CN111058004A - Chromium-silicon alloy sputtering target material and preparation method thereof - Google Patents
Chromium-silicon alloy sputtering target material and preparation method thereof Download PDFInfo
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- CN111058004A CN111058004A CN202010002184.0A CN202010002184A CN111058004A CN 111058004 A CN111058004 A CN 111058004A CN 202010002184 A CN202010002184 A CN 202010002184A CN 111058004 A CN111058004 A CN 111058004A
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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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- 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
- B22F3/093—Compacting only using vibrations or friction
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- 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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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/10—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying using centrifugal force
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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Abstract
The invention relates to a chromium-silicon alloy sputtering target material and a preparation method thereof. The preparation method comprises the following steps: (1) filling chromium-silicon alloy powder with a target mass ratio into a die, sealing the die, and performing tap treatment; (2) degassing the mould compacted in the step (1); (3) carrying out hot isostatic pressing treatment on the mould degassed in the step (2) at the temperature of 1000-; (4) and (4) obtaining the chromium-silicon alloy sputtering target after machining. The preparation method is simple in process, only needs one-time die filling treatment, reduces the risk of oxidation of the product, ensures the purity of the product, can improve the processing efficiency of the product, is convenient for large-scale mass production, and has the advantages of low energy consumption and low cost. The chromium-silicon alloy sputtering target material obtained by the preparation method has the characteristics of density being more than 99% and oxygen content being less than 0.05%, and provides a better performance guarantee for subsequent sputtering.
Description
Technical Field
The invention relates to the field of targets and target preparation, in particular to a chromium-silicon alloy sputtering target and a preparation method thereof.
Background
Physical Vapor Deposition (PVD) refers to a process of evaporating a material source by using a low-voltage and large-current arc discharge technique under a vacuum condition, ionizing both evaporated substances and gas by using gas discharge, and then depositing the evaporated substances and reaction products thereof on a workpiece by an acceleration action of an electric field to form a film with a special function. The PVD technology is the core technology of various industries such as semiconductor chip manufacturing industry, solar energy industry, LCD manufacturing industry and the like, and the main methods comprise vacuum evaporation, arc plasma plating, ion coating, molecular beam epitaxy, sputtering coating and the like.
Sputtering is one of the main techniques for preparing thin film materials, and is characterized in that ions generated by an ion source are accelerated and gathered in vacuum to form ion beam flow with high speed energy, the ion beam flows bombard the surface of a solid, kinetic energy exchange is carried out between the ions and atoms on the surface of the solid, the atoms on the surface of the solid leave the solid and are deposited on the surface of a substrate, and the bombarded solid is a raw material for preparing a thin film deposited by a sputtering method and is generally called as a sputtering target material.
Sputtering targets are generally obtained by powder metallurgy sintering molding processes because the sputtering targets prepared by the processes have unique chemical compositions and mechanical and physical properties that cannot be obtained by conventional fusion casting methods. Porous, semi-compact or fully-compact materials and products can be directly prepared by using a powder metallurgy sintering molding process. The powder metallurgy sintering molding process is divided into Hot Pressed sintering (HP) and Hot Isostatic Pressing (HIP): the HP process comprises the steps of filling dry powder into a mold, then placing the mold in a vacuum hot-pressing furnace, and heating while pressurizing from a single axial direction under the vacuum or inert condition to simultaneously complete molding and sintering; the HIP process is that the product is placed in a closed container, the powder blank in the sheath is degassed under certain temperature and vacuum degree to ensure the vacuum atmosphere in the sheath, then the same pressure is applied to all directions, and simultaneously high temperature is applied, and the product is sintered and densified under the action of high temperature and high pressure.
The chromium-silicon alloy sputtering target is a novel sputtering target, is used as a good conductor for vacuum sputtering, and can be used in the fields of electronic gate materials and electronic films. In order to make the cr-si alloy sputtering target perform well during vacuum sputtering, the cr-si alloy sputtering target is required to have high density, high uniformity of internal structure, low oxygen content and good machining conditions. However, no preparation method exists at present, so that the prepared chromium-silicon alloy sputtering target material meets the requirements.
The prior art now discloses methods for preparing some sputtering targets. For example, CN110257781A discloses a chromium-aluminum-silicon-nickel quaternary alloy target material and a preparation method thereof, wherein the preparation method comprises the steps of mixing powder, cold isostatic pressing for prepressing after die filling, crushing the prepressed alloy block into metal particles, vacuum sintering for prealloying, crushing the prealloyed block into metal powder, packing and degassing, hot isostatic pressing, and machining. Although the chromium-aluminum-silicon-nickel quaternary alloy target material prepared by the preparation method has the advantages of high density, no air holes, no looseness, no segregation, fine grains, uniform structure and the like, and can be suitable for sputtering of hard coatings required by various tools and dies, the process flow of the preparation method is too complex, the application range is limited, and the risk of oxidation of products can be increased by multi-step operation. CN105331939A discloses a silicon-containing alloy target material and a preparation method thereof, wherein the preparation method comprises five steps of prealloy powder preparation, cold isostatic pressing treatment after die filling, degassing treatment after re-sheathing, hot isostatic pressing treatment and machining treatment. Although the preparation method can prepare the target material with low impurity element content, high purity, high density, fine crystal grains and uniform microstructure, the preparation method needs at least two times of die filling treatment and pressing treatment combining cold isostatic pressing, degassing and hot isostatic pressing, and still has the defects of complex process, high energy consumption and high cost.
Although the preparation methods in the prior art all adopt the hot isostatic pressing process, the preparation methods have the defects of complex process flow, high energy consumption and high cost, and increase the risk of oxidation of products. Therefore, there is a need to develop an effective method for preparing a chromium-silicon alloy sputtering target.
Disclosure of Invention
In view of the problems in the prior art, the invention provides a chromium-silicon alloy sputtering target material and a preparation method thereof. The preparation method comprises the following steps: and (3) loading the chromium-silicon alloy powder with the target mass ratio into a mould, sealing, performing tapping treatment, degassing treatment, hot isostatic pressing treatment and machining to finally obtain the chromium-silicon alloy sputtering target material. The preparation method is simple in process, only needs one-time die filling treatment, reduces the risk of oxidation of the product, ensures the purity of the product, can improve the processing efficiency of the product, is convenient for large-scale mass production, and has the advantages of low energy consumption and low cost. The chromium-silicon alloy sputtering target material obtained by the preparation method has the characteristics of density being more than 99% and oxygen content being less than 0.05%, and provides a better performance guarantee for subsequent sputtering.
In order to achieve the purpose, the invention adopts the following technical scheme:
one of the purposes of the invention is to provide a preparation method of a chromium-silicon alloy sputtering target material, which comprises the following steps:
(1) filling chromium-silicon alloy powder with a target mass ratio into a die, sealing the die, and performing tap treatment;
(2) degassing the mould compacted in the step (1);
(3) carrying out hot isostatic pressing treatment on the mould degassed in the step (2) at the temperature of 1000-;
(4) and (4) machining the rough chromium-silicon alloy sputtering target material obtained in the step (3) to obtain the chromium-silicon alloy sputtering target material.
The preparation method provided by the invention adopts tap treatment to prepare the alloy blank before degassing treatment, on one hand, the tap density of the alloy blank is higher, the density requirement before degassing treatment can be met, on the other hand, the process flow can be simplified, the risk of oxidation of the product is reduced, the processing efficiency of the product is further improved, the large-scale mass production is facilitated, and the preparation method also has the advantages of lower energy consumption and lower cost. The preparation method adopts the high temperature of 1000-1350 ℃ during the hot isostatic pressing treatment, can ensure that the chromium-silicon alloy sputtering target material is stressed in a balanced manner in all directions, and can meet the performance requirements that the density is more than 99 percent and the oxygen content is less than 0.05 percent.
The hot isostatic pressing treatment according to the invention is carried out at a temperature of 1000-.
As a preferable technical scheme of the invention, the chromium-silicon alloy powder with the target mass ratio in the step (1) is prepared by adopting an atomization method.
Preferably, the atomization method comprises any one of, or a combination of at least two of, aerosolization, centrifugal atomization, vacuum atomization and ultrasonic atomization, typical but non-limiting examples of which are: a combination of aerosolization and vacuum atomization, a combination of centrifugal atomization and ultrasonic atomization or a combination of vacuum atomization and ultrasonic atomization, preferably aerosolization.
The principle of gas atomization is to break molten metal into fine droplets by the impact of high-pressure gas flow, and then the fine droplets are recondensed into solid powder. The gas atomization method has the advantages of high powder sphericity, low gas impurity content and the like, and becomes an important metal powder preparation method.
Preferably, the gas employed for aerosolization comprises any one or a combination of at least two of helium, nitrogen or argon, typical but non-limiting examples of which are: a combination of helium and argon, a combination of nitrogen and argon, or a combination of helium and nitrogen, etc., preferably argon.
As a preferred embodiment of the present invention, the target mass proportion in step (1) is 40% or more and 70% or less of Si (wt%), for example, 40%, 45%, 50%, 55%, 60%, 65% or 70% or more of Si (wt%), but not limited to the enumerated values, and other non-enumerated values within the range of values are also applicable, and preferably 40% or more and 55% or less of Si (wt%).
Preferably, the particle size of the chromium-silicon alloy powder with the target mass ratio in step (1) is 150-400 μm, such as 150 μm, 200 μm, 220 μm, 250 μm, 260 μm, 280 μm, 300 μm, 350 μm or 400 μm, but is not limited to the recited values, and other non-recited values within the range are equally applicable, preferably 200-350 μm.
Preferably, the purity of the chromium-silicon alloy powder with the target mass ratio in step (1) is above 3N5, such as 3N5, 3N6, 3N7, 3N8, 3N9, or 4N, but is not limited to the recited values, and other values not recited in this range are also applicable.
As a preferable technical scheme of the invention, the die in the step (1) is a stainless steel sheath.
Preferably, a cleaning step is further included before the step (1) of loading into the mold.
Preferably, the cleaning is to clean the inner wall of the mold so as to ensure no pollution in the mold.
The stainless steel sheath is welded by argon arc, and the stainless steel cover plate and the sheath are firmly welded for sealing, so that basic guarantee is provided for subsequent degassing treatment.
In a preferred embodiment of the present invention, the vibration time of the tapping process in step (1) is 3 to 30min, for example, 3min, 5min, 8min, 10min, 13min, 15min, 20min, 23min, 25min, or 30min, but is not limited to the above-mentioned values, and other values not listed in the above-mentioned range are also applicable, and preferably 3 to 15 min.
Preferably, the vibration amplitude of the tapping treatment in step (1) is 1-10mm, such as 1mm, 2mm, 3mm, 4mm, 5mm, 6mm, 7mm, 8mm, 9mm or 10mm, but not limited to the recited values, and other values not recited within the range of values are equally applicable, preferably 3-7 mm.
Preferably, the vibration frequency of the tapping treatment in step (1) is 50 to 400 times/min, such as 50 times/min, 80 times/min, 100 times/min, 120 times/min, 150 times/min, 170 times/min, 200 times/min, 230 times/min, 250 times/min, 280 times/min, 300 times/min, 350 times/min or 400 times/min, etc., but is not limited to the values listed, and other values not listed in the range of values are equally applicable, preferably 100 times/min and 300 times/min.
As a preferred embodiment of the present invention, the temperature of the degassing treatment in step (2) is 400-600 ℃, for example, 400 ℃, 450 ℃, 500 ℃, 550 ℃ or 600 ℃, but not limited to the values listed, and other values not listed in the numerical range are also applicable, preferably 450-550 ℃.
Preferably, the degassing treatment in step (2) is carried out under a vacuum of 5 to 1.5E-3Pa, for example 5E-3Pa, 4.5E-3Pa, 4E-3Pa, 3.5E-3Pa, 3E-3Pa, 2.5E-3Pa, 2E-3Pa or 1.5E-3Pa, but not limited to the recited values, and other values not recited within the range of values are equally applicable, preferably 4 to 2E-3 Pa.
According to the invention, the vacuum degree of degassing treatment is increased to 5-1.5E-3Pa, so that the gas in the jacket can be fully removed, and the gas is discharged completely, thereby further ensuring that the silicon powder is not oxidized by air, and further improving the product performance of the chromium-silicon alloy sputtering target material; in addition, the degassing effect can be better ensured under the vacuum degree, the energy consumption can be reduced to the maximum extent, and the investment of cost can be reduced.
In a preferred embodiment of the present invention, the pressure of the hot isostatic pressing treatment in step (3) is 130-180MPa, such as 130MPa, 140MPa, 150MPa, 160MPa, 170MPa or 180MPa, but not limited to the above values, and other values within the above range are also applicable, preferably 140-165 MPa.
Preferably, the holding pressure and pressure time of the hot isostatic pressing treatment in step (3) is 2-6h, such as 2h, 3h, 4h, 5h or 6h, but not limited to the recited values, and other values not recited in the range of the values are also applicable, preferably 3-5 h.
Preferably, the hot isostatic pressing treatment of step (3) is performed in a hot isostatic pressing furnace.
The hot isostatic pressing process provided by the invention is designed by combining the measured chromium-silicon alloy proportioning diagram according to the great difference of the melting point, the specific gravity and other physical properties of chromium and silicon. The high temperature of 1000-1350 ℃ and the high pressure of 130-180MPa are adopted, and the heat preservation and pressure maintaining time is 2-6h, so that the density of the chromium-silicon alloy sputtering target is greatly improved, the internal organization structure of the chromium-silicon alloy is uniform and more uniform, the energy consumption can be reduced as far as possible, and the cost is reduced to the maximum extent.
As a preferred technical scheme of the invention, the preparation method comprises the following steps:
(1) preparing chromium-silicon alloy powder with the target mass proportion of more than or equal to 40 percent and less than or equal to 70 percent of Si (wt%) by adopting an air atomization method, then filling the chromium-silicon alloy powder into a stainless steel sheath which is cleaned in advance, sealing the stainless steel sheath, and performing compaction treatment;
wherein the particle size of the chromium-silicon alloy powder is 150-400 mu m, and the purity is more than 3N 5;
the vibration time of the vibration compaction treatment is 3-30min, the vibration amplitude is 1-10mm, and the vibration frequency is 50-400 times/min;
(2) heating the mould vibrated in the step (1) to 400-600 ℃, and performing degassing treatment under the vacuum degree of 5-1.5E-3 Pa;
(3) placing the mould degassed in the step (2) into a hot isostatic pressing furnace, heating to 1000-;
(4) and (4) machining the rough chromium-silicon alloy sputtering target material obtained in the step (3) to obtain the chromium-silicon alloy sputtering target material.
The second purpose of the invention is to provide a chromium-silicon alloy sputtering target material which is prepared by the preparation method of the first purpose.
In a preferred embodiment of the present invention, the chromium-silicon alloy sputtering target has a density of > 99%, for example, 99.2%, 99.5%, 99.6%, 99.8%, or 99.9%, but is not limited to the values listed above, and other values not listed above within this range are also applicable.
Preferably, the chromium-silicon alloy sputtering target has an oxygen content of less than 0.05%, such as 0.005%, 0.01%, 0.02%, 0.03%, or 0.04%, but not limited to the recited values, and other values not recited within this range are equally applicable.
Compared with the prior art, the invention has at least the following beneficial effects:
(1) according to the preparation method of the chromium-silicon alloy sputtering target material, the alloy blank before degassing treatment is prepared by adopting the compaction treatment, only one-time die filling treatment is needed, and the preparation method has the advantages of simple process, low energy consumption and low cost;
(2) the preparation method of the chromium-silicon alloy sputtering target material can reduce the risk of oxidation of the product, ensure the purity of the product, improve the processing efficiency of the product and facilitate large-scale mass production;
(3) the chromium-silicon alloy sputtering target material has the characteristics of density of more than 99% and oxygen content of less than 0.05%, and can provide better performance guarantee for subsequent sputtering.
Drawings
FIG. 1 is a flow chart of the preparation method of the chromium-silicon alloy sputtering target material provided by the invention.
Detailed Description
The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached drawings. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Fig. 1 shows a flowchart of a method for preparing a chromium-silicon alloy sputtering target provided by the invention, which specifically includes the following steps:
(1) filling chromium-silicon alloy powder with a target mass ratio into a die, sealing the die, and performing tap treatment;
(2) degassing the mould compacted in the step (1);
(3) carrying out hot isostatic pressing treatment on the mould degassed in the step (2) at the temperature of 1000-;
(4) and (4) machining the chromium-silicon alloy sputtering target crude product obtained in the step (3) to obtain the chromium-silicon alloy sputtering target qualified in size detection.
To facilitate understanding of the invention, the following examples are set forth:
example 1
The embodiment provides a preparation method of a chromium-silicon alloy sputtering target material, which comprises the following steps:
(1) preparing chromium-silicon alloy powder with the target mass proportion of Si (wt%) -40% by adopting a gas atomization method, wherein the particle size of the chromium-silicon alloy powder is 250 micrometers, and the purity is 3N 6; then, a stainless steel sheath which is cleaned in advance is arranged, the stainless steel cover plate and the sheath are welded by argon arc welding for sealing, and the stainless steel sheath is vibrated for 20min, the vibration amplitude is 5mm, and the vibration frequency is 250 times/min;
(2) heating the mold compacted in the step (1) to 450 ℃, and degassing under the vacuum degree of 2E-3 Pa;
(3) placing the mould degassed in the step (2) into a hot isostatic pressing furnace, heating to 1100 ℃, pressurizing to 175MPa, and then carrying out hot isostatic pressing treatment for 4 hours under the condition of heat preservation and pressure maintenance to obtain a chromium-silicon alloy sputtering target crude product;
(4) and (4) machining the rough chromium-silicon alloy sputtering target material obtained in the step (3) to obtain the chromium-silicon alloy sputtering target material.
Example 2
(1) Preparing chromium-silicon alloy powder with the target mass proportion of Si (wt%) -45% by adopting an air atomization method, wherein the particle size of the chromium-silicon alloy powder is 400 mu m, and the purity is 3N 5; then, a stainless steel sheath which is cleaned in advance is arranged, the stainless steel cover plate and the sheath are welded by argon arc welding for sealing, and the stainless steel sheath is vibrated for 30min, the vibration amplitude is 10mm, and the vibration frequency is 50 times/min;
(2) heating the mold compacted in the step (1) to 450 ℃, and degassing under the vacuum degree of 1.5E-3 Pa;
(3) placing the mould degassed in the step (2) into a hot isostatic pressing furnace, heating to 1125 ℃, pressurizing to 140MPa, and then carrying out hot isostatic pressing treatment for 6h under the condition of heat preservation and pressure preservation to obtain a chromium-silicon alloy sputtering target crude product;
(4) and (4) machining the rough chromium-silicon alloy sputtering target material obtained in the step (3) to obtain the chromium-silicon alloy sputtering target material.
Example 3
(1) Preparing chromium-silicon alloy powder with the target mass proportion of 50% of Si (wt%), wherein the particle size of the chromium-silicon alloy powder is 150 mu m, and the purity is 3N 7; then, a stainless steel sheath which is cleaned in advance is arranged, the stainless steel cover plate and the sheath are welded by argon arc welding for sealing, and the stainless steel sheath is vibrated for 15min, the vibration amplitude is 3mm, and the vibration frequency is 400 times/min;
(2) heating the mold compacted in the step (1) to 450 ℃, and degassing under the vacuum degree of 5E-3 Pa;
(3) placing the mould degassed in the step (2) into a hot isostatic pressing furnace, heating to 1150 ℃, pressurizing to 150MPa, and then carrying out hot isostatic pressing treatment for 2h under the condition of heat preservation and pressure maintenance to obtain a chromium-silicon alloy sputtering target crude product;
(4) and (4) machining the rough chromium-silicon alloy sputtering target material obtained in the step (3) to obtain the chromium-silicon alloy sputtering target material.
Comparative example 1
This comparative example was conducted under the same conditions as in example 1 except that the hot isostatic pressing temperature in step (3) was replaced with 1400 ℃.
Comparative example 2
This comparative example was conducted under the same conditions as in example 1 except that the hot isostatic pressing temperature in step (3) was changed to 900 ℃.
The chromium-silicon alloy sputtering targets obtained in the above examples and comparative examples were subjected to relative tests on density, uniformity of internal texture and oxygen content, and specific results are shown in table 1.
TABLE 1
As can be seen from Table 1, the chromium-silicon alloy sputtering target material with the density of more than 99 percent and the oxygen content of less than 0.05 percent can be prepared by the preparation method, and the product is microscopic, uniform and compact and meets the performance requirements of sputtering. In addition, the preparation method provided by the invention only needs one-time die filling treatment, has a simple process flow, reduces the risk of oxidation of the product, can improve the processing efficiency of the product, and is convenient for large-scale mass production.
The applicant declares that the present invention illustrates the detailed structural features of the present invention through the above embodiments, but the present invention is not limited to the above detailed structural features, that is, it does not mean that the present invention must be implemented depending on the above detailed structural features. It should be understood by those skilled in the art that any modifications of the present invention, equivalent substitutions of selected components of the present invention, additions of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (10)
1. The preparation method of the chromium-silicon alloy sputtering target is characterized by comprising the following steps:
(1) filling chromium-silicon alloy powder with a target mass ratio into a die, sealing the die, and performing tap treatment;
(2) degassing the mould compacted in the step (1);
(3) carrying out hot isostatic pressing treatment on the mould degassed in the step (2) at the temperature of 1000-;
(4) and (4) machining the rough chromium-silicon alloy sputtering target material obtained in the step (3) to obtain the chromium-silicon alloy sputtering target material.
2. The production method according to claim 1, wherein the chromium-silicon alloy powder having the target mass ratio of step (1) is produced by an atomization method;
preferably, the atomization method comprises any one or a combination of at least two of gas atomization, centrifugal atomization, vacuum atomization and ultrasonic atomization, and preferably gas atomization;
preferably, the gas used for the aerosolization comprises any one or a combination of at least two of helium, nitrogen or argon, preferably argon.
3. The production method according to claim 1 or 2, characterized in that the target mass proportion in step (1) is 40% or more and 70% or less of Si (wt%), preferably 40% or more and 55% or less of Si (wt%);
preferably, the particle size of the chromium-silicon alloy powder with the target mass ratio in the step (1) is 150-;
preferably, the purity of the chromium-silicon alloy powder with the target mass ratio in the step (1) is more than 3N 5.
4. The production method according to any one of claims 1 to 3, wherein the mold of step (1) is a stainless steel jacket;
preferably, a cleaning step is further included before the step (1) of loading into the mold;
preferably, the cleaning is to clean the inner wall of the mold so as to ensure no pollution in the mold.
5. The production method according to any one of claims 1 to 4, wherein the vibration time of the tapping treatment of step (1) is 3 to 30min, preferably 3 to 15 min;
preferably, the vibration amplitude of the vibration compaction treatment in the step (1) is 1-10mm, preferably 3-7 mm;
preferably, the vibration frequency of the vibration compaction treatment in the step (1) is 50-400 times/min, and preferably 100-300 times/min.
6. The preparation method according to any one of claims 1 to 5, wherein the degassing treatment in step (2) is performed at a temperature of 400 ℃ and 600 ℃, preferably at a temperature of 450 ℃ and 550 ℃;
preferably, the vacuum degree of the degassing treatment in the step (2) is 5-1.5E-3Pa, and preferably 4-2E-3 Pa.
7. The method according to any one of claims 1 to 6, wherein the pressure of the hot isostatic pressing treatment in step (3) is 130-180MPa, preferably 140-165 MPa;
preferably, the heat preservation and pressure maintaining time of the hot isostatic pressing treatment in the step (3) is 2-6h, preferably 3-5 h;
preferably, the hot isostatic pressing treatment of step (3) is performed in a hot isostatic pressing furnace.
8. The production method according to any one of claims 1 to 7, characterized by comprising the steps of:
(1) preparing chromium-silicon alloy powder with the target mass proportion of more than or equal to 40 percent and less than or equal to 70 percent of Si (wt%) by adopting an air atomization method, then filling the chromium-silicon alloy powder into a stainless steel sheath which is cleaned in advance, sealing the stainless steel sheath, and performing compaction treatment;
wherein the particle size of the chromium-silicon alloy powder is 150-400 mu m, and the purity is more than 3N 5;
the vibration time of the vibration compaction treatment is 3-30min, the vibration amplitude is 1-10mm, and the vibration frequency is 50-400 times/min;
(2) heating the mould vibrated in the step (1) to 400-600 ℃, and performing degassing treatment under the vacuum degree of 5-1.5E-3 Pa;
(3) placing the mould degassed in the step (2) into a hot isostatic pressing furnace, heating to 1000-;
(4) and (4) machining the rough chromium-silicon alloy sputtering target material obtained in the step (3) to obtain the chromium-silicon alloy sputtering target material.
9. The chromium-silicon alloy sputtering target material prepared by the preparation method according to any one of claims 1 to 8.
10. The chromium silicon alloy sputtering target according to claim 9, wherein the compactness of the chromium silicon alloy sputtering target is > 99%;
preferably, the oxygen content of the chromium-silicon alloy sputtering target material is less than 0.05%.
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| CN202010002184.0A CN111058004A (en) | 2020-01-02 | 2020-01-02 | Chromium-silicon alloy sputtering target material and preparation method thereof |
| PCT/CN2020/084101 WO2021134972A1 (en) | 2020-01-02 | 2020-04-10 | Chromium-silicon alloy sputtering target material and preparation method therefor |
| SG11202007556VA SG11202007556VA (en) | 2020-01-02 | 2020-04-10 | Chromium-silicon alloy sputtering target material and preparation method thereof |
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| SG11202007556VA (en) | 2021-08-30 |
| WO2021134972A1 (en) | 2021-07-08 |
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