CN112725658A - Preparation method of titanium-aluminum alloy target - Google Patents
Preparation method of titanium-aluminum alloy target Download PDFInfo
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- CN112725658A CN112725658A CN202011432732.XA CN202011432732A CN112725658A CN 112725658 A CN112725658 A CN 112725658A CN 202011432732 A CN202011432732 A CN 202011432732A CN 112725658 A CN112725658 A CN 112725658A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C14/00—Alloys based on titanium
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/16—Both compacting and sintering in successive or repeated steps
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/045—Alloys based on refractory metals
- C22C1/0458—Alloys based on titanium, zirconium or hafnium
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Abstract
The invention discloses a preparation method of a titanium-aluminum alloy target, which comprises the following steps: weighing a titanium raw material and an aluminum raw material, dividing the titanium raw material into a first titanium raw material and a second titanium raw material, and dividing the aluminum raw material into a first aluminum raw material and a second aluminum raw material; placing a first titanium raw material and a first aluminum raw material into a water-cooled copper crucible to be smelted to obtain a first melt; cooling the first melt to obtain a first ingot; placing the first ingot at the bottom of a water-cooled copper crucible, and adding a second titanium raw material and a second aluminum raw material to carry out smelting to obtain a second melt; cooling the second melt to obtain a second ingot; heating the second cast ingot to be completely melted, refining, and quickly casting to obtain a target blank; sequentially carrying out canning, degassing and hot isostatic pressing treatment on the target blank, and finally sintering to obtain a sintered body; and taking out the sintered body, wrapping and machining to obtain the titanium-aluminum alloy target. The invention adopts a step-by-step smelting mode, and can solve the technical problems of a large amount of shrinkage cavities, looseness and the like in the titanium-aluminum alloy target material preparation in the prior art.
Description
Technical Field
The invention relates to the technical field of preparation of high-performance targets, in particular to a preparation method of a titanium-aluminum alloy target.
Background
The titanium-aluminum alloy target is mainly applied to the industry of cutter coatings, and the target is generally manufactured by adopting a smelting, hot pressing or isostatic pressing method, wherein the smelted target has better alloying, the hot pressing target has lower cost but low density, and the hot pressing target has the advantages of high density and batch production. In the using process of the target material, reactive sputtering is generally carried out in the environment of nitrogen, acetylene and other gases to form a coating. Titanium aluminum N, CrN, titanium aluminum CrN are new hard coating materials developed in recent years. Titanium aluminum N coated blades are commercially available. The chemical stability and the oxidation and wear resistance of the titanium N coating are good, and the service life of a cutter processed by the titanium N coating is 3-4 times longer than that of a cutter processed by the titanium N coating. In addition, if the titanium aluminum N coating has an appropriate aluminum concentration, a hard inert protective film is formed at the interface between the rake face of the tool and the chip during cutting, and the film has good heat insulation and can be used more effectively for high-speed cutting.
The titanium-aluminum alloy target is generally prepared by a vacuum melting technology, but the production efficiency is low in the preparation process. And the density and melting point difference of the two elements of titanium and aluminum are very large, so that it is very difficult to prepare alloy with uniform components, the titanium-aluminum alloy target material prepared by the prior art has non-uniform components and high cost, and the titanium-aluminum alloy target material has the defects of a large amount of shrinkage cavities, looseness and the like. The titanium-aluminum alloy target prepared by the prior art still has defects, and a large amount of shrinkage cavities, looseness and other defects exist in an alloy cast ingot, so that the use and development of the titanium-aluminum alloy target are seriously restricted.
For the preparation of the titanium-aluminum alloy target, powder metallurgy is also adopted in the prior art, and the titanium-aluminum alloy target is prepared by adopting the powder metallurgy, so that although the uniformity of the target can be well ensured and the forming can be realized, the defects still exist.
On one hand, the oxygen content in the target material is easy to increase due to the long-time powder mixing, and the titanium and the aluminum have larger melting point difference, and can form various metal compounds according to a titanium-aluminum alloy phase diagram, so that the complete reaction between simple substance titanium and aluminum is difficult to ensure and a completely alloyed titanium-aluminum phase is obtained in the sintering process. The Mujiangang et al researches the structure of the completely alloyed and completely unalloyed titanium-aluminum target material in the text of 'the influence of the phase structure of the titanium-aluminum target material on the structure and the performance of the coating', and the hardness of the deposited coating of the completely alloyed target is 3GPa higher than that of the completely unalloyed target material.
On the other hand, for the titanium-aluminum alloy target material, the component ratio of titanium to aluminum is close to 1:1, so that the titanium-aluminum alloy target material with high purity is difficult to prepare through simple mixing and reshaping of titanium powder and aluminum powder. The titanium-aluminum alloy target is a metal material in the semiconductor sputtering target, and the preparation method has certain defects along with the increasing requirement of the semiconductor target on the purity of the raw material.
In view of the defects of the prior art, a preparation method of a titanium-aluminum alloy target material, which can effectively solve the problems of uneven components and low purity of the alloy target material, is urgently needed in the industry.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of a titanium-aluminum alloy target.
In order to achieve the purpose, the invention adopts the following technical scheme.
The invention provides a preparation method of a titanium-aluminum alloy target, which comprises the following steps:
weighing and proportioning: weighing a titanium raw material and an aluminum raw material according to a ratio required by a titanium-aluminum alloy target material, dividing the titanium raw material into a first titanium raw material and a second titanium raw material, and dividing the aluminum raw material into a first aluminum raw material and a second aluminum raw material;
primary smelting: placing the first titanium raw material and the first aluminum raw material in a water-cooled copper crucible, vacuumizing, feeding electricity for heating, and smelting to obtain a first titanium-aluminum alloy melt;
primary cooling: cooling the first titanium-aluminum alloy melt to room temperature to obtain a first titanium-aluminum alloy ingot;
secondary smelting: placing the first titanium-aluminum alloy cast ingot at the bottom of a water-cooled copper crucible, adding a second titanium raw material and a second aluminum raw material, and repeatedly smelting according to the smelting step of one-time smelting to obtain a second titanium-aluminum alloy melt;
secondary cooling: cooling the second titanium-aluminum alloy melt to room temperature to obtain a second titanium-aluminum alloy cast ingot;
casting and molding: heating the second titanium-aluminum alloy cast ingot to be completely melted, refining, and quickly casting the second titanium-aluminum alloy cast ingot onto a water-cooling copper chassis to obtain a titanium-aluminum alloy target blank;
sintering treatment: sequentially carrying out canning, degassing and hot isostatic pressing treatment on the titanium-aluminum alloy target blank, finally sintering to obtain a titanium-aluminum alloy sintered body, and carrying out annealing treatment on the titanium-aluminum alloy sintered body;
and (3) processing and forming: and taking out the titanium-aluminum alloy sintered body, wrapping, and then machining to obtain the titanium-aluminum alloy target.
As a further improvement of the invention, the step of primary smelting specifically comprises the following steps: placing the first titanium raw material and the first aluminum raw material in a water-cooled copper crucible, placing the first aluminum raw material below the first titanium raw material, and vacuumizing the crucible to (1-3) x 10-2And (3) filling an inert atmosphere after the Pa furnace washing, vacuumizing to 0.06-0.12 Pa, and smelting in a mode of slowly increasing the smelting power at a power-increasing speed of 30-50 kw/min until the temperature is increased to 1520-1660 ℃, wherein the smelting duration is 6-10 min, and obtaining a first titanium-aluminum alloy melt after smelting.
As a further improvement of the present invention, the step of primary cooling specifically comprises: and cooling the crucible to room temperature at the speed of 50-100 ℃/min, and removing the pressure after cooling the temperature to the room temperature to obtain the first titanium-aluminum alloy cast ingot.
As a further improvement of the invention, the step of casting molding specifically comprises: and heating the second titanium-aluminum alloy ingot to 1480-1560 ℃, completely melting the second titanium-aluminum alloy ingot, refining for 4-8 min, and casting the second titanium-aluminum alloy ingot onto a water-cooled copper chassis within 3-8S after refining is finished to obtain a titanium-aluminum alloy target blank.
As a further improvement of the invention, in the casting and forming process, the water temperature below the water-cooled copper base plate is 8-12 ℃, and the water pressure is 0.24-0.28 Mpa.
As a further improvement of the invention, in the hot isostatic pressing process, the temperature is 1000-1100 ℃, the pressure is 150-300 MPa, and the heat preservation and pressure maintaining time is 4-6 h.
As a further improvement of the present invention, the degassing in the step is specifically: placing the mixture in a vacuum degassing furnace, and degassing for 2-3 hours at the temperature of 150-250 ℃.
As a further improvement of the invention, the first titanium raw material and the second titanium raw material do not exceed 60 wt% of the total amount of the titanium raw materials, and the first aluminum raw material and the second aluminum raw material do not exceed 60 wt% of the total amount of the aluminum raw materials.
As a further improvement of the invention, the mass ratio of the titanium raw material to the aluminum raw material in the weighed materials is 16:9 to 32: 9.
As a further improvement of the invention, the titanium raw material is granular or blocky metal titanium with the purity of more than 5N and the grain diameter of 1-5 mm, and the aluminum raw material is granular or blocky metal aluminum with the purity of more than 5N and the grain diameter of 1-10 mm.
According to the characteristic that the melting points of 2 metals of titanium and aluminum are different, a titanium raw material and an aluminum raw material are smelted in batches, so that the alloy target can be smelted to be completely alloyed, the prepared high-purity titanium-aluminum alloy target has excellent performance, can meet various application requirements, and solves the technical problem that alloy phase splitting is caused when the titanium-aluminum alloy target is prepared in the prior art.
Detailed Description
The technical solutions will be described clearly and completely in the following with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a preparation method of a titanium-aluminum alloy target, which comprises the following steps:
weighing and proportioning: the method comprises the steps of weighing a titanium raw material and an aluminum raw material according to the required proportion of a titanium-aluminum alloy target material, dividing the titanium raw material into a first titanium raw material and a second titanium raw material, and dividing the aluminum raw material into a first aluminum raw material and a second aluminum raw material.
According to the melting point and density difference between the titanium and the aluminum, the invention adopts a step-by-step smelting mode to carry out smelting in order to avoid incomplete smelting or component segregation.
Primary smelting: and placing the first titanium raw material and the first aluminum raw material in a water-cooled copper crucible, vacuumizing, electrically heating, and smelting to obtain a first titanium-aluminum alloy melt.
In the process of preparing the titanium-aluminum alloy target material, the weight ratio of the titanium raw material to the aluminum raw material in the weighed materials is 16: 9-32: 9, the titanium raw material is granular or blocky metal titanium with the purity of more than 5N and the grain diameter of 1-5 mm, the aluminum raw material is granular or blocky metal aluminum with the purity of more than 5N and the grain diameter of 1-10 mm, the first titanium raw material and the second titanium raw material do not exceed 60 wt% of the total amount of the titanium raw material, and the first aluminum raw material and the second aluminum raw material do not exceed 60 wt% of the total amount of the aluminum raw material.
In some embodiments of the present invention, the primary smelting may further specifically be: placing a first titanium raw material and a first aluminum raw material in a water-cooled copper crucible, placing the first aluminum raw material below the first titanium raw material, and vacuumizing the crucible to (1-3) x 10-2And (3) filling an inert atmosphere after the Pa furnace washing, and finally vacuumizing to 0.06-0.12 Pa, wherein the purpose of vacuumizing is to inhibit volatilization of metal and avoid component loss, smelting is carried out in a mode of slowly increasing the smelting power at a power-increasing speed of 30-50 kw/min until the temperature is increased to 1520-1660 ℃, the smelting duration is 6-10 min, and the first titanium-aluminum alloy melt is obtained after smelting.
Primary cooling: and cooling the first titanium-aluminum alloy melt to room temperature to obtain a first titanium-aluminum alloy ingot.
In the process of preparing the titanium-aluminum alloy target, the crucible is cooled to room temperature at the speed of 50-100 ℃/min, the pressure is removed after the temperature is reduced to the room temperature, a first titanium-aluminum alloy ingot is obtained, the temperature is greatly reduced, the situation that metal is not completely melted occurs, and the alloy composition segregation can be avoided by slowly cooling.
Secondary smelting: and placing the first titanium-aluminum alloy ingot at the bottom of the water-cooled copper crucible, adding a second titanium raw material and a second aluminum raw material, and repeatedly smelting according to the smelting steps of one-time smelting to obtain a second titanium-aluminum alloy melt.
After cooling to obtain a first titanium-aluminum alloy ingot, carrying out secondary smelting according to the primary smelting step to obtain a second titanium-aluminum alloy melt; according to the requirement, a third titanium raw material and a third aluminum raw material can be continuously added, further, a fourth titanium raw material and a fourth aluminum raw material can be added, the amount of the added titanium raw material and the amount of the added aluminum raw material can be the same or different, the amount of the added titanium raw material does not exceed 60 wt% of the total amount of the titanium raw material, the amount of the added aluminum raw material does not exceed 60 wt% of the total amount of the aluminum raw material, and the third titanium-aluminum alloy melt is obtained by smelting according to the smelting steps; the titanium raw material and the aluminum raw material are added step by step, the smelting times are not particularly limited, relevant parameters of each smelting are adjusted according to actual needs, and the details are not repeated in the application. The inert atmosphere can be argon, helium or nitrogen, in a specific embodiment, the inert atmosphere is argon, and the purity is more than or equal to 99.999%.
Secondary cooling: and cooling the second titanium-aluminum alloy melt to room temperature to obtain a second titanium-aluminum alloy cast ingot.
Casting and molding: and heating the second titanium-aluminum alloy cast ingot to be completely melted, refining, and quickly casting the second titanium-aluminum alloy cast ingot onto a water-cooling copper chassis to obtain a titanium-aluminum alloy target blank.
In some embodiments of the present invention, the step of cast molding may further be embodied as: and heating the second titanium-aluminum alloy ingot to 1480-1560 ℃, completely melting the second titanium-aluminum alloy ingot, refining for 4-8 min, casting the second titanium-aluminum alloy ingot onto a water-cooled copper chassis within 3-8S after refining is finished, controlling the water temperature below the water-cooled copper chassis to be 8-12 ℃ and the water pressure to be 0.24-0.28 Mpa, and obtaining the titanium-aluminum alloy target blank after casting.
Sintering treatment: sequentially carrying out canning, degassing and hot isostatic pressing on the titanium-aluminum alloy target blank, finally sintering to obtain a titanium-aluminum alloy sintered body, and carrying out annealing treatment on the titanium-aluminum alloy sintered body.
In some embodiments of the present invention, in the hot isostatic pressing process, the temperature is 1000 to 1100 ℃, the pressure is 150 to 300MPa, and the heat and pressure maintaining time is 4 to 6 hours. The degassing step specifically comprises: placing the mixture in a vacuum degassing furnace, and degassing for 2-3 hours at the temperature of 150-250 ℃. The degassing function is to remove water vapor existing in the target material, the hot isostatic pressing can eliminate the casting defect in the titanium-aluminum target material, the obtained crystal grains are in an ellipsoidal shape, and the target material size can be freely controlled without being influenced by the size of a hot pressing die.
And (3) processing and forming: and taking out the titanium-aluminum alloy sintered body, wrapping, and then machining to obtain the titanium-aluminum alloy target.
For further understanding of the present invention, the method and effects of the present invention will be described in further detail with reference to specific examples. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1.
(1) Weighing and proportioning: weighing a titanium raw material and an aluminum raw material according to a mass ratio of the titanium raw material to the aluminum raw material of 16:9, dividing the titanium raw material into a first titanium raw material and a second titanium raw material, and dividing the aluminum raw material into a first aluminum raw material and a second aluminum raw material, wherein the first titanium raw material accounts for 50 wt% of the total amount of the titanium raw material, the second titanium raw material accounts for 50 wt% of the total amount of the titanium raw material, the first aluminum raw material accounts for 50 wt% of the total amount of the aluminum raw material, and the second aluminum raw material accounts for 50 wt% of the total amount of the aluminum raw material;
(2) primary smelting: placing a first titanium raw material and a first aluminum raw material in a water-cooled copper crucible, placing the first aluminum raw material below the first titanium raw material, and vacuumizing the crucible to 1 x 10-2Filling an inert atmosphere after the Pa furnace washing, finally vacuumizing to 0.06Pa, and smelting in a mode of slowly increasing the smelting power at a power-increasing speed of 30kw/min until the temperature is increased to 1540 ℃, wherein the smelting duration is 8min, and obtaining a first titanium-aluminum alloy melt after smelting;
(3) primary cooling: cooling the crucible to room temperature at the speed of 60 ℃/min, and removing the pressure after the temperature is reduced to the room temperature to obtain a first titanium-aluminum alloy cast ingot;
(4) secondary smelting: placing the first titanium-aluminum alloy ingot at the bottom of a water-cooled copper crucible, adding a second titanium raw material and a second aluminum raw material, and repeatedly smelting according to the smelting steps of one-time smelting to obtain a second titanium-aluminum alloy melt;
(5) secondary cooling: cooling the second titanium-aluminum alloy melt to room temperature at the speed of 60 ℃/min, and removing the pressure after the temperature is reduced to the room temperature to obtain a second titanium-aluminum alloy cast ingot;
(6) casting and molding: heating the second titanium-aluminum alloy cast ingot to 1500 ℃, refining for 5min after the second titanium-aluminum alloy cast ingot is completely melted, and casting the second titanium-aluminum alloy cast ingot on a water-cooling copper base plate in 5S after refining is finished, wherein the water temperature under the water-cooling copper base plate is 8 ℃, the water pressure is 0.24Mpa, and a titanium-aluminum alloy target blank is obtained after casting is finished;
(7) sintering treatment: sequentially sheathing and then placing the titanium-aluminum alloy target blank in a vacuum degassing furnace, degassing for 2h at the temperature of 175 ℃, then performing hot isostatic pressing treatment, wherein the temperature is 1000 ℃, the pressure is 175MPa, the heat preservation and pressure maintaining time is 4h in the hot isostatic pressing process, finally sintering to obtain a titanium-aluminum alloy sintered body, and annealing the titanium-aluminum alloy sintered body;
(8) and (3) processing and forming: and taking out the titanium-aluminum alloy sintered body, wrapping, and then machining to obtain the titanium-aluminum alloy target.
The obtained titanium-aluminum alloy target material is tested, the component deviation of the titanium-aluminum alloy target material is less than +/-0.5 wt%, the purity is greater than 4N, the relative density is greater than 99%, and the average grain size is less than 100 mu m.
Example 2.
(1) Weighing and proportioning: weighing a titanium raw material and an aluminum raw material according to a mass ratio of the titanium raw material to the aluminum raw material of 32:9, dividing the titanium raw material into a first titanium raw material and a second titanium raw material, and dividing the aluminum raw material into a first aluminum raw material and a second aluminum raw material, wherein the first titanium raw material accounts for 60 wt% of the total amount of the titanium raw material, the second titanium raw material accounts for 40 wt% of the total amount of the titanium raw material, the first aluminum raw material accounts for 40 wt% of the total amount of the aluminum raw material, and the second aluminum raw material accounts for 60 wt% of the total amount of the aluminum raw material;
(2) primary smelting: placing a first titanium raw material and a first aluminum raw material in a water-cooled copper crucible, placing the first aluminum raw material below the first titanium raw material, and vacuumizing the crucible to 2 x 10-2After the Pa furnace washing, theFilling inert atmosphere, finally vacuumizing to 0.08Pa, and smelting in a mode of slowly increasing the smelting power at a power-increasing speed of 40kw/min until the temperature is increased to 1600 ℃, wherein the smelting duration is 6min, and obtaining a first titanium-aluminum alloy melt after smelting;
(3) primary cooling: cooling the crucible to room temperature at the speed of 50 ℃/min, and removing the pressure after the temperature is reduced to the room temperature to obtain a first titanium-aluminum alloy cast ingot;
(4) secondary smelting: placing the first titanium-aluminum alloy ingot at the bottom of a water-cooled copper crucible, adding a second titanium raw material and a second aluminum raw material, and repeatedly smelting according to the smelting steps of one-time smelting to obtain a second titanium-aluminum alloy melt;
(5) secondary cooling: cooling the second titanium-aluminum alloy melt to room temperature at the speed of 60 ℃/min, and removing the pressure after the temperature is reduced to the room temperature to obtain a second titanium-aluminum alloy cast ingot;
(6) casting and molding: heating the second titanium-aluminum alloy ingot to 1480 ℃, completely melting the second titanium-aluminum alloy ingot, refining for 6min, and casting the second titanium-aluminum alloy ingot onto a water-cooled copper chassis within 4S after refining, wherein the water temperature under the water-cooled copper chassis is 10 ℃, the water pressure is 0.26Mpa, and a titanium-aluminum alloy target blank is obtained after casting;
(7) sintering treatment: sequentially canning and then placing the titanium-aluminum alloy target blank in a vacuum degassing furnace, degassing for 3h at the temperature of 200 ℃, then performing hot isostatic pressing treatment, wherein the temperature is 1050 ℃, the pressure is 150MPa and the heat preservation and pressure maintaining time is 6h in the hot isostatic pressing process, finally sintering to obtain a titanium-aluminum alloy sintered body, and annealing the titanium-aluminum alloy sintered body;
(8) and (3) processing and forming: and taking out the titanium-aluminum alloy sintered body, wrapping, and then machining to obtain the titanium-aluminum alloy target.
The obtained titanium-aluminum alloy target material is tested, the component deviation of the titanium-aluminum alloy target material is less than +/-0.5 wt%, the purity is greater than 4.5N, the relative density is greater than 99%, and the average grain size is less than 100 mu m.
Example 3.
(1) Weighing and proportioning: weighing a titanium raw material and an aluminum raw material according to a mass ratio of the titanium raw material to the aluminum raw material of 20:9, dividing the titanium raw material into a first titanium raw material and a second titanium raw material, and dividing the aluminum raw material into a first aluminum raw material and a second aluminum raw material, wherein the first titanium raw material accounts for 55 wt% of the total amount of the titanium raw material, the second titanium raw material accounts for 45 wt% of the total amount of the titanium raw material, the first aluminum raw material accounts for 55 wt% of the total amount of the aluminum raw material, and the second aluminum raw material accounts for 45 wt% of the total amount of the aluminum raw material;
(2) primary smelting: placing a first titanium raw material and a first aluminum raw material in a water-cooled copper crucible, placing the first aluminum raw material below the first titanium raw material, and vacuumizing the crucible to 3 x 10-2Filling an inert atmosphere after the Pa furnace washing, finally vacuumizing to 0.12Pa, and smelting in a mode of slowly increasing the smelting power at a power-increasing speed of 50kw/min until the temperature is increased to 1560 ℃, wherein the smelting duration is 6min, and obtaining a first titanium-aluminum alloy melt after smelting;
(3) primary cooling: cooling the crucible to room temperature at the speed of 100 ℃/min, and removing the pressure after the temperature is reduced to the room temperature to obtain a first titanium-aluminum alloy cast ingot;
(4) secondary smelting: placing the first titanium-aluminum alloy ingot at the bottom of a water-cooled copper crucible, adding a second titanium raw material and a second aluminum raw material, and repeatedly smelting according to the smelting steps of one-time smelting to obtain a second titanium-aluminum alloy melt;
(5) secondary cooling: cooling the second titanium-aluminum alloy melt to room temperature at the speed of 60 ℃/min, and removing the pressure after the temperature is reduced to the room temperature to obtain a second titanium-aluminum alloy cast ingot;
(6) casting and molding: heating the second titanium-aluminum alloy ingot to 1480 ℃, completely melting the second titanium-aluminum alloy ingot, refining for 8min, and casting the second titanium-aluminum alloy ingot onto a water-cooled copper chassis within 8S after refining, wherein the water temperature under the water-cooled copper chassis is 12 ℃, the water pressure is 0.28Mpa, and a titanium-aluminum alloy target blank is obtained after casting;
(7) sintering treatment: sequentially canning and then placing the titanium-aluminum alloy target blank in a vacuum degassing furnace, degassing for 2.5 hours at the temperature of 250 ℃, then performing hot isostatic pressing treatment, wherein the temperature is 1100 ℃, the pressure is 300MPa, the heat preservation and pressure maintaining time is 5 hours in the hot isostatic pressing process, finally sintering to obtain a titanium-aluminum alloy sintered body, and annealing the titanium-aluminum alloy sintered body;
(8) and (3) processing and forming: and taking out the titanium-aluminum alloy sintered body, wrapping, and then machining to obtain the titanium-aluminum alloy target.
The obtained titanium-aluminum alloy target material is tested, the component deviation of the titanium-aluminum alloy target material is less than +/-0.5 wt%, the purity is greater than 4.5N, the relative density is greater than 99%, and the average grain size is less than 100 mu m.
According to the characteristic that the melting points of 2 metals of titanium and aluminum are different, a titanium raw material and an aluminum raw material are smelted in batches, so that the alloy target can be smelted to be completely alloyed, the prepared high-purity titanium-aluminum alloy target has excellent performance, can meet various application requirements, and solves the technical problem that alloy phase splitting is caused when the titanium-aluminum alloy target is prepared in the prior art.
Although the preferred embodiments of the present invention have been disclosed for illustrative purposes, those skilled in the art will appreciate that various modifications, additions and substitutions are possible, without departing from the scope and spirit of the invention as disclosed in the accompanying claims.
Claims (10)
1. The preparation method of the titanium-aluminum alloy target is characterized by comprising the following steps:
s1, weighing and proportioning: weighing a titanium raw material and an aluminum raw material according to a ratio required by a titanium-aluminum alloy target material, dividing the titanium raw material into a first titanium raw material and a second titanium raw material, and dividing the aluminum raw material into a first aluminum raw material and a second aluminum raw material;
s2, primary smelting: placing the first titanium raw material and the first aluminum raw material in a water-cooled copper crucible, vacuumizing, feeding electricity for heating, and smelting to obtain a first titanium-aluminum alloy melt;
s3, primary cooling: cooling the first titanium-aluminum alloy melt to room temperature to obtain a first titanium-aluminum alloy ingot;
s4, secondary smelting: placing the first titanium-aluminum alloy cast ingot at the bottom of a water-cooled copper crucible, adding a second titanium raw material and a second aluminum raw material, and repeatedly smelting according to the smelting step of one-time smelting to obtain a second titanium-aluminum alloy melt;
s5, secondary cooling: cooling the second titanium-aluminum alloy melt to room temperature to obtain a second titanium-aluminum alloy cast ingot;
s6, casting and forming: heating the second titanium-aluminum alloy cast ingot to be completely melted, refining, and quickly casting the second titanium-aluminum alloy cast ingot onto a water-cooling copper chassis to obtain a titanium-aluminum alloy target blank;
s7, sintering treatment: sequentially carrying out canning, degassing and hot isostatic pressing treatment on the titanium-aluminum alloy target blank, finally sintering to obtain a titanium-aluminum alloy sintered body, and carrying out annealing treatment on the titanium-aluminum alloy sintered body;
s8, processing and forming: and taking out the titanium-aluminum alloy sintered body, wrapping, and then machining to obtain the titanium-aluminum alloy target.
2. The method according to claim 1, wherein the step of primary smelting is specifically as follows: placing the first titanium raw material and the first aluminum raw material in a water-cooled copper crucible, placing the first aluminum raw material below the first titanium raw material, and vacuumizing the crucible to (1-3) x 10-2And (3) filling an inert atmosphere after the Pa furnace washing, vacuumizing to 0.06-0.12 Pa, and smelting in a mode of slowly increasing the smelting power at a power-increasing speed of 30-50 kw/min until the temperature is increased to 1520-1660 ℃, wherein the smelting duration is 6-10 min, and obtaining a first titanium-aluminum alloy melt after smelting.
3. The method according to claim 1, wherein the step of primary cooling is specifically as follows: and cooling the crucible to room temperature at the speed of 50-100 ℃/min, and removing the pressure after cooling the temperature to the room temperature to obtain the first titanium-aluminum alloy cast ingot.
4. The method according to claim 1, wherein the step of casting molding is specifically as follows: and heating the second titanium-aluminum alloy ingot to 1480-1560 ℃, completely melting the second titanium-aluminum alloy ingot, refining for 4-8 min, and casting the second titanium-aluminum alloy ingot onto a water-cooled copper chassis within 3-8S after refining is finished to obtain a titanium-aluminum alloy target blank.
5. The method as claimed in claim 4, wherein the temperature of water under the water-cooled copper base plate is 8-12 ℃ and the water pressure is 0.24-0.28 MPa in the casting process.
6. The method according to claim 1, wherein during the step of hot isostatic pressing, the temperature is 1000-1100 ℃, the pressure is 150-300 MPa, and the holding time and pressure are 4-6 h.
7. The method according to claim 1, characterized in that said step of degassing is in particular: placing the mixture in a vacuum degassing furnace, and degassing for 2-3 hours at the temperature of 150-250 ℃.
8. The method of claim 1, wherein the first titanium source material and the second titanium source material are each no more than 60 wt% of the total amount of titanium source material, and the first aluminum source material and the second aluminum source material are each no more than 60 wt% of the total amount of aluminum source material.
9. The method according to claim 1, wherein the step of weighing the titanium raw material and the aluminum raw material in the ingredient has a mass ratio of 16:9 to 32: 9.
10. The method according to claim 1, wherein the titanium raw material is granular or bulk metallic titanium with a purity of more than 5N and a particle size of 1-5 mm, and the aluminum raw material is granular or bulk metallic aluminum with a purity of more than 5N and a particle size of 1-10 mm.
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