CN114717528B - Titanium-containing target material and preparation method thereof - Google Patents

Titanium-containing target material and preparation method thereof Download PDF

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CN114717528B
CN114717528B CN202210357625.8A CN202210357625A CN114717528B CN 114717528 B CN114717528 B CN 114717528B CN 202210357625 A CN202210357625 A CN 202210357625A CN 114717528 B CN114717528 B CN 114717528B
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titanium
heat treatment
target
forging
temperature
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CN114717528A (en
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姚力军
潘杰
王学泽
周友平
周敏
陈勇军
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Ningbo Jiangfeng Electronic Material Co Ltd
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Ningbo Jiangfeng Electronic Material Co Ltd
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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
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • 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
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Abstract

The invention provides a titanium-containing target and a preparation method thereof, wherein the preparation method comprises the following steps: and forging, primary heat treatment, cold rolling and secondary heat treatment are sequentially carried out on the titanium-containing target blank, so as to obtain the titanium-containing target. According to the method, a proper preparation process is selected according to the material of the target, the internal tissue structure of the target is optimized through controlling the heat treatment and the rolling process, and the recrystallization process and the uniformity of the grain size are controlled, so that the uniformity of the coating film during sputtering of the target can be improved, and the quality of the coating film is improved; the method can effectively enhance the strength of the target material and avoid generating cracks during high-power sputtering; the method is simple to operate, low in required cost and wide in application range.

Description

Titanium-containing target material and preparation method thereof
Technical Field
The invention belongs to the technical field of target preparation, and relates to a titanium-containing target and a preparation method thereof.
Background
The magnetron sputtering technology is one of the key technologies for preparing the film material, and the target material is the key consumable in the magnetron sputtering technology. The sputtering method mainly refers to the process of bombarding the surface of a target material by adopting high-energy particles to enable atoms or molecules on the surface of the target material to be sprayed on the surface of a substrate to form a layer of compact film, and as the film material has higher requirements on uniformity when being applied to the fields of semiconductor chips, flat panel displays and the like, the uniformity of the internal tissue structure of the sputtering target material is ensured, so that the uniformity of a coating film can be ensured, and therefore, different processes are selected according to different materials for processing and preparing the target material.
The processing preparation of the target material generally adopts the processing modes of forging, hot rolling, cold rolling and the like, and then carries out heat treatment and necessary machining to prepare a target material product meeting the requirements, but the traditional operation steps often have difficulty in effectively adjusting the internal tissue structure of the target material and controlling the uniformity of the grain size of the target material, so that the uniformity of the film during sputtering coating cannot be ensured; in addition, because of different target materials, high-power sputtering is sometimes required, and cracks are easily generated on the surface of the target at the moment, so that the sputtering coating process is influenced, and a proper processing technology is required to be selected according to the different target materials, so that the internal tissue structure can be optimized, and the strength of the target can be enhanced.
CN 103215553a discloses a method for preparing a high-purity titanium plate for target materials, which comprises the following steps: pressing titanium sponge particles into electrode blocks, and then welding the electrode blocks into consumable electrodes; then the consumable electrode is subjected to vacuum consumable arc melting to obtain an ingot; carrying out first heating treatment on the cast ingot; forging the ingot by upsetting and drawing to obtain a plate blank; performing second heating treatment on the slab; then rolling to obtain a semi-finished plate; annealing, straightening and surface grinding the semi-finished plate to obtain a high-purity titanium plate for the target; the method has more operation steps, and has the advantages that important description is made for the preparation process of the cast ingot, the heat treatment and the subsequent upsetting forging are also arranged for the defects of the cast ingot, the influence of the heat treatment and the subsequent upsetting forging on the internal crystal structure is not clear, the heat treatment temperature is higher, and the energy consumption is higher.
CN 106884142a discloses a method for preparing a high quality TiN film, which comprises the following steps: selecting Ti cast ingots, forging, rolling, heat treatment, leveling and machining to prepare titanium laths; then carrying out laser engraving treatment on the titanium plate strip, rolling the engraved titanium plate strip into a titanium ring by using a rolling machine, and cleaning and drying the titanium plate strip to obtain a sputtered titanium ring; using a steel sheet as a matrix, bonding a titanium ring and titanium palladium by adopting conductive adhesive to serve as a target, and depositing a TiN film on the steel sheet; in the method, the preparation of the sputtered titanium ring is only one operation, the key point is the preparation of the TiN film, the sputtered titanium ring is not a main body part in the target material, the sputtered titanium ring is assembled with a titanium target to form the target material, and the preparation process of the titanium ring does not mention the regulation and control of the internal tissue structure.
In summary, for the preparation process of the titanium-containing target, the process steps of the preparation process are controlled according to the use requirement of the target, and the recrystallization process is regulated and controlled to optimize the internal tissue structure of the target, and meanwhile, the strength of the target is improved, so that the uniformity and the coating rate of the subsequent coating are improved.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention aims to provide a titanium-containing target material and a preparation method thereof, wherein the method selects a proper preparation process according to the material of the target material, optimizes the internal tissue structure of the target material through controlling the heat treatment and rolling process, and controls the recrystallization process and the uniformity of the grain size of the target material so as to ensure the uniformity of a coating film; meanwhile, the strength of the target material is enhanced, and cracks are avoided during high-power sputtering.
To achieve the purpose, the invention adopts the following technical scheme:
in one aspect, the invention provides a method for preparing a titanium-containing target, the method comprising the steps of:
and forging, primary heat treatment, cold rolling and secondary heat treatment are sequentially carried out on the titanium-containing target blank, so as to obtain the titanium-containing target.
According to the invention, a titanium-containing target blank, especially a high-purity titanium target blank, is firstly subjected to preliminary forging according to the material characteristics, coarse grains are thinned to obtain a compact metal structure, the mechanical property of the metal is improved, the basic shape of the metal is controlled, then, primary heat treatment is carried out, forging internal stress is mainly eliminated, the deformation and crack tendency in the subsequent processing process are reduced, cold rolling treatment is carried out after the primary heat treatment, cold deformation is controlled, the subsequent grains are driven to be recrystallized, and finally, the secondary heat treatment and rapid cooling are carried out to reorganize the structure of the target, optimize the structure of the blank, control the recrystallization process of the blank, obtain the incompletely recrystallized target, ensure the uniformity of the structure of the internal structure of the target, and further improve the uniformity of the coating film during sputtering of the target and the quality of the coating film; meanwhile, the method can also effectively enhance the strength of the target material, and cracks can not be generated even if high-power sputtering is carried out; the method is simple to operate, low in required cost and wide in application range.
The following technical scheme is a preferred technical scheme of the invention, but is not a limitation of the technical scheme provided by the invention, and the technical purpose and beneficial effects of the invention can be better achieved and realized through the following technical scheme.
As a preferable technical scheme of the invention, the titanium-containing target comprises a high-purity titanium target.
Preferably, the purity of the high purity titanium target is 4N or more, for example, 4N5, 5N or 5N5, etc., but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
As a preferable technical scheme of the invention, the titanium-containing target blank is preheated before forging.
The temperature of the preheating is preferably 450 to 550 ℃, for example, 450 ℃, 460 ℃, 480 ℃, 500 ℃, 520 ℃, 540 ℃, 550 ℃, or the like, but is not limited to the values listed, and other values not listed in the range are equally applicable.
Preferably, the preheating is performed for a period of time ranging from 90 to 150 minutes, for example, 90 minutes, 100 minutes, 110 minutes, 120 minutes, 130 minutes, 140 minutes, 150 minutes, etc., but the preheating is not limited to the recited values, and other values not recited in the range of values are equally applicable.
Preferably, the forging is performed after the heat preservation is completed, and the forging ratio per forging is 1.5 to 2.5, for example, 1.5, 1.6, 1.8, 2.0, 2.2, or 2.5, etc., but the forging ratio is not limited to the recited values, and other non-recited values within the range of the recited values are equally applicable.
Preferably, the forging is repeated 3 to 5 times, for example 3 times, 4 times or 5 times.
In the invention, the target blank is preheated before forging, mainly for facilitating deformation of the blank and reducing forging difficulty, and the preheating temperature is relatively high, mainly because the melting point of titanium is high, if the preheating temperature is too low, the effect cannot be achieved, and meanwhile, the external shape and the organization structure of the blank can be primarily adjusted; the forging ratio generally refers to the ratio of the cross-sectional areas before and after deformation.
In a preferred embodiment of the present invention, the temperature of the primary heat treatment is 400 to 500 ℃, for example 400 ℃, 420 ℃, 445 ℃, 450 ℃, 460 ℃, 480 ℃, 500 ℃, or the like, but the present invention is not limited to the above-mentioned values, and other values not mentioned in the above-mentioned value range are similarly applicable.
Preferably, the heat-retaining time of the primary heat treatment is 60 to 180min, for example, 60min, 75min, 90min, 105min, 120min, 135min, 150min or 180min, etc., but not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, air cooling is performed after the primary heat treatment and heat preservation are finished until the temperature is reduced to normal temperature.
In a preferred embodiment of the present invention, the total deformation amount of the cold rolling is 50 to 85% of the thickness before cold rolling, for example, 50%, 55%, 60%, 65%, 70%, 75%, 80% or 85%, etc., but the total deformation amount is not limited to the above-mentioned values, and other values not mentioned in the above-mentioned value range are equally applicable.
Preferably, the amount of cold rolling reduction per pass is 10 to 20mm, for example 10mm, 12mm, 15mm, 16mm, 18mm or 20mm, etc., but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
According to the invention, rolling of the target blank is performed under normal temperature, the required pressure is large according to the material selection of the titanium target, the deformation of the target blank in the process is large, the crystal grains are rotationally deformed in the rolling process, the preferential orientation is realized, and the strength is increased.
In a preferred embodiment of the present invention, the temperature of the secondary heat treatment is 300 to 400 ℃, for example 300 ℃, 320 ℃, 340 ℃, 350 ℃, 360 ℃, 380 ℃, 400 ℃, or the like, but the present invention is not limited to the above-mentioned values, and other values not mentioned in the above-mentioned value range are equally applicable.
Preferably, the heat-preserving time of the secondary heat treatment is 60 to 180min, for example, 60min, 75min, 90min, 105min, 120min, 135min, 150min or 180min, etc., but not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, water cooling is performed after the heat preservation of the secondary heat treatment is finished until the temperature is reduced to normal temperature.
Preferably, the water cooling rate is 50 to 100 ℃/s, for example, 50 ℃/s, 60 ℃/s, 70 ℃/s, 80 ℃/s, 90 ℃/s, 100 ℃/s, or the like, but is not limited to the recited values, and other non-recited values within the range are equally applicable.
In the present invention, the recrystallization process of the target blank is controlled by the secondary heat treatment and the subsequent water cooling treatment, and the incompletely recrystallized target is obtained, and the recrystallization degree at this time is about 40 to 70%, for example 40%, 45%, 50%, 55%, 60%, 65% or 70%, and the like, and the strength is remarkably improved compared with the complete recrystallization of the target.
As a preferable technical scheme of the invention, the secondary heat treatment is followed by machining.
Preferably, the machining processes the target to a desired shape and size.
As a preferable technical scheme of the invention, the preparation method comprises the following steps:
forging, primary heat treatment, cold rolling and secondary heat treatment are sequentially carried out on the titanium-containing target blank to obtain a titanium-containing target;
the titanium-containing target blank is preheated before being forged, the preheating temperature is 450-550 ℃, the heat preservation time is 90-150 min, the forging is carried out after the heat preservation is finished, the forging ratio of each forging is 1.5-2.5, and the repetition number of the forging is 3-5;
the temperature of the primary heat treatment is 400-500 ℃, the heat preservation time is 60-180 min, and air cooling is carried out after the heat preservation is finished until the temperature is reduced to normal temperature; then cold rolling is carried out, the total deformation of the cold rolling is 50-85% of the thickness before cold rolling, and the pressing amount of each pass of cold rolling is 10-20 mm;
the temperature of the secondary heat treatment is 300-400 ℃, the heat preservation time is 60-180 min, water cooling is carried out after the heat preservation is finished, and the water cooling speed is 50-100 ℃/s until the temperature is reduced to normal temperature; and machining to the required shape and size to obtain the titanium-containing target.
In another aspect, the present invention provides a titanium-containing target obtained by the above-described production method, wherein the grain size of the titanium-containing target is 10 to 15 μm, for example, 10 μm, 11 μm, 12 μm, 13 μm, 14 μm or 15 μm, etc., but the present invention is not limited to the listed values, and other non-listed values within the range of the values are equally applicable.
Compared with the prior art, the invention has the following beneficial effects:
(1) According to the method, a proper preparation process is selected according to the material of the target, the internal tissue structure of the target is optimized through controlling the heat treatment and the rolling process, the recrystallization process and the uniformity of the grain size are controlled, and the grain size can be controlled within 10-15 mu m, so that the uniformity of a coating film during sputtering of the target can be improved, and the quality of the coating film is improved;
(2) The method can effectively enhance the strength of the target material, avoid generating cracks during high-power sputtering, and ensure that the strength of the target material can reach more than 130 HV;
(3) The method disclosed by the invention is simple to operate, low in required cost and wide in application range.
Detailed Description
For better illustrating the present invention, the technical scheme of the present invention is convenient to understand, and the present invention is further described in detail below. The following examples are merely illustrative of the present invention and are not intended to represent or limit the scope of the invention as defined in the claims.
The invention provides a preparation method of a titanium-containing target in the specific embodiment part, which comprises the following steps:
and forging, primary heat treatment, cold rolling and secondary heat treatment are sequentially carried out on the titanium-containing target blank, so as to obtain the titanium-containing target.
The following are exemplary but non-limiting examples of the invention:
example 1:
the embodiment provides a preparation method of a titanium target, which comprises the following steps:
forging, primary heat treatment, cold rolling and secondary heat treatment are sequentially carried out on the titanium target blank to obtain a titanium target;
the purity of the titanium target blank is 4N5, preheating is carried out before forging, the preheating temperature is 500 ℃, the heat preservation time is 120min, forging is carried out after heat preservation is finished, the forging ratio of each forging is 2.0, and the repetition number of the forging is 4;
the temperature of the primary heat treatment is 450 ℃, the heat preservation time is 120min, and air cooling is carried out after the heat preservation is finished until the temperature is reduced to normal temperature; then cold rolling is carried out, the total deformation of the cold rolling is 70% of the thickness before cold rolling, and the pressing amount of each pass of cold rolling is 15mm;
the temperature of the secondary heat treatment is 350 ℃, the heat preservation time is 120min, water cooling is carried out after the heat preservation is finished, the water cooling speed is 100 ℃/s, and the temperature is reduced to the normal temperature; and machining to the required shape and size to obtain the high-purity titanium target.
In the embodiment, the titanium target material is prepared by adopting the method, the obtained target material has uniform tissue structure, incomplete recrystallization is controlled, the grain size is uniformly distributed, the size is controlled within the range of 10-12 mu m, and the uniformity of the coating film is controlled; the strength of the target reaches 134HV, and no crack is generated during sputtering.
Example 2:
the embodiment provides a preparation method of a titanium target, which comprises the following steps:
forging, primary heat treatment, cold rolling and secondary heat treatment are sequentially carried out on the titanium target blank to obtain a titanium target;
the purity of the titanium target blank is 4N, preheating is carried out before forging, the preheating temperature is 550 ℃, the heat preservation time is 90min, forging is carried out after heat preservation is finished, the forging ratio of each forging is 2.5, and the repetition number of the forging is 5;
the temperature of the primary heat treatment is 500 ℃, the heat preservation time is 60min, and air cooling is carried out after the heat preservation is finished until the temperature is reduced to normal temperature; then cold rolling is carried out, the total deformation of the cold rolling is 50% of the thickness before cold rolling, and the pressing amount of each pass of cold rolling is 10mm;
the temperature of the secondary heat treatment is 300 ℃, the heat preservation time is 180min, water cooling is carried out after the heat preservation is finished, and the water cooling speed is 80 ℃/s until the temperature is reduced to normal temperature; and machining to the required shape and size to obtain the high-purity titanium target.
In the embodiment, the titanium target material is prepared by adopting the method, the obtained target material has uniform tissue structure, incomplete recrystallization is controlled, the grain size is uniformly distributed, the size is controlled within the range of 10-12 mu m, and the uniformity of the coating film is controlled; the strength of the target reaches 140HV, and no crack is generated during sputtering.
Example 3:
the embodiment provides a preparation method of a titanium alloy target, which comprises the following steps:
forging, primary heat treatment, cold rolling and secondary heat treatment are sequentially carried out on the titanium target blank to obtain a titanium target;
the purity of the titanium target blank is 5N, preheating is carried out before forging, the preheating temperature is 450 ℃, the heat preservation time is 150min, forging is carried out after heat preservation is finished, the forging ratio of each forging is 1.5, and the repetition number of the forging is 3;
the temperature of the primary heat treatment is 400 ℃, the heat preservation time is 180min, and air cooling is carried out after the heat preservation is finished until the temperature is reduced to normal temperature; then cold rolling is carried out, the total deformation of the cold rolling is 80% of the thickness before cold rolling, and the pressing amount of each pass of cold rolling is 20mm;
the temperature of the secondary heat treatment is 400 ℃, the heat preservation time is 60min, water cooling is carried out after the heat preservation is finished, the water cooling speed is 50 ℃/s, and the temperature is reduced to the normal temperature; and machining to the required shape and size to obtain the high-purity titanium target.
In the embodiment, the titanium target material is prepared by adopting the method, the obtained target material has uniform tissue structure, incomplete recrystallization is controlled, the grain size is uniformly distributed, the size is controlled within the range of 10-13 mu m, and the uniformity of the coating film is controlled; the strength of the target reaches 132HV, and no crack is generated during sputtering.
Example 4:
the embodiment provides a preparation method of a titanium target, which comprises the following steps:
forging, primary heat treatment, cold rolling and secondary heat treatment are sequentially carried out on the titanium target blank to obtain a titanium target;
the purity of the titanium target blank is 4N, preheating is carried out before forging, the preheating temperature is 525 ℃, the heat preservation time is 135min, forging is carried out after heat preservation is finished, the forging ratio of each forging is 1.8, and the repetition number of the forging is 4;
the temperature of the primary heat treatment is 420 ℃, the heat preservation time is 150min, and air cooling is carried out after the heat preservation is finished until the temperature is reduced to normal temperature; then cold rolling is carried out, the total deformation of the cold rolling is 60% of the thickness before cold rolling, and the pressing amount of each pass of cold rolling is 18mm;
the temperature of the secondary heat treatment is 320 ℃, the heat preservation time is 90min, and water cooling is carried out after the heat preservation is finished, wherein the water cooling rate is 70 ℃/s until the temperature is reduced to normal temperature; and machining to the required shape and size to obtain the high-purity titanium target.
In the embodiment, the titanium target material is prepared by adopting the method, the obtained target material has uniform tissue structure, incomplete recrystallization is controlled, the grain size is uniformly distributed, the size is controlled within the range of 10-12 mu m, and the uniformity of the coating film is controlled; the strength of the target reaches 130HV, and no crack is generated during sputtering.
Example 5:
the embodiment provides a preparation method of a titanium target, which comprises the following steps:
forging, primary heat treatment, cold rolling and secondary heat treatment are sequentially carried out on the titanium target blank to obtain a titanium target;
the purity of the titanium target blank is 4N5, preheating is carried out before forging, the preheating temperature is 480 ℃, the heat preservation time is 100min, forging is carried out after heat preservation is finished, the forging ratio of each forging is 2.2, and the repetition number of the forging is 3;
the temperature of the primary heat treatment is 480 ℃, the heat preservation time is 90min, and air cooling is carried out after the heat preservation is finished until the temperature is reduced to normal temperature; then cold rolling is carried out, the total deformation of the cold rolling is 75% of the thickness before cold rolling, and the pressing amount of each pass of cold rolling is 12.5mm;
the temperature of the secondary heat treatment is 360 ℃, the heat preservation time is 150min, water cooling is carried out after the heat preservation is finished, and the water cooling speed is 80 ℃/s until the temperature is reduced to the normal temperature; and machining to the required shape and size to obtain the high-purity titanium target.
In the embodiment, the titanium target material is prepared by adopting the method, the obtained target material has uniform tissue structure, incomplete recrystallization is controlled, the grain size is uniformly distributed, the size is controlled within the range of 10-15 mu m, and the uniformity of the coating film is controlled; the strength of the target reaches 135HV, and no crack is generated during sputtering.
It can be seen from the above embodiments that, according to the method of the present invention, a suitable preparation process is selected according to the material of the target, and the internal structure of the target is optimized by controlling the heat treatment and the rolling process, and the recrystallization process and the uniformity of the grain size are controlled, and the grain size is controlled within the range of 10-15 μm, so that the uniformity of the coating film during sputtering of the target can be improved, and the quality of the coating film is improved; the method can effectively enhance the strength of the target material, avoid generating cracks during high-power sputtering, and ensure that the strength of the target material can reach more than 130 HV; the method is simple to operate, low in required cost and wide in application range.
The present invention is described in detail by the above examples, but the present invention is not limited to the above detailed methods, i.e., it does not mean that the present invention must be practiced depending on the above detailed methods. It should be apparent to those skilled in the art that any modifications of the present invention, equivalent substitutions for the method of the present invention, addition of auxiliary steps, selection of specific modes, etc., are within the scope of the present invention and the scope of the disclosure.

Claims (11)

1. The preparation method of the titanium-containing target material is characterized by comprising the following steps of:
forging, primary heat treatment, cold rolling and secondary heat treatment are sequentially carried out on the titanium-containing target blank to obtain a titanium-containing target; the repetition number of the forging is 3-5, and the forging ratio of each forging is 1.5-2.5; the temperature of the primary heat treatment is 400-500 ℃, the heat preservation time of the primary heat treatment is 60-180 min, and air cooling is carried out after the heat preservation of the primary heat treatment is finished until the temperature is reduced to normal temperature; the total deformation of the cold rolling is 50-85% of the thickness before cold rolling, and the pressing amount of each pass of cold rolling is 10-20 mm; the temperature of the secondary heat treatment is 300-400 ℃, the heat preservation time of the secondary heat treatment is 60-180 min, water cooling is carried out after the heat preservation of the secondary heat treatment is finished, and the water cooling speed is 50-100 ℃/s until the temperature is reduced to normal temperature.
2. The method of claim 1, wherein the titanium-containing target comprises a high purity titanium target.
3. The method according to claim 2, wherein the purity of the high purity titanium target is 4N or more.
4. The method of claim 1, wherein the titanium-containing target blank is preheated prior to forging.
5. The method according to claim 4, wherein the preheating temperature is 450-550 ℃.
6. The preparation method of claim 4, wherein the preheating has a holding time of 90-150 min.
7. The method according to claim 6, wherein forging is performed after the heat preservation is completed.
8. The method of claim 1, wherein the secondary heat treatment is followed by machining.
9. The method of claim 8, wherein the machining processes the target to a desired shape and size.
10. The preparation method according to claim 1, characterized in that the preparation method comprises the steps of:
forging, primary heat treatment, cold rolling and secondary heat treatment are sequentially carried out on the titanium-containing target blank to obtain a titanium-containing target;
the titanium-containing target blank is preheated before being forged, the preheating temperature is 450-550 ℃, the heat preservation time is 90-150 min, the forging is carried out after the heat preservation is finished, the forging ratio of each forging is 1.5-2.5, and the number of times of forging repetition is 3-5 times;
the temperature of the primary heat treatment is 400-500 ℃, the heat preservation time is 60-180 min, and air cooling is carried out after the heat preservation is finished until the temperature is reduced to normal temperature; then cold rolling is carried out, the total deformation of the cold rolling is 50-85% of the thickness before cold rolling, and the pressing amount of each pass of cold rolling is 10-20 mm;
the temperature of the secondary heat treatment is 300-400 ℃, the heat preservation time is 60-180 min, water cooling is carried out after the heat preservation is finished, and the water cooling speed is 50-100 ℃/s until the temperature is reduced to normal temperature; and machining to the required shape and size to obtain the titanium-containing target.
11. A titanium-containing target material obtained by the preparation method according to any one of claims 1 to 10, wherein the grain size of the titanium-containing target material is 10 to 15 μm.
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JP2000045067A (en) * 1998-07-27 2000-02-15 Nippon Steel Corp High purity titanium sheet for titanium target material and its production
CN103215553A (en) * 2013-04-27 2013-07-24 西部钛业有限责任公司 Method for preparing high-purity titanium plate for use as target
CN107523795A (en) * 2017-10-24 2017-12-29 宝鸡市铭坤有色金属有限公司 A kind of manufacture method of titanium target material

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JP3659921B2 (en) * 2002-01-15 2005-06-15 東邦チタニウム株式会社 Method for manufacturing target titanium material
CN102791905B (en) * 2010-03-11 2015-04-01 株式会社东芝 Sputtering target, method for producing same and method for producing semiconductor device
JP7179450B2 (en) * 2017-09-21 2022-11-29 Ｊｘ金属株式会社 Titanium target for sputtering, method for producing same, and method for producing titanium-containing thin film

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JP2000045067A (en) * 1998-07-27 2000-02-15 Nippon Steel Corp High purity titanium sheet for titanium target material and its production
CN103215553A (en) * 2013-04-27 2013-07-24 西部钛业有限责任公司 Method for preparing high-purity titanium plate for use as target
CN107523795A (en) * 2017-10-24 2017-12-29 宝鸡市铭坤有色金属有限公司 A kind of manufacture method of titanium target material

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