CN114959615A - TiAlCrSiY alloy target and preparation method thereof - Google Patents

TiAlCrSiY alloy target and preparation method thereof Download PDF

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Publication number
CN114959615A
CN114959615A CN202210715970.4A CN202210715970A CN114959615A CN 114959615 A CN114959615 A CN 114959615A CN 202210715970 A CN202210715970 A CN 202210715970A CN 114959615 A CN114959615 A CN 114959615A
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powder
alloy
tialcrsiy
target material
cold
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张凤戈
张欠男
魏铁峰
岳万祥
施政
王建峰
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Suzhou Liujiu New Material Technology Co ltd
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    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
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    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
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    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
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    • C22C21/00Alloys based on aluminium
    • C22C21/003Alloys based on aluminium containing at least 2.6% of one or more of the elements: tin, lead, antimony, bismuth, cadmium, and titanium
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    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
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    • C22C27/06Alloys based on chromium
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    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24Vacuum evaporation
    • C23C14/32Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
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    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
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    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
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Abstract

The invention discloses a TiAlCrSiY alloy target material and a preparation method thereof, wherein the TiAlCrSiY alloy target material comprises the following components in atomic percentage: ti10-50Percent, Al20-78 percent, Cr10-40 percent, Si1-20 percent, Y0-10 percent and Y is not 0; the preparation method comprises the steps of atomizing to prepare powder, mixing the powder, cold press molding, canning, degassing, hot isostatic pressing and the like, wherein AlY is prepared 2 Atomizing the intermediate alloy to obtain AlY 2 Alloy powder; then, raw material powders of Ti, Al, Cr, Si and AlY are added under a certain vacuum degree 2 Mixing the alloy powder to obtain mixed powder; and cold-pressing the mixed powder into a cold-pressed blank, canning, degassing and hot isostatic pressing to obtain the finished target material. The TiAlCrSiY alloy target material prepared by the invention has the advantages of high compactness, high purity, low content of gaseous impurity element O, H, uniform structure, no segregation, high material utilization rate and low cost.

Description

TiAlCrSiY alloy target and preparation method thereof
Technical Field
The invention belongs to the technical field of powder metallurgy, relates to a TiAlCrSiY alloy target material and a preparation method thereof, and particularly relates to a preparation method of a low-cost and high-performance TiAlCrSiY alloy target material for vacuum magnetron sputtering or multi-arc ion plating.
Background
Since the introduction of rare earth application to metal or alloy surface modification in the last 60 s, many material problems in industrial applications were solved. In PVD ion plating, the addition of rare earth elements is an effective and simple technical method for improving the surface quality of the coating. According to the report, rare earth elements are added into the hard coating of TiN or the system thereof, so that the compactness of a film layer, the film-substrate binding force and the oxidation resistance can be obviously improved, and the large particles and the porosity of the coating are reduced. Compared with the PVD rare earth coating cutter without rare earth, the PVD rare earth coating cutter has better high-temperature strength and is suitable for being used at higher cutting speed. The rare earth is introduced by adding rare earth elements (such as Y, Ce, La, etc.) into the target material and preparing the alloy target material containing the rare earth elements by smelting or powder metallurgy and other processes.
When the rare earth-containing alloy target is prepared by a smelting process, shrinkage cavities, looseness and macrosegregation are easily generated in the casting process, and meanwhile, the uniformity of alloy components and structures is difficult to ensure.
The powder metallurgy process is to pack the mixed powder into a sheath, and to sinter the mixture into a compact target material by hot isostatic pressing after degassing. Because the apparent density and the tap density of the titanium powder are both lower, the utilization rate of the target material prepared by the method is lower, so that the target material has higher cost and is not beneficial to industrial production. Meanwhile, rare earth elements are strong in activity and easy to oxidize, the rare earth elements are usually prepared by a hydrogenation dehydrogenation process, and the O and H contents in the target material prepared by a powder metallurgy method are high, so that the mechanical property of a film layer is reduced.
Disclosure of Invention
The invention aims to provide a TiAlCrSiY alloy target material and a preparation method thereof, wherein the TiAlCrSiY alloy target material has the characteristics of low cost and high performance; the TiAlCrSiY alloy target material obtained by the preparation method has low content of gaseous impurity element O, H, and can remarkably improve the material utilization rate in the preparation process of the target material. In order to achieve the above purpose, the following technical scheme is adopted.
A TiAlCrSiY alloy target material comprises the following components in atomic percent: ti 10-50%, Al 20-78%, Cr 10-40%, Si 1-20%, Y0-10% and Y is not 0.
The TiAlCrSiY alloy target material preferably comprises, in atomic percent, 10 to 40% (e.g., 12%, 15%, 20%, 25%, 30%, 35%, 38%) Ti, 20 to 60% (e.g., 22%, 25%, 30%, 35%, 40%, 45%, 50%, 55%, 58%) Al, 10 to 35% (e.g., 12%, 15%, 20%, 25%, 30%, 33%) Cr, 1 to 15% (e.g., 1.5%, 2%, 3%, 5%, 10%, 14%) Si, and 0.1 to 5% (e.g., 0.2%, 0.5%, 1%, 2%, 3%, 4%, 4.5%) Y.
The TiAlCrSiY alloy target material preferably comprises, in atomic percent, 15 to 20% (e.g., 16%, 17%, 18%, 19%) of Ti, 35 to 60% (e.g., 37%, 40%, 45%, 48%, 50%, 52%, 55%, 57%, 59%) of Al, 10 to 35% (e.g., 12%, 15%, 20%, 25%, 30%, 33%) of Cr, 1 to 8% (e.g., 1.5%, 2%, 3%, 5%, 6%, 7%) of Si, and 1 to 5% (e.g., 1.2%, 1.5%, 2%, 2.5%, 3%, 4%, 4.5%) of Y.
As a preferred mode, the TiAlCrSiY alloy target is prepared by adopting a powder metallurgy process, wherein the Y element is AlY 2 Adding the alloy powder.
The invention also provides a preparation method of the TiAlCrSiY alloy target, which adopts the following technical scheme.
The preparation method of the TiAlCrSiY alloy target comprises the following steps:
step 1, atomizing to prepare powder: reacting AlY 2 Preparing AlY by atomizing intermediate alloy 2 Alloy powder;
step 2, mixing powder: under a certain vacuum degree, raw material powders of Ti, Al, Cr and Si and AlY prepared in the step 1 are mixed 2 Mixing the alloy powder to obtain mixed powder;
step 3, cold press molding: uniformly filling the mixed powder in the step 2 into a cold pressing die, and pressing into a cold pressing blank;
step 4, packaging the package: stacking the cold-pressed blank obtained in the step 3 into an aluminum sheath;
step 5, degassing: placing the sheath filled with the cold pressed blank in the step 4 into a degassing furnace for degassing;
step 6, hot isostatic pressing: placing the sheath degassed in the step 5 into a hot isostatic pressing furnace for sintering densification to obtain a hot isostatic pressing ingot blank;
and 7, machining: and (4) machining and cleaning the ingot blank obtained in the step (6) to obtain the required finished target.
In the above preparation method, as a preferred mode, the atomized powder preparation refers to the preparation of AlY 2 The intermediate alloy is melted and then is made into AlY through atomization and cooling 2 The alloy powder has an atomization temperature of 1450-1500 deg.C (e.g., 1460 deg.C, 1470 deg.C, 1480 deg.C, 1490 deg.C).
In the above preparation process, as oneIn a preferred embodiment, in the step 1, the AlY obtained by atomization 2 The purity of the alloy powder is more than or equal to 99.8 percent, wherein O is less than or equal to 0.4 weight percent, H is less than or equal to 0.05 weight percent, and preferably, the AlY 2 The grain size of the alloy powder is-200 meshes to-300 meshes, and is preferably-300 meshes.
In the present invention, the AlY is 2 The intermediate alloy can be selected from commercially available AlY 2 And (4) alloy blocks. In the present invention, AlY is 2 The alloy is also called as intermediate alloy, and the simple substance Y is made into the alloy, so that the Y is convenient to be added into the alloy, and the problem that the Y is easy to burn during smelting is solved.
In addition, the invention adopts metal powder with smaller granularity, which is not only beneficial to increasing the loose packing density of the powder, but also beneficial to solving the segregation problem of the alloy target material. AlY prepared by adopting atomization method 2 The powder obtaining rate of the alloy powder in the grain size section of-300 meshes is high, so that AlY with-300 meshes is adopted on the basis of solving the segregation problem 2 The alloy powder is beneficial to reducing the production cost of the alloy target material.
In the prior art, the Y powder is usually prepared by hydrogenation dehydrogenation, because dehydrogenation is incomplete in the preparation process, the content of O and H in the Y powder obtained by hydrogenation dehydrogenation is high, wherein the content of O is 1-2 wt%, the content of H is 1-3 wt%, and the performance of a film layer formed by a target material can be reduced by the existence of high O and H.
The invention adopts atomization powder preparation process, selects commercial AlY 2 The alloy block is atomized to prepare AlY 2 The alloy powder can effectively reduce the contents of O and H in the finally prepared target material.
The invention adopts AlY 2 The alloy powder replaces a rare earth element Y simple substance, and is blended with Ti, Al, Cr and Si powder to prepare the TiAlCrSiY alloy target material, so that the defect of high content of O and H in the alloy target material due to the fact that the rare earth element Y simple substance is strong in activity and easy to oxidize and needs to be subjected to hydrogenation dehydrogenation is overcome, and the mechanical property of a film layer formed by the alloy target material is finally ensured. At the same time, AlY is adopted 2 The alloy powder replaces a rare earth element Y simple substance, and the problem that the rare earth element simple substance is easily burnt in the smelting process can be solved.
In the above production method, preferably, the particle size of the Ti powder is 35 to 45 μm, the particle size of the Al powder is 35 to 45 μm, the particle size of the Cr powder is-200 to-300 mesh, and the particle size of the Si powder is-200 to-300 mesh.
In the above-mentioned preparation method, as a preferable mode, in the step 2, the mixed powder uses a vacuum universal motion mixer, the degree of vacuum of the mixed powder is 0.1 to 10Pa (e.g., 0.5Pa, 1Pa, 2Pa, 5Pa, 7Pa, 9Pa), and the mixing time is 3 to 6h (e.g., 3.5h, 4h, 5h, 5.5 h).
In the above manufacturing method, as a preferable mode, in the step 3, the density of the cold compact is 65% to 87% (e.g., 67%, 70%, 72%, 75%, 77%, 80%, 85%), preferably 70% to 85% (e.g., 71%, 72%, 76%, 78%, 80%, 82%, 84%).
In the above production method, as a preferable mode, in the step 3, the cold press molding has a pressing pressure of 100-.
In the above-mentioned production method, as a preferable mode, in the step 3, the height of the cold compact is 10 to 100mm (e.g., 20mm, 40mm, 50mm, 60mm, 80mm, 90mm), preferably 14 to 50mm (e.g., 15mm, 20mm, 25mm, 30mm, 35mm, 40mm, 45 mm).
According to the invention, the mixed powder is subjected to cold press molding to obtain a cold pressed blank (the pressed blank for short), then the pressed blank is sheathed, compared with the method for directly sheathing the mixed powder, the mixed powder in the sheath has high loading density, the powder loading weight of an ingot blank with the same size is higher, the utilization rate of finished product processing materials is higher, and the hot isostatic pressing cost can be reduced (because one furnace can press more powder).
The height of the cold pressed compact is usually 10-100mm, and the sheath is usually 1100-1250mm (for example, 1120mm, 1150mm, 1180mm, 1200mm, 1220mm and 1240mm), so that the height difference of powder filling can be effectively reduced, and the component segregation can be reduced.
In the above preparation method, as a preferable mode, in the step 3, the material of the cold press die is tool steel or die steel.
In the invention, the cold press molding adopts a steel die, the single shaft is stressed, the external dimension of the pressed compact is standard, and the shaping is not needed, so the cost is low.
The invention can also adopt cold isostatic pressing instead of cold isostatic pressing, but because the cold isostatic pressing adopts a rubber soft sheath, the cold isostatic pressing is three-way stressed after powder is loaded in a cold isostatic pressing device. As TiAlCrSiY alloy powder containing Ti has low filling density and large shrinkage, and cold isostatic pressing compact generally has the problems of bell mouth, bending and the like, a shaping procedure needs to be added, which influences the utilization rate of finished product processing materials, so that the method is not as simple, convenient and efficient as cold pressing, and has higher cost than cold pressing.
In the above manufacturing method, as a preferable mode, in the step 4, when the cold-pressed blank is jacketed, the graphite paper is padded between the cold-pressed blanks, and the thickness of the graphite paper is preferably 0.2-1mm (for example, 0.3mm, 0.4mm, 0.5mm, 0.6mm, 0.8mm, 0.9 mm).
In the above preparation method, as a preferable mode, in the step 5, the temperature of the degassing treatment is 300- -1 Pa~10 -3 Pa (e.g. 2 x 10) -3 Pa、4*10 -3 Pa、5*10 -3 Pa、8*10 -3 Pa、1*10 -2 Pa、2*10 -2 Pa、5*10 -2 Pa、8*10 -2 Pa)。
In the above preparation method, as a preferable mode, in the step 6, the temperature of the hot isostatic pressing treatment is 350-.
In the above manufacturing method, as a preferable mode, in the step 7, the hot isostatic pressing ingot obtained in the step 6 is unpacked and then cut along a graphite paper sandwich. Because the pressed compact is padded with graphite paper, the pressed compact is easier to separate.
In the invention, in the step of cold press forming, the relative density of the pressed block obtained by cold pressing can reach 70-85% (for example, 75%, 80% and 82%) by controlling the pressing force, the pressed block is sheathed, the loading density is 70-85%, the sheath shrinkage is small during HIP, the shrinkage is regular, the reserved processing allowance is small, and the final material utilization rate of the processed finished product can reach 68-75%.
When the powder is directly sheathed, the packing density is 45-55%, the shrinkage is large and uneven when the HIP is sheathed, more processing allowance needs to be reserved, and the highest utilization rate of the final material of the processed finished product can reach-62%. Therefore, cold pressing can not only improve the powder loading weight, namely one jacket can produce more finished products, the furnace loading of subsequent HIP is improved, the cost kilogram price of HIP is reduced, and the material utilization rate of finished product processing is improved, which is detailed in the following embodiment. And is therefore more cost effective.
The TiAlCrSiY alloy target material is prepared by adopting a powder metallurgy process, and the problem of component segregation in the alloy target material can be reduced by reasonable process parameter design.
In the conventional technology, the alloy target material is prepared by adopting a conventional smelting process, a vacuum consumable furnace is used for smelting titanium alloy usually, and smelting is carried out for multiple times, so that the uniformity of components and structures is not guaranteed well. Therefore, the alloy target prepared by the method has wider component range compared with the alloy target prepared by the conventional smelting process.
Compared with the prior art, the invention has the following beneficial effects:
the TiAlCrSiY alloy target material prepared by the invention has high compactness and high purity, low contents of gas impurity elements O (less than or equal to 0.25wt percent) and H (less than or equal to 0.02wt percent), uniform tissue without segregation, high material utilization rate and lower cost benefit.
Drawings
FIG. 1 is a metallographic structure diagram of a TiAlCrSiY alloy target material obtained in example 1 of the present invention.
FIG. 2 is a metallographic structure diagram of a TiAlCrSiY alloy target material obtained in comparative example 1 of the invention.
Detailed Description
The present invention will be described in detail below with reference to examples thereof. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation. In fact, it will be apparent to those skilled in the art that modifications and variations can be made in the present invention without departing from the scope or spirit thereof. For instance, features illustrated or described as part of one embodiment, can be used with another embodiment to yield a still further embodiment. It is therefore intended that the present invention encompass such modifications and variations as fall within the scope of the appended claims and equivalents thereof.
Example 1
A TiAlCrSiY alloy target material comprises the following components in atomic percent: ti 20%, Al 55%, Cr 20%, Si 3% and Y2%. The finished size of the TiAlCrSiY alloy target material is D105 x 16 mm. The preparation method comprises the following specific steps.
Step one, atomizing to prepare powder: AlY with the purity of 99.8wt percent 2 Atomizing the alloy block to obtain AlY with the granularity of-300 meshes 2 And (3) alloying powder.
Step two, mixing powder: ti powder with the purity of 2N8 and 39 mu m, aluminum powder with the purity of 2N8 and the average grain size of 40 mu m, Cr powder with the purity of 2N8 and minus 200 meshes, Si powder with the purity of 3N6 and the grain size of minus 200 meshes, AlY with the purity of 99.8 percent and minus 300 meshes 2 Alloy powder, according to weight percentage, Ti25.576%, Al38.931%: cr27.782%, Si2.251% and AlY 2 5.46 percent of the powder is weighed and added into a universal motion mixer, and the mixture is mixed after pre-vacuumizing to 0.8Pa for 4 hours to obtain the alloy powder which is uniformly mixed.
Step three, cold press molding: uniformly filling the alloy powder obtained in the second step into a circular cold pressing die with the diameter of D132mm for pressing, wherein the pressing pressure of the cold pressing is 220MPa, the pressure maintaining time is 5s, and the alloy powder is pressed into a cold pressing blank; the density of the obtained cold compact was 70% and the height of the compact was 19.5 mm.
Step four, packaging the package: and (3) overlapping a plurality of cold pressed compacts into an aluminum sheath, and filling graphite paper between the pressed compacts, wherein the size D126 of the graphite paper is 0.3 mm.
Step five, degassing: placing the sheath filled with cold pressed blank into a degassing furnace for degassing at 400 deg.C for 4 hr, and controlling vacuum degree at 2 x 10 -3 Pa。
Step six, hot isostatic pressing: and sealing and welding the degassed sheath in the fifth step, and sintering the sheath in a hot isostatic pressing device to obtain a hot isostatic pressing ingot blank, wherein the sintering temperature is 450 ℃, the heat preservation time is 3h, and the pressure is 130 MPa.
And seventhly, peeling the ingot blank, cutting the ingot blank along the graphite paper interlayer, and processing a finished product according to the drawing requirement, wherein the size of the finished product is D105 x 16 mm.
The TiAlCrSiY alloy target prepared by the method of the embodiment has the compact density of 70%; and counting 162 TiAlCrSiY alloy target finished products prepared in 3D 141mm × 1100mm jackets, wherein the material utilization rate of the final products is 68.1%.
Here, the final material utilization rate is (finished product weight) finished product number/powder weight in the can 100%.
Examples 2 to 4
The difference between the TiAlCrSiY alloy target and the preparation method thereof and the embodiment 1 is that the compaction pressure of cold pressing molding in the embodiment 1 is changed, and the compaction density and the final material utilization rate of the TiAlCrSiY alloy target obtained under different cold pressing pressures are shown in the table 1.
TABLE 1 compaction density and final material utilization obtained at different cold pressing pressures
Figure BDA0003708800100000071
As can be seen from table 1, the higher the relative density of the resulting cold pressed blank, the higher the material utilization of the final product.
Example 5
A TiAlCrSiY alloy target material comprises the following components in atomic percent: ti 45%, Al 40%, Cr 10%, Si 4% and Y1%. The finished size of the TiAlCrSiY alloy target material is D105 x 16 mm. The preparation method is the same as that of the example 1, and in the third step, the cold pressing pressure of the cold pressing molding is 430 MPa. In this embodiment, since the content of Ti is high, the cold pressing pressure required for cold press molding is high.
The compact density and the final material utilization rate of the tialcriy alloy target material obtained in this example are shown in table 1.
Example 6
A TiAlCrSiY alloy target material comprises the following components in atomic percent: ti 35%, Al 20%, Cr 25%, Si 10% and Y10%. The finished size of the TiAlCrSiY alloy target material is D105 x 16 mm. The production method in example 1 was employed, and the cold pressing pressure of the cold press molding in step three was set to 445 MPa.
Because the aluminum content is low in the embodiment, when the atomic percentage is converted into the corresponding weight ratio, the alloy target only contains 8.68wt% of the Al, and the density of the alloy target obtained at the sintering temperature of 450 ℃ is only 90% in the hot isostatic pressing treatment process, so that the higher sintering temperature of the hot isostatic pressing can be adopted to improve the density of the alloy target.
The compact density and the final material utilization rate of the tialcriy alloy target material obtained in this example are shown in table 1.
Example 7
A TiAlCrSiY alloy target material comprises the following components in atomic percent: ti 15%, Al 45%, Cr 30%, Si 5% and Y5%. The finished size of the TiAlCrSiY alloy target material is D105 x 16 mm. The preparation method is the same as that of the example 1, and in the third step, the cold pressing pressure of the cold pressing molding is 400 MPa.
The compact density and the final material utilization rate of the tialcriy alloy target material obtained in this example are shown in table 1.
Comparative example 1
The comparative example provides a TiAlCrSiY alloy target material and a preparation method thereof, and the difference between the TiAlCrSiY alloy target material and the preparation method of the TiAlCrSiY alloy target material and the embodiment 1 is that the stepsIn the second step, conventional Y powder is adopted to replace AlY 2 And (3) mixing the powder to obtain alloy powder, and then directly canning the alloy powder without cold press molding in the third step, degassing and hot isostatic pressing treatment (namely, a conventional hot isostatic pressing process is adopted). In particular, the amount of the solvent to be used,
step two, mixing powder: ti powder with the purity of 2N8 and 39 mu m, aluminum powder with the purity of 2N8 and the average particle size of 40 mu m, Cr powder with the purity of 2N8 and-200 meshes, Si powder with the purity of 3N6 and the particle size of-200 meshes, and Y powder with the purity of 99.5 percent and-200 meshes are mixed according to the weight percentage, namely 25.576 percent, Al39.641: weighing Cr27.782%, Si2.251% and Y4.75%, adding into a universal motion mixer, pre-vacuumizing to 0.8Pa, and mixing for 4h to obtain uniformly mixed alloy powder.
And then directly mounting the alloy powder obtained in the step two in a sheath, degassing, hot isostatic pressing and machining to obtain the TiAlCrSiY alloy target.
The TiAlCrSiY alloy target prepared by the method of the comparative example is used for counting 150 TiAlCrSiY alloy target finished products prepared in 3 jackets with D150mm × 1100mm, and the material utilization rate of the final product is 62.04% according to the statistics.
As can be seen from table 1, the material utilization of the final product prepared in example 1 was significantly improved relative to the material utilization of the final product obtained by the conventional hot isostatic pressing process.
Testing the performance of the target:
sampling and analyzing the alloy target materials obtained in the example 1 and the comparative example, and measuring the density of the target material by an Archimedes drainage method; determining the purity of the target material by chemical analysis, namely determining the content of impurity elements in the target material, wherein O adopts an inert gas pulse infrared method, and H adopts an inert gas pulse thermal conductivity method; the microstructure of the target was analyzed by metallographic microscopy and the test results are shown in table 2. FIG. 1 shows the metallographic structure of the TiAlCrSiY alloy target material prepared in example 1 of the present invention. FIG. 2 shows the metallographic structure of the TiAlCrSiY alloy target material prepared in comparative example 1.
TABLE 2 TiAlCrSiY20/55/20/3/2 at% target Performance
Figure BDA0003708800100000091
*: in example 1, the TiAlCrSiY20/55/20/3/2 at% target material obtained under different cold pressing pressures in examples 1-1 to 1-4 had substantially the same density.
As can be seen from Table 2, compared with comparative example 1, the TiAlCrSiY alloy target material obtained by the preparation method of the invention has high density, low contents of O and H in the target material, and particularly, the content of H is obviously reduced.
As can be seen from FIG. 1, in the microstructure of the TiAlCrSiY alloy target material prepared in example 1, Ti, Cr, Si and AlY 2 The particles are uniformly distributed, wherein AlY 2 Is spherical particle and is a single alloy phase.
As can be seen from fig. 2, in the microstructure of the target obtained in comparative example 1, the Y particles are irregular blocks and are not completely alloyed, and the residual black material in the center of the Y particles is pure Y phase which is not alloyed.
In conclusion, the titanium-aluminum-chromium-silicon-yttrium alloy target material prepared by the preparation method provided by the invention has the advantages of high density, high purity, low content of gas impurity elements O (less than or equal to 0.25 wt%) and H (less than or equal to 0.02 wt%), uniform tissue, no segregation, high material utilization rate and more cost benefit, and is suitable for coating of coatings of various cutters and dies.

Claims (10)

1. The TiAlCrSiY alloy target is characterized by comprising the following components in atomic percent: 10-50% of Ti, 20-78% of Al, 10-40% of Cr, 1-20% of Si, 0-10% of Y and Y not being 0, wherein the TiAlCrSiY alloy target material is prepared by adopting a powder metallurgy process, and Y element is AlY 2 Adding the alloy powder.
2. The TiAlCrSiY alloy target material as claimed in claim 1, which is composed of, in atomic percent, 10-40% of Ti, 20-60% of Al, 10-35% of Cr, 1-15% of Si, and 0.1-5% of Y;
preferably, the alloy consists of, by atom, 15-20% of Ti, 35-60% of Al, 10-35% of Cr, 1-8% of Si and 1-5% of Y.
3. The preparation method of the TiAlCrSiY alloy target material according to claim 1 or 2, characterized by comprising the following steps:
step 1, atomizing to prepare powder: mixing AlY 2 Preparing AlY by atomizing intermediate alloy 2 Alloy powder;
step 2, mixing powder: under a certain vacuum degree, raw material powders of Ti, Al, Cr and Si and AlY prepared in the step 1 are mixed 2 Mixing the alloy powder to obtain mixed powder;
step 3, cold press molding: uniformly filling the mixed powder in the step 2 into a cold pressing die, and pressing into a cold pressing blank;
step 4, packaging the package: overlapping the cold-pressed blank in the step 3 into an aluminum sheath;
step 5, degassing: placing the sheath filled with the cold pressed blank in the step 4 into a degassing furnace for degassing;
step 6, hot isostatic pressing: placing the sheath degassed in the step 5 into a hot isostatic pressing furnace for sintering densification to obtain a hot isostatic pressing ingot blank;
and 7, machining: and (4) machining and cleaning the ingot blank obtained in the step (6) to obtain the required finished target.
4. The method for preparing the TiAlCrSiY alloy target material according to claim 3, wherein the atomizing pulverization is carried out by adding AlY 2 The intermediate alloy is melted and then is made into AlY through atomization and cooling 2 The atomization temperature of the alloy powder is 1450 and 1500 ℃;
preferably, in the step 1, the AlY obtained by atomization 2 The purity of the alloy powder is more than or equal to 99.8 percent, wherein O is less than or equal to 0.4 weight percent, H is less than or equal to 0.05 weight percent,
preferably, the AlY 2 The granularity of the alloy powder is-200 meshes to-300 meshes, preferably-300 meshes;
preferably, the particle size of the Ti powder is 35-45 μm, the particle size of the Al powder is 35-45 μm, the particle size of the Cr powder is-200 meshes-300 meshes, and the particle size of the Si powder is-200 meshes-300 meshes.
5. The preparation method of the TiAlCrSiY alloy target material according to claim 3 or 4, wherein in the step 2, a vacuum universal motion mixer is adopted for mixing the powder, the vacuum degree of the mixed powder is 0.1-10Pa, and the mixing time is 3-6 h.
6. The preparation method of the TiAlCrSiY alloy target material according to claim 3 or 4, wherein in the step 3, the compactness of the cold-pressed compact is 65-87%, preferably 70-85%;
preferably, in the step 3, the pressing pressure of the cold press molding is 600MPa and the pressure maintaining time is 1-30s, preferably, the pressing pressure is 150 MPa and 500MPa and the pressure maintaining time is 1-10 s;
preferably, in the step 3, the height of the cold compact is 10-100mm, preferably 14-50 mm;
preferably, in the step 3, the material of the cold-pressing die is tool steel or die steel.
7. The preparation method of the TiAlCrSiY alloy target material according to claim 3 or 4, characterized in that in the step 4, when the cold pressing blank is sheathed, graphite paper is padded between the cold pressing blanks, and preferably, the thickness of the graphite paper is 0.2-1 mm.
8. The method for preparing the TiAlCrSiY alloy target material as claimed in claim 3 or 4, wherein in the step 5, the degassing treatment temperature is 300- - 1 Pa~10 -3 Pa。
9. The method for preparing the TiAlCrSiY alloy target material according to claim 3 or 4, wherein in the step 6, the hot isostatic pressing treatment temperature is 350-.
10. The method for preparing the TiAlCrSiY alloy target material according to claim 3 or 4, wherein in the step 7, the hot isostatic pressing ingot blank obtained in the step 6 is unbacked and then cut along a graphite paper interlayer.
CN202210715970.4A 2022-06-22 2022-06-22 TiAlCrSiY alloy target and preparation method thereof Pending CN114959615A (en)

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