CN115780749A - Preparation method of high-molybdenum-equivalent titanium alloy ingot - Google Patents
Preparation method of high-molybdenum-equivalent titanium alloy ingot Download PDFInfo
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Abstract
The invention discloses a preparation method of a high molybdenum equivalent titanium alloy ingot, which is suitable for preparing a titanium alloy ingot with the diameter of more than or equal to phi 600mm and comprises the following steps: step S1: weighing various raw materials with a preset ratio respectively, and screening the raw materials to obtain various raw materials with coarse particle size which do not pass through the sieve pores and various raw materials with fine particle size which pass through the sieve pores; step S2: uniformly mixing various fine-particle-size raw materials for the first time, and preparing 9 electrode rods after uniform mixing; and step S3: uniformly mixing various raw materials with the coarse particle size for the second time, pouring the uniformly mixed raw materials into a die cavity of a hydraulic press, uniformly distributing electrode rods in the die cavity of the hydraulic press, inserting the raw materials with the coarse particle size, and pressing by using the hydraulic press to obtain an electrode block; and step S4: sequentially carrying out assembly welding and smelting processing on each electrode block to obtain a finished product titanium alloy ingot; the invention improves the distribution uniformity of the raw materials and effectively solves the problem that the segregation is easily generated in the smelting process of the high molybdenum equivalent titanium alloy ingot.
Description
Technical Field
The invention belongs to the technical field of titanium alloy, and particularly relates to a preparation method of a high-molybdenum-equivalent titanium alloy ingot.
Background
According to the method for dividing the types of titanium alloys by the equivalent weight of molybdenum, the high molybdenum equivalent weight is mainly represented by beta titanium alloys and alpha + beta two-phase titanium alloys containing Mo, V and Cr such as TC21, TC18 and TC12, and the like, because the types of alloy elements are many and the content is high, the alloys have strong solid solution strengthening and second phase dispersion strengthening effects, so that the alloys have excellent high-temperature creep property, durability and damage tolerance property, the service life and service cycle of an aeroengine structural member can be greatly prolonged, and under the large environment that the aeroengine structural member continuously pursues weight reduction in the aeronautical industry field, the titanium materials have the outstanding advantages in the aspects of light weight, high strength and high temperature resistance, so that the titanium materials can be used in related fields.
The high content of high melting point elements and easy segregation beta stable elements such as Cr, fe, V and the like is the main characteristic of the high molybdenum equivalent titanium alloy material in the aspect of element composition. At present, the alloy is generally produced by adopting a VAR smelting mode, when smelting, the intermediate alloy and the sponge titanium are uniformly mixed and pressed into an electrode block, and the electrode block is melted into an ingot after being welded. Because of the characteristics of the processing technology, the granularity of the intermediate alloy containing Mo, nb and the like is generally below 1mm at present, and the intermediate alloy is easy to cause the following problems during smelting:
1. when the raw materials are mixed and pressed, the raw materials fall to the lower part along the gaps of the raw materials to form a local accumulation layer;
2. the Mo-containing and Nb-containing small-particle intermediate alloy (the particle size is not more than 1 mm) has high melting point, and a local accumulation layer cannot be homogenized through smelting to form local accumulation, so that the macrosegregation of the material is caused, and the material is scrapped. The current commonly adopted preparation method of the electrode by pressing after mixing cannot avoid the problems.
Disclosure of Invention
The invention aims to provide a preparation method of a high molybdenum equivalent titanium alloy ingot, which aims to solve the problem of ingot segregation caused by adding a small-particle-size intermediate alloy, namely, a fine-particle-size raw material is easy to fall into the bottom of an electrode to form local accumulation when the raw material is mixed and an electrode block is pressed, and macro segregation is easy to cause if the local accumulation is not completely melted in the subsequent smelting process.
The invention adopts the following technical scheme: a preparation method of a high molybdenum equivalent titanium alloy ingot is suitable for preparing a titanium alloy ingot with the diameter of more than or equal to phi 600mm, and comprises the following steps:
step S1: weighing various raw materials with a preset ratio respectively, and screening the raw materials by using a screen with the diameter of a screen hole of 3mm to obtain various raw materials with coarse particle size which do not pass through the screen hole and various raw materials with fine particle size which pass through the screen hole;
step S2: uniformly mixing various fine-grained raw materials for the first time, pouring the uniformly mixed raw materials into a semi-continuous electrode extruder to prepare 9 electrode rods;
and step S3: uniformly mixing various raw materials with the coarse particle size for the second time, pouring the uniformly mixed raw materials into a die cavity of a hydraulic machine, uniformly distributing 9 electrode rods in the die cavity of the hydraulic machine, inserting the raw materials with the coarse particle size, and pressing by using the hydraulic machine to obtain an electrode block;
and step S4: and (5) repeating the steps S1-S3 to obtain a preset number of electrode blocks, and sequentially carrying out assembly welding and smelting processing on each electrode block to obtain a finished product of the titanium alloy ingot.
Further, when each electrode rod is inserted, the electrode rod is inserted vertically.
Further, when the electrode rods are distributed, the arrangement method of the electrode rods comprises the following steps:
1 electrode bar is placed at the center of a die cavity of a hydraulic press,
taking 4 electrode rods to be arranged in a surrounding way by taking the central position of a die cavity of the hydraulic press as an axis, leading the connecting line of the 4 electrode rods to be square,
4 electrode rods are respectively arranged at the central position of each side of the square, so that the 9 electrode rods are arranged in a shape like a Chinese character 'mi'.
Further, the blending time of the first blending in the step S2 is 60-90S.
Further, the diameter of the electrode rod is phi 20-50mm.
Further, the blending time of the second blending in the step S3 is 120-180S.
Further, the smelting in the step S4 comprises first smelting, second smelting and third smelting;
the conditions of the first smelting are as follows: the smelting current is 6-9kA, the smelting voltage is 31-33V, the arc stabilizing current is 8-10A, and the alternating current stirring time is 15s;
the conditions of the second smelting are as follows: smelting current is 13-18kA, smelting voltage is 31-33V, arc stabilizing current is 9-12A, and alternating current stirring time is 15s;
the conditions of the third smelting are as follows: the smelting current is 17-22kA, the smelting voltage is 31-33V, the arc stabilizing current is 10-14A, and the alternating current stirring time is 15-30s.
The beneficial effects of the invention are:
on the basis of combining a semi-continuous extrusion method and a traditional mixing process, raw materials are screened according to a preset proportion, fine-grain-size raw materials are mixed firstly, a semi-continuous electrode extruder is used for preparing a cylindrical electrode rod with the diameter of phi 20-50mm, then coarse-grain-size raw materials are mixed and poured into a die cavity of a hydraulic machine, the electrode rod is uniformly inserted into the die cavity of the hydraulic machine for preparing an electrode, and finally, a finished product is obtained through assembly welding and smelting;
the invention can obviously improve the electrode density and the distribution uniformity, is suitable for the production of large-specification homogeneous ingots, densifies the fine-grained raw materials through the electrode extrusion process, effectively avoids the problems of sinking and agglomeration when the small-grained raw materials are dispersed and distributed, and simultaneously adopts the combination of a material mixing and distributing mode to uniformly distribute the extruded electrode rods in the electrode block, thereby improving the distribution uniformity of the raw materials, effectively solving the problem that the high-molybdenum-equivalent titanium alloy ingot is easy to generate segregation in the smelting process and improving the component uniformity;
the invention uses the semi-continuous extruder to extrude the compact electrode bar with small specification, thereby avoiding the falling and accumulation of fine-grained raw materials in the pressing process; inserting electrode rods into the coarse-grain-diameter raw material to form a distribution pattern of the coarse-grain-diameter raw material wrapping the electrode rods at equal intervals; in the smelting process, the peripheral area of the electrode rod is preferentially melted, the wrapped electrode rod is melted by latent heat of crystallization released by the preferentially melted coarse-grain-size raw material, the melting of the coarse-grain-size raw material and the melting of the fine-grain-size raw material tend to be synchronous, metal convection and solute diffusion are more sufficient, and the distribution of alloy elements reaches homogenization, so that the problem that the high-molybdenum-equivalent ingot is easy to segregate is fundamentally solved.
Drawings
FIG. 1 is a top view of the arrangement of electrode rods according to the present invention;
figure 2 is a side view of an electrode rod according to the invention.
Wherein, 1, an electrode bar; 2. a peripheral region.
Detailed Description
The invention is described in detail below with reference to the drawings and the detailed description.
The invention discloses a preparation method of a high molybdenum equivalent titanium alloy ingot, which is suitable for preparing a titanium alloy ingot with the diameter of more than or equal to phi 600 and comprises the following steps:
step S1: weighing various raw materials with the granularity range of 0.83-25.4mm according to a preset proportion, and screening the raw materials by using a screen with the diameter of a screen hole of 3mm to obtain various raw materials with coarse particle size which do not pass through the screen hole and various raw materials with fine particle size which pass through the screen hole, wherein the raw materials at least comprise titanium sponge and aluminum molybdenum.
Step S2: uniformly mixing various fine-grained raw materials for the first time, pouring the uniformly mixed raw materials into a semi-continuous electrode extruder to prepare 9 electrode rods 1, wherein each electrode rod 1 is of a columnar structure; the length of the electrode bar 1 is equal to the height of the die cavity of the hydraulic press.
And step S3: and (2) uniformly mixing various coarse-particle-size raw materials for the second time, pouring the uniformly mixed raw materials into a die cavity of a hydraulic machine, uniformly distributing the electrode rods 1 in the die cavity of the hydraulic machine, inserting the coarse-particle-size raw materials, pressing by using the hydraulic machine to obtain an electrode block, vertically inserting the electrode rods 1 when inserting the electrode rods 1, and further preparing the electrode block with the height equal to the length of the electrode rods 1.
Uniformly laying mixtures of various coarse-particle-size raw materials in a die cavity of a hydraulic machine, sequentially inserting electrode rods 1 into the mixtures of the various coarse-particle-size raw materials and arranging the electrode rods in an array mode, wherein the electrode rods 1 in two adjacent rows are distributed in a staggered mode, namely the electrode rods 1 in two adjacent rows are distributed in a staggered mode, the arrangement mode is shown in figures 1 and 2, and when the electrode rods 1 are distributed, the arrangement method of the electrode rods 1 is as follows: the method comprises the steps of taking 1 electrode rod 1 to be placed at the central position of a die cavity of a hydraulic press, taking 4 electrode rods 1 to be arranged in a surrounding mode by taking the central position of the die cavity of the hydraulic press as an axis, enabling connecting lines of the 4 electrode rods 1 to be square, taking 4 electrode rods 1 to be respectively arranged at the central position of each side of the square, and enabling 9 electrode rods 1 to be arranged in a shape of a Chinese character 'mi'.
In the smelting process, the peripheral area 2 of the electrode rod 1 is preferentially melted, the wrapped electrode rod is melted by latent heat of crystallization released by the preferentially melted coarse-grain-size raw material, the melting of the coarse-grain-size raw material and the melting of the fine-grain-size raw material tend to be synchronous, metal convection and solute diffusion are more sufficient, the distribution of alloy elements reaches homogenization, and the problem that the ingot with high molybdenum equivalent is easy to segregate is fundamentally solved.
And step S4: and (5) repeating the steps S1-S3 to obtain a preset number of electrode blocks, and sequentially carrying out assembly welding and smelting processing on each electrode block to obtain a finished product of the titanium alloy ingot.
During preparation, when various raw materials with a preset proportion are weighed in step S1, a single electrode block can be weighed according to the using amount of the electrode block, 9 electrode rods are prepared in step S2, FIG. 1 shows the arrangement mode of the 9 electrode rods 1, the connecting line of the 8 electrode rods 1 positioned on the edge is square, 1 electrode rod 1 is inserted into the center of the square, 9 electrode rods 1 are inserted into the raw materials with the coarse grain diameter to prepare an electrode block, then the steps S1-S3 are repeated to prepare the electrode blocks with a preset number, and then the electrode blocks are sequentially subjected to assembly welding and smelting processing in step S4 to obtain the finished titanium alloy cast ingot.
Wherein the blending time of the first blending in the step S2 is 60-90S, and the diameter of the electrode rod 1 isPhi is 20-50mm, the diameter of the electrode rods 1 can be adaptively adjusted according to the die cavity area of the hydraulic press, the blending time of the second blending in the step S3 is 120-180S, the distance between the electrode rods 1 can be calculated through a formula, and the calculation formula is as follows: (D) 1 -3D 2 -60)/3, wherein D 1 Is the diagonal length of the die cavity of the hydraulic press, D 2 The diameter of the electrode rod.
Wherein the smelting in the step S4 comprises first smelting, second smelting and third smelting; the conditions of the first smelting are as follows: the smelting current is 6-9kA, the smelting voltage is 31-33V, the arc stabilizing current is 8-10A, and the alternating current stirring time is 15s; the conditions of the second smelting are as follows: smelting current is 13-18kA, smelting voltage is 31-33V, arc stabilizing current is 9-12A, and alternating current stirring time is 15s; the conditions of the third smelting are as follows: the smelting current is 17-22kA, the smelting voltage is 31-33V, the arc stabilizing current is 10-14A, and the alternating current stirring time is 15-30s.
In order to solve the segregation problem, in recent years, a method of grinding and mixing titanium sponge and Mo-containing alloy is reported (patent number: CN 200710188547.9), but the average mixing time of a single electrode block is as long as 1-5h, and the production efficiency is low; meanwhile, some methods start from improving alloy preparation means, and gradually introduce a powder metallurgy method into the preparation of the intermediate alloy, namely, firstly, preparing an intermediate alloy bar by using powder metallurgy (patent number: CN 113322388A), and then crushing the intermediate alloy into a flaky intermediate alloy with moderate granularity (patent number: CN 10527843A), but the powder metallurgy method has high cost and long flow path, and more importantly, the flaky intermediate alloy has light weight and weak bonding capacity with a base alloy during pressing, and is also easy to fall into a molten pool to form local segregation during smelting, so the segregation problem is not solved well.
Example 1
This example describes the preparation method of the present invention in detail by taking TB9 alloy as an example.
Step S1: 79.9kg of titanium sponge with the particle size of 0.83-25.4mm, 6.405kg of aluminum-molybdenum 60 alloy with the particle size of 0-0.5mm, 1.671kg of titanium-molybdenum 32 alloy with the particle size of 0-5mm, 10.5kg of aluminum-vanadium 85 alloy with the particle size of 1-6mm, 4.407kg of sponge zirconium with the particle size of 3-15mm, 6.545kg of metal chromium with the particle size of 1-3mm and 0.5712kg of ferrotitanium 32 alloy with the particle size of 3-6mm are weighed, and various raw materials are screened by using a screen with the screen mesh of 3mm to obtain a coarse-particle-size raw material and a fine-particle-size raw material.
Step S2: weighing various fine-grained raw materials, uniformly mixing for the first time for 70s, and pouring the mixture into a semi-continuous electrode extruder to prepare 9 electrode rods 1 with the diameter of phi 35mm and the length of 275 mm.
And step S3: weighing various coarse-particle-size raw materials, uniformly mixing for the second time, pouring into a 3500T hydraulic press die cavity, uniformly distributing the electrode rods 1 in the hydraulic press die cavity, inserting the coarse-particle-size raw materials, wherein the interval between the electrode rods 1 is 131mm, and pressing by using a hydraulic press to obtain electrode blocks with the specification of phi 560X 275mm; the above steps are repeated for 14 times to obtain 14 electrode blocks.
And step S4: welding, smelting and processing the electrode block according to a 1 x 14 assembly to obtain a finished product titanium alloy ingot, wherein the smelting comprises first smelting, second smelting and third smelting, and the conditions of the first smelting are as follows: the smelting current is 9kA, the smelting voltage is 31-33V, the arc stabilizing current is 10A, and the alternating-current stirring time is 15s; the conditions of the second smelting are as follows: the smelting current is 18kA, the smelting voltage is 31-33V, the arc stabilizing current is 12A, and the alternating current stirring time is 15s; the conditions of the third smelting are as follows: the smelting current is 22kA, the smelting voltage is 31-33V, the arc stabilizing current is 14A, and the alternating-current stirring time is 15s.
After the product prepared in this example was turned over and scalped by a lathe, chip-like samples were taken from the head of the ingot and from the upper, middle, and lower parts, respectively, and subjected to composition analysis, the composition analysis results being shown in table 1:
main element composition of TB9 alloy prepared in Table 1
Example 2
This example describes the preparation method of the present invention in detail by taking the TC12 alloy as an example. The preparation method of this example is the same as example 1, except that:
weighing 91.8kg of titanium sponge with the particle size of 0.83-25.4mm, 2.573kg of sponge with the particle size of 3-15mm, 3.132kg of titanium-tin 80 alloy with the particle size of 0-5mm, 6.331kg of aluminum-molybdenum 60 alloy with the particle size of 0-0.5mm, 1.872kg of aluminum-niobium 60 alloy with the particle size of 0-1.2mm, 4.699kg of chromium sheets with the particle size of 1-3mm, 2.366kg of aluminum beans with the particle size of 3-18mm in the step S1, and selecting a screen with a 3mm mesh;
the blending time for the first blending in the step S2 is 90S; the diameter of the prepared electrode rod 1 is phi 20mm, and the length is 275mm;
the blending time of the second blending in the step S3 is 150S; the spacing between the electrode rods 1 was 123mm, and electrode blocks having a specification of phi 490 x 275mm were prepared.
In step S4, the melting conditions are different: the smelting current in the first smelting is 7kA, the arc stabilizing current is 8A, the smelting current in the second smelting is 15 kA, the arc stabilizing current is 9A, the smelting current in the third smelting is 19 kA, and the arc stabilizing current is 12A.
After the product prepared in this example was turned over and scalped by a lathe, chip-like samples were taken from the head of the ingot and from the upper, middle, and lower parts, respectively, and subjected to composition analysis, the composition analysis results being shown in table 2:
table 2 preparation of main element composition of TC12 alloy
Example 3
This example illustrates the preparation method of the present invention in detail by taking the TC18 alloy as an example, and the preparation method of this example is the same as that of example 1, except that:
weighing 96.5kg of sponge titanium with the particle size of 0.83-25.4mm, 1.204kg of chromium sheets with the particle size of 1-6mm, 9.808kg of aluminum-molybdenum 60 alloy with the particle size of 0-0.5mm, 3.682kg of aluminum-vanadium 85 alloy with the particle size of 1-6mm and 1.666kg of aluminum beans with the particle size of 3-18mm in the step S1, and selecting a screen with a 3mm mesh;
the blending time for the first blending in the step S2 is 60S; the diameter of the prepared electrode rod 1 is phi 50mm, and the length is 275mm;
the blending time of the second blending in the step S3 is 120S; the interval between the electrode rods 1 was 143mm, and electrode blocks having a size of phi 640 x 275mm were prepared.
In step S4, the melting conditions are different: the smelting current in the first smelting is 6kA, the arc stabilizing current is 8A, the smelting current in the second smelting is 13kA and the arc stabilizing current is 10A, the smelting current in the third smelting is 17 kA and the arc stabilizing current is 10A, and the alternating-current stirring time is 30s.
After the product prepared in this example was turned over and scalped, chip-like samples were taken from the head of the ingot and from the upper, middle, lower, and lower parts, respectively, and subjected to component analysis, the results of which are shown in table 3:
main element composition of TC18 alloy prepared in Table 3
In examples 1 to 3, the difference between the obtained main elements of the ingots and the ingot is not more than 0.15wt.%, and the uniformity of the components is good, which indicates that the method is practical and feasible and can be used for preparing homogenized high molybdenum equivalent titanium alloy ingots.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent replacements, improvements, etc. within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. A preparation method of a high molybdenum equivalent titanium alloy ingot is characterized in that the preparation method is suitable for preparing a titanium alloy ingot with the diameter of more than or equal to phi 600mm and comprises the following steps:
step S1: weighing various raw materials with a preset ratio respectively, and screening the raw materials by using a screen with the diameter of a screen hole of 3mm to obtain various raw materials with coarse particle size which do not pass through the screen hole and various raw materials with fine particle size which pass through the screen hole;
step S2: uniformly mixing various fine-grained raw materials for the first time, pouring the uniformly mixed raw materials into a semi-continuous electrode extruder to prepare 9 electrode rods (1);
and step S3: uniformly mixing various raw materials with the coarse particle size for the second time, pouring the uniformly mixed raw materials into a die cavity of a hydraulic machine, uniformly distributing 9 electrode rods (1) in the die cavity of the hydraulic machine, inserting the raw materials with the coarse particle size, and pressing by using the hydraulic machine to obtain an electrode block;
and step S4: and (5) repeating the steps S1-S3 to obtain a preset number of electrode blocks, and sequentially carrying out assembly welding and smelting processing on each electrode block to obtain a finished product of the titanium alloy ingot.
2. A method for producing a high molybdenum equivalent titanium alloy ingot according to claim 1, wherein the electrode rods (1) are inserted vertically while inserting each of the electrode rods (1).
3. The method for preparing a high molybdenum equivalent titanium alloy ingot according to claim 1, wherein the electrode rods (1) are arranged by the following method when the electrode rods (1) are distributed:
1 electrode bar (1) is placed at the central position of a die cavity of a hydraulic press,
taking 4 electrode rods (1) to be arranged in a surrounding way by taking the central position of a die cavity of a hydraulic press as an axis, leading the connecting line of the 4 electrode rods (1) to be square,
4 electrode rods (1) are respectively arranged at the central position of each side of the square, so that the 9 electrode rods (1) are arranged in a shape like a Chinese character 'mi'.
4. The method for preparing the high molybdenum equivalent titanium alloy ingot according to claim 2 or 3, wherein the blending time of the first blending in the step S2 is 60-90S.
5. The method for preparing a high molybdenum equivalent titanium alloy ingot according to claim 4, wherein the diameter of the electrode rod (1) is phi 20-50mm.
6. The method for preparing the titanium alloy ingot with the high molybdenum equivalent weight according to claim 5, wherein the blending time of the second blending in the step S3 is 120-180S.
7. The method for preparing the titanium alloy ingot with the high molybdenum equivalent weight according to claim 6, wherein the smelting in the step S4 comprises first smelting, second smelting and third smelting;
the conditions of the first smelting are as follows: the smelting current is 6-9kA, the smelting voltage is 31-33V, the arc stabilizing current is 8-10A, and the alternating current stirring time is 15s;
the conditions of the second smelting are as follows: the smelting current is 13-18kA, the smelting voltage is 31-33V, the arc stabilizing current is 9-12A, and the alternating current stirring time is 15s;
the conditions of the third smelting are as follows: the smelting current is 17-22kA, the smelting voltage is 31-33V, the arc stabilizing current is 10-14A, and the alternating current stirring time is 15-30s.
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