CN111188016A - High-performance CrAlSiX alloy target and preparation method thereof - Google Patents
High-performance CrAlSiX alloy target and preparation method thereof Download PDFInfo
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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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/06—Alloys based on chromium
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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
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention discloses a high-performance CrAlSiX alloy target and a preparation method thereof, wherein X is one or more of W, Mo, Nb and Ta, the high-performance CrAlSiX alloy target has a double-layer structure and is formed by compounding an upper layer and a bottom layer, the upper layer is a CrAlSiX matrix target, and the CrAlSiX matrix target comprises the following components in atomic percentage: 20-70% of Cr, 20-70% of Al, 0-20% of Si and 1-20% of X; the bottom layer is a metal alloy with good heat-conducting property and mechanical property. The cutter coating prepared by the target material can obviously improve the cutting rate in high-speed dry cutting and prolong the service life of the cutter.
Description
Technical Field
The invention belongs to the technical field of powder metallurgy, and particularly relates to a high-performance CrAlSiX alloy target and a preparation method thereof.
Background
Since the 60 s in the 20 th century, the superhard film material is deposited on the surface of the metal cutting tool by the PVD technology, so that the cutting speed and the wear resistance can be obviously improved, the service life of the tool is prolonged, and the method becomes a main method for improving the performance of the tool. According to statistics, the coating proportion of the machining cutter in the developed countries exceeds 90%, the coating proportion of the cutter in China is continuously improved, and the requirement of the target material as a key source material in the coating technology is increasingly expanded.
In practical application, different types of materials are processed, and the requirements on the performance of tools and dies are various. In order to meet the requirement of high-speed dry cutting, the cutter coating must have higher red hardness and high-temperature oxidation resistance, but the existing TiN, CrN, TiAlN and CrAlN coatings cannot meet the requirement. In recent years, diversification and multilayering of film layers have become the main development direction of current cutter coatings, and thus diversification of targets is also strongly required. Due to the addition of multiple components, each component can play a special role; the multilayer film is designed to exert the excellent performance of each film layer.
The thermal hardness and the high-temperature oxidation resistance of the AlCr-based coating can be improved by adding IVA Si element or VB and VIB group refractory transition metal elements such as W, Mo, Nb and Ta. In high-speed dry machining, crescent bay abrasion can be effectively reduced, and therefore the service life of the cutter is prolonged. The milling cutter is particularly suitable for milling of materials which are difficult to machine, such as tool steel, hardened steel, stainless steel, cast iron, titanium alloy and the like.
However, the technical barrier for preparing the CrAlSiX (X ═ W, Mo, Ta and Nb) alloy target is high. On one hand, the specific gravity difference of the four components is very large, and the mutual flow of powder causes uneven tissues and easy segregation; on the other hand, as the addition amount of alloy elements such as Si, W, Mo, Ta, Nb and the like in the AlCr-based target material is increased, the intrinsic brittleness of the material is obviously increased, and the clamping area (such as ears and steps) cannot bear mechanical load in the use process of the target material, so that the target material is broken and fails. At present, the related research documents of the target materials are fewer, and the patent technology is more novel.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a high-performance CrAlSiX alloy target material, which is added with at least one of alloy elements Si, W, Mo, Ta and Nb on the basis of a CrAl target material, and can obviously improve the cutting efficiency and prolong the service life of a coating.
The second purpose of the invention is to provide a preparation method of a high-performance CrAlSiX alloy target material. The prepared alloy target has the characteristics of high purity, high density, accurate component control, uniform structure, no segregation, good heat conductivity and mechanical properties, excellent coating performance, large specification and size and the like.
The technical scheme adopted by the invention for solving the technical problem is as follows:
a high-performance CrAlSiX alloy target comprises a CrAlSiX matrix target, wherein the CrAlSiX matrix target comprises the following components in atomic percent: 20-70% (e.g., 25%, 30%, 35%, 40%, 45%, 50%, 55%, 60%, 65%) Cr, 20-70% (e.g., 25%, 30%, 35%, 40%, 45%, 50%, 55%, 60%, 65%) Al, 0-20% (e.g., 0%, 2%, 4%, 6%, 8%, 10%, 12%, 14%, 16%, 18%) Si, 1-20% (e.g., 2%, 3%, 5%, 7%, 9%, 11%, 13%, 15%, 17%, 19%) X; wherein X is one or more of W, Mo, Nb and Ta.
In the above-mentioned high-performance craalsix alloy target material, as a preferred embodiment, the craalsix matrix target is composed of the following components in atomic percent: 20-70% of Cr, 20-70% of Al, 0-15% of Si and 1-10% of X.
In the above-mentioned high-performance craalsix alloy target material, as a preferred embodiment, the craalsix matrix target is composed of the following components in atomic percent: 20-70% of Cr, 20-70% of Al, 2-10% of Si and 1-5% of X.
In the high-performance CrAlSiX alloy target material, as a preferred embodiment, the CrAlSiX matrix target has a relative density of more than 99% and an average grain size of not more than 100 μm.
In the above-mentioned high-performance CrAlSiX alloy target, as a preferred embodiment, the high-performance CrAlSiX alloy target is formed by compounding an upper layer and a bottom layer, the upper layer is the CrAlSiX base target, and the bottom layer is an alloy having both good heat conductivity and mechanical properties; more preferably, the thermal conductivity of the underlayer is not less than 150W/(m.k), the tensile strength is not less than 100MPa, the yield strength is not less than 75MPa, and the plasticity is not less than 2%.
In the high-performance CrAlSiX alloy target, as a preferred embodiment, the bottom layer is an aluminum alloy, a copper alloy or a molybdenum alloy.
In the high-performance CrAlSiX alloy target, as a preferred embodiment, the bottom layer is an aluminum alloy, and the aluminum alloy contains at least one of alloy elements of Si, Cu, Mn, Mg, Zn, Ti, and Cr; more preferably, the aluminum alloy is AlY, wherein Y is selected from one or more of Cr, Ti, Si, Cu, Mn and Zn, and the content of Y element is 2-40% by atomic percentage (for example, 3%, 5%, 10%, 15%, 20%, 25%, 30%, 35%).
In the high-performance CrAlSiX alloy target material, as a preferred embodiment, the bottom layer is tightly welded to the upper layer by a hot isostatic pressing diffusion welding technique (i.e., hot isostatic pressing treatment).
In the high-performance CrAlSiX alloy target material, as a preferred embodiment, the thickness of the target material is 12-32mm for a single-layer CrAlSiX base target; for the double-layer target material, the thickness of the upper layer is 3-27mm, and the thickness of the bottom layer is 2-10 mm.
According to another aspect of the invention, a preparation method of the high-performance CrAlSiX alloy target is also provided, which comprises the following steps:
firstly, weighing raw material powder according to the component design of the target material to prepare alloy powder; if the double-layer alloy target material is prepared, respectively preparing upper-layer CrAlSiX alloy powder and bottom-layer alloy powder;
step two, carrying out die pressing treatment on the alloy powder to obtain a die pressing compact; if the double-layer alloy target material is prepared, respectively carrying out die pressing treatment on the upper-layer CrAlSiX alloy powder (matrix alloy powder) and the bottom-layer alloy powder to respectively obtain an upper-layer die pressing compact and a bottom-layer die pressing compact;
step three, the die pressing compact is placed into a sheath, sealed and then subjected to degassing treatment to obtain a degassed sheath; if the double-layer alloy target material is prepared, overlapping the upper layer die pressing compact and the bottom layer die pressing compact and filling the upper layer die pressing compact and the bottom layer die pressing compact into a package;
step four, performing hot isostatic pressing treatment on the degassed sheath to obtain a pressed ingot blank;
and fifthly, machining the pressed ingot blank, and cleaning to obtain the high-performance composite alloy target material.
In the above method for preparing a high-performance CrAlSiX alloy target, as a preferred embodiment, when the preparation of the alloy powder is not specifically described, a method conventional in the art may be adopted, that is, a method conventional in the art is adopted to prepare the raw material into the alloy powder. In the first step, preferably, the raw material powder is prepared by an atomization powder preparation method or directly mixed in a mixer, wherein the raw material powder has a desired particle size (hereinafter referred to as an element powder mixing method). When the element powder mixing method is adopted, the element powder is more preferably mixed in a V-shaped mixer or a three-dimensional mixer under the protection of vacuum or inert gas for 3-10 hours (such as 4 hours, 5 hours, 6 hours, 7 hours and 8 hours).
In the above method for preparing a high-performance CrAlSiX alloy target, as a preferred embodiment, in the step one, the raw material powder is chromium powder, silicon powder, aluminum powder, W powder, Mo powder, Nb powder, or Ta powder, wherein an average particle size of the chromium powder and the silicon powder is 35 to 100 μm (e.g., 40 μm, 50 μm, 60 μm, 70 μm, 80 μm, 90 μm, or 95 μm); the average particle size D50 of the aluminum powder is 2-40 μm (such as 5 μm, 10 μm, 15 μm, 20 μm, 25 μm, 30 μm, 35 μm); the average particle size of the W, Mo, Nb and Ta powders is 5-70 μm (for example, 6 μm, 10 μm, 15 μm, 20 μm, 25 μm, 30 μm, 35 μm, 40 μm, 45 μm, 50 μm, 55 μm, 60 μm and 65 μm); preferably, the bottom layer alloy powder is an aluminum alloy powder, and the average particle size of the aluminum alloy powder is 35-100 μm (such as 40 μm, 50 μm, 60 μm, 70 μm, 80 μm, 90 μm, 95 μm); more preferably, the purity of the raw material powder is preferably 99.8 wt% or more.
In the above method for preparing a high-performance CrAlSiX alloy target, as a preferred embodiment, in the second step, the pressing process is performed at a pressure of 30-330 tons (e.g. 32t, 50t, 100t, 150t, 200t, 250t, 300t, 320t, 325t), a dwell time of 0-5min (e.g. (0.5min, 1min, 1.5min, 2min, 2.5min, 3min, 3.5min, 4min, 4.5min), the pressing process is performed in a single-piece pressing process, preferably, the relative densities of the pressed compacts are both 60-90% (e.g. 65%, 70%, 75%, 80%, 85%), the pressed compacts are each D (80-200) h (16-42) mm for a single-layer target, and the upper and lower pressed compacts are each D (80-200) h (6-35) and D (80-200) h (4-15 mm) for a double-layer target, d represents the diameter of the compact in mm, and h represents the thickness of the compact in mm. In the mould pressing treatment, the mould pressing height is low, so that the height drop can be reduced, and the segregation is further improved; and the application does not need reshaping in cold isostatic pressing after the molding process, so that the process is less and the cost is lower.
In the above method for preparing a high performance CrAlSiX alloy target, as a preferred embodiment, in the third step, the degassing treatment temperature is 300-The vacuum degree of the degassing treatment was controlled to 10-1Pa～10-3Pa (e.g. 5 x 10)-2Pa、10-2Pa、5*10-3Pa)。
In the above method for preparing a high-performance CrAlSiX alloy target, as a preferred embodiment, in the fourth step, the hot isostatic pressing treatment is performed at a temperature of 400-. If the hot isostatic pressing treatment temperature is too high, Cr and Al in the upper-layer target material have alloying reaction, so that an alloy phase is generated to influence the film coating performance; if the hot isostatic pressing treatment temperature is too low, the obtained target material has low density and many gaps, and the use is affected.
Compared with the prior art, the invention has the following beneficial effects:
(1) the CrAlSiX alloy target material prepared by the invention has the advantages of high purity, high density, uniform structure, no segregation, good heat-conducting property and comprehensive mechanical property, excellent coating performance and the like.
(2) According to the high-performance CrAlSiX alloy target material prepared by the invention, the bottom alloy (such as aluminum-based alloy) stabilizing layer is tightly welded on the back surface of the CrAlSiX matrix target material by a hot isostatic pressing diffusion welding connection technology (hot isostatic pressing treatment), so that the prepared double-layer alloy target material is ensured to have high thermal conductivity and good comprehensive mechanical property, when the target material is used under high sputtering power or power density, a target material clamping part can bear the action of larger mechanical stress and thermal stress, and the target material clamping part cannot be brittle fracture or stressed, bent and warped due to too good plasticity.
(3) The introduction of the bottom layer material (for example, the cheap aluminum alloy powder is adopted), the use of rare or precious metal materials such as W, Mo, Ta, Nb and the like can be effectively saved, the development cost of the target and the corresponding film layer is reduced, the popularization of the novel target and the coating in the domestic market is promoted, and the cost benefit is achieved.
(4) The cutter coating prepared by the target material has improved red hardness, high-temperature oxidation resistance and extremely smooth surface, remarkably improves the cutting rate in high-speed dry cutting and prolongs the service life of the cutter, and is particularly suitable for milling of tool steel, hardened steel, stainless steel, cast iron, titanium and titanium alloy.
Drawings
FIG. 1 is a microstructure diagram of a CrAlSiW alloy target obtained in example 5 of the present invention.
Fig. 2 is a structural diagram corresponding to the double-layer target of the present invention, wherein (a) is a front view of the double-layer target, and (b) is a side sectional view of a section a-a of the double-layer target, wherein 1 in (b) denotes a substrate CrAlSiX target, and 2 denotes an underlying aluminum alloy material.
Detailed Description
In order to highlight the objects, technical solutions and advantages of the present invention, the present invention is further illustrated by the following examples, which are presented by way of illustration of the present invention and are not intended to limit the present invention. The technical solution of the present invention is not limited to the specific embodiments listed below, and includes any combination of the specific embodiments.
Examples 1 to 9
The single-layer and double-layer target materials of CrAl, CrAlSi, CrAlW and CrAlSiX (X is W, Mo, Ta and Nb) are sequentially prepared by the preparation method provided by the invention, and the bottom layer material is aluminum alloy (according to atomic percentage, 70 percent of Al and 30 percent of Cr).
The starting powders used in examples 1 to 9 are commercially available in the following purities and particle sizes:
cr powder with purity of 99.8 wt.% and granularity of-200 meshes;
al powder, 99.8 wt.% purity, particle size-325 mesh;
si powder with purity of 99.8 wt.% and granularity of-200 meshes;
powder W, purity 99.9 wt.%, particle size-200 mesh;
mo powder, purity 99.9 wt.%, particle size D50 ═ 8 μm;
ta powder, 99.7 wt.% purity, particle size D50 ═ 8 μm;
nb powder, 99.5 wt.% purity, particle size D50 ═ 8 μm.
The target material is prepared by the following specific steps:
step one, preparing mixed powder of a base body and a bottom layer alloy: respectively taking raw material powder according to the component design in the following table 1, and mixing the powder by using a three-dimensional mixer for 8 hours;
step two, placing the alloy powder obtained in the step one into a die pressing mold, maintaining the pressure for 0.5min under the pressure of 240 tons, and demolding to obtain die pressing compacts with different components, wherein the density is 70%; wherein the size of a green compact for manufacturing the single-layer target material is D200 x 20 mm; the size of the upper laminate used for the bi-layer target fabrication was D200 x 15mm and the size of the bottom laminate was D200 x 5 mm.
Step three, for the preparation of the single-layer target material, directly putting the pressed compact into an aluminum sheath with proper size; for the double-layer target material, an upper layer green compact and a bottom layer green compact are stacked into an aluminum ladle sleeve with a proper size; placing the sheath into a mold pressing compact, degassing at 400 deg.C for 5 hr, and controlling vacuum degree at 10-3Pa or so.
And step four, sealing and welding the degassed sheath, and sintering in hot isostatic pressing equipment, wherein the sintering temperature is 460 ℃, the pressure is 120MPa, and the heat preservation and pressure maintaining time is 3 h.
Step five, machining the ingot blank subjected to the hot isostatic pressing treatment, and cleaning to obtain a required finished target material, wherein the size of the obtained round target material is D160 x 12 mm; the thickness of the substrate (upper layer) A is 8mm, and the thickness of the bottom layer B is 4mm, wherein the alloy target material with the double-layer structure is shown in figure 2.
Measuring the density of the target material by an Archimedes drainage method; measuring the purity of the target material by a GDMS method; and grading the grain size of the prepared target material by using NanoMeasurer grain size grading software. Table 1 shows the composition and basic performance parameters of the targets prepared in examples 1-9, wherein the target composition CrAl30/70 of example 1 indicates that the target is, in atomic percent, Cr 30%, Al 65%, W5%, and so on for other examples, and so on for Table 2.
TABLE 1
In table 1 above, the symbol "r ═ to" means approximately equal to.
The alloy target finished product with the size D160 x 12mm prepared in the above example is subjected to a coating experiment, and the sputtering performance of the target is tested. The substrate is made of hard alloy (WC-6% Co) with the specification of 15 x 6mm, and the substrate is polished, mirror-polished, ultrasonically cleaned and dried by hot air for later use. Selecting the same coating experiment parameters: background vacuum 5 x 10-4Pa, heating the substrate to 500 deg.C, and then charging pure N2The pressure was 3.5Pa, the substrate bias was-100V, and the power density was 17W/cm2And adjusting the deposition time to obtain a coating with the thickness of about 3 mu m. The sputtering properties of the target are shown in table 2.
The discharge stabilization time refers to the idle burning time, which is the time for idle sputtering before the target material meets the requirement of depositing the film (the discharge frequency reaches a certain value). The longer the discharge stabilization time is, the more defects such as pores, inclusions, non-conductive oxides and the like in the target material are, and the uniformity of the phase and the structure is poor. The shorter the discharge stabilization time is, the higher the target material density and the better the tissue uniformity are.
The surface roughness of the coating is measured using a surface profiler or an atomic force microscope.
The coating hardness was measured using a microhardness tester with a load of 0.05 kgf.
TABLE 2
The CrAl30/70 at% and CrAlSi30/60/10 at% alloy targets prepared in examples 1 and 2 begin to bend and warp at the clamped part after sputtering for 120min, and the deformation degree is increased along with the increase of the sputtering time, which obviously reduces the number of furnaces for using the targets.
The CrAlSiW30/60/8/2 at% single-layer target prepared in example 5 is high in intrinsic brittleness, and the clamping position is broken in the Ar gas etching process before film coating, so that continuous sputtering cannot be carried out.
The double-layer craalsix (X ═ W, Mo, Ta, Nb) composite target materials prepared in examples 6 to 9 have better coating hardness, and when the target material is used under high sputtering power or power density, the target material clamping part can bear higher mechanical stress and thermal stress, and the target material clamping part is not brittle fracture or bending warpage, which benefits from the high thermal conductivity and excellent comprehensive mechanical property of the bottom layer aluminum alloy material. Meanwhile, due to the addition of high-melting-point metals W, Mo, Ta and Nb, the melting point of the alloy is increased, the area of a molten pool formed by arc ablation is reduced, large particles accumulated around the molten pool are reduced, the surface roughness is reduced, and the target can be used more continuously. After the molten pool is reduced, the arc energy can be concentrated on a smaller area for sputtering, and the deposition rate of the coating is obviously improved. In addition, the introduction of the bottom aluminum-based alloy material can obviously reduce the use amount of noble metals W, Mo, Ta and Nb, and can obviously reduce the cost of the target material and the corresponding coating.
Using the target materials prepared in the examples 1, 2, 3, 4, 6-9, a CrAlN + CrAlSiXN (X ═ W, Mo, Nb, Ta) double-layer coating is synthesized on the surface of a hard alloy milling cutter through cathodic arc evaporation, the total thickness of the coating is about 3 mu m, the thickness of a CrAlN transition layer is about (approximately equal to) 0.5 mu m, and the thickness of a CrAlSiXN main layer is about 2.5 mu m. Coating deposition temperature at 500 ℃ and N at a pressure of 3.5Pa2The process was carried out under an atmosphere, substrate bias voltages of-80V and-100V, respectively, were applied, and target current 150A was applied.
The end mill with the two-layer coating deposited as described above was used for roughing stainless steel and the tool life of the coatings of different compositions was tested and is shown in table 3.
Milling conditions are as follows:
cutting tool: the diameter D of the end mill is 10mm, and the tooth number Z is 4;
workpiece: austenitic stainless steel, 0Cr18Ni12Mo2 Ti;
cutting parameters: cutting speed VC60m/min, feed speed fv252mm/min, cutting depth ap7 mm; and (3) cooling: 5% of emulsion;
the process comprises the following steps: forward milling;
tool life standard: when the width of the side wear area of the cutter reaches 0.2mm, the total length of cutting is taken as the cutting life of the cutter in meters.
TABLE 3 coating composition and tool cutting life
The cutting tests described above compare the cutting life of coated cemented carbide end mills machining stainless steel. The processing of stainless steel is a very difficult process, and the difficulty lies in that the cutting force is large, the work hardening is serious, the cutter is easy to stick, and the cutter is easy to wear. The coatings 34, 35, 36, 37 give the best results in terms of tool cutting life. The increased cutting life of the tool is related to the increased high temperature hardness and oxidation resistance exhibited by the addition of Si, W, Mo, Ta, Nb to the CrAlN coating, and thus the wear resistance is increased.
Examples 10 to 12
Compared with the double-layer target material of the embodiment 6, the composition ratio of only the upper substrate layer in the embodiments 10 to 12 is different, and other preparation processes are the same. The composition of the upper layer of the targets used alone and the corresponding target properties in examples 10-12 are shown in table 4.
TABLE 4
Examples 13 to 16
Compared with the dual layer target of example 6, examples 13-16 differ only in the hot isostatic pressing process, and all other fabrication processes are the same. The particle sizes of the raw material powders used alone and the corresponding target properties in examples 13-16 are shown in Table 7.
TABLE 5
Claims (10)
1. The high-performance CrAlSiX alloy target is characterized by comprising a CrAlSiX matrix target, wherein the CrAlSiX matrix target comprises the following components in atomic percent: 20-70% of Cr, 20-70% of Al, 0-20% of Si and 1-20% of X; wherein X is one or more of W, Mo, Nb and Ta.
2. The target material according to claim 1, wherein the CrAlSiX base target consists of, in atomic percent: 20-70% of Cr, 20-70% of Al, 0-15% of Si and 1-10% of X; preferably, the CrAlSiX matrix target consists of the following components in atomic percent: 20-70% of Cr, 20-70% of Al, 2-10% of Si and 1-5% of X.
3. A target material according to claim 1 or 2, wherein the CrAlSiX matrix target has a relative density of more than 99% and an average grain size of not more than 100 μm.
4. The target according to any one of claims 1 to 3, wherein the target is formed by compounding an upper layer and a bottom layer, the upper layer is the CrAlSiX substrate target, and the bottom layer is an alloy having both good heat conductivity and mechanical properties; preferably, the thermal conductivity of the bottom layer is not less than 150W/(m.K), the tensile strength is not less than 100MPa, the yield strength is not less than 75MPa, and the plasticity is not less than 2%; more preferably, the bottom layer is an aluminum alloy, a copper alloy or a molybdenum alloy; more preferably, the bottom layer is an aluminum alloy containing at least one of the alloying elements of Si, Cu, Mn, Mg, Zn, Ti and Cr; further preferably, the aluminum alloy is AlY, wherein Y is selected from one or more of Cr, Ti, Si, Cu, Mn and Zn, and the content of Y element is 2-40% by atomic percentage.
5. The target of claim 4, wherein the bottom layer is tightly welded to the upper layer by a hot isostatic pressure diffusion welding technique; preferably, the target material thickness is 12-32mm for a single layer CrAlSiX substrate target; for the double-layer target material, the thickness of the upper layer is 3-27mm, and the thickness of the bottom layer is 2-10 mm.
6. The preparation method of the high-performance CrAlSiX alloy target is characterized by comprising the following steps of:
firstly, weighing raw material powder according to the component design of the target material of any one of claims 1 to 5 to prepare alloy powder; if the double-layer alloy target material is prepared, respectively preparing upper-layer CrAlSiX alloy powder and bottom-layer alloy powder;
step two, carrying out die pressing treatment on the alloy powder to obtain a die pressing compact; if the double-layer alloy target material is prepared, respectively carrying out die pressing treatment on the upper-layer CrAlSiX alloy powder and the bottom-layer alloy powder to respectively obtain an upper-layer die pressing compact and a bottom-layer die pressing compact;
step three, the die pressing compact is placed into a sheath, sealed and then subjected to degassing treatment to obtain a degassed sheath; if the double-layer alloy target material is prepared, overlapping the upper layer die pressing compact and the bottom layer die pressing compact and filling the upper layer die pressing compact and the bottom layer die pressing compact into a package;
step four, performing hot isostatic pressing treatment on the degassed sheath to obtain the high-performance CrAlSiX alloy target material;
preferably, the method further comprises a fifth step of machining and cleaning the high-performance CrAlSiX alloy target to obtain a high-performance composite alloy target finished product.
7. The preparation method according to claim 6, wherein in the first step, the alloy powder is prepared by an atomization powder preparation method or directly mixing raw material powder with a required particle size in a mixer; preferably, the alloy powder is prepared by mixing in a V-shaped mixer or a three-dimensional mixer under the protection of vacuum or inert gas for 3-10 h.
Preferably, the raw material powder is chromium powder, silicon powder, aluminum powder, W powder, Mo powder, Nb powder and Ta powder, wherein the average particle size of the chromium powder and the silicon powder is 35-100 mu m; the average particle size D50 of the aluminum powder is 2-40 μm; the average particle size of the W, Mo, Nb and Ta powder is 5-70 μm; preferably, the bottom layer alloy powder is aluminum alloy powder, and the average particle size of the aluminum alloy powder is 35-100 μm; more preferably, the purity of the raw material powder is preferably 99.8 wt% or more.
8. The production method according to claim 6 or 7, wherein in the second step, the pressure of the molding treatment is 30 to 330 tons, the dwell time is 0 to 5min, and the molding treatment is unidirectional molding. Preferably, the relative density of the pressed compact is 60-90%; for a single layer target, the sizes of the pressed compacts are respectively D (80-200) × h (16-42) mm; for the bi-layer target, the sizes of the upper layer die pressed compact and the bottom layer die pressed compact are respectively D (80-200) × h (6-35) mm and D (80-200) × h (4-15) mm, D represents the diameter of the compact in mm, and h represents the thickness of the compact in mm.
9. The method according to any one of claims 6 to 8, wherein in the third step, the degassing treatment temperature is 300 ℃ and the holding time is 4 to 40 hours, and the vacuum degree of the degassing treatment is controlled to 10-1Pa～10-3Pa。
10. The preparation method according to any one of claims 6 to 9, wherein in the fourth step, the hot isostatic pressing treatment temperature is 400-.
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