CN113005314A - Preparation method of high-uniformity NbTi alloy ingot - Google Patents
Preparation method of high-uniformity NbTi alloy ingot Download PDFInfo
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Abstract
A preparation method of a high-uniformity NbTi alloy ingot comprises the following preparation steps: 1) preparing the titanium sponge and the niobium rod according to the proportion; 2) preparing a titanium electrode block: pressing titanium sponge to form a titanium electrode block, wherein grooves penetrating through two opposite side ends of the titanium electrode block are formed in the surface of the titanium electrode block; 3) assembling a consumable electrode: assembling and welding a plurality of titanium electrode blocks and niobium rods to form a rod-shaped consumable electrode, wherein the consumable electrode is in a structure that the titanium electrode blocks are wrapped on the peripheries of the niobium rods; 4) and smelting the prepared consumable electrode for three times to obtain an NbTi alloy ingot. The ingot prepared by the method has no Nb fritting blocks and black spots, and can be produced in batch.
Description
Technical Field
The invention belongs to the technical field of nonferrous metal processing, and particularly relates to a preparation method of NbTi (niobium-titanium) alloy ingots with phi of 280-640 mm.
Background
Since 1911, Dutch physicist K. Onnas discovered superconducting properties, it was discovered that tens of metals and nearly 4000 alloys and compounds were superconducting. Since the discovery of superconductivity, the superconducting technology is developed at a high speed and is widely applied to high-tech fields such as high-energy physics, controlled thermonuclear fusion, energy storage, magnetic suspension, nuclear magnetic resonance and the like. The superconducting material is the basis of the superconducting technology, and the application range and the application degree of the superconducting technology are closely related to the superconducting material.
NbTi alloy is the most widely used superconducting material at present due to its high mechanical properties and excellent superconducting properties. The melting point of Nb element is up to 2410 ℃, the density is up to 8.57g/cm3, while the melting point of active metal Ti is only 1687 ℃, the density is only 4.50g/cm3, the difference between the melting point and the density of the two is large, and the risk of Nb unfreezing block is large; meanwhile, due to the difference between the component density and the melting point, the alloy is easy to generate component segregation, and the X-ray detection shows that the alloy is black spot. At present, an ingot of niobium-titanium alloy is usually prepared by mixing titanium sponge and niobium scraps to prepare an electrode for smelting for multiple times. However, the preparation method still has the phenomena of Nb unfreezing blocks, black spots and the like.
Disclosure of Invention
The invention aims to provide a preparation method of NbTi alloy ingot with the specification of phi 280-phi 640mm, which solves the problems of Nb fritting failure and uneven components in the ingot.
In order to realize the aim, the technical scheme adopted by the invention is a preparation method of a high-uniformity NbTi alloy ingot, which comprises the following preparation steps:
1) preparing the titanium sponge and the niobium rod according to the proportion;
2) preparing a titanium electrode block: pressing titanium sponge to form a titanium electrode block, wherein grooves penetrating through two opposite side ends of the titanium electrode block are formed in one surface of the titanium electrode block;
3) assembling the consumable electrode: assembling and welding a plurality of titanium electrode blocks and niobium rods to form a rod-shaped consumable electrode, wherein the consumable electrode is in a structure that the titanium electrode blocks are wrapped on the peripheries of the niobium rods;
4) and smelting the prepared consumable electrode for three times to obtain an NbTi alloy ingot.
In the step 1), the content of the titanium element is 40-60 wt%.
In the step 2), the pressure strength of the titanium electrode block formed by pressing the titanium sponge is 10-30 MPa.
In the step 3), a plurality of titanium electrode blocks are sequentially distributed to form a strip-shaped groove; placing a niobium rod in the strip-shaped groove; covering the titanium electrode blocks and the niobium rods which are arranged well with the titanium electrode blocks corresponding to the titanium electrode blocks to form a structure that the outer peripheral surface of the niobium rod is wrapped with the titanium electrode blocks; and welding the assembled titanium electrode block and the niobium rod to form the consumable electrode.
In the step 4), smelting for the first time: vacuum before melting is 5.0Pa, melting voltage is 30-40V, melting current is 8-30 KA, air leakage rate is controlled to be below 1.2Pa/min, arc stabilizing current adopts direct current of 3-18A, cooling time after melting is more than or equal to 3 hours, and flat head treatment is carried out on the cast ingot after melting is finished;
smelting for the second time: turning around and smelting the cast ingot subjected to flat head treatment; the vacuum before melting is 2.0Pa, the melting voltage is 30-45V, and the melting current is 10-30 kA; controlling the air leakage rate to be below 1.0Pa/min, adopting alternating current of 5-20A for arc stabilizing current, and cooling for more than or equal to 4 hours after smelting; performing flat head treatment on the cast ingot after the smelting is finished;
smelting for the third time: turning around and smelting the cast ingot subjected to the flat head treatment after the second smelting; 1.0Pa of vacuum before melting, 32-45V of melting voltage and 8-30 kA of melting current; the air leakage rate is 0.8Pa/min, the arc stabilizing current is 8-25A alternating current, and the cooling time after smelting is more than or equal to 5 hours.
And during the third smelting, the mode of reducing the input power step by step is adopted to keep the depth of the molten pool stable.
And during the third smelting, the arc stabilizing period is kept between 5 and 300 s.
And during the third smelting, the input power is reduced step by step in the feeding stage, and the bottom of the second smelting ingot is completely remained on the auxiliary electrode after the smelting is finished.
The first smelting crystallizer is phi 160-440 mm, the second smelting crystallizer is phi 220-560 mm, and the third smelting crystallizer is phi 280-640 mm.
According to the niobium-titanium alloy ingot, the Ti element is introduced in a sponge titanium form, the Nb element is introduced in an Nb rod form, and the content of the Ti element in the NbTi alloy is 40-60 wt%.
The consumable electrode is manufactured in a mode that the peripheral surface of a niobium rod is wrapped with titanium metal, and the niobium metal is assembled into the consumable electrode in an integral rod shape, so that the phenomenon that niobium is not melted in a niobium-titanium alloy ingot is avoided. The principle lies in that when the niobium scrap and titanium metal mixed material is adopted to manufacture the electrode, the formed density is not high as that of a niobium rod. When in smelting, the highest melting point of an arc region reaches 4700 ℃, an electrode block added in a Nb scrap mode is difficult to reach a sufficiently compact state, and the Nb scrap falls into a molten pool before being melted in the smelting process. Since the lower bath temperature is only 100 c (about 2300 c) above the melting point of the NbTi alloy, the melting point of pure niobium reaches 2477 c. Once the Nb shavings fall into the molten pool, it is difficult to fully alloy, resulting in the formation of Nb-unfrozen cakes. And the Nb rod mode is adopted to be introduced into the consumable electrode, the density of the Nb rod is high, and the situation that chips fall off during melting can not occur, so that the phenomenon that Nb is not melted in ingot casting can be avoided.
And smelting for three times is adopted, and the depth of a molten pool is kept stable by adopting a mode of reducing input power step by step in the third smelting. The arc stabilizing period is kept between 5 and 300 seconds, and the stirring intensity in the molten pool is ensured to be proper and uniform. And in the feeding stage, the input power is further reduced step by step, and the bottom of the niobium-titanium alloy ingot is completely remained on the auxiliary electrode after the smelting is finished. The smelting process can ensure that niobium-titanium metal is fully melted and uniformly mixed, and the condition of ingot casting black spots is avoided.
The invention has the beneficial effects that: the invention provides a preparation method of a high-uniformity NbTi alloy ingot, which solves the problems of Nb fritting failure and black spots by changing the structural form of raw materials and changing the distribution mode and the smelting times of a consumable electrode, realizes the engineering batch production of the NbTi alloy ingot, and can provide high-quality NbTi ingots for the fields of ITER projects, medical MRI equipment and the like.
Drawings
Fig. 1 is a schematic structural diagram of a titanium electrode block after titanium sponge is pressed and formed.
Fig. 2 is a schematic view of the structure of the consumable electrode after assembly and welding.
FIG. 3 is a diagram showing the X-ray detection result of the middle part of an NbTi ingot with the phi 280mm specification.
FIG. 4 is a diagram showing the X-ray detection result of the middle part of an NbTi ingot with a diameter of 520 mm.
FIG. 5 is a diagram showing the X-ray detection result of the middle part of an NbTi ingot with a diameter of 640 mm.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
The preparation method of the high-uniformity NbTi alloy ingot specifically comprises the following steps:
1) preparing the titanium sponge and the niobium rod according to the proportion;
2) preparing a titanium electrode block: pressing titanium sponge to form a titanium electrode block 1, wherein grooves 11 penetrating through two opposite side ends of the titanium electrode block are formed on the surface of one side of the titanium electrode block, referring to fig. 1;
3) assembling a consumable electrode: referring to fig. 2, a plurality of titanium electrodes 1 and niobium rods 2 are assembled and welded to form a rod-shaped consumable electrode, and the consumable electrode is in a structure that the periphery of the niobium rod is wrapped with a titanium electrode block;
4) and smelting the prepared consumable electrode for three times to obtain an NbTi alloy ingot. The Ti content in the niobium-titanium alloy ingot is 40-60 wt%.
5) And processing the obtained NbTi alloy ingot, peeling the surface of the obtained NbTi alloy ingot, and sawing a dead head to obtain a marketable NbTi alloy finished product ingot.
The titanium sponge and the niobium rod are made of materials meeting the national standard.
The parameters of the third smelting are as follows:
smelting for the first time: the vacuum before smelting is 5.0Pa, the smelting voltage is 30-40V, the smelting current is 8-30 KA, the gas leakage rate is controlled to be below 1.2Pa/min, the arc stabilizing current adopts direct current of 3-18A, and the cooling time after smelting is more than or equal to 3 hours;
smelting for the second time: the vacuum before melting is 2.0Pa, the melting voltage is 30-45V, and the melting current is 10-30 kA; controlling the air leakage rate to be below 1.0Pa/min, adopting alternating current of 5-20A for arc stabilizing current, and cooling for more than or equal to 4 hours after smelting;
smelting for the third time: 1.0Pa of vacuum before melting, 32-45V of melting voltage and 8-30 kA of melting current; the air leakage rate is 0.8Pa/min, the arc stabilizing current is 8-25A alternating current, and the cooling time after smelting is more than or equal to 5 hours.
The above-mentioned preparation steps will be described in detail.
Example 1
Step 1): preparing titanium sponge and niobium rods according to the proportion requirement of 40 wt% of Ti content in the alloy;
step 2): pouring the titanium sponge into a special die, pressing the titanium sponge into a titanium electrode block 1 by using an oil press, wherein the pressing strength is 25 MPa;
and step 3: sequentially arranging and combining the three titanium electrode blocks 1 pressed in the step 2 with the surfaces with the grooves facing upwards, forming long-strip-shaped grooves on the three arranged titanium electrode blocks, and placing the niobium rod 2 in the long-strip-shaped grooves formed by combining the three titanium electrode blocks; and then covering the titanium electrode block with the surface of which the three grooves are located at the corresponding positions of the three titanium electrode blocks, wherein the peripheral surface of the niobium rod is completely wrapped by a hollow part formed by the grooves of the six oppositely arranged titanium electrode blocks, and the end surfaces of two ends of the niobium rod are flush with the end surfaces of the combined titanium electrode blocks. Welding the combined titanium electrode block and niobium rod into a rod-shaped consumable electrode by adopting a non-tungsten argon shield plasma welding box;
and 4, step 4: carrying out three times of smelting on the consumable electrode obtained in the step 3 in a consumable vacuum electric arc furnace:
smelting for the first time: the crystallizer specification is phi 160mm, the vacuum is 5.0Pa before melting, the melting voltage is 30-40V, the melting current is 8-30 KA, the air leakage rate is controlled below 1.2Pa/min, the arc stabilizing current adopts direct current of 3-18A, the cooling time after melting is more than or equal to 3 hours, and flat head treatment needs to be carried out on a lathe after melting;
smelting for the second time: turning around and smelting the cast ingot subjected to flat head treatment; the specification of the crystallizer is phi 220mm, the vacuum before melting is 2.0Pa, the melting voltage is 30-45V, and the melting current is 10-30 kA; controlling the air leakage rate to be below 1.0Pa/min, adopting alternating current of 5-20A for arc stabilizing current, and cooling for more than or equal to 4 hours after smelting;
smelting for the third time: turning around and smelting the cast ingot subjected to the flat head treatment after the second smelting; the specification of the crystallizer is phi 280mm, the vacuum before melting is 1.0Pa, the melting voltage is 32-45V, and the melting current is 8-30 kA; the air leakage rate is 0.8Pa/min, the arc stabilizing current is 8-25A alternating current, and the cooling time after smelting is more than or equal to 5 hours. And during the third smelting, the mode of reducing the input power step by step is adopted to keep the depth of the molten pool stable. The arc stabilization period is maintained at 5-300 s. And the input power is reduced step by step in the feeding stage, so that the bottom of the second smelting ingot is completely remained on the auxiliary electrode after the smelting is finished.
And 5: and (4) peeling the surface of the ingot smelted in the vacuum arc furnace in the step (4), and sawing a dead head to obtain a NbTi alloy finished product ingot.
The NbTi alloy ingot with the diameter of 280mm melted in the present example was subjected to middle transverse X-ray detection, and as shown in fig. 3, no niobium non-melting block and no black spot were found.
Example 2
Step 1): preparing titanium sponge and niobium rods according to the proportion requirement of 47 wt% of Ti content in the alloy;
step 2): pouring the titanium sponge into a special die, pressing the titanium sponge into a titanium electrode block 1 by using an oil press, wherein the pressing strength is 25 MPa;
and step 3: sequentially arranging and combining the six titanium electrode blocks 1 pressed in the step 2 with the surfaces with the grooves facing upwards, forming long-strip-shaped grooves on the six arranged titanium electrode blocks, and placing the niobium rod 2 in the long-strip-shaped grooves formed by combining the six titanium electrode blocks; and then covering the titanium electrode block with the six grooves on the corresponding positions of the six titanium electrode blocks, wherein the titanium electrode block faces downwards, completely wrapping the peripheral surface of the niobium rod through a hollow part formed by the grooves of the twelve oppositely arranged titanium electrode blocks, and the end surfaces of the two ends of the niobium rod are flush with the end surfaces of the combined titanium electrode block. Welding the combined titanium electrode block and niobium rod into a rod-shaped consumable electrode by adopting a non-tungsten argon shield plasma welding box;
and 4, step 4: and (3) carrying out three times of smelting on the consumable electrode obtained in the step (3) in a consumable vacuum arc furnace:
smelting for the first time: the crystallizer specification is phi 360mm, the vacuum is 5.0Pa before melting, the melting voltage is 30-40V, the melting current is 15-30 KA, the air leakage rate is controlled to be below 1.2Pa/min, the arc stabilizing current adopts direct current of 3-18A, the cooling time after melting is more than or equal to 4 hours, and flat head treatment needs to be carried out on a lathe after melting;
smelting for the second time: turning around and smelting the cast ingot subjected to flat head treatment; the specification of the crystallizer is phi 440mm, the vacuum before melting is 2.0Pa, the melting voltage is 30-45V, and the melting current is 10-30 kA; controlling the air leakage rate to be below 1.0Pa/min, adopting alternating current of 5-20A for arc stabilizing current, and cooling for more than or equal to 5 hours after smelting;
smelting for the third time: turning around and smelting the cast ingot subjected to the flat head treatment after the second smelting; the specification of the crystallizer is phi 520mm, the vacuum before melting is 1.0Pa, the melting voltage is 32-45V, and the melting current is 8-30 kA; the air leakage rate is 0.8Pa/min, the arc stabilizing current is 8-25A alternating current, and the cooling time after smelting is more than or equal to 6 hours. And during the third smelting, the mode of reducing the input power step by step is adopted to keep the depth of the molten pool stable. The arc stabilization period is maintained at 5-300 s. And the input power is reduced step by step in the feeding stage, so that the bottom of the second smelting ingot is completely remained on the auxiliary electrode after the smelting is finished.
And 5: and (4) peeling the surface of the ingot smelted in the vacuum arc furnace in the step (4), and sawing a dead head to obtain a NbTi alloy finished product ingot.
The cast ingot with the diameter of 520mm melted in the embodiment is subjected to middle transverse X-ray detection, and referring to FIG. 4, the cast ingot has no niobium non-melting blocks and no black spots.
Example 3
Step 1: preparing titanium sponge and niobium rods according to the proportion requirement of 60 wt% of Ti content in the alloy;
step 2: pouring the titanium sponge into a special die, pressing the titanium sponge into a titanium electrode block 1 by using an oil press, wherein the pressing strength is 25 MPa;
and step 3: sequentially arranging and combining the eight titanium electrode blocks 1 pressed in the step 2 with the surfaces with the grooves facing upwards, forming long-strip-shaped grooves on the arranged eight titanium electrode blocks, and placing the niobium rod 2 in the long-strip-shaped grooves formed by combining the eight titanium electrode blocks; and then covering the titanium electrode block with the surface facing downwards with the eight grooves at the corresponding positions of the eight titanium electrode blocks, completely wrapping the peripheral surface of the niobium rod through a hollow part formed by the grooves of the sixteen titanium electrode blocks which are oppositely arranged, and enabling the end surfaces of two ends of the niobium rod to be flush with the end surfaces of the combined titanium electrode blocks. Welding the combined titanium electrode block and niobium rod into a rod-shaped consumable electrode by adopting a non-tungsten argon shield plasma welding box;
and 4, step 4: carrying out three times of smelting on the consumable electrode obtained in the step 3 in a consumable vacuum electric arc furnace;
smelting for the first time: the crystallizer specification is phi 440mm, the vacuum is 5.0Pa before melting, the melting voltage is 30-40V, the melting current is 20-30 KA, the air leakage rate is controlled below 1.2Pa/min, the arc stabilizing current adopts direct current of 3-18A, the cooling time after melting is more than or equal to 5 hours, and flat head treatment needs to be carried out on a lathe after melting;
smelting for the second time: turning around and smelting the cast ingot subjected to flat head treatment; the specification of the crystallizer is phi 560mm, the vacuum before melting is 2.0Pa, the melting voltage is 30-45V, and the melting current is 10-30 kA; controlling the air leakage rate to be below 1.0Pa/min, adopting alternating current of 5-20A for arc stabilizing current, and cooling for 6 hours or more after smelting;
smelting for the third time: turning around and smelting the cast ingot subjected to the flat head treatment after the second smelting; the specification of the crystallizer is phi 640mm, the vacuum before melting is 1.0Pa, the melting voltage is 32-45V, and the melting current is 12-30 kA; the air leakage rate is 0.8Pa/min, the arc stabilizing current is 8-25A alternating current, and the cooling time after smelting is more than or equal to 6 hours. And during the third smelting, the mode of reducing the input power step by step is adopted to keep the depth of the molten pool stable. The arc stabilization period is maintained at 5-300 s. And the input power is reduced step by step in the feeding stage, so that the bottom of the second smelting ingot is completely remained on the auxiliary electrode after the smelting is finished.
And 5: and (4) peeling the surface of the ingot smelted in the vacuum arc furnace in the step (4), and sawing a dead head to obtain a NbTi alloy finished product ingot.
The ingots with the diameter of 640mm melted in the example were subjected to middle transverse X-ray detection, and as shown in fig. 5, there were no niobium non-melting blocks and no black spots.
From the above embodiments, the preparation method of the NbTi alloy ingot provided by the invention can be used for performing three times of smelting in a consumable electrode structure mode that the titanium electrode block wraps the niobium rod, so that the NbTi alloy ingot which is uniformly distributed, has no niobium fritting blocks and has no black spots can be obtained, the quality of the NbTi alloy ingot is improved, and the batch production can be met.
Claims (11)
1. A preparation method of a high-uniformity NbTi alloy ingot comprises the following preparation steps:
1) preparing the titanium sponge and the niobium rod according to the proportion;
2) preparing a titanium electrode block: pressing titanium sponge to form a titanium electrode block, wherein grooves penetrating through two opposite side ends of the titanium electrode block are formed in one surface of the titanium electrode block;
3) assembling a consumable electrode: assembling and welding a plurality of titanium electrode blocks and niobium rods to form a rod-shaped consumable electrode, wherein the consumable electrode is in a structure that the titanium electrode blocks are wrapped on the peripheries of the niobium rods;
4) and smelting the prepared consumable electrode for three times to obtain an NbTi alloy ingot.
2. The method of preparing a high homogeneity NbTi alloy ingot according to claim 1, characterized in that in step 1), the titanium element content is 40-60 wt%.
3. The method for preparing the high-uniformity NbTi alloy ingot according to claim 1, wherein in the step 2), the pressure strength of the titanium electrode block formed by pressing the titanium sponge is 10-30 MPa.
4. The method for preparing the high-uniformity NbTi alloy ingot according to claim 1, wherein in the step 3), a plurality of titanium electrode blocks are sequentially arranged and distributed to form a strip-shaped groove; placing a niobium rod in the strip-shaped groove; covering the titanium electrode blocks and the niobium rods which are arranged well with the titanium electrode blocks corresponding to the titanium electrode blocks to form a structure that the outer peripheral surface of the niobium rod is wrapped with the titanium electrode blocks; and welding the assembled titanium electrode block and the niobium rod to form the consumable electrode.
5. The method of preparing a high uniformity ingot of NbTi alloy of claim 1, wherein the welding in step 3) is performed using non-tungsten argon shield plasma welding.
6. The method of preparing a high homogeneity NbTi alloy ingot according to claim 1, characterized in that in step 4), the first melting: vacuum before melting is 5.0Pa, melting voltage is 30-40V, melting current is 8-30 KA, air leakage rate is controlled to be below 1.2Pa/min, arc stabilizing current adopts direct current of 3-18A, cooling time after melting is more than or equal to 3 hours, and flat head treatment is carried out on the cast ingot after melting is finished;
smelting for the second time: turning around and smelting the cast ingot subjected to flat head treatment; the vacuum before melting is 2.0Pa, the melting voltage is 30-45V, and the melting current is 10-30 kA; controlling the air leakage rate to be below 1.0Pa/min, adopting alternating current of 5-20A for arc stabilizing current, and cooling for more than or equal to 4 hours after smelting; performing flat head treatment on the cast ingot after the smelting is finished;
smelting for the third time: turning around and smelting the cast ingot subjected to the flat head treatment after the second smelting; 1.0Pa of vacuum before melting, 32-45V of melting voltage and 8-30 kA of melting current; the air leakage rate is 0.8Pa/min, the arc stabilizing current is 8-25A alternating current, and the cooling time after smelting is more than or equal to 5 hours.
7. The method of claim 6, wherein the third melting step comprises a step-wise reduction of input power to maintain a constant depth of the molten pool.
8. The method of claim 6, wherein during the third melting, the arc stabilization period is maintained between 5 and 300 seconds.
9. The method of claim 6, wherein during the third melting, the input power is reduced step by step during the feeding stage to ensure that the bottom of the second melted ingot remains on the auxiliary electrode after the melting is completed.
10. The method of preparing a highly homogeneous ingot of NbTi alloy according to claim 6, wherein the cooling time after melting is 6 hours or more in the third melting.
11. The method for preparing the high-uniformity NbTi alloy ingot according to claim 6, wherein the first smelting crystallizer is phi 160-440 mm in specification, the second smelting crystallizer is phi 220-560 mm in specification, and the third smelting crystallizer is phi 280-640 mm in specification.
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| CN113245681A (en) * | 2021-07-14 | 2021-08-13 | 西部超导材料科技股份有限公司 | Vacuum plasma welding method for niobium-titanium alloy cast ingot |
| CN114318021A (en) * | 2021-11-19 | 2022-04-12 | 成都先进金属材料产业技术研究院股份有限公司 | Vacuum consumable melting method for Ti45Nb titanium alloy |
| CN115029570A (en) * | 2022-06-15 | 2022-09-09 | 西部超导材料科技股份有限公司 | Preparation method of titanium-niobium alloy ingot |
| CN115896507A (en) * | 2022-11-23 | 2023-04-04 | 宁夏中色金航钛业有限公司 | Niobium hafnium titanium zirconium tantalum tungsten alloy and preparation process thereof |
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