CN115838876B - Preparation method of niobium-titanium-aluminum-based alloy cast ingot - Google Patents
Preparation method of niobium-titanium-aluminum-based alloy cast ingot Download PDFInfo
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 87
- 239000000956 alloy Substances 0.000 title claims abstract description 87
- -1 niobium-titanium-aluminum Chemical compound 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 229910001275 Niobium-titanium Inorganic materials 0.000 claims abstract description 63
- RJSRQTFBFAJJIL-UHFFFAOYSA-N niobium titanium Chemical compound [Ti].[Nb] RJSRQTFBFAJJIL-UHFFFAOYSA-N 0.000 claims abstract description 63
- 239000000203 mixture Substances 0.000 claims abstract description 61
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000003825 pressing Methods 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 17
- 229910001257 Nb alloy Inorganic materials 0.000 claims abstract description 15
- QNTVPKHKFIYODU-UHFFFAOYSA-N aluminum niobium Chemical compound [Al].[Nb] QNTVPKHKFIYODU-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000137 annealing Methods 0.000 claims abstract description 12
- 238000003466 welding Methods 0.000 claims description 68
- 238000003723 Smelting Methods 0.000 claims description 60
- 238000000034 method Methods 0.000 claims description 25
- 239000004744 fabric Substances 0.000 claims description 12
- 239000010936 titanium Substances 0.000 claims description 12
- 229910052719 titanium Inorganic materials 0.000 claims description 10
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 6
- 239000010949 copper Substances 0.000 claims description 6
- 229910052802 copper Inorganic materials 0.000 claims description 6
- 238000005554 pickling Methods 0.000 claims description 5
- 241001417935 Platycephalidae Species 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 230000008439 repair process Effects 0.000 claims description 2
- 239000010955 niobium Substances 0.000 abstract description 19
- 238000009826 distribution Methods 0.000 abstract description 15
- 239000002994 raw material Substances 0.000 abstract description 10
- 238000005204 segregation Methods 0.000 abstract description 8
- 238000009776 industrial production Methods 0.000 abstract description 6
- 238000002844 melting Methods 0.000 abstract description 6
- 230000008018 melting Effects 0.000 abstract description 6
- 239000002253 acid Substances 0.000 abstract description 2
- 238000005406 washing Methods 0.000 abstract description 2
- 230000008569 process Effects 0.000 description 20
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 16
- 229910052758 niobium Inorganic materials 0.000 description 13
- 239000012535 impurity Substances 0.000 description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 229910001069 Ti alloy Inorganic materials 0.000 description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 6
- 230000007547 defect Effects 0.000 description 6
- 238000003892 spreading Methods 0.000 description 6
- 230000007480 spreading Effects 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 5
- 229910052786 argon Inorganic materials 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000001514 detection method Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 229910001182 Mo alloy Inorganic materials 0.000 description 2
- UNQHSZOIUSRWHT-UHFFFAOYSA-N aluminum molybdenum Chemical compound [Al].[Mo] UNQHSZOIUSRWHT-UHFFFAOYSA-N 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910000599 Cr alloy Inorganic materials 0.000 description 1
- QQHSIRTYSFLSRM-UHFFFAOYSA-N alumanylidynechromium Chemical compound [Al].[Cr] QQHSIRTYSFLSRM-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000000788 chromium alloy Substances 0.000 description 1
- 239000002173 cutting fluid Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 229910002058 ternary alloy Inorganic materials 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 229910006281 γ-TiAl Inorganic materials 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention discloses a preparation method of a niobium-titanium-aluminum-based alloy cast ingot, which comprises the following steps: 1. crushing the niobium-titanium cast ingot to obtain niobium-titanium scraps, and carrying out acid washing and vacuum annealing treatment to obtain pretreated niobium-titanium scraps; 2. mixing part of the pretreated niobium-titanium scraps with titanium sponge to obtain a mixture A, and mixing the rest of the pretreated niobium-titanium scraps with aluminum-niobium alloy and other intermediate alloys to obtain a mixture B; 3. distributing and pressing the mixture A serving as an upper layer, a lower layer and the mixture B serving as an intermediate layer to obtain an electrode block; 4. the electrode block is assembled and welded to obtain an electrode rod; 5. the electrode rod is subjected to three times of vacuum consumable arc melting. According to the invention, niobium-titanium scraps are adopted and preprocessed, and the design of mixing and pressing distribution modes of the niobium-titanium scraps and other raw materials is combined, so that micro-zone segregation and inclusion of Nb element and loss of Al element are avoided, uniformity and content accuracy of alloy components in the niobium-titanium-aluminum-based alloy cast ingot are improved, and the requirement of industrial production is met.
Description
Technical Field
The invention belongs to the technical field of niobium alloy preparation, and particularly relates to a preparation method of a niobium-titanium-aluminum-based alloy cast ingot.
Background
Compared with gamma-TiAl alloy, the Ti-AlNb alloy has higher strength and better fracture toughness, and the excellent performance of the Ti-AlNb alloy meets the urgent requirements of the future aeroengine on the light high-temperature structural material with high specific strength and high specific rigidity, and has important significance for reducing the dead weight of the aircraft and improving the fuel efficiency and the high-temperature service performance. The mechanical and thermal processing forming properties of the niobium-titanium-aluminum-based alloy are seriously affected by the uniformity of alloy components and structures and the content of impurity elements, so that the proper raw materials and smelting methods are selected to prepare the cast ingot with accurate and pure components, uniform alloy element distribution and compact solidification structure, particularly low-gap element O, N, H content, which is a precondition for ensuring the mechanical properties of the niobium-titanium-aluminum-based alloy. From the viewpoint of smelting the Ti-Al-Nb ternary alloy, the low-density and low-melting-point Al element in the smelting process of the niobium-titanium-aluminum-based alloy volatilizes more, and meanwhile, the Nb element content is high, micro-region segregation and inclusion are easy to occur, and the accuracy and uniformity of alloy components are difficult to ensure.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a niobium-titanium-aluminum-based alloy cast ingot aiming at the defects in the prior art. According to the method, niobium-titanium scraps are adopted as raw materials and are preprocessed, the niobium-titanium scraps are respectively mixed with other raw materials and are subjected to three-layer distribution design, so that the introduction amount of impurity elements is reduced, micro-zone segregation and inclusion of Nb elements in the smelting process are avoided, aluminum-niobium alloy with a lower melting point is selected as an intermediate alloy for adding the aluminum element and the niobium element, the loss of low-density and low-melting-point Al elements in the smelting process is reduced, the uniformity and content accuracy of alloy components in the niobium-titanium-aluminum-based alloy cast ingot are improved, and the problem of uneven distribution of alloy elements in the niobium-titanium-aluminum-based alloy is solved.
In order to solve the technical problems, the invention adopts the following technical scheme: the preparation method of the niobium-titanium-aluminum-based alloy cast ingot is characterized by comprising the following steps of:
crushing a niobium-titanium cast ingot to obtain niobium-titanium scraps, pickling the niobium-titanium scraps, and then carrying out vacuum annealing treatment to obtain pretreated niobium-titanium scraps;
step two, mixing part of the pretreated niobium-titanium scraps obtained in the step one with titanium sponge to obtain a mixture A, and mixing the pretreated niobium-titanium scraps obtained in the rest step one with aluminum-niobium alloy and other intermediate alloys to obtain a mixture B;
step three, taking the mixture A obtained in the step two as an upper layer and a lower layer and taking the mixture B as an intermediate layer to perform cloth in a pressing die, and then performing pressing treatment to obtain an electrode block;
fourthly, performing assembly welding treatment on the electrode block obtained in the third step, and performing repair welding on a titanium sheet at an assembly welding position to obtain an electrode rod;
and fifthly, placing the electrode rod obtained in the step four as a consumable electrode in a vacuum consumable arc furnace for primary smelting to obtain primary ingots, sequentially connecting the heads and the tails of the 4 primary ingots after the flat heads, placing the primary ingots in the vacuum consumable arc furnace for assembly welding to obtain 2 electrodes, carrying out secondary smelting on the 2 electrodes to obtain 2 secondary ingots, connecting the heads and the tails of the 2 secondary ingots after the flat heads, placing the 2 secondary ingots in the vacuum consumable arc furnace for assembly welding to obtain 1 electrode, and carrying out tertiary smelting on the 1 electrode to obtain tertiary ingots, namely niobium-titanium-aluminum-based alloy ingots.
Firstly, pretreating niobium-titanium scraps, removing oxide impurities on the surfaces of the niobium-titanium scraps by acid washing, softening the niobium-titanium scraps by combining vacuum annealing treatment so as to have higher ductility, reducing the content of partial gas impurity elements such as O, N, H in the niobium-titanium scraps, and simultaneously further removing greasy dirt on the surfaces of the niobium-titanium scraps and impurities such as adhered cutting fluid to obtain niobium-titanium scraps with lower impurity element content, thereby being beneficial to realizing the subsequent electrode block pressing process; secondly, the invention adopts niobium-titanium scraps and aluminum-niobium alloy as raw materials of niobium elements in the niobium-titanium-aluminum-based alloy cast ingot of target products, the pretreated niobium-titanium scraps are divided into two parts, one part is mixed with sponge titanium to obtain a mixture A, the other part is mixed with aluminum-niobium alloy and other intermediate alloy to obtain a mixture B, and the mixture A and the mixture B are subjected to cloth pressing to prepare the target products of the electrode block, so that the niobium-containing raw materials are dispersed in each position of the electrode block, the distribution uniformity of the niobium elements in the niobium-titanium-aluminum-based alloy cast ingot is improved, the micro-region segregation and inclusion of the Nb elements due to high content are avoided, and the uniformity and content accuracy of alloy components in the niobium-titanium-aluminum-based alloy cast ingot are improved; and the mixture A is used as a wrapping material to be paved on the upper layer and the lower layer in the distribution process of the pressed electrode block, and the mixture B of the aluminum-containing raw material is used as a middle layer to be wrapped between the upper layer and the lower layer, so that volatilization of low-density and low-melting-point Al elements in the subsequent smelting process is greatly reduced, uniformity and content accuracy of alloy components in the niobium-titanium-aluminum-based alloy ingot are further improved, and edge arcs caused by material dropping of the two intermediate alloys of the aluminum-niobium alloy and the other intermediate alloys are avoided, uneven alloy components in the niobium-titanium-aluminum-based alloy ingot are avoided, and smooth proceeding of the subsequent smelting process is ensured.
The preparation method of the niobium-titanium-aluminum-based alloy cast ingot is characterized in that the granularity of the niobium-titanium scraps in the first step is 1mm to over3mm, wherein the conditions of the vacuum annealing treatment are as follows: vacuum degree is less than 5×10 -2 The temperature is 900-950 ℃ under MPa, and the time is more than 60 min. According to the invention, the scraps produced after the niobium-titanium ingot casting is adopted as the raw material of niobium element, so that the preparation cost is reduced, the granularity of the niobium-titanium scraps is controlled to be 1-3 mm, the granularity difference between the niobium-titanium scraps and other intermediate alloys is reduced, the alloy is more uniformly distributed in the electrode block after being mixed, and inclusion and component segregation are not easy to generate in the smelting process.
The preparation method of the niobium-titanium-aluminum-based alloy cast ingot is characterized in that the titanium sponge in the second step is 0-grade titanium sponge with the granularity of 3-12.7 mm, the titanium sponge is mixed by a mixer for 3min to obtain a mixture A, and the mixture B is obtained by mixing by the mixer for 5 min. The 0-grade titanium sponge with the granularity of 3-12.7 mm has a spongy pore structure and a smaller volume, ensures that niobium-titanium scraps are completely adhered to the surface of the titanium sponge after pressing treatment, and avoids component segregation caused by falling of the niobium-titanium scraps in the smelting treatment process. Meanwhile, the invention adopts a mixer to mix, which is favorable for fully and uniformly mixing each component in the mixture A and the mixture B, and further is favorable for uniformly distributing each element in the niobium-titanium-aluminum-based alloy cast ingot.
The preparation method of the niobium-titanium-aluminum-based alloy cast ingot is characterized in that the mass of the mixture A of the upper layer and the lower layer in the third step is equal. According to the invention, the mixture A of the upper layer and the lower layer is controlled to have equal mass, so that the mixture B of the aluminum-containing raw material is fully wrapped between the mixture A of the upper layer and the lower layer, the wrapping effect is ensured, volatilization of low-density and low-melting-point Al elements in the subsequent smelting process is effectively reduced, and uniformity and accurate content of alloy components in the niobium-titanium-aluminum-based alloy cast ingot are improved.
The preparation method of the niobium-titanium-aluminum-based alloy cast ingot is characterized in that the assembly welding treatment in the fourth step is performed by adopting vacuum welding box copper electrode plasma arc welding. The invention uses vacuum argon-filled atmosphere as welding environment, reduces the oxidation condition of welding spots during welding, improves the position firmness degree of the welding spots in the welding process of the electrode blocks, thoroughly avoids the problem of tungsten inclusion in titanium alloy by using a copper electrode welding gun, and has the advantages of small welding heat affected zone, small welding deformation, high welding quality and the like.
Compared with the prior art, the invention has the following advantages:
1. according to the invention, niobium-titanium scraps are adopted as raw materials, the niobium-titanium scraps are pretreated, so that the pressing process is facilitated, the introduction amount of impurity elements is reduced, the niobium-titanium scraps are divided into two parts and are respectively mixed with titanium sponge, aluminum-niobium alloy and other intermediate alloys, so that the niobium elements are uniformly distributed, meanwhile, the volatilization of low-density and low-melting-point Al elements in the smelting process is reduced by adopting a three-layer distribution mode, the micro-region segregation of the Nb elements and the impurity and Al element loss are avoided by commonly controlling all links, and the uniformity and content accuracy of alloy components in the niobium-titanium-aluminum-based alloy cast ingot are improved.
2. The niobium-titanium-aluminum-based alloy cast ingot prepared by the method improves the mass content of niobium element in the cast ingot to more than 40% on the premise of ensuring the uniformity of the integral components, has the advantages of uniform distribution of each alloy component in the cast ingot, small fluctuation, no defects of niobium inclusion and the like, has good surface quality, and meets the requirement of industrial production on the uniformity of the component distribution of the niobium-titanium-aluminum-based alloy homogeneous cast ingot.
3. According to the invention, niobium titanium scraps are used as one of sources of niobium elements, aluminum-niobium alloy is used as the sources of other niobium elements and part of aluminum elements, and the aluminum-niobium alloy has a low melting point, so that the aluminum-niobium alloy is easier to uniformly distribute in the smelting process, the segregation risk of alloy components is reduced, other intermediate alloys and sponge titanium are selected to supplement other alloy components, and the distribution uniformity of the alloy components in the niobium-titanium-aluminum alloy cast ingot is ensured.
4. According to the invention, the particle size of the niobium-titanium scraps is controlled in combination with pretreatment, and the distribution mode, the electrode block assembly welding mode and the smelting mode of the pressed electrode block are controlled, so that the distribution uniformity of alloy components in the niobium-titanium-aluminum-based alloy cast ingot is further synergistically improved, metallurgical defects are avoided, and the surface quality of the cast ingot is improved.
5. According to the invention, the electrode block is prepared by adopting a three-layer material distribution mode, the mixture of niobium titanium scraps and titanium sponge is used as an upper layer coating material and a lower layer coating material, and the mixture of the aluminum-containing intermediate alloy is used as an intermediate layer, so that the aluminum-containing intermediate alloy is ensured to be completely coated, the volatilization of Al element in the smelting process is reduced, the side arc caused by material dropping of the intermediate layer is avoided, and the smooth proceeding of the smelting process is ensured.
6. The invention adopts three times of vacuum consumable arc melting, and the next melting is carried out after each melting cast ingot is assembled and welded in the vacuum consumable arc furnace, so that the introduction of impurity elements is further avoided, the uniformity of alloy components of the niobium-titanium-aluminum-based alloy cast ingot is improved, and the process is simple and easy to control.
7. The invention has simple production process, low cost and easy realization of industrial production.
The technical scheme of the invention is further described in detail by examples.
Detailed Description
Example 1
The embodiment comprises the following steps:
crushing the niobium-titanium cast ingot to obtain niobium-titanium scraps with granularity of 1-3 mm, pickling the niobium-titanium scraps, and then placing the pickled niobium-titanium scraps into a vacuum annealing furnace, wherein the vacuum degree is 4.5 multiplied by 10 -2 Heating to 900-950 ℃ under the condition of MPa, and preserving heat for 70min to perform vacuum annealing treatment to obtain pretreated niobium-titanium scraps;
step two, mixing the pretreated niobium-titanium scraps obtained in the step one with 0-grade sponge titanium with the granularity of 3-12.7 mm for 3min by a mixer to obtain a mixture A, and mixing the pretreated niobium-titanium scraps obtained in the step one with aluminum-niobium alloy and aluminum-molybdenum alloy for 5min by the mixer to obtain a mixture B;
step three, dividing the mixture A obtained in the step two into two parts with equal mass, namely the mixture A 1 And mixture A 2 First, the mixture A is mixed 1 Pouring the mixture into a pressing mold, spreading cloth to form a lower layer, pouring the mixture B into the pressing mold, spreading cloth to form an intermediate layer, and pouring the mixture A 2 Pouring the mixture into a pressing die, paving cloth to form an upper layer, and pressing by adopting an oil press to obtain an electrode block with a single weight of 15kg, wherein the total number of the electrode blocks is 20;
dividing the 20 electrode blocks obtained in the step three into 4 groups, performing assembly welding treatment by adopting copper electrode plasma arc welding of a vacuum welding box, and performing assembly welding by adopting a titanium thin plate at an assembly welding position, wherein 1 electrode rod is obtained by assembly welding of every 5 electrode blocks, and 4 electrode rods are obtained in total; the electrode blocks are arranged in a vacuum welding box and are uniformly and symmetrically placed in the assembly welding treatment process, the clamp is adjusted and tightened, the air leakage rate is tested when the vacuum degree in the vacuum welding box is not more than 3Pa, and the air leakage rate is not more than 2.5 Pa.min -1 Then argon is filled until the pressure is 45kPa, welding is started, the adopted welding current is 320A-370A, and the welding voltage is 50V-70V;
and fifthly, respectively placing the 4 electrode rods obtained in the step four as consumable electrodes in a vacuum consumable arc furnace for primary smelting, wherein a crucible with the diameter phi of 220mm is used for primary smelting, the smelting flow is 5-9 kA, the smelting voltage is 29-32V, the smelting vacuum degree is 1.0-3.0 Pa, 4 primary ingots are obtained, then the head and the tail of the 4 primary ingots are sequentially connected and placed in the vacuum consumable arc furnace for assembly welding to obtain 2 electrodes, the 2 electrodes are subjected to secondary smelting, a crucible with the diameter phi of 280mm is used for secondary smelting, the smelting flow is 5-10 kA, the smelting voltage is 29-33V, the smelting vacuum degree is 0.5-1.6 Pa, 2 secondary ingots are obtained, then the head and the tail of the 2 secondary ingots are connected and placed in the vacuum consumable arc furnace for assembly welding to obtain 1 electrode, the three electrodes are smelted, the three times are used for smelting, the crucible with the diameter phi of 360mm is 7-12 kA, the smelting flow is 5-10 kA, the smelting voltage is 3-20 Pa, the nominal Ti is 3-0.28 Pa, and the three-dimensional Ti alloy is obtained.
The niobium-titanium-aluminum-based alloy cast ingot prepared in the embodiment is subjected to lathe facing and peeling, then the cast ingot is subjected to middle-section sawing, and chemical components are detected by respectively sampling blocks at the upper part, the middle part and the lower part of the cast ingot, and the result shows that the mass content of niobium elements at the upper part, the middle part and the lower part of the niobium-titanium-aluminum-based alloy cast ingot is 47.02%, 46.07% and 46.08%, the absolute value of fluctuation deviation of components is less than 1%, and the uniformity of components of each alloy is good. Meanwhile, through further detection, the niobium-titanium-aluminum-based alloy cast ingot prepared by the embodiment has no defects of niobium inclusion and the like, and meets the requirement of large-scale industrial production on the uniformity of the component distribution of the niobium-titanium-aluminum-based alloy cast ingot alloy.
Example 2
The embodiment comprises the following steps:
crushing the niobium-titanium cast ingot to obtain niobium-titanium scraps with granularity less than 3mm, pickling the niobium-titanium scraps, and then placing the pickled niobium-titanium scraps into a vacuum annealing furnace, wherein the vacuum degree is less than 5 multiplied by 10 -2 Heating to 900 ℃ under the condition of MPa, and preserving heat for 60min to perform vacuum annealing treatment to obtain pretreated niobium-titanium scraps;
step two, mixing the pretreated niobium-titanium scraps obtained in the step one with 0-grade sponge titanium with the granularity of 3-12.7 mm for 3min by a mixer to obtain a mixture A, and mixing the pretreated niobium-titanium scraps obtained in the step one with aluminum-niobium alloy and aluminum-molybdenum alloy for 5min by the mixer to obtain a mixture B;
step three, dividing the mixture A obtained in the step two into two parts, namely the mixture A 1 And mixture A 2 First, the mixture A is mixed 1 Pouring the mixture into a pressing mold, spreading cloth to form a lower layer, pouring the mixture B into the pressing mold, spreading cloth to form an intermediate layer, and pouring the mixture A 2 Pouring the mixture into a pressing die, paving cloth to form an upper layer, and pressing by adopting an oil press to obtain an electrode block with a single weight of 15kg, wherein the total number of the electrode blocks is 20;
dividing the 20 electrode blocks obtained in the step three into 4 groups, performing assembly welding treatment by adopting copper electrode plasma arc welding of a vacuum welding box, and performing assembly welding by adopting a titanium thin plate at an assembly welding position, wherein 1 electrode rod is obtained by assembly welding of every 5 electrode blocks, and 4 electrode rods are obtained in total; the electrode blocks are arranged in a vacuum welding box and are uniformly and symmetrically placed in the assembly welding treatment process, the clamp is adjusted and tightened, the air leakage rate is tested when the vacuum degree in the vacuum welding box is not more than 3Pa, and the air leakage rate is not more than 2.5 Pa.min -1 Then argon is filled until the pressure is 45kPa, welding is started, the adopted welding current is 320A-370A, and the welding voltage is 50V-70V;
and fifthly, respectively placing the 4 electrode rods obtained in the step four as consumable electrodes in a vacuum consumable arc furnace for primary smelting, wherein a crucible with the diameter phi of 220mm is used for primary smelting, the smelting flow is 5-9 kA, the smelting voltage is 29-32V, the smelting vacuum degree is 1.0-3.0 Pa, 4 primary ingots are obtained, then the head and the tail of the 4 primary ingots are sequentially connected and placed in the vacuum consumable arc furnace for assembly welding to obtain 2 electrodes, the 2 electrodes are subjected to secondary smelting, a crucible with the diameter phi of 280mm is used for secondary smelting, the smelting flow is 5-10 kA, the smelting voltage is 29-33V, the smelting vacuum degree is 0.5-1.6 Pa, 2 secondary ingots are obtained, then the head and the tail of the 2 secondary ingots are connected and placed in the vacuum consumable arc furnace for assembly welding to obtain 1 electrode, the three electrodes are smelted, the three times are used for smelting, the crucible with the diameter phi of 360mm is 7-12 kA, the smelting flow is 5-10 kA, the smelting voltage is 3.6 Pa, the nominal titanium alloy is 3-30 Pa, and the three-dimensional titanium alloy is obtained after the three times of 3-16 Pa, and the nominal titanium alloy is cooled, and the nominal titanium alloy is obtained.
The niobium-titanium-aluminum-based alloy cast ingot prepared in the embodiment is subjected to lathe facing and peeling, then the cast ingot is subjected to middle-section sawing, and chemical components are detected by respectively sampling blocks at the upper part, the middle part and the lower part of the cast ingot, and the result shows that the mass content of niobium elements at the upper part, the middle part and the lower part of the niobium-titanium-aluminum-based alloy cast ingot is 47.56%, 48.01% and 47.92%, the absolute value of fluctuation deviation of components is less than 1%, and the uniformity of components of each alloy is good. Meanwhile, through further detection, the niobium-titanium-aluminum-based alloy cast ingot prepared by the embodiment has no defects of niobium inclusion and the like, and meets the requirement of large-scale industrial production on the uniformity of the component distribution of the niobium-titanium-aluminum-based alloy cast ingot alloy.
Example 3
The embodiment comprises the following steps:
crushing the niobium-titanium cast ingot to obtain niobium-titanium scraps with granularity less than 3mm, pickling the niobium-titanium scraps, and then placing the pickled niobium-titanium scraps into a vacuum annealing furnace, wherein the vacuum degree is less than 5 multiplied by 10 -2 Heating to 900 ℃ under the condition of MPa, and preserving heat for 60min to perform vacuum annealing treatment to obtain pretreated niobium-titanium scraps;
step two, mixing the pretreated niobium-titanium scraps obtained in the step one with 0-grade sponge titanium with the granularity of 3-12.7 mm for 3min by a mixer to obtain a mixture A, and mixing the pretreated niobium-titanium scraps obtained in the step one with aluminum-niobium alloy and aluminum-chromium alloy for 5min by the mixer to obtain a mixture B;
step three, dividing the mixture A obtained in the step two into two parts, namely the mixture A 1 And mixture A 2 First, the mixture A is mixed 1 Pouring the mixture into a pressing mold, spreading cloth to form a lower layer, pouring the mixture B into the pressing mold, spreading cloth to form an intermediate layer, and pouring the mixture A 2 Pouring the mixture into a pressing die, paving cloth to form an upper layer, and pressing by adopting an oil press to obtain an electrode block with a single weight of 15kg, wherein the total number of the electrode blocks is 20;
dividing the 20 electrode blocks obtained in the step three into 4 groups, performing assembly welding treatment by adopting copper electrode plasma arc welding of a vacuum welding box, and performing assembly welding by adopting a titanium thin plate at an assembly welding position, wherein 1 electrode rod is obtained by assembly welding of every 5 electrode blocks, and 4 electrode rods are obtained in total; the electrode blocks are arranged in a vacuum welding box and are uniformly and symmetrically placed in the assembly welding treatment process, the clamp is adjusted and tightened, the air leakage rate is tested when the vacuum degree in the vacuum welding box is not more than 3Pa, and the air leakage rate is not more than 2.5 Pa.min -1 Then argon is filled until the pressure is 45kPa, welding is started, the adopted welding current is 320A-370A, and the welding voltage is 50V-70V;
and fifthly, respectively placing the 4 electrode rods obtained in the step four as consumable electrodes in a vacuum consumable arc furnace for primary smelting, wherein a crucible with the diameter phi of 220mm is used for primary smelting, the smelting flow is 5-9 kA, the smelting voltage is 29-32V, the smelting vacuum degree is 1.0-3.0 Pa, 4 primary ingots are obtained, then the heads and tails of the 4 primary ingots are sequentially connected and placed in the vacuum consumable arc furnace for assembly welding to obtain 2 electrodes, the 2 electrodes are subjected to secondary smelting, a crucible with the diameter phi of 280mm is used for secondary smelting, the smelting flow is 5-10 kA, the smelting voltage is 29-33V, the smelting vacuum degree is 0.5-1.6 Pa, 2 secondary ingots are obtained, the heads and tails of the 2 secondary ingots are connected and placed in the vacuum consumable arc furnace for assembly welding to obtain 1 electrode, the three electrodes are smelted, the three electrodes are used for smelting, the crucible with the diameter phi of 360mm is 7-12 kA, the smelting flow is 5-10 kA, the smelting voltage is 3-3.6 Pa, the nominal Ti is 3-32 Pa, and the three-3-13 Pa of the alloy is obtained.
The niobium-titanium-aluminum-based alloy cast ingot prepared in the embodiment is subjected to lathe facing and peeling, then the cast ingot is subjected to middle-section sawing, and chemical components are detected by respectively sampling blocks at the upper part, the middle part and the lower part of the cast ingot, and the result shows that the mass contents of niobium elements at the upper part, the middle part and the lower part of the niobium-titanium-aluminum-based alloy cast ingot are 49.92%, 49.75% and 49.55%, the absolute value of fluctuation deviation of the components is less than 1%, and the uniformity of the components of each alloy is good. Meanwhile, through further detection, the niobium-titanium-aluminum-based alloy cast ingot prepared by the embodiment has no defects of niobium inclusion and the like, and meets the requirement of large-scale industrial production on the uniformity of the component distribution of the niobium-titanium-aluminum-based alloy cast ingot alloy.
The above description is only of the preferred embodiments of the present invention, and is not intended to limit the present invention. Any simple modification, variation and equivalent variation of the above embodiments according to the technical substance of the invention still fall within the scope of the technical solution of the invention.
Claims (5)
1. The preparation method of the niobium-titanium-aluminum-based alloy cast ingot is characterized by comprising the following steps of:
crushing a niobium-titanium cast ingot to obtain niobium-titanium scraps, pickling the niobium-titanium scraps, and then carrying out vacuum annealing treatment to obtain pretreated niobium-titanium scraps; the granularity of the niobium-titanium scraps is 1 mm-3 mm;
step two, mixing part of the pretreated niobium-titanium scraps obtained in the step one with titanium sponge to obtain a mixture A, and mixing the pretreated niobium-titanium scraps obtained in the rest step one with aluminum-niobium alloy and other intermediate alloys to obtain a mixture B; the titanium sponge is 0-grade titanium sponge with granularity of 3-12.7 mm;
step three, taking the mixture A obtained in the step two as an upper layer and a lower layer and taking the mixture B as an intermediate layer to perform cloth in a pressing die, and then performing pressing treatment to obtain an electrode block;
fourthly, performing assembly welding treatment on the electrode block obtained in the third step, and performing repair welding on a titanium sheet at an assembly welding position to obtain an electrode rod;
and fifthly, placing the electrode rod obtained in the step four as a consumable electrode in a vacuum consumable arc furnace for primary smelting to obtain primary ingots, sequentially connecting the heads and the tails of the 4 primary ingots after the flat heads, placing the primary ingots in the vacuum consumable arc furnace for assembly welding to obtain 2 electrodes, carrying out secondary smelting on the 2 electrodes to obtain 2 secondary ingots, connecting the heads and the tails of the 2 secondary ingots after the flat heads, placing the 2 secondary ingots in the vacuum consumable arc furnace for assembly welding to obtain 1 electrode, and carrying out tertiary smelting on the 1 electrode to obtain tertiary ingots, namely niobium-titanium-aluminum-based alloy ingots.
2. The method for producing a niobium-titanium-aluminum-based alloy ingot according to claim 1, wherein the vacuum annealing treatment conditions in the step one are: vacuum degree is less than 5×10 -2 The temperature is 900-950 ℃ under MPa, and the time is more than 60 min.
3. The method for preparing the niobium-titanium-aluminum-based alloy ingot according to claim 1, wherein in the second step, the mixture A is obtained by mixing for 3min by a mixer, and the mixture B is obtained by mixing for 5min by a mixer.
4. The method for producing a niobium-titanium-aluminum-based alloy ingot according to claim 1, wherein the mass of the mixture a of the upper layer and the lower layer in the third step is equal.
5. The method for preparing a niobium-titanium-aluminum-based alloy ingot according to claim 1, wherein the assembly welding treatment in the fourth step is performed by vacuum welding box copper electrode plasma arc welding.
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