CN113373317A - Preparation method of zero shrinkage cavity titanium or titanium alloy ingot and ingot - Google Patents

Preparation method of zero shrinkage cavity titanium or titanium alloy ingot and ingot Download PDF

Info

Publication number
CN113373317A
CN113373317A CN202110521942.4A CN202110521942A CN113373317A CN 113373317 A CN113373317 A CN 113373317A CN 202110521942 A CN202110521942 A CN 202110521942A CN 113373317 A CN113373317 A CN 113373317A
Authority
CN
China
Prior art keywords
current
ingot
smelting
titanium
feeding stage
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202110521942.4A
Other languages
Chinese (zh)
Inventor
黄立清
李超
樊凯
焦毅柱
胡珊珊
郭文军
彭晖
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hunan Goldsky Titanium Industry Technology Co ltd
Original Assignee
Hunan Goldsky Titanium Industry Technology Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Hunan Goldsky Titanium Industry Technology Co ltd filed Critical Hunan Goldsky Titanium Industry Technology Co ltd
Priority to CN202110521942.4A priority Critical patent/CN113373317A/en
Publication of CN113373317A publication Critical patent/CN113373317A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B9/00General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C22B9/16Remelting metals
    • C22B9/20Arc remelting
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22DCASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D7/00Casting ingots, e.g. from ferrous metals
    • B22D7/005Casting ingots, e.g. from ferrous metals from non-ferrous metals
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00Obtaining refractory metals
    • C22B34/10Obtaining titanium, zirconium or hafnium
    • C22B34/12Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
    • C22B34/1295Refining, melting, remelting, working up of titanium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C14/00Alloys based on titanium

Abstract

The invention relates to a preparation method of a zero shrinkage cavity titanium or titanium alloy ingot and the ingot, wherein the preparation method of the titanium or titanium alloy ingot comprises the following steps: taking a titanium or titanium alloy non-finished product ingot as a consumable electrode, and carrying out final smelting by adopting vacuum consumable arc smelting, wherein the final smelting comprises a smelting stage and a feeding stage which are sequentially carried out; the feeding stage process comprises a step-by-step current reduction feeding stage and a step-by-step current increase feeding stage which are sequentially carried out, wherein the smelting current of the step-by-step current reduction feeding stage is greater than the end point smelting current of the step-by-step current reduction feeding stage. According to the invention, on the basis of the stage of feeding by reducing current step by step, the smelting current is increased again to feed in the stage of feeding by increasing current, so that the baking on the end part of the ingot is increased, the end part of the ingot obtains enough energy input, the solidification shrinkage characteristic of the unset melt in the ingot is further coordinated, shrinkage cavities which are originally formed are eliminated, finally no shrinkage cavity is formed in the ingot, the loss of the portion containing the shrinkage cavity at the head part of the ingot is avoided, and the yield of the ingot is improved.

Description

Preparation method of zero shrinkage cavity titanium or titanium alloy ingot and ingot
Technical Field
The invention relates to the technical field of titanium or titanium alloy, in particular to a preparation method of a zero-shrinkage-cavity titanium or titanium alloy ingot and the ingot.
Background
Titanium is an active metal element, titanium and titanium alloy contact with air in the smelting process, and the titanium element is easily combined with elements such as oxygen, nitrogen and the like in the air to make the material brittle. Therefore, melting of titanium and titanium alloys needs to be performed in a vacuum or an inert atmosphere. Vacuum consumable arc melting is the main preparation method for preparing high-quality titanium alloy at present, and the ingot prepared by the method has the advantages of high uniformity and high purity, but in the process, feeding is generally needed to reduce the depth of a shrinkage cavity so as to improve the yield when the ingot is smelted in the last time.
At present, a method of reducing current step by step is generally adopted in the industry for feeding. However, the method has high control difficulty and general effect, a certain shrinkage cavity still exists after the ingot casting of each furnace is fed, the fluctuation of the depth range of the shrinkage cavity is large, the cutting amount of the portion containing the shrinkage cavity at the head of the ingot casting is large (the weight is generally more than 2 percent), and the improvement of the yield is limited. Therefore, the conventional method for preparing a titanium or titanium alloy ingot is desired to be improved.
Disclosure of Invention
Accordingly, there is a need for a titanium or titanium alloy ingot and a method for producing the same that can effectively eliminate shrinkage cavities and improve yield.
Specifically, the invention is realized by the following technical scheme:
in one aspect of the present invention, a method for preparing a titanium or titanium alloy ingot comprises the following steps:
taking a titanium or titanium alloy non-finished product ingot as a consumable electrode, and carrying out final smelting by adopting vacuum consumable arc smelting, wherein the final smelting comprises a smelting stage and a feeding stage which are sequentially carried out; the feeding stage process comprises a step-by-step current reduction feeding stage and a step-by-step current increase feeding stage which are sequentially carried out, wherein the smelting current of the step-by-step current reduction feeding stage is larger than the end point smelting current of the step-by-step current reduction feeding stage.
In some embodiments, the titanium or titanium alloy unfinished ingot is solid, has a diameter of phi 500mm to phi 1100mm, and has a total weight of 2000Kg to 15000 Kg.
In some embodiments, the smelting current in the smelting stage is 12KA to 40KA, the smelting voltage is 24V to 40V, the arc stabilizing current is AC 8A to 20A, and the stirring period is 5S to 30S.
In some embodiments, the feeding stage is started when the weight of the unfused consumable electrode remaining from the last smelting is 100Kg to 500 Kg.
In some embodiments, the end-point smelting current of the step-by-step reduced current feeding stage is 3KA to 5 KA; the total time of the step-by-step current reduction feeding stage is 60-240 min, and the current increasing stage is started when the weight of the remaining unfused consumable electrode in the step-by-step current reduction feeding stage is 10-50 Kg.
In some embodiments, the smelting current of the current increasing and feeding stage is 6 KA-12 KA, and the total time of the current increasing and feeding stage is 5 min-30 min.
In some embodiments, the difference between the melting current of the current increasing feeding stage and the end melting current of the current decreasing feeding stage is 3KA to 7 KA.
In some of these embodiments, the method of manufacturing further comprises the step of manufacturing the titanium or titanium alloy unfinished ingot by:
preparing raw materials required for preparing a titanium or titanium alloy ingot into an electrode block, and performing vacuum consumable arc melting for at least 1 time by taking the electrode block as a consumable electrode to obtain the titanium or titanium alloy non-finished ingot.
In some embodiments, in the step of preparing the titanium or titanium alloy non-finished product ingot, the melting current of the vacuum consumable arc melting is 8KA to 35KA, the melting voltage is 20V to 36V, and the arc stabilizing current is AC/DC 6A to 16A, wherein the stirring period of AC is 5S to 20S.
In another aspect of the invention, a titanium or titanium alloy ingot is provided, which is prepared by the preparation method of any one of the above.
The invention has the following beneficial effects:
the researchers of the invention find that on the basis of the traditional step-by-step current reduction feeding stage, a current increasing feeding stage can be further added: namely, when the feeding in the current-decreasing feeding stage is completed, the smelting current is increased again to perform the feeding in the current-increasing feeding stage, the baking on the end part of the ingot is increased, so that the end part of the ingot obtains enough energy input, the solidification shrinkage characteristic of the unset melt in the ingot is coordinated, the shrinkage cavity is further lifted to the upper surface of the ingot and is finally eliminated, the shrinkage cavity which is originally formed is finally realized, the shrinkage cavity is not formed in the ingot, the sawing loss of the portion, containing the shrinkage cavity, of the head part of the ingot is avoided, the yield of the titanium or titanium alloy ingot is improved, and the method has great economic value.
Drawings
FIG. 1 is a flaw detection signal chart of a finished titanium alloy ingot produced in example 1;
FIG. 2 is a flaw detection signal chart of the finished titanium alloy ingot produced in comparative example 1.
Detailed Description
In order that the invention may be more fully understood, a more particular description of the invention will now be rendered by reference to specific embodiments thereof that are illustrated in the appended drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
An embodiment of the present invention provides a method for producing a titanium or titanium alloy ingot, including the steps of:
and taking a titanium or titanium alloy non-finished product ingot as a consumable electrode, and carrying out final smelting by adopting vacuum consumable arc smelting. Wherein, the last smelting comprises a smelting stage and a feeding stage which are carried out in sequence.
The feeding stage process comprises a step-by-step current reduction feeding stage and a step-by-step current increase feeding stage which are sequentially carried out, wherein the smelting current of the step-by-step current reduction feeding stage is greater than the end point smelting current of the step-by-step current reduction feeding stage.
Consumable electrode smelter is also called vacuum consumable electrode arc smelting (VAR), and is a consumable electrode produced by an induction smelter in a vacuum environment is heated and smelted by controllable alternating current arc.
Researchers of the invention find that titanium or titanium alloy prepared by a method of reducing current step by step for feeding commonly adopted in the industry still has a certain shrinkage cavity, and the depth of the shrinkage cavity is large, the range fluctuation of the depth is large, so that the cutting amount of the shrinkage cavity-containing part at the head of an ingot is large, and the improvement of the yield is limited.
Based on this, the researchers of the present invention found that, on the basis of the conventional step-by-step decreasing current feeding stage, an increasing current feeding stage can be further added: namely, when the feeding in the current-decreasing feeding stage is completed, the smelting current is increased again to perform the feeding in the current-increasing feeding stage, the baking on the end part of the ingot is increased, so that the end part of the ingot obtains enough energy input, the solidification shrinkage characteristic of the unset melt in the ingot is coordinated, the shrinkage cavity is further lifted to the upper surface of the ingot and is finally eliminated, the shrinkage cavity which is originally formed is finally realized, the shrinkage cavity is not formed in the ingot, the sawing loss of the portion, containing the shrinkage cavity, of the head part of the ingot is avoided, the yield of the titanium or titanium alloy ingot is improved, and the method has great economic value.
In some of these embodiments, the titanium or titanium alloy unfinished ingot is solid, with a diameter specification of phi 500mm to phi 1100mm, and a total weight of 2000Kg to 15000 Kg.
In some embodiments, the smelting current in the smelting stage is 12 KA-40 KA, the smelting voltage is 24V-40V, the arc stabilizing current is AC 8A-20A, and the stirring period is 10 s-30 s, wherein AC refers to alternating current.
Furthermore, the smelting current in the smelting stage is 18KA to 35KA, the smelting voltage is 28V to 38V, the arc stabilizing current is AC 8A to 18A, and the stirring period is 10s to 30 s.
In some embodiments, the feeding stage is started when the weight of the remaining unfused consumable electrode in the last smelting is 100 Kg-500 Kg.
In some embodiments, the end-point smelting current of the step-by-step reduced current feeding stage is 3-5 KA; further, the total time of the step-by-step current reduction feeding stage is 60-180 min; further, when the weight of the remaining unfused consumable electrode in the stage of gradually reducing current feeding is 10 Kg-50 Kg, the current feeding stage is started to be increased.
In some of these embodiments, the process of the step-down current feeding stage is (KA/V/min):
(25~10)/(33~27)/(2~10)→(10~6)/(30~26)/(5~20)→(6~4)/(26~23)/(10~40)→(5~3)/(26~23)/(40~170)。
further, when the target ingot is a TC4 titanium alloy ingot with the phi 880mm specification, the process of the step-by-step current reduction feeding stage is as follows (KA/V/min): (21-19)/29.5/2 → 8.5/26/15 → 5/25/30 → 4/25/(90-140).
Further, when the target ingot is TC11 titanium alloy ingot with phi 680mm specification, the process of the step-by-step current reduction feeding stage is as follows (KA/V/min): (20-18)/29/2 → 8/26/15 → 4.5/25/30 → 4/25/(60-100).
Further, when the target ingot is a TA15 titanium alloy ingot with the specification of phi 780mm, the process of the step-by-step current reduction feeding stage is as follows (KA/V/min): (21-19)/29.5/2 → 8/26/12 → 4.5/25/25 → 3.5/25/(70-120).
In some embodiments, the smelting current in the current rise feeding stage is 6 KA-12 KA, and the total time of the current rise feeding stage is 5 min-30 min.
Further, the process of the current rise feeding stage is (KA/V/min):
(6~12)/(22~28)/(2~5)→(6~12)/(22~28)/(3~25)。
further, when the target ingot is a TC4 titanium alloy ingot with a phi 880mm specification, the process at the current rise feeding stage is as follows (KA/V/min): 9.5/26/2 → 10/26/15. (in this case: within 2min, the current KA/voltage V is changed to 9.5/26, and then within 15min, the current KA/voltage V is changed to 10/26 in a linear way, namely, within 15min, the current linear change is increased by 0.5KA, and the voltage is kept unchanged; the same meaning is provided in the context of the labels).
Further, when the target ingot is a TC11 titanium alloy ingot with the specification of phi 680mm, the process at the current rise feeding stage is as follows (KA/V/min): 7/26/2 → 7/26/10.
Further, when the target ingot is a TA15 titanium alloy ingot with the phi 780mm specification, the process at the current increasing feeding stage is as follows (KA/V/min): 9/26/2 → 9/26/12.
In some embodiments, the difference between the smelting current in the current increasing feeding stage and the end-point smelting current in the current decreasing feeding stage is 3KA to 7 KA; furthermore, the difference value of the smelting current in the current increasing and feeding stage and the end-point smelting current in the current decreasing and feeding stage is 3-6 KA.
In some of these embodiments, the method of preparation further comprises the step of preparing an unfinished ingot of titanium or titanium alloy:
preparing raw materials required for preparing the titanium or titanium alloy ingot into an electrode block, and performing vacuum consumable arc melting for at least 1 time by taking the electrode block as a consumable electrode to obtain a titanium or titanium alloy non-finished ingot. Further, in the step of preparing the titanium or titanium alloy non-finished product ingot, the smelting current of vacuum consumable arc smelting is 8 KA-35 KA, the smelting voltage is 20V-36V, the arc stabilizing current is AC/DC 6A-16A, and the stirring period of AC is 5S-20S.
In some specific examples, the number of heats of the vacuum consumable arc melting in the step of preparing the non-finished ingot of titanium or titanium alloy is 2. The melting current of the 1 st vacuum consumable arc melting is 8 KA-18 KA, the melting voltage is 20V-28V, and the arc stabilizing current is DC 6A-12A. The melting current of the 2 nd vacuum consumable electrode arc melting is 12 KA-35 KA, the melting voltage is 24V-36V, the arc stabilizing current is AC 8A-16A, and the stirring period is 5S-20S.
Further, the electrode block is a cylinder.
Specifically, the preparation method of the titanium or titanium alloy non-finished ingot comprises the following steps: preparing materials and mixing materials according to raw materials required for preparing a titanium or titanium alloy ingot, and then pressing into an electrode block; typically, these raw materials need to be pressed into a plurality of electrode blocks; and then stacking and welding a plurality of electrode blocks obtained by pressing into a long cylindrical welding electrode, wherein the welding electrode can be used as a consumable electrode to perform vacuum consumable arc melting for at least 1 time to obtain a titanium or titanium alloy non-finished product ingot. Wherein, the welding step can be carried out by adopting a vacuum plasma welding mode.
Further, the total weight of the electrode block is 40Kg to 120 Kg. Furthermore, the diameter specification of the welding electrode is phi 400 mm-phi 1000 mm.
An embodiment of the invention provides a titanium or titanium alloy ingot prepared by any one of the above preparation methods.
The titanium ingot or the titanium alloy ingot is prepared by the preparation method and has zero shrinkage cavity.
The titanium ingot or the titanium alloy ingot prepared by the invention can eliminate shrinkage cavities in the titanium and titanium alloy finished product ingot, so that the ingot does not need to be cut off from the head part containing the shrinkage cavities, and the yield of the ingot is further improved.
In some of these embodiments, the titanium alloy ingot is a TC4 (nominal composition Ti-6Al-4V) titanium alloy ingot, a TC11 (nominal composition Ti-6.5Al-3.5Mo-1.5Zr-0.3Si) titanium alloy ingot, a TA15 (nominal composition Ti-7.5Al-1Mo-1V-2Zr) titanium alloy ingot, a TA11 (nominal composition Ti-8Al-1Mo-1V) titanium alloy ingot, a TC18 (nominal composition Ti-5Al-4.75Mo-4.75V-1Cr-1Fe) titanium alloy ingot, or a TC32 (nominal composition Ti-5Al-3Mo-3Cr-1Zr-0.15Si) titanium alloy ingot.
In order to make the objects, technical solutions and advantages of the present invention more concise and clear, the present invention is described with the following specific embodiments, but the present invention is by no means limited to these embodiments. The following described examples are only preferred embodiments of the present invention, which can be used to describe the present invention and should not be construed as limiting the scope of the present invention. It should be understood that any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
In order to better illustrate the invention, the following examples are given to further illustrate the invention. The following are specific examples.
Example 1:
the process for preparing the titanium alloy ingot with zero shrinkage cavity phi 880mmTC4 (nominal component Ti-6Al-4V) comprises the following steps:
stacking and welding TC4 electrode blocks with the unit weight of 90Kg and the diameter of phi 580mm to prepare 6840Kg of welding electrode, and smelting the welding electrode for 2 times by adopting vacuum consumable arc to obtain phi 780mmTC4 titanium alloy cast ingot. The melting current of the 1 st vacuum consumable arc melting is 15KA, the melting voltage is 25V, and the arc stabilizing current is DC 10A. The melting current of the 2 nd vacuum consumable electrode arc melting is 25KA, the melting voltage is 32V, the arc stabilizing current is AC 12A, and the stirring period is 14S.
Taking a phi 780mmTC4 titanium alloy cast ingot (subjected to 2 times of VAR smelting) as a consumable electrode, carrying out the last smelting in a vacuum consumable arc furnace, wherein the specification of a crucible is phi 880mm, the smelting current is 32KA, the smelting voltage is 36V, the arc stabilizing current is AC 14A, the stirring period is 15S, and when the consumable electrode is remained 300Kg, feeding is carried out by adopting step-by-step current reduction, and the process of current reduction is (KA/V/min): 20/29.5/2 → 8.5/26/15 → 5/25/30 → 4/25/(90-140), when the weight of the consumable electrode is 30Kg, then the current is increased, and the current increasing process is (KA/V/min): 9.5/26/2 → 10/26/15, then tripping and cooling to obtain the finished titanium alloy ingot.
Flaw detection is carried out on the whole cast ingot, a shrinkage cavity signal is not found (as shown in figure 1), and zero shrinkage cavity of the cast ingot is confirmed; the ingot is subsequently longitudinally cut, and no shrinkage cavity is found. The abscissa in fig. 1 is the acoustic depth, and no other peak is found in the diameter range of 0 to 880mm except for the initial wave and the bottom.
Example 2:
the process for preparing the titanium alloy ingot with zero shrinkage cavity phi of 680mmTC11 (nominal component Ti-6.5Al-3.5Mo-1.5Zr-0.3Si) comprises the following steps:
stacking and welding TC11 electrode blocks with the unit weight of 40Kg and the diameter of phi 420mm to prepare 3840Kg of welding electrodes, and smelting the welding electrodes for 2 times by adopting vacuum consumable arc to obtain phi 580mmTC11 titanium alloy cast ingots. The melting current of the 1 st vacuum consumable arc melting is 10KA, the melting voltage is 22V, and the arc stabilizing current is DC 7A. The melting current of the 2 nd vacuum consumable electrode arc melting is 16KA, the melting voltage is 26V, the arc stabilizing current is AC 8A, and the stirring period is 10S. Using phi 580mmTC11 titanium alloy cast ingot (which is subjected to 2 times of VAR smelting) as a consumable electrode, carrying out the last smelting in a vacuum consumable arc furnace, wherein the specification of a crucible is phi 680mm, the smelting current is 25KA, the smelting voltage is 32V, the arc stabilizing current is AC 8A, the stirring period is 15S, and when the consumable electrode is remained 250Kg, feeding is carried out by adopting step-by-step current reduction, and the process of current reduction is (KA/V/min): 18/29/2 → 8/26/15 → 4.5/25/30 → 4/25/(60-100), when the weight of the consumable electrode is 15Kg, then the current is increased, and the current increasing process is (KA/V/min): 7/26/2 → 7/26/10, then tripping and cooling to obtain the finished titanium alloy ingot. Flaw detection is carried out on the whole cast ingot, no shrinkage cavity signal is found, and zero shrinkage cavity of the cast ingot is confirmed; the ingot is subsequently longitudinally cut, and no shrinkage cavity is found.
Example 3:
the process for preparing the titanium alloy ingot with zero shrinkage cavity phi 780mmTA15 (nominal component Ti-7.5Al-1Mo-1V-2Zr) comprises the following steps:
stacking and welding TA15 electrode blocks with the unit weight of 60Kg and the diameter of phi 480mm to prepare 4800Kg welding electrodes, and smelting the welding electrodes for 2 times by adopting vacuum consumable arc to obtain phi 680mmTA15 titanium alloy cast ingots. The melting current of the 1 st vacuum consumable arc melting is 12KA, the melting voltage is 24V, and the arc stabilizing current is DC 9A. The melting current of the 2 nd vacuum consumable electrode arc melting is 22KA, the melting voltage is 30V, the arc stabilizing current is AC 12A, and the stirring period is 14S. Using a phi 680mmTA15 titanium alloy cast ingot (which is subjected to 2 times of VAR smelting) as a consumable electrode, carrying out the last smelting in a vacuum consumable arc furnace, wherein the specification of a crucible is phi 780mm, the smelting current is 29KA, the smelting voltage is 35V, the arc stabilizing current is AC 14A, the stirring period is 20s, and when the consumable electrode is remained 270Kg, feeding is carried out by adopting step-by-step current reduction, and the process of current reduction is (KA/V/min): 20/29.5/2 → 8/26/12 → 4.5/25/25 → 3.5/25/(70-120), when the weight of the consumable electrode is 20Kg, then the current is increased, and the current-increasing process is (KA/V/min): 9/26/2 → 9/26/12, then tripping and cooling to obtain the finished titanium alloy ingot. Flaw detection is carried out on the whole cast ingot, no shrinkage cavity signal is found, and zero shrinkage cavity of the cast ingot is confirmed; the ingot is subsequently longitudinally cut, and no shrinkage cavity is found.
Example 4
The preparation process of example 4 is substantially the same as that of example 1, except that: a finished TA1 pure titanium ingot was prepared using a TA1 (nominal composition Ti, i.e., pure titanium) electrode block. Flaw detection is carried out on the whole cast ingot, no shrinkage cavity signal is found, and zero shrinkage cavity of the cast ingot is confirmed; the ingot is subsequently longitudinally cut, and no shrinkage cavity is found.
Example 5
The preparation process of example 5 is substantially the same as that of example 2, except that: TC18 (nominal component Ti-5Al-4.75Mo-4.75V-1Cr-1Fe) electrode block is adopted to prepare TC18 alloy finished product cast ingot. Flaw detection is carried out on the whole cast ingot, no shrinkage cavity signal is found, and zero shrinkage cavity of the cast ingot is confirmed; the ingot is subsequently longitudinally cut, and no shrinkage cavity is found.
Example 6
The preparation process of example 6 is substantially the same as that of example 3, except that: and preparing a finished TC32 alloy ingot by using a TC32 (nominal component Ti-5Al-3Mo-3Cr-1Zr-0.15Si) electrode block. Flaw detection is carried out on the whole cast ingot, no shrinkage cavity signal is found, and zero shrinkage cavity of the cast ingot is confirmed; the ingot is subsequently longitudinally cut, and no shrinkage cavity is found.
Comparative example 1:
comparative example 1 is essentially the same as example 1, except that: omitting "then boost current, the boost current process is (KA/V/min): 9.5/26/2 → 10/26/15'.
After obtaining a finished titanium alloy ingot, when flaw detection is carried out on the side surface of the ingot, a shrinkage cavity signal is found to exist at a position 90mm away from the end surface of the head of the ingot, as shown in figure 2, besides an initial wave and a bottom wave, an obvious defect reflection signal is also found at a position 400mm away from the surface of the ingot; the ingot was sawed at the shrinkage cavity signal position (feeder sawing amount-240 Kg), and a shrinkage cavity with a diameter of about 20mm was found. Specifically, the preparation process of comparative example 1 is as follows:
stacking and welding TC4 electrode blocks with the unit weight of 90Kg and the diameter of phi 580mm to prepare 6840Kg of welding electrode, and smelting the welding electrode for 2 times by adopting vacuum consumable arc to obtain phi 780mmTC4 titanium alloy cast ingot. The melting current of the 1 st vacuum consumable arc melting is 15KA, the melting voltage is 25V, and the arc stabilizing current is DC 10A. The melting current of the 2 nd vacuum consumable electrode arc melting is 25KA, the melting voltage is 32V, the arc stabilizing current is AC 12A, and the stirring period is 14S.
Taking a phi 780mmTC4 titanium alloy cast ingot (subjected to 2 times of VAR smelting) as a consumable electrode, carrying out the last smelting in a vacuum consumable arc furnace, wherein the specification of a crucible is phi 880mm, the smelting current is 32KA, the smelting voltage is 36V, the arc stabilizing current is AC 14A, the stirring period is 15S, and when the consumable electrode is remained 300Kg, feeding is carried out by adopting step-by-step current reduction, and the process of current reduction is (KA/V/min): 20/29.5/2 → 8.5/26/15 → 5/25/30 → 4/25/(90-140), when the weight of the consumable electrode is 30Kg, tripping and cooling to obtain the finished titanium alloy ingot.
Comparative example 2:
the preparation process of comparative example 2 is substantially the same as that of example 2 except that: omitting "then boost current, the boost current process is (KA/V/min): 7/26/2 → 7/26/10 "; after obtaining a finished titanium alloy ingot, when flaw detection is carried out on the side surface of the ingot, a shrinkage cavity signal is found to exist at a position 60mm away from the end surface of the head of the ingot; the ingot was sawed at the shrinkage cavity signal position (feeder sawing amount-100 Kg), and a shrinkage cavity with a diameter of about 15mm was found. Specifically, the preparation process of comparative example 2 is as follows:
stacking and welding TC11 electrode blocks with the unit weight of 40Kg and the diameter of phi 420mm to prepare 3840Kg of welding electrodes, and smelting the welding electrodes for 2 times by adopting vacuum consumable arc to obtain phi 580mmTC11 titanium alloy cast ingots. The melting current of the 1 st vacuum consumable arc melting is 10KA, the melting voltage is 22V, and the arc stabilizing current is DC 7A. The melting current of the 2 nd vacuum consumable electrode arc melting is 16KA, the melting voltage is 26V, the arc stabilizing current is AC 8A, and the stirring period is 10S. Using phi 580mmTC11 titanium alloy cast ingot (which is subjected to 2 times of VAR smelting) as a consumable electrode, carrying out the last smelting in a vacuum consumable arc furnace, wherein the specification of a crucible is phi 680mm, the smelting current is 25KA, the smelting voltage is 32V, the arc stabilizing current is AC 8A, the stirring period is 15S, and when the consumable electrode is remained 250Kg, feeding is carried out by adopting step-by-step current reduction, and the process of current reduction is (KA/V/min): 18/29/2 → 8/26/15 → 4.5/25/30 → 4/25/(60-100), when the weight of the consumable electrode is 15Kg, tripping and cooling to obtain the finished titanium alloy ingot.
Comparative example 3:
comparative example 3 is substantially the same as example 3 except that: omitting "then boost current, the boost current process is (KA/V/min): 9/26/2 → 9/26/12 "; after obtaining a finished titanium alloy ingot, when flaw detection is carried out on the side surface of the ingot, a shrinkage cavity signal is found to exist at a position 80mm away from the end surface of the head of the ingot; the ingot was sawed at the shrinkage cavity signal position (feeder sawing amount-160 Kg), and a shrinkage cavity with a diameter of about 15mm was found. Specifically, the preparation process of comparative example 3 is as follows:
stacking and welding TA15 electrode blocks with the unit weight of 60Kg and the diameter of phi 480mm to prepare 4800Kg welding electrodes, and smelting the welding electrodes for 2 times by adopting vacuum consumable arc to obtain phi 680mmTA15 titanium alloy cast ingots. The melting current of the 1 st vacuum consumable arc melting is 12KA, the melting voltage is 24V, and the arc stabilizing current is DC 9A. The melting current of the 2 nd vacuum consumable electrode arc melting is 22KA, the melting voltage is 30V, the arc stabilizing current is AC 12A, and the stirring period is 14S. Using a phi 680mmTA15 titanium alloy cast ingot (which is subjected to 2 times of VAR smelting) as a consumable electrode, carrying out the last smelting in a vacuum consumable arc furnace, wherein the specification of a crucible is phi 780mm, the smelting current is 29KA, the smelting voltage is 35V, the arc stabilizing current is AC 14A, the stirring period is 20s, and when the consumable electrode is remained 270Kg, feeding is carried out by adopting step-by-step current reduction, and the process of current reduction is (KA/V/min): 20/29.5/2 → 8/26/12 → 4.5/25/25 → 3.5/25/(70-120), when the weight of the consumable electrode is 20Kg, tripping and cooling to obtain the finished titanium alloy ingot.
Some key process parameters of examples 1-3 are shown in the following table:
Figure BDA0003064316180000111
compared with the comparative example 1, the comparison of the example 1 and the comparative example 1 shows that under the condition of no change of other conditions, the TC4 titanium alloy ingot preparation process can effectively eliminate shrinkage cavity in the TC4 titanium alloy ingot on the basis of the feeding process of gradually reducing current, and the subsequent current increasing feeding stage is further added, so that zero shrinkage cavity is finally achieved.
Compared with the comparative example 2, the comparison of the example 2 and the comparative example 2 shows that under the condition of no change of other conditions, the TC11 titanium alloy ingot preparation process can effectively eliminate shrinkage cavity in the TC11 titanium alloy ingot on the basis of the feeding process of gradually reducing current, and the subsequent current increasing feeding stage is further added, so that zero shrinkage cavity is finally achieved.
Compared with the comparative example 3, the embodiment 3 shows that under the condition that other conditions are not changed, the TA15 titanium alloy ingot preparation process can effectively eliminate shrinkage cavity in the TA15 titanium alloy ingot and finally achieve zero shrinkage cavity by further increasing the current increasing stage on the basis of the feeding process of gradually decreasing the current.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (10)

1. A preparation method of a titanium or titanium alloy ingot is characterized by comprising the following steps:
taking a titanium or titanium alloy non-finished product ingot as a consumable electrode, and carrying out final smelting by adopting vacuum consumable arc smelting, wherein the final smelting comprises a smelting stage and a feeding stage which are sequentially carried out; the feeding stage process comprises a step-by-step current reduction feeding stage and a step-by-step current increase feeding stage which are sequentially carried out, wherein the smelting current of the step-by-step current reduction feeding stage is larger than the end point smelting current of the step-by-step current reduction feeding stage.
2. The method of claim 1, wherein the non-finished ingot of titanium or titanium alloy is solid, has a diameter of phi 500mm to phi 1100mm, and has a total weight of 2000Kg to 15000 Kg.
3. The preparation method of claim 1, wherein the smelting current in the smelting stage is 12KA to 40KA, the smelting voltage is 24V to 40V, the arc stabilizing current is AC 8A to 20A, and the stirring period is 5S to 30S.
4. The method of claim 1, wherein the feeding stage is initiated when the weight of the remaining unmelted consumable electrodes from the last smelt is between 100Kg and 500 Kg.
5. The method of claim 1, wherein an end-point melting current of the step-down current feeding stage is 3KA to 5KA, a total duration of the step-down current feeding stage is 60min to 240min, and the step-up current feeding stage is started when a weight of unfused consumable electrodes remaining in the step-down current feeding stage is 10Kg to 50 Kg.
6. The method of claim 1, wherein the end-point smelting current of the current-increasing feeding stage is 6KA to 12KA, and the total duration of the current-increasing feeding stage is 5min to 30 min.
7. The process of claim 1, wherein the difference between the melting current in the up-current feeding stage and the end-point melting current in the down-current feeding stage is 3KA to 7 KA.
8. The method of claim 1 to 7, further comprising the step of preparing the non-finished ingot of titanium or titanium alloy by:
preparing raw materials required for preparing a titanium or titanium alloy ingot into an electrode block, and performing vacuum consumable arc melting for at least 1 time by taking the electrode block as a consumable electrode to obtain the titanium or titanium alloy non-finished ingot.
9. The method of claim 8, wherein in the step of preparing the non-finished titanium or titanium alloy ingot, the consumable vacuum arc melting has a melting current of 8KA to 35KA, a melting voltage of 20V to 36V, and an arc stabilizing current of AC/DC 6A to 16A, wherein the AC has a stirring period of 5S to 20S.
10. A titanium or titanium alloy ingot produced by the production method according to any one of claims 1 to 9.
CN202110521942.4A 2021-05-13 2021-05-13 Preparation method of zero shrinkage cavity titanium or titanium alloy ingot and ingot Pending CN113373317A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110521942.4A CN113373317A (en) 2021-05-13 2021-05-13 Preparation method of zero shrinkage cavity titanium or titanium alloy ingot and ingot

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110521942.4A CN113373317A (en) 2021-05-13 2021-05-13 Preparation method of zero shrinkage cavity titanium or titanium alloy ingot and ingot

Publications (1)

Publication Number Publication Date
CN113373317A true CN113373317A (en) 2021-09-10

Family

ID=77570912

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110521942.4A Pending CN113373317A (en) 2021-05-13 2021-05-13 Preparation method of zero shrinkage cavity titanium or titanium alloy ingot and ingot

Country Status (1)

Country Link
CN (1) CN113373317A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113881854A (en) * 2021-10-28 2022-01-04 西部钛业有限责任公司 Method for eliminating low-density inclusion defect source of titanium alloy ingot
CN114015891A (en) * 2021-11-11 2022-02-08 云南钛业股份有限公司 VAR pure titanium ingot feeding method based on feeding electrode and ingot

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0931558A (en) * 1995-07-19 1997-02-04 Daido Steel Co Ltd Vacuum arc remelting method
CN102438764A (en) * 2009-04-30 2012-05-02 塞菲瓦尔公司 Method for producing elongate products made of titanium
CN109082536A (en) * 2018-08-23 2018-12-25 河南中原特钢装备制造有限公司 A kind of electroslag remelting production technology
CN109706332A (en) * 2018-12-19 2019-05-03 西部超导材料科技股份有限公司 A method of improving titan alloy casting ingot surface quality
CN110951974A (en) * 2019-11-20 2020-04-03 湖南金天钛业科技有限公司 Titanium alloy ingot and preparation method thereof
CN110964932A (en) * 2019-11-18 2020-04-07 西部超导材料科技股份有限公司 Arc-extinguishing process of VAR titanium alloy primary ingot

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0931558A (en) * 1995-07-19 1997-02-04 Daido Steel Co Ltd Vacuum arc remelting method
CN102438764A (en) * 2009-04-30 2012-05-02 塞菲瓦尔公司 Method for producing elongate products made of titanium
CN109082536A (en) * 2018-08-23 2018-12-25 河南中原特钢装备制造有限公司 A kind of electroslag remelting production technology
CN109706332A (en) * 2018-12-19 2019-05-03 西部超导材料科技股份有限公司 A method of improving titan alloy casting ingot surface quality
CN110964932A (en) * 2019-11-18 2020-04-07 西部超导材料科技股份有限公司 Arc-extinguishing process of VAR titanium alloy primary ingot
CN110951974A (en) * 2019-11-20 2020-04-03 湖南金天钛业科技有限公司 Titanium alloy ingot and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113881854A (en) * 2021-10-28 2022-01-04 西部钛业有限责任公司 Method for eliminating low-density inclusion defect source of titanium alloy ingot
CN113881854B (en) * 2021-10-28 2023-08-15 西部钛业有限责任公司 Method for eliminating sources of low-density inclusion defects of titanium alloy cast ingot
CN114015891A (en) * 2021-11-11 2022-02-08 云南钛业股份有限公司 VAR pure titanium ingot feeding method based on feeding electrode and ingot

Similar Documents

Publication Publication Date Title
CN110951974B (en) Titanium alloy ingot and preparation method thereof
CN113373317A (en) Preparation method of zero shrinkage cavity titanium or titanium alloy ingot and ingot
CN112481513B (en) Process for preparing copper-chromium alloy electrical contact consumable electrode by using CuCr metal powder
CN111519066B (en) Preparation method for improving component uniformity of large-size titanium alloy ingot
CN111225990A (en) Method for producing a nickel-base alloy
CN110527843B (en) Preparation method of high-niobium titanium alloy homogeneous ingot
CN107022696B (en) A kind of bio-medical metastable beta-type Zr-Nb alloy cast ingots and preparation method thereof
CN113832363B (en) Titanium alloy ingot and preparation method thereof
CN108546850A (en) A kind of production method of 6101 aluminum alloy plate materials of high conductivity
CN111842855B (en) Method for preparing TA10 residual material into cast ingot by using duplex process
CN113462904B (en) Pressing method of Ti-Mo alloy vacuum consumable electrode bar with high Mo content
CN111549244A (en) Preparation method of Ti35 titanium alloy ingot
CN111304493A (en) Superstrong high-plasticity titanium alloy and preparation method thereof
CN109371255A (en) A kind of 6N high-purity cobalt ingot casting method
CN113512657A (en) Preparation method of high-uniformity boron-containing titanium alloy ingot
CN105603283A (en) Method for preparing and forming high-strength high-toughness wrought magnesium alloy
CN111575572A (en) B-doped TiZrNb multi-principal-element alloy and preparation method thereof
JPH05214458A (en) Method for melting titanium alloy ingot by var process
CN110669974A (en) Preparation method of niobium-zirconium alloy cast ingot
CN116287807A (en) Preparation method of short-process alloy forging
CN102409184B (en) Preparation method of pure nickel slab
CN110257783B (en) Low-cost preparation method of titanium-silicon alloy target material
CN111286638A (en) (ScAl)3+Al2O3+Sc2O3) Al-based composite inoculant, and preparation method and application thereof
CN111945032A (en) 3D printing fine-grain titanium alloy and preparation method thereof
CN115287498B (en) TiC reinforced titanium-based composite material and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20210910