting to prepare the Mo-containing titanium alloy.
Vacuum consumable arc melting: and carrying out vacuum consumable arc melting on the prepared consumable electrode to obtain a high-Mo titanium alloy ingot with the Mo content of 10-40% by mass percent.
The first time and the second time of vacuum arc furnace smelting respectively adopt crucibles with the diameters of 360 mm-440 mm and 440 mm-560 mm, the leakage rate is controlled to be below 1.2Pa/min, the vacuum degree is controlled to be below 20.0Pa, the smelting current is controlled to be 6-40 kA, the smelting voltage is controlled to be 25-40V, and the cooling time after smelting is not less than 6.0 hours;
and a crucible with the diameter of 520-640 mm is adopted for the third vacuum arc furnace smelting, the leakage rate is controlled to be below 0.8Pa/min, the vacuum degree is controlled to be below 5.0Pa, the smelting current is 6-40 kA, the smelting voltage is 25-45V, feeding is carried out when the consumable electrode smelting residual mass is 100-1000 kg, the smelting current is reduced step by step, the complete reservation of the molten tail is finally ensured, and the cooling time after smelting is not less than 6.0 hours.
The binary alloy, such as AlV alloy, AlFe alloy, NbTi alloy, TiSi alloy and the like, related to the invention are all the alloys existing in the market, and can be purchased in the market or prepared by the existing alloy technology.
The Chinese names corresponding to the elements related by the invention are as follows: ti (titanium), Mo (molybdenum), Al (aluminum), V (vanadium), Nb (niobium), Si (silicon), O (oxygen).
The above technical solutions are specifically described by way of example.
Example 1
Preparing a Ti-Mo intermediate alloy core rod:
step 1: mixing Mo powder which meets the national standard and contains 0.095% of O element by mass and Ti powder which contains 0.19% of O element by mass according to the mass ratio of 3:7, and uniformly mixing by using a mixer; pressing the mixed powder into a blank by using a cold isostatic press, wherein the pressing pressure is 125MPa, and the pressure maintaining time is 7 min.
Step 2: and (3) sintering the blank obtained in the step (1) by using a vacuum sintering furnace, wherein the sintering temperature is 1150 ℃, and the heat preservation time is 14 h.
And step 3: and (3) forging the sintered blank obtained in the step (2) by using a precision forging machine. The heating temperature before finish forging is 1100 ℃, the asbestos is wrapped in the forging process for slow cooling, the single-pass deformation is 3%, and the single-fire forging is carried out for 5 passes; then forging to the required specification according to the mode; and (3) carrying out mechanical processing such as peeling and head cutting on the forged bar, and then requiring 100% light to obtain the Ti-Mo intermediate alloy core rod with the diameter of 85 mm.
Preparing a Mo-free electrode block:
and 4, step 4: adopting HTi particles, AlV alloy particles, AlFe alloy particles and simple substance Al particles which are in national standard, preparing the components of an electrode block according to the mass ratio of Ti-3.5Al-10Mo-8V-1Fe of TB3 titanium alloy, the specification of a consumable electrode and the specification of a Ti-Mo intermediate alloy core rod which needs 85mm, mixing the materials and pressing to prepare the electrode block; the pressing strength of the electrode block is 22MPa, the pressed electrode block is in an annular semicircular shape, and the diameter of the semicircular shape on the inner side of the electrode block is 85mm consistent with the outer diameter of the Ti-Mo intermediate alloy core rod machined in the step 3;
when the components of the electrode block are proportioned, the mass of each component of the consumable electrode is calculated according to the mass of the consumable electrode and the mass ratio of each component of the titanium alloy mark; calculating the length of the needed Ti-Mo intermediate alloy core rod according to the mass of the Mo element; then subtracting the mass of the Mo element according to the mass of the Ti-Mo intermediate alloy core rod to obtain the mass of the Ti element of the Ti-Mo intermediate alloy core rod; the mass of the Ti element of the Ti-Mo intermediate alloy core rod is subtracted according to the mass of the Ti component of the consumable electrode, and the mass is the mass of the titanium sponge particles required in the electrode block; and calculating the mass of the alloy to be introduced and the mass of the simple substance Al according to the mass of the components of Al, V and Fe, and batching the electrode block.
Preparing a consumable electrode:
and 5: placing the Ti-Mo intermediate alloy core rod in the step 3 in the middle, placing an electrode block on the outer peripheral side of the Ti-Mo intermediate alloy core rod, and welding the assembled electrode block into a consumable electrode for smelting in a non-tungsten electrode plasma welding box protected by argon; the mass ratio of each component in the consumable electrode is consistent with that of Ti-3.5Al-10Mo-8V-1Fe, in the consumable electrode, Mo component is introduced by a Ti-Mo intermediate alloy core rod, V element and Fe element are introduced by intermediate alloy, Al element is introduced by intermediate alloy and simple substance Al, one part of Ti element is introduced by the Ti-Mo intermediate alloy core rod, and the other part of Ti element is introduced by sponge titanium.
Vacuum consumable arc melting:
step 6: carrying out three times of vacuum arc melting on the consumable electrode obtained in the step 4, and specifically:
the first time and the second time of vacuum arc furnace smelting respectively adopt crucibles with the diameters of 280mm and 360mm, and in the smelting process, the leakage rate is 0.95Pa/min, the vacuum degree is 18Pa, the smelting current is 6.5kA, the smelting voltage is 26V, and the cooling time after smelting is 3.5 hours;
the third vacuum arc furnace smelting adopts a crucible with the diameter of 440mm, in the smelting process, the leakage rate is 0.78Pa/min, the vacuum degree is 4.7Pa, the smelting current is 7.5kA, the smelting voltage is 26.5V, feeding is started when 200kg of the consumable electrode smelting residual mass is carried out, the current reduction rate is gradually reduced, and the cooling time after smelting is 6.5 hours.
The TB3 titanium alloy ingot obtained after the smelting is finished has no clinker, and the content of each element is calculated by mass ratio: the Al content is 3.2%, the Mo content is 10.4%, the V content is 7.9%, the Fe content is 1.1%, and the chemical components meet the national standard requirements.
Example 2
Preparing a Ti-Mo intermediate alloy core rod:
step 1: mixing Mo powder which meets the national standard and contains 0.06 percent of O element by mass and Ti powder which contains 0.14 percent of O element by mass according to the mass ratio of 3.5:6.5, and uniformly mixing by using a mixer; pressing the mixed powder into a blank by using a cold isostatic press, wherein the pressing pressure is 160MPa, and the pressure maintaining time is 12 min.
Step 2: and (3) sintering the blank obtained in the step (1) by using a vacuum sintering furnace, wherein the sintering temperature is 1250 ℃, and the heat preservation time is 10 hours.
And step 3: and (3) forging the sintered blank obtained in the step (2) by using a precision forging machine. The heating temperature before finish forging is 900 ℃, the asbestos is wrapped in the forging process for slow cooling, the single-pass deformation is 6%, and the single-fire forging is carried out for 3 passes; then forging to the required specification according to the mode; and (3) machining the forged bar, and then requiring 100% of light to obtain the Ti-Mo intermediate alloy core rod with the diameter of 130 mm.
Preparing a Mo-free electrode block:
and 4, step 4: adopting sponge titanium HTi, NbTi scraps, TiSi particles and simple substance Al which are in national standard, preparing electrode blocks according to the mass ratio of Ti-3.0Al-15Mo-3.0Nb-0.2Si, the specification of a consumable electrode and the specification of a Ti-Mo intermediate alloy core rod of TB8 titanium alloy, mixing the materials, and pressing to form the electrode blocks; the pressing strength of the electrode block is 35MPa, the pressed electrode block is in an annular semicircular shape, and the diameter of the semicircular shape on the inner side of the electrode block is 130mm consistent with the outer diameter of the Ti-Mo intermediate alloy core rod machined in the step 3;
when the components of the electrode block are proportioned, the mass of each component of the consumable electrode is calculated according to the mass of the consumable electrode and the mass ratio of each component of the titanium alloy mark; calculating the length of the needed Ti-Mo intermediate alloy core rod according to the mass of the Mo element; then subtracting the mass of the Mo element according to the mass of the Ti-Mo intermediate alloy core rod to obtain the mass of the Ti element of the Ti-Mo intermediate alloy core rod; the mass of the Ti element of the Ti-Mo intermediate alloy core rod is subtracted according to the mass of the Ti component of the consumable electrode, and the mass is the mass of the titanium sponge particles required in the electrode block; and then calculating the mass of the alloy to be introduced and the mass of the simple substance Al according to the mass of the required components of Al, Nb and Si, and batching the electrode block.
Preparing a consumable electrode:
and 5: placing the Ti-Mo intermediate alloy core rod in the step 3 in the middle, placing an electrode block on the outer peripheral side of the Ti-Mo intermediate alloy core rod, and welding the assembled electrode block into a consumable electrode for smelting in a non-tungsten electrode plasma welding box protected by argon;
the mass ratio of each component in the consumable electrode is consistent with that of Ti-3.0Al-15Mo-3.0Nb-0.2Si, in the consumable electrode, the Mo component is introduced by a Ti-Mo intermediate alloy core rod, the Nb element and the Si element are introduced by an intermediate alloy, the Al element is introduced by simple substance Al, one part of the Ti element is introduced by the Ti-Mo intermediate alloy core rod, one part of the Ti element is introduced by the intermediate alloy, and one part of the Ti element is introduced by the titanium sponge.
Vacuum consumable arc melting:
step 6: carrying out three times of vacuum arc melting on the consumable electrode obtained in the step 4, and specifically:
the first time and the second time of vacuum arc furnace smelting respectively adopt crucibles with the diameters of 360mm and 440mm, and in the smelting process, the leakage rate is 0.75Pa/min, the vacuum degree is 10Pa, the smelting current is 12kA, the smelting voltage is 32V, and the cooling time after smelting is 5 hours;
the third vacuum arc furnace smelting adopts a crucible with the diameter of 520mm, in the smelting process, the leakage rate is 0.50Pa/min, the vacuum degree is 2.2Pa, the smelting current is 18kA, the smelting voltage is 34V, feeding is started when the consumable electrode smelting residual mass is 600kg, the current reduction rate is gradually reduced, and the cooling time after smelting is 8.0 hours.
The TB8 titanium alloy ingot prepared in example 2 has no clinker, the Al content is 2.9, the Mo content is 15.1, the Nb content is 3.0, the Si content is 0.18, and the chemical composition meets the national standard requirement.
Example 3
Preparing a Ti-Mo intermediate alloy core rod:
step 1: mixing Mo powder which meets the national standard and contains 0.04 percent of O element by mass and Ti powder which contains 0.16 percent of O element by mass according to the mass ratio of 4:6, and uniformly mixing by using a mixer; pressing the uniformly mixed powder into a blank by using a cold isostatic press, wherein the pressing pressure is 190MPa, and the pressure maintaining time is 18 min.
Step 2: and (3) sintering the blank obtained in the step (1) by using a vacuum sintering furnace, wherein the sintering temperature is 1450 ℃, and the heat preservation time is 5 h.
And step 3: and (3) forging the sintered blank obtained in the step (2) by using a precision forging machine. The heating temperature before finish forging is 600 ℃, asbestos is wrapped in the forging process for slow cooling, the single-pass deformation is 9%, and the single-fire forging is carried out for 2 passes; then forging to the required specification according to the mode; after the forged bar is machined, 100% of light is required, and the Ti-Mo intermediate alloy core rod with the diameter of 190mm is obtained.
Preparing a Mo-free electrode block:
and 4, step 4: adopting national standard HTi, carrying out electrode block titanium sponge proportioning according to the mass ratio of Ti to 15Mo of the TB11 titanium alloy, the specification of a consumable electrode and the specification of a required Ti-Mo intermediate alloy core rod, and pressing the weighed titanium sponge particles to form an electrode block; the pressing strength of the electrode block is 45MPa, the pressed electrode block is in an annular semicircular shape, and the diameter of the semicircular shape on the inner side of the electrode block is 190mm consistent with the outer diameter of the Ti-Mo intermediate alloy core rod machined in the step 3;
when the components of the electrode block are proportioned, the mass of each component of the consumable electrode is calculated according to the mass of the consumable electrode and the mass ratio of each component of the titanium alloy mark; calculating the length of the needed Ti-Mo intermediate alloy core rod according to the mass of the Mo element; then subtracting the mass of the Mo element according to the mass of the Ti-Mo intermediate alloy core rod to obtain the mass of the Ti element of the Ti-Mo intermediate alloy core rod; the mass of the Ti element of the Ti-Mo intermediate alloy core rod is subtracted according to the mass of the Ti component of the consumable electrode, and the mass is the mass of the titanium sponge particles required in the electrode block; and then batching the titanium sponge electrode block according to the mass of the required titanium sponge particles.
Preparing a consumable electrode:
and 5: placing the Ti-Mo intermediate alloy core rod in the step 3 in the middle, placing a titanium sponge electrode block on the outer peripheral side of the Ti-Mo intermediate alloy core rod, and welding the assembled titanium sponge electrode block into a consumable electrode for smelting in a non-tungsten electrode plasma welding box under the protection of argon;
the mass ratio of each component in the consumable electrode is consistent with that of Ti-15Mo, in the consumable electrode, the Mo component is introduced by a Ti-Mo intermediate alloy core rod, one part of Ti element is introduced by the Ti-Mo intermediate alloy core rod, and the other part of Ti element is introduced by an electrode block.
Vacuum consumable arc melting:
step 6: carrying out three times of vacuum arc melting on the consumable electrode obtained in the step 4, and specifically:
the first time and the second time of vacuum arc furnace smelting respectively adopt crucibles with the diameter of 440mm and 560mm, and in the smelting process, the leakage rate is 0.80Pa/min, the vacuum degree is 8Pa, the smelting current is 18kA, the smelting voltage is 38V, and the cooling time after smelting is 6 hours;
the third vacuum arc furnace smelting adopts a crucible with the diameter of 640mm, in the smelting process, the leakage rate is 0.60Pa/min, the vacuum degree is 1.2Pa, the smelting current is 28kA, the smelting voltage is 42V, feeding is started when the consumable electrode smelting residual mass is 900kg, the current reduction rate is gradually reduced, and the cooling time after smelting is 12 hours.
The TB11 titanium alloy ingot prepared by the embodiment has no clinker, the Mo content is 14.9, and the chemical composition meets the national standard requirement.
Example 4
Preparing a Ti-Mo intermediate alloy core rod:
step 1: mixing Mo powder which meets the national standard and contains 0.04 percent of O element by mass and Ti powder which contains 0.14 percent of O element by mass according to the mass ratio of 3.2:6.8, and uniformly mixing by using a mixer; pressing the uniformly mixed powder into a blank by using a cold isostatic press, wherein the pressing pressure is 150MPa, and the pressure maintaining time is 15 min.
Step 2: and (3) sintering the blank obtained in the step (1) by using a vacuum sintering furnace, wherein the sintering temperature is 1350 ℃, and the heat preservation time is 12 h.
And step 3: and (3) forging the sintered blank obtained in the step (2) by using a precision forging machine. The heating temperature before finish forging is 700 ℃, the asbestos is wrapped in the forging process for slow cooling, the single-pass deformation is 5%, and the single-fire forging is carried out for 4 passes; then forging to the required specification according to the mode; after the forged bar is machined, 100% of light is required, and the Ti-Mo intermediate alloy core rod with the diameter of 200mm is obtained.
Vacuum consumable arc melting:
and 4, step 4: and 3, taking the Ti-Mo intermediate alloy core rod obtained in the step 3 as a consumable electrode to carry out three times of vacuum consumable electrode arc furnace smelting, specifically:
the first time and the second time of vacuum consumable electrode arc furnace smelting respectively adopt crucibles with the diameters of 280mm and 360mm, and in the smelting process, the leakage rate is 0.9Pa/min, the vacuum degree is 16Pa, the smelting current is 8kA, the smelting voltage is 28V, and the cooling time after smelting is 4 hours;
the third vacuum consumable electrode electric arc furnace adopts a crucible with the diameter of 440mm for smelting, the leakage rate is 0.60Pa/min, the vacuum degree is 2Pa, the smelting current is 9kA, the smelting voltage is 30V, feeding is started when the consumable electrode smelting residual mass is 150kg, the current reduction rate is gradually reduced, and the cooling time after smelting is 6 hours.
The TB7 titanium alloy ingot prepared by the embodiment has no unfixed block, the Mo content is 32.5, and the chemical composition meets the national standard requirement.
From the above examples, it can be seen that the titanium alloy with high Mo content can be prepared by preparing a Ti — Mo master alloy core rod and a prepared electrode block, assembling and welding the Ti — Mo master alloy core rod and the electrode block to form a consumable electrode, and performing vacuum consumable arc melting. The content of each component of the consumable electrode is consistent with that of each component of the corresponding titanium alloy, and the Mo element in the titanium alloy is ensured to be completely introduced from the Ti-Mo intermediate alloy. Mo element introduced by the intermediate alloy does not generate Mo unfixed blocks in the titanium alloy, and is suitable for mass production, popularization and application.
Claims (12)
1. A preparation method of a high Mo titanium alloy ingot specifically comprises the following steps:
preparing a Ti-Mo intermediate alloy core rod: mixing Mo powder and Ti powder in proportion, molding, vacuum sintering and fine forging to obtain a Ti-Mo intermediate alloy core rod;
preparing a Mo-free electrode block: preparing a corresponding electrode block without Mo element according to the content of each component of the prepared titanium alloy containing Mo element;
preparing a consumable electrode: assembling and welding the electrode block without Mo element and the prepared Ti-Mo intermediate alloy core rod to form a consumable electrode, wherein the content of each element component in the consumable electrode is consistent with that of the titanium alloy corresponding to the electrode block without Mo element; in the consumable electrode, Mo element is introduced by a Ti-Mo intermediate alloy core rod, Ti element is introduced by an electrode block and the Ti-Mo intermediate alloy core rod together, and other elements are introduced by the electrode block;
vacuum consumable arc melting: and carrying out vacuum consumable arc melting on the prepared consumable electrode to obtain a high-Mo titanium alloy ingot with the Mo content of 10-40% by mass.
2. The method of claim 1, wherein in the step of preparing the Ti-Mo master alloy core rod, the ratio of Mo powder to Ti powder is 3: 7-4: 6 by mass ratio.
3. The method of manufacturing a high Mo titanium alloy ingot according to claim 1, wherein in the step of manufacturing the Ti-Mo master alloy core rod, the sintered compact is heated and then finish forged; the single-pass deformation is not more than 15mm, and the single-pass forging is carried out for 2-5 passes; and (3) machining the forged bar, and then requiring 100% of light to obtain the Ti-Mo intermediate alloy core rod.
4. The method of claim 3, wherein the heating temperature before finish forging is 500 ℃ to 1200 ℃.
5. The method of claim 3, wherein the forging is conducted by slow cooling with asbestos.
6. The method of manufacturing a high Mo titanium alloy ingot according to claim 1, wherein in the step of manufacturing the Mo-free electrode block, when the electrode block is manufactured, Ti element is mainly introduced by sponge titanium, and other elements are introduced by binary alloy; when a certain element is introduced from a binary alloy and cannot meet the matching amount, the deficiency is introduced from the simple substance metal of the element.
7. The method of claim 1, wherein in the step of preparing the consumable electrode, the consumable electrode has a structure in which a Ti — Mo master alloy core rod is centered, and the electrode block wraps an outer circumferential surface of the Ti — Mo master alloy core rod.
8. The method of producing a high Mo titanium alloy ingot according to claim 1, wherein in the step of vacuum consumable arc melting, the parameters of vacuum consumable arc melting are: controlling the leakage rate to be below 1.2Pa/min, controlling the vacuum degree to be below 5.0Pa, controlling the smelting current to be 6-40 kA, controlling the smelting voltage to be 25-45V, controlling the cooling time to be not less than 6 hours after smelting, entering a feeding stage at the later stage of smelting, reducing the smelting current step by step, and finally ensuring that the molten powder is completely reserved.
9. The method of claim 8, wherein the vacuum consumable arc melting is performed three times: the first and second vacuum consumable arc melting parameters are as follows: controlling the leakage rate to be below 1.2Pa/min, the vacuum degree to be below 20.0Pa, the smelting current to be 6-40 kA, the smelting voltage to be 25-40V and the cooling time to be not less than 6.0 hours after smelting in the smelting process;
the parameters of the third vacuum consumable arc melting are as follows: controlling the leakage rate to be below 0.8Pa/min, controlling the vacuum degree to be below 5.0Pa, controlling the smelting current to be 6-40 kA and the smelting voltage to be 25-45V in the smelting process, feeding when the consumable electrode is smelted to obtain 100-1000 kg of residual mass, reducing the smelting current step by step, finally ensuring that the molten powder is completely reserved, and controlling the cooling time to be not less than 6.0 hours after smelting.
10. A preparation method of a high Mo titanium alloy ingot specifically comprises the following steps:
preparing a consumable electrode: mixing Mo powder and Ti powder according to the proportion of the components of the titanium-molybdenum-titanium alloy, uniformly mixing, forming, vacuum sintering and precisely forging to obtain a Ti-Mo consumable electrode;
vacuum consumable arc melting: and (3) carrying out vacuum consumable arc melting on the Ti-Mo consumable electrode obtained in the step to obtain a titanium alloy ingot with the Mo content of 10-40% by mass.
11. The method of claim 10, wherein in the step of preparing the consumable electrode, the precision forging process parameters are as follows: the single-pass deformation is not more than 15mm, and the single-pass forging is carried out for 2-5 passes; the forged bar requires 100% light after machining.
12. The method of claim 10, wherein the vacuum consumable arc melting is performed three times, and the first and second vacuum arc furnace melting parameters are: controlling the leakage rate to be below 1.2Pa/min, the vacuum degree to be below 20.0Pa, the smelting current to be 6-40 kA, the smelting voltage to be 25-40V and the cooling time to be not less than 6.0 hours after smelting in the smelting process;
the parameters of the third vacuum consumable arc melting are as follows: in the smelting process, the leakage rate is controlled to be below 0.8Pa/min, the vacuum degree is controlled to be below 5.0Pa, the smelting current is 6-40 kA, the smelting voltage is 25-45V, the feeding stage is carried out in the later stage of smelting, the smelting current is reduced step by step, the complete reservation of the molten metal is finally ensured, and the cooling time after smelting is not less than 6.0 hours.
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| CN102367523A (en) * | 2011-10-08 | 2012-03-07 | 中南大学 | Method for melting titanium alloy containing high-melting point alloy element |
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| CN110551919A (en) * | 2019-09-23 | 2019-12-10 | 西安赛特金属材料开发有限公司 | Preparation method of titanium-molybdenum alloy |
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| CN102367523A (en) * | 2011-10-08 | 2012-03-07 | 中南大学 | Method for melting titanium alloy containing high-melting point alloy element |
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