CN112391596A - Preparation method of high-quality tungsten-titanium sputtering target material - Google Patents
Preparation method of high-quality tungsten-titanium sputtering target material Download PDFInfo
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- CN112391596A CN112391596A CN202011114954.7A CN202011114954A CN112391596A CN 112391596 A CN112391596 A CN 112391596A CN 202011114954 A CN202011114954 A CN 202011114954A CN 112391596 A CN112391596 A CN 112391596A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- 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
- B22F3/02—Compacting only
- B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
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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
- B22F3/14—Both compacting and sintering simultaneously
- B22F3/15—Hot isostatic pressing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/04—Alloys based on tungsten or molybdenum
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Abstract
A preparation method of a high-quality tungsten titanium sputtering target material combines a cold isostatic pressing treatment process and a hot isostatic pressing sintering process, adopts a staged heat preservation and pressure maintaining process in the hot isostatic pressing sintering process, has simple steps, is easy to operate, and the prepared tungsten titanium target material has uniform tissue, fine grains, high purity and density of more than or equal to 99 percent, completely meets the use requirements in the field of high-end electronic product coating, has low production cost, is convenient for industrial batch production, and can meet the requirements of high-end target materials. The process is particularly suitable for industrial mass production of high-quality tungsten-titanium circular sputtering targets.
Description
Technical Field
The invention relates to the technical field of target processing, in particular to a preparation method of a high-quality circular tungsten-titanium sputtering target.
Background
The tungsten alloy has relatively stable physical and chemical properties, particularly has relatively high conductivity and high electromigration resistance, so the tungsten alloy is widely applied to semiconductor technology, particularly industries such as large scale integrated circuits (LSIs), Photovoltaics (PVs), Touch Screens (TFTs) and the like, and is an indispensable key material in the technical field of electronic information.
With the rapid development of semiconductor and electronic information technologies, the demand for high-quality tungsten alloy sputtering target materials is increasing as the application of the tungsten alloy sputtering target materials in magnetron sputtering control.
For the target material, the performance indexes such as purity, density, microstructure and the like influence the performance of the target material sputtering film. Generally, the higher the purity of the target material is, the better the sputtering film performance is, the higher the density of the target material is, the air holes in the target material can be reduced, the film deposition rate during sputtering is improved, and the discharge phenomenon of sputtered film particles is reduced; the more uniform the microstructure and the finer the grain size of the target material, the faster the sputtering rate and the more uniform the thickness of the sputtered film. Therefore, high-quality tungsten-titanium alloy target materials are required to have high purity, high compactness, and fine and uniform microstructure.
In the prior art, the tungsten titanium target material is usually produced by a method of first cold isostatic pressing and then vacuum sintering. The tungsten titanium target prepared by the traditional method has the advantages of low purity, low density and uneven microstructure, and causes the problems of poor coating quality, poor thickness uniformity and the like in the sputtering coating process of the target. Therefore, the research on the preparation method of the high-quality tungsten alloy target is imperative.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of a high-quality tungsten-titanium sputtering target material.
The technical scheme adopted by the invention to solve the technical problems is as follows: a preparation method of a high-quality tungsten-titanium sputtering target material comprises the following steps:
1. selecting tungsten powder and titanium powder, mixing according to the mass ratio to obtain tungsten-titanium mixed powder;
2) filling the tungsten-titanium mixed powder obtained in the step 1) into a rubber sleeve mold, sealing the rubber sleeve mold, then putting the sealed rubber sleeve mold into a cold isostatic press for cold isostatic pressing treatment to obtain a pressed blank, and demoulding the pressed blank to obtain a pressed powder blank;
3) and putting the pressed powder blank obtained in the step 2) into a sheath die, reserving an air outlet in the sheath die, vacuumizing the sheath die from the air outlet, sealing the air outlet, putting the sheath die into a hot isostatic pressing machine for hot isostatic pressing sintering treatment, and obtaining a hot pressed blank after the hot isostatic pressing sintering is finished.
4) And carrying out annealing treatment on the hot-pressed blank obtained in the step 3) in a hot isostatic pressing machine along with furnace cooling, taking out the hot-pressed blank, and carrying out mechanical processing to obtain the tungsten-titanium target material.
Preferably, in the step 1), the purity of the tungsten powder is more than or equal to 99.95 percent, the purity of the titanium powder is more than or equal to 99.95 percent, and in the tungsten-titanium mixed powder obtained by mixing the materials: according to the mass percentage, the titanium powder accounts for 8-12%, and the balance is tungsten powder.
Further, in the tungsten-titanium mixed powder obtained by mixing in the step 1): according to the mass percentage, the titanium powder is 10 percent, and the rest is tungsten powder, and the mixture is sieved by a 200-mesh sieve before being mixed.
Further, in the step 1), mixing the tungsten powder and the titanium powder in an argon atmosphere for 10-16 hours.
Preferably, in the step 2), the rubber sleeve mold is mechanically vibrated in the process of loading the tungsten-titanium mixed powder into the rubber sleeve mold, so as to ensure uniformity of powder loading.
Further, in the step 2), the pressing pressure adopted during the cold isostatic pressing treatment is 100-200 MPa, the pressing time is 4-10 minutes, and the pressurizing and depressurizing speeds are 10-15 MPa/min.
Preferably, in the step 3), a mechanical processing and shaping step is added before the pressed powder blank is filled into the sheath.
In a preferable embodiment, in the step 3), the pressure before the hot isostatic pressing sintering is finished is 150-200MPa, the temperature is 1301-1500 ℃, and the holding time is 4-6 h.
As another preferred embodiment, in step 3), the hot isostatic pressing sintering is performed by using a staged heat and pressure maintaining process, which is as follows:
in the first stage, pre-inflating is carried out in a furnace chamber of a hot isostatic pressing machine: filling inert gas to the pressure of 18-22 MPa;
and in the second stage, heating and pressurizing the furnace chamber of the hot isostatic pressing machine, which comprises the following steps:
firstly, raising the temperature to 500-600 ℃ at a temperature raising speed of 5-15 ℃/min, and then preserving heat and pressure for 0.8-1.2 h under the pressure of 20 MPa;
and then raising the temperature to 1301-1500 ℃ at a temperature raising speed of 5-15 ℃/min, and raising the pressure to 150-200MPa at a speed of 5-30 MPa/h.
And a third stage: and (3) heat preservation and pressure maintaining sintering: and preserving heat and pressure for 3-5 h under the conditions that the temperature in the furnace cavity is 1301-1500 ℃ and the pressure is 150-200 MPa.
Further, the annealing treatment in the step 4) is as follows: and after the third stage, removing the pressure of the inert gas, closing a heating switch of the hot isostatic pressing machine, cooling the sheath die coated with the tungsten-titanium blank to below 300 ℃ along with the furnace, and taking out the sheath die coated with the tungsten-titanium blank.
Has the advantages that:
according to the invention, the cold isostatic pressing treatment process and the hot isostatic pressing sintering process are combined, and the staged heat preservation and pressure maintaining process is adopted in the hot isostatic pressing sintering process, so that the method has the advantages of simple steps, easiness in operation, uniform structure of the prepared tungsten-titanium target material, fine crystal grains, high purity and high density (the density is more than or equal to 99%), completely meets the use requirements in the field of film coating of high-end electronic products, has low production cost, is convenient for industrial batch production, and can meet the requirements of the high-end target material. The process is particularly suitable for industrial mass production of high-quality tungsten-titanium circular sputtering targets.
The present invention will be described in further detail with reference to the drawings and specific examples.
Drawings
Fig. 1 is a schematic view of a gum cover mold.
Fig. 2 is a schematic diagram of a jacket mold.
FIG. 3 is a microstructure of a tungsten titanium sputtering target prepared in accordance with example one.
FIG. 4 is a microstructure of a tungsten titanium sputtering target prepared in example two.
FIG. 5 is a microstructure of a tungsten titanium sputtering target prepared in example III.
In the figure: 1. gum cover mould, 101, dress powder opening, 2, stopper, 3, tube-shape spare, 4, bottom plate, 401, cylindrical protrusion, 5, top cap, 6, gas vent.
Detailed Description
A preparation method of a high-quality tungsten-titanium sputtering target material comprises the following steps:
1. selecting tungsten powder and titanium powder, mixing according to the mass ratio to obtain tungsten-titanium mixed powder; in the step, the purity of the tungsten powder is preferably more than or equal to 99.95%, the purity of the titanium powder is preferably more than or equal to 99.95%, and in the tungsten-titanium mixed powder obtained by mixing, the titanium powder accounts for 8-12% by mass, and the balance is the tungsten powder. And preferably, the tungsten powder and the titanium powder are sieved by a 200-mesh sieve before proportioning and mixing. The tungsten powder and the titanium powder can be mixed in a V-shaped mixer in an argon atmosphere, and the powder mixing time is preferably 10-16 h.
2) And (2) filling the tungsten-titanium mixed powder obtained in the step 1) into a rubber sleeve mould, sealing the rubber sleeve mould, compacting the mould, putting the mould into a cold isostatic press for cold isostatic pressing treatment to obtain a pressed blank after ensuring the regular shape, and demoulding the pressed blank to obtain a pressed powder blank.
In the step, the rubber sleeve die is mechanically vibrated in the process of loading the tungsten-titanium mixed powder into the rubber sleeve die so as to ensure the uniformity of powder loading. The pressing pressure adopted during cold isostatic pressing treatment is 100-200 MPa, the pressing time is 4-10 minutes, and the speed of pressurization and depressurization is 10-15 MPa/min.
The step adopts a cold isostatic pressing treatment process, and can uniformly apply pressure to the rubber sleeve filled with the tungsten-titanium mixed powder from all directions by utilizing the pressure intensity characteristic of a liquid medium, so that the tungsten-titanium mixed powder is formed. In the process of fully compacting the tungsten-titanium mixed powder, the tungsten-titanium mixed powder is subjected to plastic deformation, so that gaps among particles of the tungsten-titanium mixed powder can be reduced, the defects of poor quality such as cavities, holes, fine gaps and cracks in the blank in the traditional hot isostatic pressing process are avoided, and the quality of the powder blank is ensured.
3) And machining and shaping the pressed powder blank obtained in the step 2), and then filling the pressed powder blank into a packaging mold.
The pressed powder blank obtained after the cold isostatic pressing treatment generally has the conditions of irregular shape and poor flatness and verticality, and if the subsequent hot isostatic pressing treatment is directly carried out, the difficulty of a sheath manufacturing procedure is increased, the sheath sealing effect is influenced, and the slab forming is not favorable. Therefore, the pressed powder blank is preferably subjected to shaping before being placed into a sheathing die, so that the shape is regular.
The canning material can adopt the stainless steel, and thickness is 2~3mm, reserves the gas vent, adopts the welding mode to carry out the canning processing. And then vacuumizing from the exhaust port, welding and sealing the exhaust port, putting the sheath die filled with the pressed powder blank into a hot isostatic pressing machine for hot isostatic pressing sintering treatment, and obtaining a hot pressed blank after the hot isostatic pressing sintering is finished.
In the step, hot isostatic pressing sintering is preferably carried out by adopting a staged heat preservation and pressure maintaining process, which comprises the following steps:
in the first stage, pre-inflating is carried out in a furnace chamber of a hot isostatic pressing machine: filling inert gas to the pressure of 18-22 MPa;
and in the second stage, heating and pressurizing the furnace chamber of the hot isostatic pressing machine, which comprises the following steps:
firstly, raising the temperature to 500-600 ℃ at a temperature raising speed of 5-15 ℃/min, and then preserving heat and pressure for 0.8-1.2 h under the pressure of 20 MPa;
and then, increasing the temperature to 1300-1500 ℃ at a temperature increasing speed of 5-15 ℃/min, and increasing the pressure to 150-200MPa at a speed of 5-30 MPa/h. At this stage, sintering necks begin to form between the tungsten-titanium mixed powder particles, while reduction of oxides on the particle surfaces and recrystallization within the powder particles also occur.
And a third stage: and (3) heat preservation and pressure maintaining sintering: and keeping the temperature and pressure for 4-6 h under the conditions that the temperature in the furnace cavity is 1301-1500 ℃ and the pressure is 150-200MPa to obtain the hot isostatic pressed blank.
The hot isostatic pressing sintering process may also be performed as follows:
filling inert gas into a compressor, pressurizing the cavity of the hot isostatic pressing machine at a pressurizing speed of 18-22Mpa/h, finally pressurizing to the maximum pressure of 150-200MPa, heating the cavity of the hot isostatic pressing machine at a heating speed of 5-15 ℃/min to 1301-1500 ℃, and then preserving heat and pressure for 4-6 h at the temperature of 150-200MPa and 1301-1500 ℃ to obtain the blank after hot isostatic pressing.
When the pressure is lower than 150MPa, the density of the final product cannot meet the use requirement, and when the pressure is higher than 200MPa, waste can be caused. The temperature 1301 + 1500 ℃ was also chosen based on the same reasons.
At this stage, growth of the sintering necks, grain boundary migration, and particle coalescence occur. As the sintering proceeds, the internal voids of the sintered body are closed and spheroidized, and the sintered body shrinks.
The hot isostatic pressing process uses inert gas as medium to conduct pressure, can uniformly apply pressure to the sheath die from all directions, and simultaneously heats up in a furnace chamber, so that the pressed blank realizes pressing, sintering and forming by using the static pressure at high temperature. According to the invention, the hot isostatic pressing treatment of the steps is carried out on the basis of carrying out cold isostatic pressing treatment on the tungsten-titanium mixed powder to prepare the tungsten-titanium target material, the density of the material can be improved, and the sintered target material has fine and uniform grains and meets the requirement of sputtering target materials.
The invention adopts a staged heat preservation and pressure maintaining process to prepare the target material, is more favorable for ensuring the sintering effect and improving the quality of the tungsten-titanium target material.
And 4), annealing the hot-pressed blank obtained in the step 3) in a hot isostatic pressing machine along with furnace cooling, taking out the hot-pressed blank, and obtaining the tungsten-titanium target material through mechanical processing.
The annealing treatment in the step is as follows: and after the third stage, removing the pressure of the inert gas, closing a heating switch of the hot isostatic pressing machine, cooling the sheath die coated with the tungsten-titanium blank to below 300 ℃ along with the furnace, and taking out the sheath die coated with the tungsten-titanium blank.
And then, cutting the sheath by using a water knife, and removing the sheath to obtain the tungsten-titanium blank.
The targets manufactured in this embodiment are all circular, so that the rubber sleeve die used in step 2) is a cylindrical rubber sleeve die as shown in fig. 1, and finally, a lathe is used for cutting an outer circle of the tungsten-titanium blank, then, the tungsten-titanium blank is cut into slices by linear cutting with a tolerance of +/-0.1 mm, then, the slices are transferred to a grinding machine for processing, and finally, the slices are polished to obtain the disc-shaped tungsten-titanium target with the surface roughness of less than 0.8 μm.
The preparation method of the tungsten-titanium sputtering target material can also be applied to the preparation of the square target material, and a rubber sleeve mold and a sheath with corresponding shapes are adopted in the preparation process.
The first embodiment is as follows:
1. selecting tungsten powder and titanium powder, mixing the tungsten powder and the titanium powder according to the mass ratio to obtain tungsten-titanium mixed powder: tungsten powder and titanium powder with the purity of more than or equal to 99.95 percent are selected to be screened (usually, a 200-mesh sieve is selected) to remove agglomerated particles, so that the tungsten powder and the titanium powder can be fully mixed. Then, mixing the tungsten powder and the titanium powder according to the mass percentage of 90 percent of the tungsten powder and 10 percent of the titanium powder, and putting the mixed powder after mixing into a V-shaped mixer for mixing. The protection of argon gas is let in before V type blendor starts, and the argon gas atmospheric pressure is positive in guaranteeing V type blendor, and this embodiment mixes the powder time and is 14 h.
2) And (2) filling the tungsten-titanium mixed powder obtained in the step 1) into a rubber sleeve die, as shown in figure 1. In this embodiment, the rubber sleeve mold 1 is cylindrical, and the upper end of the rubber sleeve mold 1 is provided with a powder loading opening 101, and after the tungsten-titanium mixed powder is loaded from the powder loading opening, the powder loading opening is sealed by a plug 2 (if necessary, glue can be applied to ensure sealing). In the step, the rubber sleeve die 1 is mechanically vibrated in the process of loading the tungsten-titanium mixed powder into the rubber sleeve die so as to ensure the uniformity of powder loading.
Sealing the rubber sleeve mould, compacting the mould, putting the mould into a cold isostatic press for cold isostatic pressing after ensuring the regular shape to obtain a pressed blank, and demoulding the pressed blank to obtain a pressed powder blank; the pressing pressure adopted during cold isostatic pressing treatment is 180MPa, the pressing time is 5 minutes, and the pressurizing and depressurizing speed is 10 MPa/min.
3) And machining and shaping the pressed powder blank obtained in the step 2), and then filling the pressed powder blank into a packaging mold. The sheath die is designed according to the shape of the target product and the size of the blank after the cold isostatic pressing treatment, so that the requirement of the subsequent hot isostatic pressing treatment process is met.
In this embodiment, the sheath is made of stainless steel, has a thickness of 2-3 mm, and has a shape as shown in fig. 2, and includes a cylindrical barrel 3, a bottom plate 4 is disposed at one end of the barrel 3, the bottom plate has a cylindrical protrusion 401 hermetically fitted with the corresponding end of the barrel 3, a top cover 5 is disposed at the other end of the barrel 3, and an air outlet 6 is reserved on the top cover 5. Sealing the sheathing die by adopting an argon arc welding mode, and firstly welding and sealing the whole joint of the sheathing die in the process, wherein the exhaust port is not sealed; and after the pressed powder blank is placed into a sheathing die, vacuumizing from an exhaust port 6 to ensure that the vacuum degree in the sheathing die is at least 3 x 10 < -3 > Pa, then welding and sealing the exhaust port to form a closed environment inside the sheathing die, and then placing the sheathing die filled with the pressed powder blank into a hot isostatic pressing machine to carry out hot isostatic pressing sintering to obtain a hot pressed blank.
In the step, the hot isostatic pressing sintering is carried out by adopting a staged heat preservation and pressure maintaining process, which comprises the following steps:
in the first stage, pre-inflating is carried out in a furnace chamber of a hot isostatic pressing machine: filling inert gas argon until the pressure is 20 MPa;
and in the second stage, heating and pressurizing the furnace chamber of the hot isostatic pressing machine, which comprises the following steps:
firstly, raising the temperature to 500 ℃ according to the temperature rise speed of 5 ℃/min (about 1.6h is needed), and then keeping the temperature and the pressure for 1 h under the pressure of 20 MPa;
then, the temperature is increased from 500 ℃ to 1400 ℃ according to the temperature increase speed of 5 ℃/min, and the pressure is increased from 20MPa to 200MPa at the speed of 10MPa/h (the process needs about 3 h);
and a third stage: and (3) heat preservation and pressure maintaining sintering: keeping the temperature and pressure in the furnace chamber at 1400 ℃ and 200Mpa for 5 h.
And 4), removing the pressure of the inert gas of the hot isostatic pressing machine, closing a heating switch of the hot isostatic pressing machine, cooling the sheath die coated with the tungsten-titanium blank to below 300 ℃ along with the furnace (namely, in the annealing process), and taking out the sheath die coated with the tungsten-titanium blank.
And then, cutting the sheath by using a water knife, and removing the sheath to obtain the tungsten-titanium blank. In this embodiment, a high-speed water jet is used to cut the sheath, and the sintered billet is obtained after the sheath mold is removed. The quality test result of the cut sample is that the purity of the target material is more than or equal to 99.95 percent, the impurity content is less than or equal to 500ppm, the microstructure of the target material is shown in figure 3, the crystal grain size of the matrix is fine and uniform, part of titanium element is dispersed and distributed, no segregation exists, and the requirement of the microstructure of the sputtering target material is met. The target density was 14.58g/cm3, and the relative density (compactness) corresponding to the theoretical density (14.59 g/cm 3) was 99.96%. And (3) carrying out ultrasonic nondestructive inspection on the sintered billet before machining, and inspecting the integral internal quality of the billet, wherein the internal defects such as cracks, delamination, holes and the like do not exist.
Example two:
1. selecting tungsten powder and titanium powder, mixing the tungsten powder and the titanium powder according to the mass ratio to obtain tungsten-titanium mixed powder: tungsten powder and titanium powder with the purity of more than or equal to 99.95 percent are selected to be screened (usually, a 200-mesh sieve is selected) to remove agglomerated particles, so that the tungsten powder and the titanium powder can be fully mixed. Then, mixing the tungsten powder and the titanium powder according to the mass percentage of 88 percent of the tungsten powder and 12 percent of the titanium powder, and putting the mixed powder after mixing into a V-shaped mixer for mixing. The protection of argon gas is let in before V type blendor start, and it is positive to guarantee that the argon gas atmospheric pressure is in the V type blendor, and this embodiment mixes the powder time and is 10 h.
2) And (2) filling the tungsten-titanium mixed powder obtained in the step 1) into a rubber sleeve die, as shown in figure 1. In this embodiment, the rubber sleeve mold 1 is cylindrical, and the upper end of the rubber sleeve mold 1 is provided with a powder loading opening 101, and after the tungsten-titanium mixed powder is loaded from the powder loading opening, the powder loading opening is sealed by a plug 2 (if necessary, glue can be applied to ensure sealing). In the step, the rubber sleeve die 1 is mechanically vibrated in the process of loading the tungsten-titanium mixed powder into the rubber sleeve die so as to ensure the uniformity of powder loading.
Sealing the rubber sleeve mould, compacting the mould, putting the mould into a cold isostatic press for cold isostatic pressing after ensuring the regular shape to obtain a pressed blank, and demoulding the pressed blank to obtain a pressed powder blank; the pressing pressure adopted during the cold isostatic pressing treatment is 100MPa, the pressing time is 4 minutes, and the pressurizing and depressurizing speeds are 12 MPa/min.
3) And machining and shaping the pressed powder blank obtained in the step 2), and then filling the pressed powder blank into a packaging mold. The sheath die is designed according to the shape of the target product and the size of the blank after the cold isostatic pressing treatment, so that the requirement of the subsequent hot isostatic pressing treatment process is met.
In this embodiment, the sheath is made of stainless steel, has a thickness of 2-3 mm, and has a shape as shown in fig. 2, and includes a cylindrical barrel 3, a bottom plate 4 is disposed at one end of the barrel 3, the bottom plate has a cylindrical protrusion 401 hermetically fitted with the corresponding end of the barrel 3, a top cover 5 is disposed at the other end of the barrel 3, and an air outlet 6 is reserved on the top cover 5. Sealing the sheathing die by adopting an argon arc welding mode, and firstly welding and sealing the whole joint of the sheathing die in the process, wherein the exhaust port is not sealed; and after the pressed powder blank is placed into a sheathing die, vacuumizing from an exhaust port 6 to ensure that the vacuum degree in the sheathing die is at least 3 x 10 < -3 > Pa, then welding and sealing the exhaust port to form a closed environment inside the sheathing die, and then placing the sheathing die filled with the pressed powder blank into a hot isostatic pressing machine to carry out hot isostatic pressing sintering to obtain a hot pressed blank.
In the step, the hot isostatic pressing sintering is carried out by adopting a staged heat preservation and pressure maintaining process, which comprises the following steps:
in the first stage, pre-inflating is carried out in a furnace chamber of a hot isostatic pressing machine: filling inert gas argon until the pressure is 18 MPa;
and in the second stage, heating and pressurizing the furnace chamber of the hot isostatic pressing machine, which comprises the following steps:
firstly, raising the temperature to 550 ℃ at a temperature rise speed of 10 ℃/min, and then preserving heat and pressure for 0.8 h under the pressure of 18 MPa;
then raising the temperature from 550 ℃ to 1360 ℃ at a temperature raising speed of 10 ℃/min, and raising the pressure from 18MPa to 180MPa at a speed of 5 MPa/h;
and a third stage: and (3) heat preservation and pressure maintaining sintering: keeping the temperature and pressure in the furnace chamber at 1360 deg.C and 180Mpa for 4 h.
And 4), removing the pressure of the inert gas of the hot isostatic pressing machine, closing a heating switch of the hot isostatic pressing machine, cooling the sheath die coated with the tungsten-titanium blank to below 300 ℃ along with the furnace (namely, in the annealing process), and taking out the sheath die coated with the tungsten-titanium blank.
And then, cutting the sheath by using a water knife, and removing the sheath to obtain the tungsten-titanium blank. In this embodiment, a high-speed water jet is used to cut the sheath, and the sintered billet is obtained after the sheath mold is removed. The quality test result of the cut sample is that the purity of the target material is more than or equal to 99.95 percent, the impurity content is less than or equal to 500ppm, the microstructure of the target material is shown in figure 4, the crystal grain size of the matrix is fine and uniform, part of titanium element is dispersed and distributed, no segregation exists, and the requirement of the microstructure of the sputtering target material is met. The density of the target material is equal to-13.87 g/cm3, and the density (relative density) corresponding to the theoretical density (13.91 g/cm 3) is 99.71%. And (3) carrying out ultrasonic nondestructive inspection on the sintered billet before machining, and inspecting the integral internal quality of the billet, wherein the internal defects such as cracks, delamination, holes and the like do not exist.
Example three:
1. selecting tungsten powder and titanium powder, mixing the tungsten powder and the titanium powder according to the mass ratio to obtain tungsten-titanium mixed powder: tungsten powder and titanium powder with the purity of more than or equal to 99.95 percent are selected to be screened (usually, a 200-mesh sieve is selected) to remove agglomerated particles, so that the tungsten powder and the titanium powder can be fully mixed. And then mixing the tungsten powder and the titanium powder according to the mass percentage of 92 percent of the tungsten powder and 8 percent of the titanium powder, and putting the mixed powder after mixing into a V-shaped mixer for mixing. The protection of argon gas is let in before V type blendor start, and it is positive to guarantee that the argon gas atmospheric pressure is in the V type blendor, and this embodiment mixes the powder time and is 16 h.
2) And (2) filling the tungsten-titanium mixed powder obtained in the step 1) into a rubber sleeve die, as shown in figure 1. In this embodiment, the rubber sleeve mold 1 is cylindrical, and the upper end of the rubber sleeve mold 1 is provided with a powder loading opening 101, and after the tungsten-titanium mixed powder is loaded from the powder loading opening, the powder loading opening is sealed by a plug 2 (if necessary, glue can be applied to ensure sealing). In the step, the rubber sleeve die 1 is mechanically vibrated in the process of loading the tungsten-titanium mixed powder into the rubber sleeve die so as to ensure the uniformity of powder loading.
Sealing the rubber sleeve mould, compacting the mould, putting the mould into a cold isostatic press for cold isostatic pressing after ensuring the regular shape to obtain a pressed blank, and demoulding the pressed blank to obtain a pressed powder blank; the pressing pressure adopted during cold isostatic pressing treatment is 200MPa, the pressing time is 10 minutes, and the pressurizing and depressurizing speeds are 15 MPa/min.
3) And machining and shaping the pressed powder blank obtained in the step 2), and then filling the pressed powder blank into a packaging mold. The sheath die is designed according to the shape of the target product and the size of the blank after the cold isostatic pressing treatment, so that the requirement of the subsequent hot isostatic pressing treatment process is met.
In this embodiment, the sheath is made of stainless steel, has a thickness of 2-3 mm, and has a shape as shown in fig. 2, and includes a cylindrical barrel 3, a bottom plate 4 is disposed at one end of the barrel 3, the bottom plate has a cylindrical protrusion 401 hermetically fitted with the corresponding end of the barrel 3, a top cover 5 is disposed at the other end of the barrel 3, and an air outlet 6 is reserved on the top cover 5. Sealing the sheathing die by adopting an argon arc welding mode, and firstly welding and sealing the whole joint of the sheathing die in the process, wherein the exhaust port is not sealed; and after the pressed powder blank is placed into a sheathing die, vacuumizing from an exhaust port 6 to ensure that the vacuum degree in the sheathing die is at least 3 x 10 < -3 > Pa, then welding and sealing the exhaust port to form a closed environment inside the sheathing die, and then placing the sheathing die filled with the pressed powder blank into a hot isostatic pressing machine to carry out hot isostatic pressing sintering to obtain a hot pressed blank.
In the step, the hot isostatic pressing sintering is carried out by adopting a staged heat preservation and pressure maintaining process, which comprises the following steps:
in the first stage, pre-inflating is carried out in a furnace chamber of a hot isostatic pressing machine: filling inert gas argon until the pressure is 22 MPa;
and in the second stage, heating and pressurizing the furnace chamber of the hot isostatic pressing machine, which comprises the following steps:
firstly, raising the temperature to 600 ℃ at a temperature rise speed of 15 ℃/min, and then preserving heat and pressure for 1.2h under the pressure of 18 MPa;
then, the temperature is increased from 600 ℃ to 1320 ℃ at the temperature increasing speed of 15 ℃/min, and the pressure is increased from 22MPa to 160MPa at the speed of 30 MPa/h;
and a third stage: and (3) heat preservation and pressure maintaining sintering: keeping the temperature and pressure in the furnace chamber at 1320 deg.C and 160Mpa for 3 h.
And 4), removing the pressure of the inert gas of the hot isostatic pressing machine, closing a heating switch of the hot isostatic pressing machine, cooling the sheath die coated with the tungsten-titanium blank to below 300 ℃ along with the furnace (namely, in the annealing process), and taking out the sheath die coated with the tungsten-titanium blank.
And then, cutting the sheath by using a water knife, and removing the sheath to obtain the tungsten-titanium blank. In this embodiment, a high-speed water jet is used to cut the sheath, and the sintered billet is obtained after the sheath mold is removed. The quality test result of the cut sample is that the purity of the target material is more than or equal to 99.95 percent, the impurity content is less than or equal to 500ppm, the microstructure of the target material is shown in figure 5, the crystal grain size of the matrix is fine and uniform, part of titanium element is dispersed and distributed, no segregation exists, and the requirement of the microstructure of the sputtering target material is met. The target density was equal to 15.25g/cm3, corresponding to a theoretical density (15.35 g/cm 3) and a compactness (relative density) of 99.34%. And (3) carrying out ultrasonic nondestructive inspection on the sintered billet before machining, and inspecting the integral internal quality of the billet, wherein the internal defects such as cracks, delamination, holes and the like do not exist.
Example four:
1. selecting tungsten powder and titanium powder, mixing the tungsten powder and the titanium powder according to the mass ratio to obtain tungsten-titanium mixed powder: tungsten powder and titanium powder with the purity of more than or equal to 99.95 percent are selected to be screened (usually, a 200-mesh sieve is selected) to remove agglomerated particles, so that the tungsten powder and the titanium powder can be fully mixed. Then, mixing the tungsten powder and the titanium powder according to the mass percentage of 90 percent of the tungsten powder and 10 percent of the titanium powder, and putting the mixed powder after mixing into a V-shaped mixer for mixing. The protection of argon gas is let in before V type blendor start, and it is positive to guarantee that the argon gas atmospheric pressure is in the V type blendor, and this embodiment mixes the powder time and is 12 h.
2) And (2) filling the tungsten-titanium mixed powder obtained in the step 1) into a rubber sleeve die, as shown in figure 1. In this embodiment, the rubber sleeve mold 1 is cylindrical, and the upper end of the rubber sleeve mold 1 is provided with a powder loading opening 101, and after the tungsten-titanium mixed powder is loaded from the powder loading opening, the powder loading opening is sealed by a plug 2 (if necessary, glue can be applied to ensure sealing). In the step, the rubber sleeve die 1 is mechanically vibrated in the process of loading the tungsten-titanium mixed powder into the rubber sleeve die so as to ensure the uniformity of powder loading.
Sealing the rubber sleeve mould, compacting the mould, putting the mould into a cold isostatic press for cold isostatic pressing after ensuring the regular shape to obtain a pressed blank, and demoulding the pressed blank to obtain a pressed powder blank; the pressing pressure adopted during cold isostatic pressing treatment is 200MPa, the pressing time is 10 minutes, and the pressurizing and depressurizing speeds are 15 MPa/min.
3) And machining and shaping the pressed powder blank obtained in the step 2), and then filling the pressed powder blank into a packaging mold. The sheath die is designed according to the shape of the target product and the size of the blank after the cold isostatic pressing treatment, so that the requirement of the subsequent hot isostatic pressing treatment process is met.
In this embodiment, the sheath is made of stainless steel, has a thickness of 2-3 mm, and has a shape as shown in fig. 2, and includes a cylindrical barrel 3, a bottom plate 4 is disposed at one end of the barrel 3, the bottom plate has a cylindrical protrusion 401 hermetically fitted with the corresponding end of the barrel 3, a top cover 5 is disposed at the other end of the barrel 3, and an air outlet 6 is reserved on the top cover 5. Sealing the sheathing die by adopting an argon arc welding mode, and firstly welding and sealing the whole joint of the sheathing die in the process, wherein the exhaust port is not sealed; and after the pressed powder blank is placed into a sheathing die, vacuumizing from an exhaust port 6 to ensure that the vacuum degree in the sheathing die is at least 3 x 10 < -3 > Pa, then welding and sealing the exhaust port to form a closed environment inside the sheathing die, and then placing the sheathing die filled with the pressed powder blank into a hot isostatic pressing machine to carry out hot isostatic pressing sintering to obtain a hot pressed blank.
In the step, the hot isostatic pressing sintering is carried out by adopting a staged heat preservation and pressure maintaining process, which comprises the following steps:
in the first stage, pre-inflating is carried out in a furnace chamber of a hot isostatic pressing machine: filling inert gas argon until the pressure is 20 MPa;
and in the second stage, heating and pressurizing the furnace chamber of the hot isostatic pressing machine, which comprises the following steps:
firstly, raising the temperature to 600 ℃ at a temperature rise speed of 15 ℃/min, and then preserving heat and pressure for 1.2h under the pressure of 18 MPa;
then, the temperature is increased from 600 ℃ to 1500 ℃ at the temperature increasing speed of 15 ℃/min, and the pressure is increased from 22MPa to 150MPa at the speed of 30 MPa/h;
and a third stage: and (3) heat preservation and pressure maintaining sintering: keeping the temperature and pressure in the furnace chamber at 1500 deg.C and 150Mpa for 4 hr.
And 4), removing the pressure of the inert gas of the hot isostatic pressing machine, closing a heating switch of the hot isostatic pressing machine, cooling the sheath die coated with the tungsten-titanium blank to below 300 ℃ along with the furnace (namely, in the annealing process), and taking out the sheath die coated with the tungsten-titanium blank.
And then, cutting the sheath by using a water knife, and removing the sheath to obtain the tungsten-titanium blank. In this embodiment, a high-speed water jet is used to cut the sheath, and the sintered billet is obtained after the sheath mold is removed. The quality test result of the cut sample shows that the purity of the target material is more than or equal to 99.95 percent, the impurity content is less than or equal to 500ppm, and a microstructure picture (similar to the microstructure picture of the first three embodiments and omitted) of the target material shows that the matrix crystal grain size is fine and uniform, part of titanium element is dispersed and distributed without segregation, and the microstructure requirement of the sputtering target material is met. The target density was equal to 14.48g/cm3, corresponding to a theoretical density (14.59 g/cm 3) and a compactness (relative density) of 99.25%. And (3) carrying out ultrasonic nondestructive inspection on the sintered billet before machining, and inspecting the integral internal quality of the billet, wherein the internal defects such as cracks, delamination, holes and the like do not exist.
Example five:
1. selecting tungsten powder and titanium powder, mixing the tungsten powder and the titanium powder according to the mass ratio to obtain tungsten-titanium mixed powder: tungsten powder and titanium powder with the purity of more than or equal to 99.95 percent are selected to be screened (usually, a 200-mesh sieve is selected) to remove agglomerated particles, so that the tungsten powder and the titanium powder can be fully mixed. Then, mixing the tungsten powder and the titanium powder according to the mass percentage of 90 percent of the tungsten powder and 10 percent of the titanium powder, and putting the mixed powder after mixing into a V-shaped mixer for mixing. The protection of argon gas is let in before V type blendor start, and it is positive to guarantee that the argon gas atmospheric pressure is in the V type blendor, and this embodiment mixes the powder time and is 10 h.
2) And (2) filling the tungsten-titanium mixed powder obtained in the step 1) into a rubber sleeve die, as shown in figure 1. In this embodiment, the rubber sleeve mold 1 is cylindrical, and the upper end of the rubber sleeve mold 1 is provided with a powder loading opening 101, and after the tungsten-titanium mixed powder is loaded from the powder loading opening, the powder loading opening is sealed by a plug 2 (if necessary, glue can be applied to ensure sealing). In the step, the rubber sleeve die 1 is mechanically vibrated in the process of loading the tungsten-titanium mixed powder into the rubber sleeve die so as to ensure the uniformity of powder loading.
Sealing the rubber sleeve mould, compacting the mould, putting the mould into a cold isostatic press for cold isostatic pressing after ensuring the regular shape to obtain a pressed blank, and demoulding the pressed blank to obtain a pressed powder blank; the pressing pressure adopted during the cold isostatic pressing treatment is 100MPa, the pressing time is 4 minutes, and the pressurizing and depressurizing speeds are 12 MPa/min.
3) And machining and shaping the pressed powder blank obtained in the step 2), and then filling the pressed powder blank into a packaging mold. The sheath die is designed according to the shape of the target product and the size of the blank after the cold isostatic pressing treatment, so that the requirement of the subsequent hot isostatic pressing treatment process is met.
In this embodiment, the sheath is made of stainless steel, has a thickness of 2-3 mm, and has a shape as shown in fig. 2, and includes a cylindrical barrel 3, a bottom plate 4 is disposed at one end of the barrel 3, the bottom plate has a cylindrical protrusion 401 hermetically fitted with the corresponding end of the barrel 3, a top cover 5 is disposed at the other end of the barrel 3, and an air outlet 6 is reserved on the top cover 5. Sealing the sheathing die by adopting an argon arc welding mode, and firstly welding and sealing the whole joint of the sheathing die in the process, wherein the exhaust port is not sealed; and after the pressed powder blank is placed into a sheathing die, vacuumizing from an exhaust port 6 to ensure that the vacuum degree in the sheathing die is at least 3 x 10 < -3 > Pa, then welding and sealing the exhaust port to form a closed environment inside the sheathing die, and then placing the sheathing die filled with the pressed powder blank into a hot isostatic pressing machine to carry out hot isostatic pressing sintering to obtain a hot pressed blank.
In the step, the hot isostatic pressing sintering is carried out by adopting a staged heat preservation and pressure maintaining process, which comprises the following steps:
in the first stage, pre-inflating is carried out in a furnace chamber of a hot isostatic pressing machine: filling inert gas argon until the pressure is 18 MPa;
and in the second stage, heating and pressurizing the furnace chamber of the hot isostatic pressing machine, which comprises the following steps:
firstly, raising the temperature to 550 ℃ at a temperature rise speed of 10 ℃/min, and then preserving heat and pressure for 0.8 h under the pressure of 18 MPa;
then raising the temperature from 550 ℃ to 1360 ℃ at a temperature raising speed of 10 ℃/min, and raising the pressure from 18MPa to 200MPa at a speed of 5 MPa/h;
and a third stage: and (3) heat preservation and pressure maintaining sintering: keeping the temperature and pressure in the furnace chamber at 1301 deg.C and 200Mpa for 5 h.
And 4), removing the pressure of the inert gas of the hot isostatic pressing machine, closing a heating switch of the hot isostatic pressing machine, cooling the sheath die coated with the tungsten-titanium blank to below 300 ℃ along with the furnace (namely, in the annealing process), and taking out the sheath die coated with the tungsten-titanium blank.
And then, cutting the sheath by using a water knife, and removing the sheath to obtain the tungsten-titanium blank. In this embodiment, a high-speed water jet is used to cut the sheath, and the sintered billet is obtained after the sheath mold is removed. The quality test result of the cut sample shows that the purity of the target material is more than or equal to 99.95 percent, the impurity content is less than or equal to 500ppm, and a microstructure picture (similar to the microstructure pictures of the previous three embodiments and omitted) of the target material shows that the matrix crystal grain size is fine and uniform, part of titanium element is dispersed and distributed without segregation, and the microstructure requirement of the sputtering target material is met. The target density was equal to 14.47g/cm3, corresponding to a density (relative density) of 99.18% for the theoretical density (14.59 g/cm 3). And (3) carrying out ultrasonic nondestructive inspection on the sintered billet before machining, and inspecting the integral internal quality of the billet, wherein the internal defects such as cracks, delamination, holes and the like do not exist.
The targets manufactured in the above embodiments are all circular, so the rubber sleeve die used in step 2) is a cylindrical rubber sleeve die, and finally, a lathe is used for cutting an outer circle of the tungsten-titanium blank, then, the tungsten-titanium blank is cut into slices by linear cutting with a tolerance of +/-0.1 mm, then, the tungsten-titanium blank is transferred to a grinding machine for processing, and finally, the tungsten-titanium blank is polished and processed into a circular tungsten-titanium target with a surface roughness of less than 0.8 μm.
The preparation method of the tungsten-titanium sputtering target material can also be applied to the preparation of the square target material, and a rubber sleeve mold and a sheath with corresponding shapes are adopted in the preparation process.
It should be noted that the above embodiments are only for illustrating the present invention, but the present invention is not limited to the above embodiments, and any simple modification, equivalent change and modification made to the above embodiments according to the technical essence of the present invention fall within the protection scope of the present invention.
Claims (10)
1. A preparation method of a high-quality tungsten-titanium sputtering target material is characterized by comprising the following steps:
1. selecting tungsten powder and titanium powder, mixing according to the mass ratio to obtain tungsten-titanium mixed powder;
2) filling the tungsten-titanium mixed powder obtained in the step 1) into a rubber sleeve mold, sealing the rubber sleeve mold, then putting the sealed rubber sleeve mold into a cold isostatic press for cold isostatic pressing treatment to obtain a pressed blank, and demoulding the pressed blank to obtain a pressed powder blank;
3) placing the pressed powder blank obtained in the step 2) into a sheath die, reserving an air outlet in the sheath die, vacuumizing the sheath die from the air outlet, sealing the air outlet, then placing the sheath die into a hot isostatic pressing machine for hot isostatic pressing sintering treatment, and obtaining a hot pressed blank after the hot isostatic pressing sintering is finished;
4) and carrying out annealing treatment on the hot-pressed blank obtained in the step 3) in a hot isostatic pressing machine along with furnace cooling, taking out the hot-pressed blank, and carrying out mechanical processing to obtain the tungsten-titanium target material.
2. The method for preparing a high-quality tungsten-titanium sputtering target according to claim 1, wherein the method comprises the following steps: the purity of the tungsten powder selected in the step 1) is more than or equal to 99.95%, the purity of the titanium powder is more than or equal to 99.95%, and in the tungsten-titanium mixed powder obtained by mixing the materials: according to the mass percentage, the titanium powder accounts for 8-12%, and the balance is tungsten powder.
3. The method for preparing a high-quality tungsten-titanium sputtering target according to claim 2, wherein the method comprises the following steps: mixing the materials in the step 1) to obtain tungsten-titanium mixed powder: according to the mass percentage, the titanium powder is 10 percent, and the rest is tungsten powder, and the mixture is sieved by a 200-mesh sieve before being mixed.
4. The method for preparing a high-quality circular tungsten-titanium sputtering target according to claim 1, wherein the method comprises the following steps: in the step 1), mixing tungsten powder and titanium powder in an argon atmosphere for 10-16 h.
5. The method for preparing a high-quality tungsten-titanium sputtering target according to claim 1, wherein the method comprises the following steps: and in the step 2), the rubber sleeve die is mechanically vibrated in the process of loading the tungsten-titanium mixed powder into the rubber sleeve die so as to ensure the uniformity of powder loading.
6. The method for preparing a high-quality tungsten-titanium sputtering target according to claim 1, wherein the method comprises the following steps: in the step 2), the pressing pressure adopted during the cold isostatic pressing treatment is 100-200 MPa, the pressing time is 4-10 minutes, and the pressurizing and depressurizing speeds are 10-15 MPa/min.
7. The method for preparing a high-quality tungsten-titanium sputtering target according to claim 1, wherein the method comprises the following steps: and 3) adding a mechanical processing and shaping step before the pressed powder blank is packaged into a sheath.
8. The method for preparing a high-quality tungsten-titanium sputtering target according to claim 1, wherein the method comprises the following steps: in the step 3), the pressure before hot isostatic pressing sintering is finished is 150-200MPa, the temperature is 1301-1500 ℃, and the heat preservation time is 4-6 h.
9. The method for preparing a high-quality tungsten-titanium sputtering target according to claim 1, wherein the method comprises the following steps: in the step 3), the hot isostatic pressing sintering is carried out by adopting a staged heat preservation and pressure maintaining process, which comprises the following steps:
in the first stage, pre-inflating is carried out in a furnace chamber of a hot isostatic pressing machine: filling inert gas to the pressure of 18-22 MPa;
and in the second stage, heating and pressurizing the furnace chamber of the hot isostatic pressing machine, which comprises the following steps:
firstly, raising the temperature to 500-600 ℃ at a temperature raising speed of 5-15 ℃/min, and then preserving heat and pressure for 0.8-1.2 h under the pressure of 20 MPa;
then, increasing the temperature to 1301-1500 ℃ at a temperature increasing speed of 5-15 ℃/min, and increasing the pressure to 150-200MPa at a speed of 5-30 MPa/h;
and a third stage: and (3) heat preservation and pressure maintaining sintering: and preserving heat and pressure for 3-5 h under the conditions that the temperature in the furnace cavity is 1301-1500 ℃ and the pressure is 150-200 MPa.
10. The method for preparing a high-quality tungsten-titanium sputtering target according to claim 9, wherein the method comprises the following steps: the annealing treatment in the step 4) comprises the following steps: and after the third stage, removing the pressure of the inert gas, closing a heating switch of the hot isostatic pressing machine, cooling the sheath die coated with the tungsten-titanium blank to below 300 ℃ along with the furnace, and taking out the sheath die coated with the tungsten-titanium blank.
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