CN116079055A - CrAlFe-based alloy target and preparation method thereof - Google Patents
CrAlFe-based alloy target and preparation method thereof Download PDFInfo
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- B22—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
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/052—Metallic powder characterised by the size or surface area of the particles characterised by a mixture of particles of different sizes or by the particle size distribution
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/0408—Light metal alloys
- C22C1/0416—Aluminium-based alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
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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
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- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
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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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- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
Abstract
The invention belongs to the technical field of powder metallurgy materials and manufacturing thereof, and particularly relates to a CrAlFe-based alloy target and a preparation method thereof, wherein the preparation method comprises the following steps: s1, performing high-energy ball milling treatment on Al powder and Fe powder to obtain prealloyed AlFe alloy powder; s2, uniformly mixing AlFe alloy powder and the rest raw material powder of the CrAlFe-based alloy target to obtain CrAlFe-based alloy powder; s3, carrying out hot-press sintering on the CrAlFe-based alloy powder under a vacuum condition, releasing pressure after the hot-press sintering is finished, and then cooling and demolding to obtain a CrAlFe-based alloy sintered blank; s4, machining the CrAlFe-based alloy sintered blank to obtain the CrAlFe-based alloy target. According to the invention, the cracking phenomenon of the CrAlFe-based alloy target can be improved by removing the pressure before cooling.
Description
Technical Field
The invention belongs to the technical field of powder metallurgy materials and manufacturing thereof, and particularly relates to a CrAlFe-based alloy target and a preparation method thereof.
Background
Since the 60 s of the 20 th century, superhard film materials are deposited on the surface of a metal cutting tool by PVD technology, so that the cutting speed and the wear resistance can be remarkably improved, the service life of the tool is prolonged, and the method becomes a main method for improving the performance of the tool. With the continuous development and progress of coating technology, the first generation of TiN and CrN coatings are developed into the current AlTiN and AlCrN composite coatings, and the diversification, the nanocrystallization and the multilayering are gradually carried out. By adding Fe element into the AlCrN coating, the high-temperature oxidation resistance and the thermal strength of the film layer can be obviously improved; the refractory transition metal elements such as W, mo, ta, nb, V and the like are added into the AlCrFeN coating, so that the hot hardness and high-temperature oxidation resistance of the coating can be further improved, and the cutting performance of the cutter is obviously improved.
However, the preparation technology of the CrAlFe and CrAlFeX (one or more of X= W, mo, ta, nb, V) alloy targets has high barriers. When the target material is prepared by adopting a conventional hot isostatic pressing process, the external part and the core part of the target material are severely cracked.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide the CrAlFe-based alloy target and the preparation method thereof.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
in a first aspect, the invention provides a preparation method of a CrAlFe-based alloy target, which comprises the following steps:
s1, performing high-energy ball milling treatment on Al powder and Fe powder to obtain prealloyed AlFe alloy powder;
s2, uniformly mixing the AlFe alloy powder and the rest raw material powder of the CrAlFe-based alloy target material to obtain CrAlFe-based alloy powder, wherein the rest raw material powder of the CrAlFe-based alloy target material is Cr powder or consists of Cr powder and X powder, and the X powder comprises at least one of W powder, mo powder, ta powder, nb powder and V powder;
S3, carrying out hot-press sintering on the CrAlFe-based alloy powder under a vacuum condition, releasing pressure after the hot-press sintering is finished, and then cooling and demolding to obtain a CrAlFe-based alloy sintered blank;
and S4, machining the CrAlFe-based alloy sintered blank to obtain the CrAlFe-based alloy target.
According to the invention, the vacuum hot-pressing sintering process is adopted, the pressure is removed before cooling, and the CrAlFe-based alloy target is prepared, so that the cracking phenomenon of the CrAlFe-based alloy target can be improved.
According to the invention, al powder and Fe powder are subjected to high-energy ball milling treatment, and then the AlFe alloy powder, cr powder and X powder are uniformly mixed, so that metal Fe and Al are fully alloyed to form AlFe alloy powder, the problem that the severe alloying reaction of pure Al powder and Fe powder is exothermic, so that Cr and matrix Al in a target material generate alloying reaction to generate more brittle alloy phases is effectively avoided, less brittle alloy phases in the target material are ensured, the brittleness of CrAlFe and CrAlFeX alloy target materials can be effectively improved, and the cracking problem of blanks is improved.
In the preparation method of the CrAlFe-based alloy target, as a preferred embodiment, the CrAlFe-based alloy target comprises the following chemical components in percentage by atom: cr 10-70at% (e.g., 10at%, 30at%, 50at%, 70at%, etc.), al 20-85at% (e.g., 20at%, 40at%, 60at%, 85at%, etc.), fe 0-20at% (e.g., 1at%, 3at%, 5at%, 10at%, 15at%, 20at%, etc.), X0-20 at% (e.g., 0at%, 5at%, 10at%, 15at%, 20at%, etc.), wherein X represents at least one of W, mo, ta, nb, V.
In the preparation method of the CrAlFe-based alloy target, as a preferred embodiment, the mass of the required raw materials is calculated according to the atomic percentage of each element in the CrAlFe-based alloy target.
In the preparation method of the CrAlFe-based alloy target, as a preferable implementation mode, the purity of the Fe powder is more than or equal to 99.5wt percent, and the Fisher granularity F.S.S. is 5-8 mu m; the Al powder is air atomized aluminum powder, the purity is more than or equal to 99.7wt percent, and the granularity is-200 meshes; the purity of the Cr powder is more than or equal to 99.8wt percent, and the granularity is-200 meshes; the purity of the W powder is more than or equal to 99.9wt percent, and the Fisher particle size F.S.S. is 5-8 mu m; the purity of the Mo powder is more than or equal to 99.9wt percent, and the Fisher granularity F.S.S. is 5-8 mu m; the purity of the Ta powder is more than or equal to 99.8 weight percent, and D50=15-20 mu m; the purity of the Nb powder is more than or equal to 99.5 weight percent, and the granularity is-300 meshes; the purity of the V powder is more than or equal to 99.8wt% and the granularity is minus 325 meshes.
The invention improves the fluidity between mixed powders and reduces segregation by adopting non-spherical aluminum powder, so that the microstructure of the prepared alloy target is uniform and has no segregation.
In the preparation method of the CrAlFe-based alloy target material, in the step S1, the ball milling medium comprises one of zirconia balls, steel balls and stainless steel balls, and the diameter of the ball milling medium is 20-30mm, for example, 20mm, 25mm or 30 mm.
In the above-mentioned method for producing a CrAlFe-based alloy target, in step S1, the mass ratio of the spheres to the powder raw material= (10 to 20): 1 may be, for example, 10:1, 15:1, or 20:1.
In the preparation method of the CrAlFe-based alloy target, as a preferred embodiment, in the step S1, the vacuum degree is pre-pumped to be less than or equal to 0.1Pa, ar gas of 0.5-2Pa is then filled, high-energy ball milling treatment is carried out under the protection of the Ar gas, the ball milling rotating speed is 100-150r/min (for example, 100r/min, 120r/min or 150r/min and the like), the ball milling time is 20-50h (for example, 20h, 40h or 50h and the like), and if the ball milling time is too long, the oxygen content in the target can be increased.
In the preparation method of the CrAlFe-based alloy target, in step S1, after the high-energy ball milling treatment is completed, the AlFe alloy powder is screened to remove large powder particles, wherein the pore diameter of the screened screen is 1-2mm.
In the preparation method of the CrAlFe-based alloy target material, in the step S2, the mixing is performed in a mixer, and a mode of adding zirconia balls for dry mixing is adopted, wherein the ball mass ratio (the weight ratio of the balls to mixed powder) corresponding to the zirconia balls is 1 (5-10) (for example, 1:5, 1:7 or 1:10) and the mixing time is 3-10h (for example, 3h, 5h, 7h or 10 h). The embodiment of the invention adds balls to accelerate the diffusion, convection and shearing among powder particles, thereby achieving the ideal mixing effect rapidly.
In the preparation method of the CrAlFe-based alloy target, as a preferred embodiment, the mixer is at least one of a universal motion mixer, a three-dimensional mixer and a double-cone mixer, and preferably a universal motion mixer.
In the above method for preparing a CrAlFe-based alloy target, in step S3, the pressure relief includes maintaining pressure and cooling to 400-460 ℃ (for example, 400 ℃, 410 ℃, 430 ℃ or 460 ℃), and then linearly releasing pressure to 0MPa (removing the pressure applied to the CrAlFe-based alloy sintered blank).
Here, linear pressure relief refers to pressure relief at a fixed pressure relief rate.
In the above method for preparing a CrAlFe-based alloy target, as a preferred embodiment, in step S3, the hot press sintering has a maximum sintering temperature of 500-600 ℃.
In the above method for preparing a CrAlFe-based alloy target, as a preferred embodiment, in step S3, the hot press sintering includes: firstly, under the room temperature state, an initial pressure of 5-12Mpa (for example, 5Mpa, 7Mpa, 10Mpa or 12Mpa and the like) is applied to the CrAlFe-based alloy powder, vacuum pumping is carried out to 0.1-0.5Pa, then vacuum hot-pressing sintering is carried out, the temperature is increased to 120-180 ℃ (for example, 120 ℃ and 140 ℃, 160 ℃ or 180 ℃ and the like from room temperature, if the temperature is too high, the O content in a target material is increased, preferably 120-150 ℃, the temperature increasing rate is 1-5 ℃/min, when the vacuum degree reaches 0.01Pa-0.05Pa, the timing, the heat preservation and the pressure maintaining are started, the heat preservation and the pressure maintaining time is 1-5h under 120-180 ℃ and 5-12Mpa, the temperature rising rate is 2-10 ℃/min (for example, 2 ℃/min, 4 ℃/min, 6 ℃/min, 8 ℃/min or 10 ℃/min and the like) is continued to be increased to the sintering temperature of 500-600 ℃ (for example, 500 ℃ and 530 ℃, 550 ℃ or 600 ℃ and the like, if the temperature is too low, the porosity is low, the target material is easy to cause gas release, and the quality of a film, the film and the like are easily generated when the film is in the vacuum state; when the temperature is too high, the Al and other components are subjected to alloying reaction to generate a brittle alloy phase, the pressed compact starts to crack, and meanwhile, the pressure is linearly increased to 20-50MPa (for example, 20MPa, 30MPa, 40MPa or 50MPa, and the like, preferably 30-50 MPa), and the temperature and the pressure are maintained for 1-6h (for example, 1h, 3h, 5h or 6h, and the like) at 500-600 ℃ and 20-50 MPa.
Here, the time from 5-12MPa to 20-50MPa is the same as the time from 120-180deg.C to 500-600deg.C.
In the preparation method of the CrAlFe-based alloy target, as a preferred embodiment, in the step S3, the pressure relief time is 20min-60min (for example, 20min, 25min, 30min, 35min, 40min, 45min, 50min or 60min, etc.).
In the above method for preparing a CrAlFe-based alloy target, as a preferred embodiment, in step S3, the cooling and demolding includes: air cooling along with the furnace after pressure relief, discharging and demoulding when the furnace temperature is lower than 200 ℃ (for example, the furnace temperature can be 100 ℃, 120 ℃, 140 ℃, 160 ℃ or 200 ℃ and the like).
In the above method for preparing a CrAlFe-based alloy target, as a preferred embodiment, the machining includes at least one of grinding, wire cutting, turning, and milling.
In the above method for preparing a CrAlFe-based alloy target, in step S3, the hot press sintering of the CrAlFe-based alloy powder includes: filling the CrAlFe-based alloy powder into a die, and then performing hot-pressing sintering, wherein the die is a graphite die, and the size of an inner cavity of the die is (D108-D300) mm (150-300) mm (die depth).
In the above method for preparing a CrAlFe-based alloy target, in step S4, the size of the CrAlFe-based alloy target is D (60-300) mm x (10-40) mm.
In a second aspect, the present invention provides a CrAlFe-based alloy target made by the method of preparation provided in the first aspect.
In the CrAlFe-based alloy target, as a preferable implementation mode, the relative density of the CrAlFe-based alloy target is more than or equal to 99%. Relative density = actual density value/theoretical density value.
Compared with the prior art, the invention has the beneficial effects that at least one of the following is included:
(1) According to the invention, the vacuum hot-pressing sintering process is adopted, the pressure is removed before cooling, and the CrAlFe-based alloy target is prepared, so that the cracking phenomenon of the CrAlFe-based alloy target can be improved.
(2) The fluidity of ternary or higher alloy powder is improved by controlling the granularity and the form of the powder (such as adopting air atomized aluminum powder, selecting finer powder for mixing), and simultaneously, a mixer is selected, so that the uniformity of powder mixing is improved, and the problem of nonuniform structure in an alloy target is effectively solved.
(3) The Al powder and the Fe powder are subjected to high-energy ball milling, so that metal Fe and Al are fully alloyed to form AlFe alloy powder, severe alloying reaction heat release of pure Al powder and Fe powder in the hot-press sintering process is effectively avoided, the Cr and matrix Al in the target material are caused to generate more brittle alloy phases, the brittleness of the CrAlFe and CrAlFeX alloy target material can be effectively improved, and the cracking problem of the blank is improved.
(4) The alloy target is prepared by the hot-pressing sintering process, and no pressure can be realized in the cooling process due to the fact that the pressure head is lifted during cooling, residual internal stress in the CrAlFe and CrAlFeX alloy targets after cooling is small, and the prepared alloy target is high in density, uniform in structure and free of cracking.
Drawings
FIG. 1 is a microstructure of the CrAlFe alloy target provided in example 1;
FIG. 2 is a microstructure of the CrAlFe alloy target provided in comparative example 1;
FIG. 3 is an external view of the CrAlFe alloy target product provided in example 1;
FIG. 4 is an external view of the CrAlFe alloy target product provided in comparative example 1;
fig. 5 is another appearance of the CrAlFe alloy target product provided in comparative example 1.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The examples of the present invention are implemented on the premise of the technical scheme of the present invention, and detailed implementation modes and processes are given, but the protection scope of the present invention is not limited to the following examples, in which the process parameters of specific conditions are not noted, and generally according to conventional conditions.
The endpoints of the ranges and any values disclosed in the present invention are not limited to the precise range or value, and the range or value should be understood to include values close to the range or value. For numerical ranges, one or more new numerical ranges may be obtained in combination with each other between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point values, and are to be considered as specifically disclosed in the present invention.
The process parameters for the specific conditions not noted in the examples below are generally as usual. The experimental reagents used in the following examples, unless otherwise specified, are all conventional biochemical reagents; the dosage of the experimental reagent is the dosage of the reagent in the conventional experimental operation unless specified.
In a first aspect, the invention provides a preparation method of a CrAlFe-based alloy target, which comprises the following steps:
S1, pre-vacuumizing to the vacuum degree of less than or equal to 0.1Pa, filling Ar gas of 0.5-2Pa, performing high-energy ball milling treatment on Al powder and Fe powder under the protection of Ar gas, sieving the AlFe alloy powder after the high-energy ball milling treatment is finished to remove large powder particles, wherein the aperture of a sieving screen is 1-2mm, and obtaining prealloyed AlFe alloy powder, wherein a ball milling medium comprises one of zirconia balls, steel balls and stainless steel balls, the diameter of the ball milling medium is 20-30mm, the ball material mass ratio is ball/powder raw material= (10-20): 1, the ball milling rotating speed is 100-150r/min, and the ball milling time is 20-50h.
S2, uniformly mixing the AlFe alloy powder and Cr powder in a mixer, or uniformly mixing the AlFe alloy powder, cr powder and X powder in the mixer, and adopting a mode of adding zirconia balls for dry mixing to obtain CrAlFe-based alloy powder, wherein the X powder comprises at least one of W powder, mo powder, ta powder, nb powder and V powder, the purity of the Fe powder is more than or equal to 99.5wt%, and the Fisher particle size F.S.S.S is 5-8 mu m; the Al powder is air atomized aluminum powder, the purity is more than or equal to 99.7wt percent, and the granularity is-200 meshes; the purity of the Cr powder is more than or equal to 99.8wt percent, and the granularity is-200 meshes; the purity of the W powder is more than or equal to 99.9wt percent, and the Fisher particle size F.S.S. is 5-8 mu m; the purity of the Mo powder is more than or equal to 99.9wt percent, and the Fisher granularity F.S.S. is 5-8 mu m; the purity of the Ta powder is more than or equal to 99.8 weight percent, and D50=15-20 mu m; the purity of the Nb powder is more than or equal to 99.5 weight percent, and the granularity is-300 meshes; the purity of the V powder is more than or equal to 99.8wt%, the granularity is minus 325 meshes, the ball material mass ratio (the weight ratio of balls to mixed powder) corresponding to the zirconia balls is 1 (5-10), the mixing time is 3-10h, and the mixer is at least one of a universal motion mixer, a three-dimensional mixer and a double-cone mixer.
S3, filling the CrAlFe-based alloy powder into a graphite mold under a vacuum condition, and then performing hot-pressing sintering, wherein after the hot-pressing sintering is finished, pressure relief, cooling and demolding are performed to obtain a CrAlFe-based alloy sintered blank, and the size of an inner cavity of the graphite mold is (D108-D300) mm (150-300) mm (mold depth), and the hot-pressing sintering comprises: firstly, under the room temperature state, applying an initial pressure of 5-12Mpa to CrAlFe-based alloy powder, vacuumizing to 0.1-0.5Pa, then performing vacuum hot-pressing sintering, raising the temperature from room temperature to 120-180 ℃ at a temperature raising rate of 1-5 ℃/min, starting timing, keeping the temperature and pressure after the vacuum degree reaches 0.01-0.05 Pa, keeping the temperature and pressure for 1-5h at 120-180 ℃ and 5-12Mpa, continuously raising the temperature to 500-600 ℃ at a temperature raising rate of 2-10 ℃/min, simultaneously raising the pressure to 20-50MPa, keeping the temperature and pressure for 1-6h at 500-600 ℃ and 20-50MPa, keeping the pressure and cooling to 400-460 ℃, then keeping the pressure and the pressure for 20-60 min, and cooling and demoulding comprises the steps of: and (5) air cooling along with the furnace after pressure relief, discharging and demoulding when the furnace temperature is lower than 200 ℃.
S4, machining (grinding, wire cutting, turning and milling) the CrAlFe-based alloy sintered blank to obtain the CrAlFe-based alloy target, wherein the size of the CrAlFe-based alloy target is D (60-300) mm (10-40) mm, and the chemical components of the CrAlFe-based alloy target are calculated according to atomic percent: 10-70at% of Cr, 20-85at% of Al, 0-20at% of Fe which is not 0at%, and 0-20at% of X, wherein X represents at least one of W, mo, ta, nb, V.
The invention adopts a vacuum hot-pressing sintering process, and the relative density is more than or equal to 99 percent, the structure is uniform, and the CrAlFe and CrAlFeX alloy targets without cracking are produced by powder screening and powder mechanical alloying pretreatment, so that the target coating performance is excellent.
The high-energy ball milling prealloying treatment of the Al powder and the Fe powder ensures that the alloy phase content in the target is low, and reduces the intrinsic brittleness of the target; the pressure head is lifted in the cooling process of the hot-pressing sintering process, so that the residual internal stress in the pressed compact is ensured to be small, and the prepared target is not easy to crack.
In a second aspect, the invention provides a CrAlFe-based alloy target material, which is prepared by the preparation method provided in the first aspect, and the relative density of the CrAlFe-based alloy target material is more than or equal to 99%.
In order to further understand the present invention, the CrAlFe-based alloy target material and the preparation method thereof provided by the present invention are described in detail with reference to the following examples, and the scope of protection of the present invention is not limited by the following examples.
Example 1
The CrAlFe-based alloy target provided by the embodiment is a CrAlFe alloy target, and comprises the following chemical components in percentage by atom: cr (Cr) 40 Al 50 Fe 10 The method comprises the following steps of: 40at% of Cr, 50at% of Al and 10at% of Fe, and the weight percentages are as follows: cr 52.16wt%, al 33.83wt% and Fe 14.01wt%.
The preparation method of the CrAlFe-based alloy target provided by the embodiment comprises the following steps:
s1, calculating and weighing raw materials required by preparing the CrAlFe-based alloy target according to the mass of the prepared CrAlFe-based alloy target, wherein the raw materials comprise Cr powder, al powder and Fe powder, the purity of the Fe powder is more than or equal to 99.5wt%, and the Fisher granularity F.S.S.S=6.0 mu m; the Al powder is air atomized aluminum powder, the purity is more than or equal to 99.7wt percent, and the granularity is-200 meshes; the purity of Cr powder is more than or equal to 99.8wt percent, and the granularity is-200 meshes;
filling Al powder and Fe powder into a high-energy ball mill for high-energy ball milling treatment to obtain prealloyed AlFe alloy powder, wherein the high-energy ball milling parameters are as follows: the ball milling process comprises the steps of taking a steel ball with the diameter of D25mm as a ball milling medium, wherein the ball material ratio is ball and powder raw material mass ratio=15:1, pre-vacuumizing to the vacuum degree of 0.05Pa, filling Ar gas with the pressure of 0.5Pa into a high-energy ball mill, performing high-energy ball milling treatment under the protection of the Ar gas, wherein the ball milling rotating speed is 120r/min, the ball milling time is 24 hours, sieving alloy powder to remove large powder particles after ball milling, and the sieve aperture is 1mm.
S2, uniformly mixing the AlFe alloy powder obtained in the step S1 and Cr powder in a universal motion mixer to obtain CrAlFe alloy powder, wherein the mixing adopts a mode of adding zirconia balls for dry mixing, and the ball-to-material ratio is ZrO 2 Ball weight: mix weight = 1:10, mixing time 6h.
S3, uniformly filling the CrAlFe alloy powder obtained in the step S2 into a round graphite die, wherein the effective size of the inner cavity of the die is D165 x 200mm (the effective inner diameter of the die is 165mm, the depth of the die is 200 mm), performing hot-press sintering under a vacuum condition, continuously vacuumizing in the hot-press sintering process, maintaining the pressure and cooling to 450 ℃ along with a furnace after the hot-press sintering is finished, linearly releasing the pressure to 0MPa, releasing the pressure for 30min, naturally cooling to 150 ℃ along with the furnace, discharging from the furnace, and demoulding to obtain a CrAlFe sintered blank with high density, wherein the hot-press sintering comprises: firstly, under the room temperature state, the initial pressure of 10Mpa is applied to CrAlFe alloy powder, meanwhile, the vacuum pumping is carried out to 0.1Pa, then the vacuum hot-pressing sintering procedure is started, the temperature is raised to 150 ℃ from room temperature, the heating rate is 2 ℃/min, the timing, the heat preservation and the pressure maintaining are started after the vacuum degree reaches 0.05Pa, the heat preservation and the pressure maintaining are carried out for 3 hours at 150 ℃ and 10Mpa, the temperature is continuously raised to the sintering temperature 535 ℃ (the heating rate is 4 ℃/min), meanwhile, the linear pressure is raised to the sintering pressure of 35MPa, the time of the pressure rise from 10Mpa to 35Mpa is the same as the time of the temperature rise from 150 ℃ to the sintering temperature 535 ℃, and the heat preservation and the pressure maintaining are carried out for 2.5 hours at 535 ℃ and 35 MPa.
S4, grinding, wire cutting, turning and milling are carried out on the CrAlFe sintered blank, so that a CrAlFe alloy target (finished target) meeting the requirements of size and surface quality is obtained, wherein the target is a round target, and the size is as follows: diameter d156.3mm and height 20mm.
Fig. 1 is a microstructure diagram (SEM image) of the CrAlFe alloy target provided in this embodiment, and fig. 3 is an appearance diagram of the CrAlFe alloy target provided in this embodiment, as can be seen from fig. 1 and 3, the CrAlFe alloy target provided in this embodiment has a uniform structure, cr and Al matrix do not undergo alloying reaction, and the target has no cracking phenomenon.
Example 2
The CrAlFe-based alloy target provided by the embodiment is a CrAlFeMo alloy target, and the chemical components and the atomic percentages thereof are as follows: cr (Cr) 15 Al 60 Fe 20 Mo 5 The method comprises the following steps of: 15at% of Cr, 60at% of Al, 20at% of Fe and 5at% of Mo, and the weight percentages are as follows: 19.52wt% of Cr, 40.51wt% of Al, 27.96wt% of Fe and 12.01wt% of Mo.
The preparation method of the CrAlFe-based alloy target provided by the embodiment comprises the following steps:
s1, calculating and weighing raw materials required by preparing the CrAlFe-based alloy target according to the mass of the prepared CrAlFe-based alloy target, wherein the raw materials comprise Cr powder, al powder, fe powder and Mo powder, the purity of the Fe powder is more than or equal to 99.5wt%, and the Fisher granularity F.S.S.S=6.0 mu m; the Al powder is air atomized aluminum powder, the purity is more than or equal to 99.7wt percent, and the granularity is-200 meshes; the purity of Cr powder is more than or equal to 99.8wt percent, and the granularity is-200 meshes; the purity of Mo powder is more than or equal to 99.9wt percent, and the Fisher particle size F.S.S. is 6.7 mu m;
Filling Al powder and Fe powder into a high-energy ball mill for high-energy ball milling treatment to obtain prealloyed AlFe alloy powder, wherein the high-energy ball milling parameters are as follows: the ball milling process comprises the steps of taking a steel ball with the diameter of D25mm as a ball milling medium, wherein the ball material ratio is ball and powder raw material mass ratio=15:1, pre-vacuumizing to the vacuum degree of 0.05Pa, filling Ar gas with the pressure of 0.5Pa into a high-energy ball mill, performing high-energy ball milling treatment under the protection of the Ar gas, wherein the ball milling rotating speed is 120r/min, the ball milling time is 24 hours, sieving alloy powder to remove large powder particles after ball milling, and the sieve aperture is 1mm.
S2, uniformly mixing the AlFe alloy powder obtained in the step S1, cr powder and Mo powder in a universal motion mixer to obtain CrAlFeMo alloy powder, wherein the mixing adopts a mode of adding zirconia balls for dry mixing, and the ball-to-material ratio is ZrO 2 Ball weight: mix weight = 1:10, mixing time 6h.
S3, uniformly filling the CrAlFeMo alloy powder obtained in the step S2 into a round graphite mold, wherein the effective size of the inner cavity of the mold is D165 x 200mm, carrying out hot-press sintering under vacuum conditions, continuously vacuumizing in the hot-press sintering process, maintaining the pressure and cooling to 450 ℃ along with a furnace after the hot-press sintering is finished, linearly releasing the pressure to 0MPa, releasing the pressure for 0.5h, naturally cooling to 150 ℃ along with the furnace, discharging from the furnace, and demoulding to obtain a high-density CrAlFeMo sintered blank, wherein the hot-press sintering comprises the following steps: firstly, under the room temperature state, applying an initial pressure of 8Mpa to CrAlFeMo alloy powder, vacuumizing to 0.1Pa, starting a vacuum hot-pressing sintering program, heating to 135 ℃ from room temperature, heating at a heating rate of 2 ℃/min, starting timing, preserving heat and pressure after the vacuum degree reaches 0.03Pa, preserving heat and pressure for 4h at 135 ℃ and 8Mpa, continuously heating to a sintering temperature of 520 ℃ (heating rate of 5 ℃/min), linearly boosting to a sintering pressure of 40Mpa, wherein the time from 8Mpa to 40Mpa is the same as the time from 135 ℃ to 520 ℃, and preserving heat and pressure for 3h at 520 ℃ and 40 Mpa.
S4, grinding, wire cutting, turning and milling are carried out on the CrAlFeMo sintered blank, so that the CrAlFeMo alloy target (finished target) meeting the requirements of the size and the surface quality is obtained, and the target is a round target with the size: diameter D160mm and height 14mm.
The microstructure diagram of the CrAlFeMo alloy target prepared in the embodiment is similar to that of the embodiment 1, the alloy target prepared in the embodiment has uniform structure, cr and Al do not generate alloying reaction, and the target has no cracking phenomenon.
Example 3
The CrAlFe-based alloy target provided by the embodiment is a CrAlFeNb alloy target, and comprises the following chemical components in percentage by atom: cr (Cr) 55 Al 40 Fe 3 Nb 2 The method comprises the following steps of: 55at% of Cr, 40at% of Al, 3at% of Fe, 2at% of Nb, and the weight percentages are as follows: 66.63wt% of Cr, 25.14wt% of Al, 3.9wt% of Fe and 4.33wt% of Nb.
The preparation method of the CrAlFe-based alloy target provided by the embodiment comprises the following steps:
s1, calculating and weighing raw materials required by preparing the CrAlFe-based alloy target according to the mass of the prepared CrAlFe-based alloy target, wherein the raw materials comprise Cr powder, al powder, fe powder and Nb powder, the purity of the Fe powder is more than or equal to 99.5wt%, and the Fisher granularity F.S.S.S=6.0 mu m; the Al powder is air atomized aluminum powder, the purity is more than or equal to 99.7wt percent, and the granularity is-200 meshes; the purity of Cr powder is more than or equal to 99.8wt percent, and the granularity is-200 meshes; the purity of the Nb powder is more than or equal to 99.5 weight percent, and the granularity is-300 meshes;
Filling Al powder and Fe powder into a high-energy ball mill for high-energy ball milling treatment to obtain prealloyed AlFe alloy powder, wherein the high-energy ball milling parameters are as follows: the ball milling process comprises the steps of taking a steel ball with the diameter of D25mm as a ball milling medium, wherein the ball material ratio is ball and powder raw material mass ratio=15:1, pre-vacuumizing to the vacuum degree of 0.05Pa, filling Ar gas with the pressure of 0.5Pa into a high-energy ball mill, performing high-energy ball milling treatment under the protection of the Ar gas, wherein the ball milling rotating speed is 120r/min, the ball milling time is 24 hours, sieving alloy powder to remove large powder particles after ball milling, and the sieve aperture is 1mm.
S2, uniformly mixing the AlFe alloy powder obtained in the step S1, cr powder and Nb powder in a universal motion mixer to obtain CrAlNb alloy powder, wherein the mixing adopts a mode of adding zirconia balls for dry mixing, and the ball-to-material ratio is ZrO 2 Ball weight: mix weight = 1:10, mixing time 6h.
S3, uniformly filling the CrAlNb alloy powder obtained in the step S2 into a round graphite mold, wherein the effective size of the inner cavity of the mold is D165 x 200mm (the effective inner diameter of the mold is 165mm, the depth is 200 mm), performing hot-press sintering under a vacuum condition, continuously vacuumizing in the hot-press sintering process, maintaining the pressure and cooling to 450 ℃ along with a furnace after the hot-press sintering is finished, linearly releasing the pressure to 0MPa, releasing the pressure for 0.5h, naturally cooling to 150 ℃ along with the furnace, discharging from the furnace, and demolding to obtain a high-density CrAlNb sintered blank, wherein the hot-press sintering comprises: firstly, under the room temperature state, the initial pressure of 10Mpa is applied to CrAlNb alloy powder, meanwhile, the vacuum pumping is carried out to 0.1Pa, then, a vacuum hot-pressing sintering program is started, the temperature is raised to 170 ℃ from room temperature, the heating rate is 2 ℃/min, after the vacuum degree reaches 0.02Pa, the timing, the heat preservation and the pressure maintaining are started, the heat preservation and the pressure maintaining are carried out for 3 hours at 170 ℃ and 10Mpa, the temperature is continuously raised to 550 ℃ (the heating rate is 4 ℃/min), meanwhile, the linear pressure is raised to 35MPa, the time for raising the pressure from 10Mpa to 35MPa is the same as the time for raising the temperature from 170 ℃ to 550 ℃, and the heat preservation and the pressure maintaining are carried out for 1.5 hours at 550 ℃ and 35 MPa.
S4, grinding, wire cutting, turning and milling are carried out on the CrAlNb sintered blank, so that a CrAlNb alloy target (finished target) meeting the requirements of size and surface quality is obtained, and the target is a round target with the size: diameter D160.0mm, height 12mm.
The microstructure diagram of the CrAlNb alloy target prepared in the embodiment is similar to that of the embodiment 1, the microstructure of the alloy target prepared in the embodiment is uniform, the Cr and Al do not generate alloying reaction, and the target does not have cracking phenomenon.
Example 4
The CrAlFe-based alloy target provided by the embodiment is a CrAlFeV alloy target, and the chemical components and the atomic percentages thereof are as follows: cr (Cr) 22 Al 60 Fe 3 V 15 The method comprises the following steps of: cr 22at%, al 60at%, fe 3at%, V15 at%, and the weight percentages are: 30.96wt% of Cr, 43.82wt% of Al, 4.54wt% of Fe and 20.68wt% of V.
The preparation method of the CrAlFe-based alloy target provided by the embodiment comprises the following steps:
s1, calculating and weighing raw materials required by preparing the CrAlFe-based alloy target according to the mass of the prepared CrAlFe-based alloy target, wherein the raw materials comprise Cr powder, al powder, fe powder and V powder, the purity of the Fe powder is more than or equal to 99.5wt%, and the Fisher granularity F.S.S.S=6.0 mu m; the Al powder is air atomized aluminum powder, the purity is more than or equal to 99.7wt percent, and the granularity is-200 meshes; the purity of Cr powder is more than or equal to 99.8wt percent, and the granularity is-200 meshes; the purity of the V powder is more than or equal to 99.8wt percent, and the granularity is minus 325 meshes;
Filling Al powder and Fe powder into a high-energy ball mill for high-energy ball milling treatment to obtain prealloyed AlFe alloy powder, wherein the high-energy ball milling parameters are as follows: the ball milling process comprises the steps of taking a steel ball with the diameter of D25mm as a ball milling medium, wherein the ball material ratio is ball and powder raw material mass ratio=15:1, pre-vacuumizing to the vacuum degree of 0.05Pa, filling Ar gas with the pressure of 0.5Pa into a high-energy ball mill, performing high-energy ball milling treatment under the protection of the Ar gas, wherein the ball milling rotating speed is 120r/min, the ball milling time is 32h, sieving alloy powder to remove large powder particles after ball milling, and the sieve aperture is 1mm.
S2, uniformly mixing the AlFe alloy powder obtained in the step S1, cr powder and V powder in a universal motion mixer to obtain CrAlFeV alloy powder, wherein the mixing adopts a mode of adding zirconia balls for dry mixing, and the ball-to-material ratio is ZrO 2 Ball weight: mix weight = 1:10, mixing time 6h.
S3, uniformly filling the CrAlFeV alloy powder obtained in the step S2 into a round graphite mold, wherein the effective size of the inner cavity of the mold is D165 x 200mm (the effective inner diameter of the mold is 165mm, the depth is 200 mm), performing hot-press sintering under a vacuum condition, continuously vacuumizing in the hot-press sintering process, maintaining the pressure and cooling to 450 ℃ along with a furnace after the hot-press sintering is finished, linearly releasing the pressure to 0MPa, releasing the pressure for 0.5h, naturally cooling to 150 ℃ along with the furnace, discharging from the furnace, and demolding to obtain a high-density CrAlFeV sintered blank, wherein the hot-press sintering comprises: firstly, under the room temperature state, applying an initial pressure of 12Mpa to CrAlFeV alloy powder, vacuumizing to 0.1Pa, starting a vacuum hot-pressing sintering program, heating to 160 ℃ from room temperature, heating at a heating rate of 2 ℃/min, starting timing, preserving heat and pressure after the vacuum degree reaches 0.05Pa, preserving heat and pressure for 4 hours at 160 ℃ and 12Mpa, continuously heating to a sintering temperature of 530 ℃ (heating rate of 4 ℃/min), linearly boosting to the sintering pressure of 35MPa, wherein the time for boosting to 35MPa from 12Mpa is the same as the time for heating to the sintering temperature of 530 ℃, and preserving heat and pressure for 3 hours at 530 ℃ and 35 MPa.
S4, grinding, wire cutting, turning and milling are carried out on the CrAlFeV sintered blank, so that the CrAlFeV alloy target (finished target) meeting the requirements of the size and the surface quality is obtained, and the target is a round target with the size: diameter D154.0mm and height 20mm.
The microstructure diagram of the CrAlFeV alloy target prepared in the embodiment is similar to that of the embodiment 1, the alloy target prepared in the embodiment has uniform structure, cr and Al do not generate alloying reaction, and the target has no cracking phenomenon.
Example 5
The CrAlFe-based alloy target provided by the embodiment is a CrAlFe alloy target, and comprises the following chemical components in percentage by atom: cr (Cr) 70 Al 25 Fe 5 The method comprises the following steps of: 70at% of Cr, 25at% of Al and 5at% of Fe, and the weight percentages are as follows: 79.24wt% of Cr, 14.68wt% of Al and 6.08wt% of Fe.
The preparation method of the CrAlFe-based alloy target provided by the embodiment comprises the following steps:
s1, preparing prealloyed AlFe alloy powder in the step S1 of reference example 1.
S2, uniformly mixing the AlFe alloy powder obtained in the step S1 and Cr powder in a universal motion mixer to obtain CrAlFe alloy powder, wherein the mixing adopts a mode of adding zirconia balls for dry mixing, and the ball-to-material ratio is ZrO 2 Ball weight: mix weight = 1:5, mixing time 4h.
S3, uniformly filling the CrAlFe alloy powder obtained in the step S2 into a round graphite die, wherein the effective size of the inner cavity of the die is D165 x 200mm (the effective inner diameter of the die is 165mm, the depth of the die is 200 mm), performing hot-press sintering under a vacuum condition, continuously vacuumizing in the hot-press sintering process, maintaining the pressure and cooling to 450 ℃ along with a furnace after the hot-press sintering is finished, linearly releasing the pressure to 0MPa, releasing the pressure for 0.5h, naturally cooling to 100 ℃ along with the furnace, discharging from the furnace, and demoulding to obtain a CrAlFe sintered blank with high density, wherein the hot-press sintering comprises: firstly, under the room temperature state, the initial pressure of 10Mpa is applied to CrAlFe alloy powder, meanwhile, the vacuum pumping is carried out to 0.1Pa, then the vacuum hot-pressing sintering procedure is started, the temperature is raised to 150 ℃ from room temperature, the heating rate is 2 ℃/min, the timing, the heat preservation and the pressure maintaining are started after the vacuum degree reaches 0.01Pa, the heat preservation and the pressure maintaining are carried out for 4 hours at 150 ℃ and 10Mpa, the temperature is continuously raised to the sintering temperature 600 ℃ (the heating rate is 4 ℃/min), meanwhile, the linear pressure is raised to the sintering pressure of 25MPa, the time of the pressure rise from 10Mpa to 25Mpa is the same as the time of the temperature rise from 150 ℃ to the sintering temperature of 600 ℃, and the heat preservation and the pressure maintaining are carried out for 5 hours at 600 ℃ and 25 MPa.
S4, grinding, wire cutting, turning and milling are carried out on the CrAlFe sintered blank, so that a CrAlFe alloy target (finished target) meeting the requirements of size and surface quality is obtained, wherein the target is a round target, and the size is as follows: diameter d156.3mm and height 20mm.
The microstructure diagram of the CrAlFe alloy target prepared in the embodiment is similar to that of the embodiment 1, the microstructure of the alloy target prepared in the embodiment is uniform, the Cr and Al do not generate alloying reaction, and the target does not have cracking phenomenon.
Comparative example 1
The CrAlFe-based alloy target provided in the comparative example is a CrAlFe alloy target, and comprises the following chemical components in percentage by atom: cr (Cr) 40 Al 50 Fe 10 The method comprises the following steps of: 40at% of Cr, 50at% of Al and 10at% of Fe, and the weight percentages are as follows: cr 52.16wt%, al 33.83wt% and Fe 14.01wt%.
The preparation method of the CrAlFe-based alloy target provided by the comparative example is a HIP process, and specifically comprises the following steps:
s1, calculating and weighing raw materials required by preparing the CrAlFe-based alloy target according to the mass of the prepared CrAlFe-based alloy target, wherein the raw materials comprise Cr powder, al powder and Fe powder, the purity of the Fe powder is more than or equal to 99.5wt%, and the Fisher granularity F.S.S.S=6.0 mu m; the Al powder is air atomized aluminum powder, the purity is more than or equal to 99.7wt percent, and the granularity is-200 meshes; the purity of Cr powder is more than or equal to 99.8wt percent, and the granularity is-200 meshes; mixing Al powder, fe powder and Cr powder in a universal motion mixer for 6 hours, wherein the ball-to-material ratio is 1:10, and obtaining CrAlFe alloy powder.
S2, packing the powder prepared in the step S1 into a sleeve, and degassing in a degassing furnace at a degassing temperature of 350 ℃ and a degassing vacuum degree of 0.005Pa for 4 hours; hot Isostatic Pressing (HIP) after sheath sealing, HIP temperature 450 ℃, pressure 115MPa, heat preservation and pressure maintaining for 4 hours, cooling to 150 ℃ along with a furnace, releasing pressure, evacuating, discharging from the furnace, cooling to room temperature and removing sheath to obtain the CrAlFe-based alloy sintered blank.
And S3, performing linear cutting and turning/milling processing on the CrAlFe-based alloy sintered blank to obtain the CrAlFe-based alloy target.
Fig. 2 is a microstructure view (SEM image of scanning electron microscope) of the CrAlFe alloy target provided in this comparative example, fig. 4 is an appearance view of the CrAlFe alloy target provided in this comparative example, and fig. 5 is another appearance view of the CrAlFe alloy target provided in this comparative example, as can be seen from fig. 2, fig. 4 and fig. 5, the outer circle and the core of the CrAlFe alloy target provided in this comparative example have a large number of annular cracks, and the edges of Cr particles have a large number of cracks, so that serious cracking phenomenon occurs. The applicant speculates that the reasons may be: al and Fe react to release heat, so that Cr and Al are alloyed to generate more alloy phases, the brittleness of the target is increased, and the target is easy to crack; as the conventional hot isostatic pressing process is to cool down in a pressed state, residual stress in the cooled target is large, and the brittle target is easy to crack.
Comparative example 2
The CrAlFe-based alloy target provided in this comparative example is a CrAlFe alloy target, and has the same chemical composition and atomic percentage as those in example 1, specifically: cr (Cr) 40 Al 50 Fe 10 The method comprises the following steps of: 40at% of Cr, 50at% of Al and 10at% of Fe.
The preparation method of the CrAlFe-based alloy target provided in this comparative example is basically the same as that of example 1, except that all the alloy powders are mixed together, specifically including the steps of:
s1, calculating and weighing raw materials required by preparing the CrAlFe-based alloy target according to the mass of the prepared CrAlFe-based alloy target, wherein the raw materials comprise Cr powder, al powder and Fe powder, the purity of the Fe powder is more than or equal to 99.5wt%, and the Fisher granularity F.S.S.S=6.0 mu m; the Al powder is air atomized aluminum powder, the purity is more than or equal to 99.7wt percent, and the granularity is-200 meshes; the purity of Cr powder is more than or equal to 99.8wt percent, and the granularity is-200 meshes;
uniformly mixing Al powder, fe powder and Cr powder in a universal motion mixer to obtain CrAlFe alloy powder, wherein the mixing adopts a mode of adding zirconia balls for dry mixing, and the ball-to-material ratio is ZrO 2 Ball weight: mix weight = 1:10, mixing time 8h.
S2, the same as step S3 in example 1.
S3, the same as the step S4 in the embodiment 1.
Cr and Al in the CrAlFe alloy target provided in the comparative example have alloying reaction, and microcracks are arranged in the target.
Comparative example 3
The CrAlFe-based alloy target provided in this comparative example is a CrAlFe alloy target, and has the same chemical composition and atomic percentage as those in example 1, specifically: cr (Cr) 40 Al 50 Fe 10 The method comprises the following steps of: 40at% of Cr, 50at% of Al and 10at% of Fe.
The preparation method of the CrAlFe-based alloy target provided in the comparative example is basically the same as that of the example 1, except that the temperature is raised to 300 ℃ from room temperature in the step S3, and the preparation method specifically comprises the following steps:
S1-S2 the same procedure as in examples 1S 1-S2.
S3, uniformly filling the CrAlFe alloy powder obtained in the step S2 into a round graphite die, wherein the effective size of the inner cavity of the die is D165 x 200mm (the effective inner diameter of the die is 165mm, the depth of the die is 200 mm), performing hot-press sintering under a vacuum condition, continuously vacuumizing in the hot-press sintering process, maintaining the pressure and cooling to 450 ℃ along with a furnace after the hot-press sintering is finished, linearly releasing the pressure to 0MPa, releasing the pressure for 0.5h, naturally cooling to 150 ℃ along with the furnace, discharging from the furnace, and demoulding to obtain a CrAlFe sintered blank with high density, wherein the hot-press sintering comprises: firstly, under the room temperature state, the initial pressure of 10Mpa is applied to CrAlFe alloy powder, meanwhile, the vacuum pumping is carried out to 0.1Pa, then, the vacuum hot-pressing sintering procedure is started, the temperature is raised to 300 ℃ from room temperature, the heating rate is 2 ℃/min, the timing, the heat preservation and the pressure maintaining are started after the vacuum degree reaches 0.05Pa, the heat preservation and the pressure maintaining are carried out for 3 hours at 300 ℃ and 10Mpa, the temperature is continuously raised to the sintering temperature 535 ℃ (the heating rate is 4 ℃/min), meanwhile, the linear pressure is raised to 35MPa, and the heat preservation and the pressure maintaining are carried out for 2.5 hours at 535 ℃ and 35 MPa.
S4 is the same as the step S4 of example 1.
Comparative example 4
The CrAlFe-based alloy target provided in this comparative example is a CrAlFe alloy target, and has the same chemical composition and atomic percentage as those in example 1, specifically: cr (Cr) 40 Al 50 Fe 10 I.e. by atomic percentThe ratio is as follows: 40at% of Cr, 50at% of Al and 10at% of Fe.
The preparation method of the CrAlFe-based alloy target provided in the comparative example is basically the same as that of the example 1, except that the sintering temperature in the step S3 is 660 ℃, and specifically comprises the following steps:
S1-S2 the same procedure as in examples 1S 1-S2.
S3, uniformly filling the CrAlFe alloy powder obtained in the step S2 into a round graphite die, wherein the effective size of the inner cavity of the die is D165 x 200mm (the effective inner diameter of the die is 165mm, the depth of the die is 200 mm), performing hot-press sintering under a vacuum condition, continuously vacuumizing in the hot-press sintering process, maintaining the pressure and cooling to 450 ℃ along with a furnace after the hot-press sintering is finished, linearly releasing the pressure to 0MPa, releasing the pressure for 0.5h, naturally cooling to 150 ℃ along with the furnace, discharging from the furnace, and demoulding to obtain a CrAlFe sintered blank with high density, wherein the hot-press sintering comprises: firstly, under the room temperature state, the initial pressure of 10Mpa is applied to CrAlFe alloy powder, meanwhile, the vacuum is pumped to 0.1Pa, then, a vacuum hot-pressing sintering procedure is started, the temperature is raised to 150 ℃ from room temperature, the heating rate is 2 ℃/min, after the vacuum degree reaches 0.05Pa, the timing, the heat preservation and the pressure maintaining are started, the heat preservation and the pressure maintaining are carried out for 3 hours at 150 ℃ and 10Mpa, the temperature is continuously raised to the sintering temperature of 660 ℃ (the heating rate is 4 ℃/min), meanwhile, the linear pressure is raised to 35MPa, and the heat preservation and the pressure maintaining time at 660 ℃ and 35MPa is 1 hour.
S4 is the same as the step S4 of example 1.
Cr and Al in the CrAlFe alloy target provided by the comparative example are seriously alloyed, and microcracks appear in the target.
Comparative example 5
The CrAlFe-based alloy target provided in this comparative example is a CrAlFe alloy target, and has the same chemical composition and atomic percentage as those in example 1, specifically: cr (Cr) 40 Al 50 Fe 10 The method comprises the following steps of: 40at% of Cr, 50at% of Al and 10at% of Fe.
The preparation method of the CrAlFe-based alloy target material provided by the comparative example is basically the same as that of the example 1, except that the ball milling time is 60h in the step S1, and the preparation method specifically comprises the following steps:
s1 is basically the same as step S1 in example 1, except that the ball milling time is 60h.
S2-S4 steps are identical to those of examples 1S 2-S4.
Comparative example 6
The CrAlFe-based alloy target provided in the comparative example is a CrAlFe alloy target, and comprises the following chemical components in percentage by atom: cr (Cr) 40 Al 50 Fe 10 The method comprises the following steps of: 40at% of Cr, 50at% of Al and 10at% of Fe, and the weight percentages are as follows: cr 52.16wt%, al 33.83wt% and Fe 14.01wt%.
The preparation method of the CrAlFe-based alloy target provided by the comparative example is basically the same as that of the example 1, and is characterized in that in the step S3, after hot-pressed sintering is finished, the target is naturally cooled to 150 ℃ along with a furnace, pressure relief is carried out, and the target is discharged and demoulded, and specifically comprises the following steps:
Steps S1 and S2 are the same as steps S1 and S2 in example 1.
S3, uniformly filling the CrAlFe alloy powder obtained in the step S2 into a round graphite die, wherein the effective size of an inner cavity of the die is D165 x 200mm (the effective inner diameter of the die is 165mm, the depth of the die is 200 mm), performing hot-press sintering under a vacuum condition, continuously vacuumizing in the hot-press sintering process, naturally cooling to 150 ℃ along with a furnace after the hot-press sintering is finished, linearly releasing pressure to be 0MPa, releasing pressure for 30min, discharging and demoulding to obtain a CrAlFe sintered blank, wherein the hot-press sintering comprises the following steps: firstly, under the room temperature state, the initial pressure of 10Mpa is applied to CrAlFe alloy powder, meanwhile, the vacuum pumping is carried out to 0.1Pa, then the vacuum hot-pressing sintering procedure is started, the temperature is raised to 150 ℃ from room temperature, the heating rate is 2 ℃/min, the timing, the heat preservation and the pressure maintaining are started after the vacuum degree reaches 0.05Pa, the heat preservation and the pressure maintaining are carried out for 3 hours at 150 ℃ and 10Mpa, the temperature is continuously raised to the sintering temperature 535 ℃ (the heating rate is 4 ℃/min), meanwhile, the linear pressure is raised to the sintering pressure of 35MPa, the time of the pressure rise from 10Mpa to 35Mpa is the same as the time of the temperature rise from 150 ℃ to the sintering temperature 535 ℃, and the heat preservation and the pressure maintaining are carried out for 2.5 hours at 535 ℃ and 35 MPa.
Step S4 is the same as step S4 in example 1.
Cracks with a depth of 2-3mm appear on the surface of the alloy target prepared in the comparative example.
Performance testing
The CrAlFe alloy targets provided in examples 1-5 and comparative examples 1-5 were tested for relative density, brittleness and oxygen content in the targets, and the test results are shown in Table 1.
The detection method of the relative density comprises the following steps: the relative density is measured by Archimedes drainage according to the measured density value divided by the theoretical density value of the target.
The method for detecting the brittleness (bending strength) of the target comprises the following steps: the mechanical properties are measured by an Instron 3369 universal material tester, and according to the industry standard YB/T5349-2014, test method for bending mechanical properties of metallic materials.
The O content in the target material is measured by an inert gas melting infrared thermal conductivity method.
TABLE 1
From table 1, the following points can be seen:
(1) The alloy targets prepared in the examples 1-5 have lower oxygen content, larger bending strength and high compactness; the higher the degree of alloying in the target, the higher the relative density of the target, which will generally exceed the theoretical density value, and thus a relative density greater than 100% will occur in the comparative example.
(2) As can be seen from the examples 1 and 2, the invention can effectively improve the brittleness of the CrAlFe alloy target material and increase the bending strength of the target material by performing high-energy ball milling treatment on the Al powder and the Fe powder and then uniformly mixing the AlFe alloy powder and the Cr powder, and the higher the bending strength of the target material is, the stronger the cracking resistance of the material is shown. The applicant speculates that the reasons may be: according to the invention, the Al powder and the Fe powder are subjected to high-energy ball milling treatment, and then the AlFe alloy powder and the Cr powder are uniformly mixed, so that metal Fe and Al are fully alloyed to form the AlFe alloy powder, the severe alloying reaction heat release of pure Al powder and Fe powder is effectively avoided, the Cr and matrix Al in the target material are caused to generate more brittle alloy phases, the less brittle alloy phases in the target material are ensured, the brittleness of the target material is reduced, and the bending strength of the target material is improved.
(3) As is clear from example 1 and comparative example 3, in the hot press sintering process, when the temperature of the first temperature rise is too high, the oxygen content in the target increases.
(4) As is clear from example 1 and comparative example 4, in the hot press sintering process, when the temperature of the second temperature rise (sintering temperature) is too high, the flexural strength of the target material is lowered.
(5) As is clear from example 1 and comparative example 5, when the ball milling time is too long, the oxygen content in the target increases.
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. While still being apparent from variations or modifications that may be made by those skilled in the art are within the scope of the invention.
Claims (10)
1. The preparation method of the CrAlFe-based alloy target is characterized by comprising the following steps of:
s1, performing high-energy ball milling treatment on Al powder and Fe powder to obtain prealloyed AlFe alloy powder;
s2, uniformly mixing the AlFe alloy powder and the rest raw material powder of the CrAlFe-based alloy target material to obtain CrAlFe-based alloy powder, wherein the rest raw material powder of the CrAlFe-based alloy target material is Cr powder or consists of Cr powder and X powder, and the X powder comprises at least one of W powder, mo powder, ta powder, nb powder and V powder;
S3, carrying out hot-press sintering on the CrAlFe-based alloy powder under a vacuum condition, releasing pressure after the hot-press sintering is finished, and then cooling and demolding to obtain a CrAlFe-based alloy sintered blank;
and S4, machining the CrAlFe-based alloy sintered blank to obtain the CrAlFe-based alloy target.
2. The method for preparing a CrAlFe-based alloy target according to claim 1, wherein the CrAlFe-based alloy target comprises the following chemical components in atomic percent: 10-70at% of Cr, 20-85at% of Al, 0-20at% of Fe which is not 0at%, and 0-20at% of X, wherein X represents at least one of W, mo, ta, nb, V.
3. The method for producing a target of CrAlFe-based alloy according to claim 1, wherein the purity of the Fe powder is not less than 99.5wt%, and the Fisher particle size F.S.S. is 5 to 8. Mu.m; the Al powder is air atomized aluminum powder, the purity is more than or equal to 99.7wt percent, and the granularity is-200 meshes; the purity of the Cr powder is more than or equal to 99.8wt percent, and the granularity is-200 meshes; the purity of the W powder is more than or equal to 99.9wt percent, and the Fisher particle size F.S.S. is 5-8 mu m; the purity of the Mo powder is more than or equal to 99.9wt percent, and the Fisher granularity F.S.S. is 5-8 mu m; the purity of the Ta powder is more than or equal to 99.8 weight percent, and D50=15-20 mu m; the purity of the Nb powder is more than or equal to 99.5 weight percent, and the granularity is-300 meshes; the purity of the V powder is more than or equal to 99.8wt% and the granularity is minus 325 meshes.
4. The preparation method of the CrAlFe-based alloy target according to claim 1, wherein in the step S1, the ball milling medium comprises one of zirconia balls, steel balls and stainless steel balls, and the diameter of the ball milling medium is 20-30mm;
and/or in the step S1, the mass ratio of the ball materials is (10-20): 1;
and/or in the step S1, pre-vacuumizing to the vacuum degree of less than or equal to 0.1Pa, then charging Ar gas of 0.5-2Pa, and performing high-energy ball milling treatment under the protection of Ar gas, wherein the ball milling rotating speed is 100-150r/min, and the ball milling time is 20-50h;
and/or, in the step S1, sieving the AlFe alloy powder after the high-energy ball milling treatment is finished to remove large powder particles, wherein the pore diameter of the sieved screen is 1-2mm.
5. The preparation method of the CrAlFe-based alloy target material according to claim 1, wherein in the step S2, the mixing is performed in a mixer, a mode of adding zirconia balls for dry mixing is adopted, the ball material mass ratio corresponding to the zirconia balls is 1 (5-10), and the mixing time is 3-10h, wherein the mixer is at least one of a universal motion mixer, a three-dimensional mixer and a double-cone mixer.
6. The method for producing a CrAlFe-based alloy target according to claim 1, wherein in step S3, the pressure relief includes maintaining the pressure and cooling to 400-460 ℃, followed by linear pressure relief to a pressure of 0MPa;
And/or, in step S3, the maximum sintering temperature of the hot press sintering is 500-600 ℃.
7. The method for producing a CrAlFe-based alloy target according to claim 1, wherein in step S3, the hot press sintering comprises: firstly, under the room temperature state, applying an initial pressure of 5-12Mpa to CrAlFe-based alloy powder, vacuumizing to 0.1-0.5Pa, then performing vacuum hot-pressing sintering, raising the temperature from room temperature to 120-180 ℃ at a heating rate of 1-5 ℃/min, starting timing, preserving heat and pressure after the vacuum degree reaches 0.01-0.05 Pa, preserving heat and pressure for 1-5h at 120-180 ℃ and 5-12Mpa, continuously raising the temperature to 500-600 ℃ at a heating rate of 2-10 ℃/min, linearly raising the sintering pressure to 20-50MPa, and preserving heat and pressure for 1-6h at 500-600 ℃ and 20-50 MPa.
8. The method for producing a CrAlFe-based alloy target according to claim 6, wherein the pressure relief time is 20min-60min in step S3.
9. The method for producing a CrAlFe-based alloy target according to claim 1, wherein in step S3, the cooling and demolding includes: air cooling along with the furnace after pressure relief, discharging and demoulding when the furnace temperature is lower than 200 ℃;
And/or, in the step S4, the size of the CrAlFe-based alloy target material is D (60-300) mm (10-40) mm.
10. A CrAlFe-based alloy target, characterized in that the CrAlFe-based alloy target is made by the preparation method of any one of claims 1-9.
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