JP7116794B2 - Tantalum-silicon alloy sputtering target material and manufacturing method thereof - Google Patents

Description

The present application relates to the field of target materials and target material manufacturing, such as tantalum-silicon alloy sputtering target materials and methods of manufacturing the same.

Physical Vapor Deposition (PVD) is under vacuum conditions, using an arc discharge technology with low voltage and high current to evaporate the material with gas discharge, ionize the vaporized substance and gas, and then , to form a thin film having a special function by evaporating the vaporized substance and its reaction product on the workpiece by the accelerating action of the electric field. PVD technology is an important core technology in many fields such as semiconductor chip manufacturing, solar energy, LCD manufacturing, etc. Main methods include vacuum deposition, arc plasma plating, ion plating, molecular beam epitaxy and sputtering plating. is.

Sputtering is one of the main techniques for manufacturing thin film materials. It utilizes ions generated in an ion source and accelerated coalescence in a vacuum to form an ion beam stream with high velocity energy, thereby forming solids. Upon impacting the surface, the ions exchange kinetic energy with the atoms of the solid surface, causing the atoms of the solid surface to move away from the solid and deposit on the basal plane. The collided solid is a raw material for depositing a thin film by a sputtering method, and is generally called a sputtering target material.

Sputtering target materials are commonly obtained by a powder metallurgical sintering process. This is because the sputtering target material produced by this process has a unique chemical composition and mechanical and physical properties that are not available from conventional melting and casting methods. The powder metallurgy sintering process is divided into two methods: hot press sintering and hot isostatic pressing. Hot isostatic pressing is a method in which molding and sintering are completed at the same time. The product is sintered and densified.

Tantalum-silicon alloy sputtering target material is a novel sputtering target material, as a good conductor in vacuum sputtering, it can be applied in the field of electronic gate materials and electronic films. In order for the tantalum-silicon alloy sputtering target material to have good performance during vacuum sputtering, it is required that the tantalum-silicon alloy sputtering target material has a high density and a uniform internal structure. However, at present, there is no manufacturing method that allows the obtained tantalum silicon alloy sputtering target material to satisfy the above requirements.

The prior art currently discloses several methods of manufacturing sputtering target materials. For example, China Patent Application No. 102321871 discloses a method for producing molybdenum alloy sputtering target material for flat panel display by hot isostatic pressing, comprising powder preparation, hydraulic pressing, cold isostatic pressing, It includes sintering, machining, filling into capsules, hot isostatic pressing and other processes, and with the synergistic effect of high temperature and high pressure, the workpiece is evenly pressed in all directions, and the target material is highly dense. A manufacturing method with good uniformity and excellent performance is disclosed. However, this manufacturing method has limited application scope due to its complicated process, long production cycle and lack of powder mixing process for non-metallic powders. In China Patent Application No. 105624619, including powder production, cold isostatic pressing, vacuum sintering, hot isostatic pressing, machining, indium bonding, etc., aluminum rare earth alloy rotating sputtering target for tablet touch panel A method of making a material and a target material made thereby are disclosed. This manufacturing method simplifies the process and makes it easier to operate, but there is also no powder mixing process for non-metallic powders.

The manufacturing methods in the above prior art all adopt the hot isostatic pressing process, but since there is no powder mixing process for non-metallic powders, it is not possible to ensure the purity of the final sputtering target material. , In addition, due to the large difference in physical properties such as melting point and specific gravity of tantalum and silicon, demanding higher requirements for process parameters such as powder mixing process, degassing treatment and hot isostatic pressing, tantalum silicon alloy It cannot meet the requirements for compactness and uniformity of internal structure of the sputtering target material. Therefore, there is currently a need to develop methods for producing effective tantalum-silicon alloy sputtering target materials.

The following provides an overview of the themes detailed in this specification. This summary is not intended to limit the scope of the claims.

Objects of the present application include providing a tantalum-silicon alloy sputtering target material and a method of making the same. The manufacturing method includes six steps of powder mixing, charging into a mold, cold isostatic pressing, degassing, hot isostatic pressing, and machining. It can not only effectively prevent oxidation and ensure the purity of the product, but also can meet the requirements of tantalum silicon alloy sputtering target material denseness and internal structure uniformity, and the process is simple and the operation is simple. is simple and has a short production cycle. The tantalum silicon alloy sputtering target material manufactured by the above manufacturing method not only has a uniform structure inside the tantalum silicon alloy, but also can be formed with a density of 99% or more, ensuring better performance in subsequent sputtering. can provide

In order to achieve this purpose, the present application adopts the following technical solutions.

In one aspect, the present application is a method of making a tantalum silicon alloy sputtering target material comprising:
(1) mixing tantalum powder and silicon powder in atomic ratio;
(2) a step of charging the tantalum silicon powder mixed in step (1) into a mold and sealing the mold;
(3) a step of cold isostatically treating the mold sealed in step (2) to obtain a tantalum silicon material;
(4) a step of encapsulating the tantalum silicon material obtained in step (3), sealing the capsule, and performing a degassing treatment;
(5) subjecting the degassed capsules in step (4) to hot isostatic pressure treatment at 1050 to 1350° C. to obtain a crude tantalum silicon alloy sputtering target material;
(6) machining the crude tantalum silicon alloy sputtering target material obtained in step (5) to obtain a tantalum silicon alloy sputtering target material;
A manufacturing method is provided comprising:

The manufacturing method according to the present application employs a combination of cold isostatic pressing, degassing, and hot isostatic pressing to evenly distribute the tantalum silicon alloy sputtering target material in each direction. Applying pressure, we have achieved the high requirements of a compactness of 99% or more and a uniform internal structure.

At the same time, the present application performs hot isostatic pressure treatment at a high temperature of 1050-1350 ° C., such a high hot isostatic pressure treatment temperature greatly improves the compactness of the tantalum silicon alloy sputtering target material and , the oxygen content can be effectively controlled and contamination can be effectively avoided, thus ensuring the purity of the product.

The hot isostatic pressure treatment temperature described in this application is 1050-1350°C, such as 1050°C, 1100°C, 1150°C, 1200°C, 1250°C, 1300°C and 1350°C, etc. It is not intended to be limited to the numerical values listed, and applies equally to other unlisted numerical values within this numerical range.

As a preferred embodiment of the present application, said mixing in step (1) is performed in an inert gas atmosphere.

Preferably, the inert gas includes any one of helium gas, nitrogen gas, or argon gas, or a combination of at least two or more. A typical example of this combination is a combination of helium gas and argon gas. , a combination of nitrogen gas and argon gas, or a combination of helium gas and nitrogen gas, but not limited to these examples, and argon gas is preferred.

Preferably, the pressure of said inert gas is 0.02-0.06 MPa, such as 0.02 MPa, 0.03 MPa, 0.04 MPa, 0.05 MPa or 0.06 MPa, but the listed The numerical values are not limiting and other non-listed numerical values within this numerical range apply as well, preferably between 0.03 and 0.05 MPa.

In the present application, the mixing operation of tantalum powder and silicon powder is performed in an inert gas atmosphere, and the pressure of the inert gas is in the range of 0.02 to 0.06 MPa to ensure the uniformity of the mixed powder. On the other hand, the air content is reduced, the risk of air adsorption and oxidation caused by the fine particle size of the non-metallic silicon powder is reduced, and thus the product purity of the tantalum silicon alloy sputtering target material is finally improved.

As a preferred embodiment of the present application, the time of said mixing in step (1) is 12 to 48 h, such as 12 h, 18 h, 24 h, 30 h, 36 h, 42 h or 48 h, but limited to the numerical values recited. , other non-recited values within this numerical range apply as well, preferably between 12 and 24 h.

Preferably, said mixing in step (1) is carried out in a powder mixer.

Preferably, said powder mixer is a V-type powder mixer.

Preferably, the powder mixer is provided with an inner liner.

Preferably, said innerliner is a polyurethane innerliner.

The powder mixer described in this application is provided with a polyurethane inner liner to prevent direct contact between the tantalum silicon powder and the inner wall of the powder mixer, effectively avoiding contamination of the tantalum silicon powder, can further ensure the purity of

Preferably, the mixing speed of the powder mixer is 5-20 r/min, such as 5 r/min, 8 r/min, 10 r/min, 12 r/min, 15 r/min, 17 r/min or 20 r/min However, it is not intended to be limited to the listed values, and other non-listed values within this numerical range apply as well, preferably between 8 and 12 r/min.

Preferably, said mixing in step (1) includes stopping and beating.

Preferably, the time interval between stops is 3-6 h, such as 3 h, 3.5 h, 4 h, 4.5 h, 5.5 h, 6 h, but not limited to the values recited. , other unlisted values within this numerical range apply as well, preferably between 4 and 5h.

Preferably, the tapping process uses a rubber hammer.

Preferably, a washing step is further included prior to said mixing in step (1).

Preferably, the washing step is to wash the powder mixer so as not to contaminate the inside of the powder mixer.

As a preferred embodiment of the present application, said mold in step (2) is a rubber capsule.

Preferably, after charging the mold in step (2), it is hardened with a tool, covered with a mold cover, and sealed.

As a preferred embodiment of the present application, said cold isostatic pressure in step (3) is 140-250 MPa, such as 140 MPa, 160 MPa, 180 MPa, 200 MPa, 220 MPa or 250 MPa, but limited to the numerical values recited. other non-recited values within that numerical range apply as well, preferably between 160 and 200 MPa.

Preferably, the cold isostatic holding time in step (3) is 15-60 min, such as 15 min, 20 min, 25 min, 30 min, 35 min, 40 min, 45 min, 50 min, 55 min or 60 min. is not limited to the listed values, and other non-listed values within that numerical range apply as well, preferably between 20 and 40 min.

Preferably, said cold isostatic treatment in step (3) is performed in a cold isostatic press.

Cold isostatic pressing is a process that uses rubber or plastic as the capsule mold material and liquid as the pressure medium at room temperature, and is mainly used for molding powder materials. Provides the substrate to carry out the process.

As a preferred embodiment of the present application, said capsule in step (4) is a stainless steel capsule.

The stainless steel capsule of the present application is strongly welded and sealed with the capsule by arc welding, thus providing a basic guarantee for the subsequent degassing process.

Preferably, the temperature of said degassing treatment in step (4) is from 400 to 600° C., such as 400° C., 450° C., 500° C., 550° C. or 600° C., but limited to the values recited. other non-cited values within this numerical range apply as well, preferably 450-550°C.

Preferably, the degree of vacuum of the degassing treatment in step (4) is 5E-3Pa to 1.5E-3Pa, for example, 5E-3Pa, 4.5E-3Pa, 4E-3Pa, 3.5E-3Pa. , 3E-3Pa, 2.5E-3Pa, 2E-3Pa, 1.5E-3Pa, etc., but are not limited to the numerical values listed, and other unlisted numerical values within this numerical range. The same applies, preferably between 4E-3Pa and 2E-3Pa.

In the present application, by increasing the degree of vacuum in the degassing process to 5E-3Pa to 1.5E-3Pa, the gas inside the capsule is sufficiently degassed, the gas is completely discharged, and the silicon powder is removed from the air. It can further ensure that it will not be oxidized at , and finally further improve the product performance of the tantalum-silicon alloy sputtering target material. In addition, the degassing effect can be better ensured at the vacuum degree, which can minimize energy consumption and reduce cost input.

As a preferred embodiment of the present application, the temperature of the hot isostatic pressure treatment in step (5) is 1150 to 1250° C., such as 1150° C., 1170° C., 1200° C., 1230° C. or 1250° C., It is not intended to be limiting to the numerical values recited, and other non-recited numerical values within this numerical range apply as well.

Preferably, said hot isostatic pressure in step (5) is between 130 and 180 MPa, such as 130 MPa, 140 MPa, 150 MPa, 160 MPa, 170 MPa or 180 MPa, but limited to the values recited. other non-cited values within this numerical range apply as well, preferably between 140 and 165 MPa.

Preferably, the hot isostatic pressure retention time in step (5) is 2 to 6 h, such as 2 h, 3 h, 4 h, 5 h or 6 h, but is limited to the numerical values listed. other non-recited values within this numerical range apply as well, preferably between 3 and 5h.

Preferably, said hot isostatic treatment in step (5) is performed in a hot isostatic furnace.

The HIP process according to the present application is designed with the measured tantalum-silicon alloy recipes for the large differences in physical properties such as melting points and specific gravities of tantalum and silicon. At a high temperature of 1050 to 1350° C. and a high pressure of 130 to 180 MPa, the heat and pressure holding time is set to 2 to 6 hours. The tissue structure can be homogenized to minimize energy consumption and minimize costs.

As a preferred embodiment of the present application, the production method comprises
(1) Tantalum powder and silicon powder are charged in atomic proportions into a V-type powder mixer with a polyurethane inner liner, in an inert gas atmosphere at a pressure of 0.02 to 0.06 MPa, at a mixing speed of 8 to 12 r/min. Mixing for 12-24 h, stopping every 4-5 h in the mixing period and hitting the V-type powder mixer using a rubber hammer;
(2) a step of charging the tantalum silicon powder mixed in step (1) into a rubber capsule mold, solidifying it with a tool, and sealing;
(3) Place the mold sealed in step (2) into a cold isostatic press, pressurize to 160-200 MPa, hold pressure for 20-40 minutes and perform cold isostatic treatment to obtain a tantalum silicon material. process and
(4) putting the tantalum silicon material obtained in step (3) into a stainless capsule, sealing it, heating it to 400 to 600° C., and degassing it at a degree of vacuum of 4E-3Pa to 2E-3Pa;
(5) Put the degassed capsules in step (4) in a hot isostatic furnace, heat to 1050-1350°C, pressurize to 130-180 MPa, heat and hold for 2-6 hours, and heat. a step of subjecting to a pressure treatment to obtain a crude product of a tantalum silicon alloy sputtering target material;
(6) machining the crude tantalum silicon alloy sputtering target material obtained in step (5) to obtain a tantalum silicon alloy sputtering target material;
including.

In a preferred embodiment of the present application, the tantalum-silicon alloy sputtering target material in step (6) passes the size detection, and then undergoes the processes of washing, drying and packaging in order to achieve shipping standards.

A second object of the present application is to provide a tantalum-silicon alloy sputtering target material produced by the production method described in the first object.

As a preferred embodiment of the present application, the compactness of said tantalum silicon alloy sputtering target material is greater than 99%, such as 99.2%, 99.5%, 99.6%, 99.8% or 99.9% etc., but are not intended to be limited to the numerical values recited, and other non-recited numerical values within this numerical range apply as well.

The present application has at least the following effects when compared with the prior art.
(1) The method for producing a tantalum silicon alloy sputtering target material according to the present application combines a cold isostatic treatment, a degassing treatment, and a hot isostatic treatment, and furthermore, the temperature of the hot isostatic treatment is is 1050 to 1350° C., it is possible to obtain a tantalum silicon target material that can be applied to the production of a semiconductor target material having a denseness of 99% or more and a uniform microstructure.
(2) In the production method according to the present application, the powder mixing process is performed under an inert atmosphere, the pressure of the inert gas is in the range of 0.02 to 0.06 MPa, and the powder is stopped during mixing and beaten. Through the treatment, the powder mixer is further provided with a polyurethane inner liner to avoid the silicon powder from being adsorbed by the powder mixer, which not only ensures the uniformity of powder mixing, but also improves the mixing It can effectively reduce the air content in the subsequent tantalum silicon powder and ensure the purity of the product.
(3) In the production method according to the present application, by setting the degree of vacuum in the degassing process to a range of 5E-3Pa to 1.5E-3Pa, a better degassing effect is achieved, and the silicon powder is oxidized with air. to avoid as much as possible and further ensure the purity of the product.
(4) The method for producing the tantalum-silicon alloy sputtering target material according to the present application is also characterized by a simple process, easy operation, and a short production cycle.

Other aspects will be appreciated upon reading and understanding the detailed description and drawings.

FIG. 1 is a flowchart of a method for manufacturing a tantalum-silicon alloy sputtering target material according to the present application.

Aspects of the present application will now be further described by way of specific embodiments with reference to the accompanying drawings. As will be apparent to those skilled in the art, the above embodiments only aid in understanding the present application and should not be considered as specific limitations to the present application.

FIG. 1 shows a flow chart of a method for producing a tantalum silicon alloy sputtering target material according to the present application.
(1) mixing tantalum powder and silicon powder;
(2) a step of charging the tantalum silicon powder mixed in step (1) into a mold and sealing the mold;
(3) a step of cold isostatically treating the mold sealed in step (2) to obtain a tantalum silicon material;
(4) a step of welding the tantalum silicon material obtained in step (3) to a capsule and subjecting it to degassing;
(5) subjecting the degassed capsules in step (4) to hot isostatic pressure treatment at 1050 to 1350° C. to obtain a crude tantalum silicon alloy sputtering target material;
(6) machining the crude tantalum silicon alloy sputtering target material obtained in step (5) to obtain a tantalum silicon alloy sputtering target material;
(7) a step of detecting the size of the tantalum silicon alloy sputtering target material obtained in step (6), and successively washing, drying, and packaging the passed product;
(8) shipping the packaged product.

To facilitate understanding of the application, the application provides the following examples.

Example 1
This example is a method for producing a tantalum silicon alloy sputtering target material,
(1) A tantalum powder and a silicon powder with an atomic ratio of Si (at %) = 50% are charged into a V-type powder mixer with a polyurethane inner liner, and mixed at 6 r/min in an argon gas atmosphere at a pressure of 0.04 MPa. mixing at speed for 36 h, stopping every 6 h for the mixing period and hitting the V-type powder mixer with a rubber hammer;
(2) a step of charging the tantalum silicon powder mixed in step (1) into a rubber capsule mold, solidifying it with a tool, and sealing;
(3) A step of placing the rubber sleeve mold sealed in step (2) in a cold isostatic press, pressurizing to 200 MPa and holding pressure for 15 minutes to perform cold isostatic treatment to obtain a tantalum silicon material; ,
(4) Put the tantalum silicon material obtained in step (3) into a stainless capsule, weld the stainless steel cover and the capsule by arc welding, seal the capsule, heat to 550°C, and deaerate at a degree of vacuum of 2E-3Pa. and
(5) Put the degassed capsule in step (4) into a hot isostatic furnace, raise the temperature to 1250 ° C., pressurize to 175 MPa, and hold and heat for 3 hours to perform hot isostatic treatment, obtaining a crude tantalum-silicon alloy sputtering target material;
(6) machining the crude tantalum silicon alloy sputtering target material obtained in step (5) to obtain a tantalum silicon alloy sputtering target material;
(7) a step of detecting the size of the tantalum silicon alloy sputtering target material obtained in step (6), and successively washing, drying, and packaging the passed product;
(8) shipping the packaged product;
A manufacturing method is provided comprising:

Example 2
This example is a method for producing a tantalum silicon alloy sputtering target material,
(1) A tantalum powder and a silicon powder with an atomic ratio of Si (at %) = 50% are charged into a V-type powder mixer with a polyurethane inner liner, and mixed at 20 r/min in an argon gas atmosphere at a pressure of 0.05 MPa. Mixing at speed for 20 hours, stopping during the mixing period, and performing a beating process;
(2) a step of putting the tantalum silicon powder mixed in step (1) into a rubber capsule mold, then hardening it with a tool and sealing it;
(3) A step of placing the rubber sleeve mold sealed in step (2) in a cold isostatic press, pressurizing to 160 MPa and holding pressure for 20 minutes to perform cold isostatic treatment to obtain a tantalum silicon material; ,
(4) Put the tantalum silicon material obtained in step (3) into a stainless capsule, weld the stainless steel cover and the capsule by arc welding, seal the capsule, heat to 550°C, and deaerate at a degree of vacuum of 2E-3Pa. and
(5) Put the degassed capsule in step (4) into a hot isostatic furnace, raise the temperature to 1300 ° C., pressurize to 165 MPa, and hold and heat for 3 hours to perform hot isostatic treatment, obtaining a crude tantalum-silicon alloy sputtering target material;
(6) machining the crude tantalum silicon alloy sputtering target material obtained in step (5) to obtain a tantalum silicon alloy sputtering target material;
(7) a step of detecting the size of the tantalum silicon alloy sputtering target material obtained in step (6), and successively washing, drying, and packaging the passed product;
(8) shipping the packaged product;
A manufacturing method is provided comprising:

Example 3
This example is a method for producing a tantalum silicon alloy sputtering target material,
(1) Tantalum powder and silicon powder with an atomic ratio of Si (at %) = 56% are charged into a V-type powder mixer with a polyurethane inner liner, and mixed at 12 r/min in an argon gas atmosphere with a pressure of 0.05 MPa. mixing at speed for 12 h, stopping every 3 h for the mixing period and hitting the V-type powder mixer with a rubber hammer;
(2) a step of charging the tantalum silicon powder mixed in step (1) into a rubber capsule mold, solidifying it with a tool, and sealing;
(3) A step of placing the rubber sleeve mold sealed in step (2) in a cold isostatic press, pressurizing to 250 MPa and holding pressure for 40 minutes to perform cold isostatic treatment to obtain a tantalum silicon material; ,
(4) Put the tantalum silicon material obtained in step (3) into a stainless steel capsule, weld the stainless steel cover and the capsule by arc welding to seal the seal, heat to 450 ° C., and desorb at a degree of vacuum of 5.5E-3 Pa. a step of air-treating;
(5) Put the degassed capsule in step (4) into a hot isostatic furnace, raise the temperature to 1150 ° C., pressurize to 150 MPa, and heat and hold for 4 h to perform hot isostatic treatment, obtaining a crude tantalum-silicon alloy sputtering target material;
(6) machining the crude tantalum silicon alloy sputtering target material obtained in step (5) to obtain a tantalum silicon alloy sputtering target material;
(7) a step of detecting the size of the tantalum silicon alloy sputtering target material obtained in step (6), and successively washing, drying, and packaging the passed product;
(8) shipping the packaged product;
A manufacturing method is provided comprising:

Example 4
This example is a method for producing a tantalum silicon alloy sputtering target material,
(1) Tantalum powder and silicon powder with an atomic ratio of Si (at %) = 65% are charged into a V-type powder mixer with a polyurethane inner liner, and mixed at 10 r/min in an argon gas atmosphere with a pressure of 0.05 MPa. Mixing at speed for 20 h, stopping every 4 h for the mixing period and hitting the V-type powder mixer with a rubber hammer;
(2) a step of charging the tantalum silicon powder mixed in step (1) into a rubber capsule mold, solidifying it with a tool, and sealing;
(3) A step of placing the rubber sleeve mold sealed in step (2) in a cold isostatic press, pressurizing to 140 MPa and holding pressure for 60 minutes to perform cold isostatic treatment to obtain a tantalum silicon material; ,
(4) Put the tantalum silicon material obtained in step (3) into a stainless capsule, seal the capsule by welding the stainless steel cover and the capsule by arc welding, heat to 500°C, and deaerate at a degree of vacuum of 5E-3Pa. and
(5) Put the degassed capsule in step (4) into a hot isostatic furnace, raise the temperature to 1200 ° C., pressurize to 140 MPa, and hold and heat for 4 h to perform hot isostatic treatment, obtaining a crude tantalum-silicon alloy sputtering target material;
(6) machining the crude tantalum silicon alloy sputtering target material obtained in step (5) to obtain a tantalum silicon alloy sputtering target material;
(7) a step of detecting the size of the tantalum silicon alloy sputtering target material obtained in step (6), and successively washing, drying, and packaging the passed product;
(8) shipping the packaged product;
A manufacturing method is provided comprising:

Comparative example 1
In this comparative example, the process conditions are the same as those in Example 1, except that the hot isostatic pressure temperature in step (5) was changed to 1400°C.

Comparative example 2
In this comparative example, the process conditions are the same as in Example 1, except that the hot isostatic pressure temperature in step (5) was changed to 1000°C.

The tantalum silicon alloy sputtering target materials obtained in the above examples and comparative examples were evaluated for compactness, uniformity of the internal structure, and product appearance. Table 1 shows the specific results.

From Table 1, the following conclusions can be drawn.
(1) The tantalum silicon alloy sputtering target materials obtained in Examples 1 to 4 not only have a density of 99% or more, but also have a microscopically uniform and dense structure without cavities and a layered structure. It has the feature that it does not have any, and it meets the manufacturing requirements of semiconductor target materials.
(2) In Example 2, since the tantalum silicon powder was not stopped during mixing and the beating treatment was not performed, a small amount of the silicon powder agglomerated, resulting in a small amount of fine black spots on the product appearance of the obtained tantalum silicon alloy sputtering target material. was generated. In Example 3, since the degree of vacuum during the degassing treatment was 5.5E-3 Pa, the degassing effect was slightly deteriorated, and the compactness of the obtained tantalum silicon alloy sputtering target material had just reached 99.1%. is.
(3) In Comparative Example 1, the hot isostatic pressure temperature is 1400°C, which is relatively high, so the product density is not high, and the product has microscopic cavities, making the product fragile and easy to break. caused a problem. In Comparative Example 2, the temperature of hot isostatic pressing was relatively low at 1000°C, so not only was the density of the product low, but the product had microscopic cavities and had a layered structure. . Therefore, the tantalum-silicon alloy sputtering target materials obtained in the two comparative examples do not satisfy the standard in terms of uniformity of density and internal structure.

As described above, the production method according to the present application not only effectively prevents the oxidation of the silicon powder and ensures the purity of the product, but also allows the tantalum silicon alloy sputtering target material to have a denseness greater than 99% and an internal It can meet the requirement of uniform structure, and has the characteristics of simple process, easy operation and short production cycle.

Applicant believes that although the application describes the detailed structural features of the present application through the above examples, the application is not limited to the above detailed structural features, and that the application is not limited to the above detailed structural features. It did not imply that it must be implemented in reliance on structural features.

Although the preferred embodiments of the present application have been described in detail above, the present application is not limited to the specific details in the above-described embodiments, and within the scope of the technical concept of the present application, Various simple modifications can be added to the technical scheme.

It should be noted that the individual specific technical features described in the specific embodiments above may be combined in any suitable manner if not contradictory, and in order to avoid unnecessary duplication, the The application omits the various possible combinations.

Claims (10)

A method for producing a tantalum silicon alloy sputtering target material, comprising:
(1) tantalum powder and silicon powder are mixed in an atomic ratio , mixing is performed in a powder mixer, mixing includes stopping and beating, and the interval time between stopping is 3 to 6 hours; a process and
(2) a step of charging the tantalum silicon powder mixed in step (1) into a mold and sealing the mold;
(3) a step of cold isostatically treating the mold sealed in step (2) to obtain a tantalum silicon material;
(4) The tantalum silicon material obtained in step (3) is placed in a capsule, sealed, and degassed. process and
(5) subjecting the capsule deaerated in step (4) to hot isostatic pressure treatment at 1050 to 1350° C. to obtain a crude tantalum silicon alloy sputtering target material;
(6) machining the crude tantalum silicon alloy sputtering target material obtained in step (5) to obtain a tantalum silicon alloy sputtering target material;
Manufacturing method including. The mixing in step (1) is performed in an inert gas atmosphere,
The manufacturing method according to claim 1. The pressure of the inert gas is 0.02 to 0.06 MPa,
The manufacturing method according to claim 2. The interval time between stops in step (1) is 4 to 5 h.
The production method according to any one of claims 1 to 3. Mixing in step (1) includes stopping, beating,
The manufacturing method according to claim 4. The mold in step (2) is a rubber capsule,
The production method according to any one of claims 1 to 5. The pressure of the cold isostatic treatment in step (3) is 140 to 250 MPa,
The production method according to any one of claims 1 to 6. The capsule in step (4) is a stainless capsule,
The production method according to any one of claims 1 to 7. The temperature of the hot isostatic treatment in step (5) is 1150 to 1250 ° C.
The production method according to any one of claims 1 to 8. The manufacturing method is
(1) Tantalum powder and silicon powder are charged in atomic proportions into a V-type powder mixer with a polyurethane inner liner , in an inert gas atmosphere at a pressure of 0.02 to 0.06 MPa, at a mixing speed of 8 to 12 r/min. Mixing for 12 to 24 hours, stopping every 4 to 5 hours in the mixing period and hitting the V-type powder mixer with a rubber hammer;
(2) a step of charging the tantalum silicon powder mixed in step (1) into a rubber capsule mold, solidifying it with a tool, and sealing;
(3) Place the mold sealed in step (2) into a cold isostatic press, pressurize to 160-200 MPa, hold pressure for 20-40 minutes and perform cold isostatic treatment to obtain a tantalum silicon material. process and
(4) putting the tantalum silicon material obtained in step (3) into a stainless capsule, sealing it, heating it to 400 to 600° C., and degassing it at a degree of vacuum of 4E-3Pa to 2E-3Pa;
(5) Put the degassed capsules in step (4) in a hot isostatic furnace, heat to 1050-1350°C, pressurize to 130-180 MPa, heat and hold for 2-6 hours, and heat. a step of subjecting to a pressure treatment to obtain a crude product of a tantalum silicon alloy sputtering target material;
(6) machining the crude tantalum silicon alloy sputtering target material obtained in step (5) to obtain a tantalum silicon alloy sputtering target material;
The production method according to any one of claims 1 to 9, comprising

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