Aluminum-yttrium alloy composite target material and preparation method thereof

Through powder metallurgy and vacuum hot press sintering technology, combined with the design of AlSi alloy base material and AlY13/87wt% alloy powder, the problems of coarse grains and serious segregation in the preparation of high yttrium content aluminum yttrium alloy targets are solved, and high density and excellent mechanical properties are achieved.

CN118910568BActive Publication Date: 2025-05-09苏州六九科技股份有限公司
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Patent Information

Application Number
CN202410997385.7
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-07-24
Publication Date
2025-05-09
Estimated Expiration
2044-07-24

AI Technical Summary

Technical Problem

In the preparation of high-yttrium aluminum yttrium alloy targets, the presence of coarse grains, severe segregation, poor mechanical properties, high oxygen content, low density and large intrinsic brittleness of the material, it is difficult to meet the requirements of mechanical processing and coating and carding.

Method used

The powder metallurgy method is adopted, and through the vacuum hot press sintering process, AlY13/87wt% alloy powder is used instead of pure Y powder, the composite target structure is designed, the AlSi alloy base material is equipped, the heating rate and insulation steps are controlled, and the cooling treatment is carried out to prevent the violent alloying reaction of aluminum yttrium.

Benefits of technology

The preparation of high-yttrium content aluminum-yttrium alloy composite target with high density, low impurity content, uniform and unsegregated components is achieved, solving the problems of material brittleness and processing difficulty, and improving the mechanical and thermal conductivity of the target.

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Abstract

The present application relates to the technical field of powder metallurgy materials, and specifically discloses an aluminum-yttrium alloy composite target and a preparation method thereof. The preparation method of the aluminum-yttrium alloy composite target disclosed in the present application is: using powder to mix evenly and mold to obtain AlSi cold pressed blanks; then vacuum hot pressing sintering treatment is carried out, and after slow cooling, the composite target blank is demoulded, and the target product is obtained by post-processing; the parameter conditions of the hot pressing sintering treatment are: after loading the powder, a pressure of 3‑8MPa is applied, and the temperature is kept at 150‑250°C for 1‑4h; then the temperature is increased to 480‑580°C at a heating rate of 3‑10°C / min, and the temperature is kept for 1‑3h; then the temperature is increased to 600‑650°C at a heating rate of 0.5‑3°C / min, and the temperature is kept for 0.5‑2h. The present application realizes the preparation of aluminum-yttrium alloy composite targets with high density, low impurity element content, uniform composition and no segregation through the above-mentioned preparation method.
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Description

Technical Field

[0001] The present application relates to the technical field of powder metallurgy materials, and in particular to an aluminum-yttrium alloy composite target material and a preparation method thereof. Background Art

[0002] Since the service life of hard-coated tools and molds is much longer than that of ordinary tools and molds, it is very common to use hard-coated tools and molds in manufacturing companies. It is known that adding rare earth elements to hard coatings can significantly improve the density of the film layer, the bonding strength of the film base and the antioxidant properties, and reduce the large particles and porosity of the coating. At present, aluminum-yttrium alloy targets are widely used in the coating industry. Adding a certain amount of yttrium to aluminum can play a role in refining grains, resisting oxidation, improving corrosion resistance, and improving strength and plasticity. Therefore, aluminum-yttrium alloys have the comprehensive properties of high strength, corrosion resistance, high temperature resistance and good weldability, and are widely used in aerospace, electronics, optics, coatings and other fields. With the continuous development of coating applications, aluminum-yttrium alloy targets are becoming more and more widely used, especially aluminum-yttrium alloy targets with high yttrium content (yttrium content ≥ 40wt%).

[0003] At present, there are two main methods for preparing high-purity aluminum-yttrium alloys: smelting and powder metallurgy. On the one hand, due to the huge difference in the melting points of yttrium (melting point 1522°C) and aluminum (melting point 660°C), the two are not easy to mix evenly during casting, and there are problems such as coarse grains, severe segregation, and poor mechanical properties. Usually, an aluminum-yttrium intermediate alloy is prepared first, and then aluminum and the aluminum-yttrium intermediate alloy are smelted together. In order to ensure uniform composition, the aluminum-yttrium intermediate alloy needs to be smelted repeatedly, and the process steps are cumbersome. And as the yttrium content in the aluminum-yttrium alloy target increases, brittle second phase particles such as Al 3 Y.Al 2 Y、AlY、Al 2 Y 3 , AlY 2 One or more of them may easily cause shrinkage cavities and cracks during smelting. On the other hand, powder metallurgy usually directly mixes aluminum powder and yttrium powder of different particle sizes and then sinters them into shape. Aluminum powder and yttrium powder are easy to oxidize and difficult to prepare. In the subsequent sintering process, there are problems of high oxygen content and low density, especially when the yttrium content increases, which affects the use effect of the target material. At present, high yttrium content alloy targets still have the problem of high intrinsic brittleness of the material, and the target material is easy to collapse when processing threads or steps. The material cannot meet the requirements of mechanical processing and coating clamping. Therefore, the research and development of a method for high-quality high-yttrium content aluminum-yttrium alloy is of great significance to the development of coating targets for key fields. Summary of the invention

[0004] In order to solve the above technical problems, the present application provides an aluminum-yttrium alloy composite target and a preparation method thereof.

[0005] The present application provides a method for preparing an aluminum-yttrium alloy composite target, which specifically comprises the following steps:

[0006] Mixing powder: Al powder and AlY13 / 87wt% alloy powder are weighed and mixed evenly according to a proportion to obtain an AlY alloy target layer powder composed of Al=20-60wt% and Y=40-80wt%; at the same time, Al powder and AlSi10 gold powder are weighed and mixed evenly according to a proportion to obtain an AlSi alloy bottom layer powder composed of Al=20-100wt% and AlSi10=0-80wt%;

[0007] Compression molding: The AlSi alloy bottom layer powder is subjected to compression molding to obtain an AlSi alloy bottom layer cold pressed billet with a density of 80-95%;

[0008] Mold loading: Load the AlSi alloy bottom cold pressed billet into the mold, and evenly fill the AlY alloy target layer powder on top;

[0009] Hot pressing sintering: in 10 -1 -10 -3 The composite target blank is obtained by vacuum hot pressing and sintering under vacuum conditions of 1000 Pa and slowly cooling and demoulding.

[0010] The parameters of the hot pressing sintering treatment are as follows: after powder loading, a pressure of 3-8 MPa is applied, and the temperature is kept at 150-250°C for 1-4 hours; then the temperature is increased to 480-580°C at a heating rate of 3-10°C / min, and the temperature is kept for 1-3 hours, and the pressure is linearly increased to a set value of 20-50 MPa; then the temperature is increased to 600-650°C at a heating rate of 0.5-3°C / min, and the temperature is kept for 0.5-2 hours;

[0011] Post-processing: machining the composite slab to obtain a target product.

[0012] This application adopts a powder metallurgy method, and adds AlY13 / 87wt% alloy powder instead of pure Y powder to the AlY target material, and realizes the preparation of a high-yttrium-content aluminum-yttrium alloy composite target material with high density, low content of impurity elements N, O, and H, and uniform composition without segregation through a vacuum hot pressing sintering process. At the same time, an AlSi alloy bottom material with excellent comprehensive mechanical properties is configured on the bottom surface of the AlY alloy, and a composite target material structure is designed to solve the problem that the threads and steps cannot be machined due to the intrinsic brittleness of the AlY alloy target material as the Y content increases.

[0013] AlSi10 is a conventional alloy powder, with the national standard grade of 4045 aluminum alloy. Adding AlSi10 alloy powder to the underlying pure Al matrix forms a complex phase structure in which the AlSi10 alloy phase is embedded in the aluminum matrix, which can improve the tensile strength and yield strength of the underlying layer, thereby improving the deformation resistance of the underlying layer. The steps, ears and other mounting positions are not easy to bend or warp, while also having good thermal conductivity. In addition, by adding a certain proportion of AlSi10 alloy powder to the Al matrix, the underlying layer has good thermal conductivity, which is equivalent to the improved thermal conductivity of the AlY-AlSi composite target. In the subsequent PVD coating, it can significantly reduce the appearance of large droplets and large particles, and the resulting film surface is more delicate and smooth, and the film performance is better.

[0014] During the experiment, the inventor found that during the vacuum hot pressing sintering process, when the heating rate is too fast, aluminum yttrium undergoes a violent alloying reaction and releases a large amount of heat, causing the temperature in the furnace to instantly rush to a higher than the set value of 650°C, which is not controlled by the hot pressing furnace temperature controller. Liquid phases will appear in both the bottom layer and the target layer. Under the action of pressure, the liquid phase splashes, aluminum segregation occurs, and microcracks appear in the internal microstructure of the target material. This application controls the aluminum yttrium alloying reaction rate by setting multiple insulation steps and setting different heating rates at different stages (the heating rate is controlled by the heating time). Therefore, this application is designed to be kept warm at 480-580°C, first allowing aluminum yttrium to fully undergo an alloying reaction, and then slowly heating to 600-650°C at a slower heating rate, so that the unreacted aluminum yttrium further slowly alloys, which effectively prevents the problem of uncontrollable temperature caused by concentrated heat release due to the intense alloying of aluminum yttrium.

[0015] In addition, in the vacuum hot pressing sintering process, after the heat preservation is completed, the present application adopts temperature-controlled cooling, and the slow cooling rate can effectively prevent the target material from producing stress cracks.

[0016] The present application adopts the form of powder + cold pressed billet. The bottom layer is molded to obtain an AlSi cold pressed billet of a certain density, and then AlY alloy target layer powder is evenly filled on it, thereby improving the problem of the non-straight boundary line between the target layer and the bottom layer in the double-layer target material obtained by vacuum hot pressing sintering.

[0017] The parameters of the powder mixing are: mixing with a three-dimensional mixer, a rotation speed of 500-900 r / min, and a mixing time of 3-8 h.

[0018] Preferably, in the compression molding, the density of the AlSi alloy bottom cold pressed billet is 80-90%.

[0019] Preferably, the AlSi alloy bottom cold-pressed billet has a diameter of D60-D185 mm and a thickness of 10-30 mm.

[0020] Preferably, the parameters of the compression molding are: the compression pressure is 150-800 tons, and the holding time is 0-10s and is not 0.

[0021] Preferably, the parameter conditions of the hot pressing sintering treatment are: after powder loading, a pressure of 3-8 MPa is applied, and the temperature is kept at 150-250°C for 1-4 hours; then the temperature is increased to 500-580°C at a heating rate of 3-9°C / min, and the temperature is kept for 1-3 hours, and the pressure is linearly increased to a set value of 20-50 MPa; then the temperature is increased to 600-640°C at a heating rate of 0.5-2°C / min, and the temperature is kept for 0.5-2 hours.

[0022] Preferably, during the hot pressing sintering process, the specific parameters of the slow cooling are: cooling the hot pressing sintering temperature of 600-650°C to 350-450°C at a cooling rate of 0.5-5°C / min, then unloading the pressure and cooling to room temperature with the furnace.

[0023] Furthermore, the specific parameters of the slow cooling are: cooling the hot pressing sintering temperature of 600-650°C to 350-400°C at a cooling rate of 0.5-3°C / min, then unloading the pressure and cooling to room temperature along with the furnace.

[0024] On the other hand, the present application provides an aluminum-yttrium alloy composite target material, which is prepared using the above-mentioned method for preparing the aluminum-yttrium alloy composite target material. The preparation method adopts a composite structure design and is prepared by the above-mentioned vacuum hot pressing sintering process.

[0025] In summary, the technical solution of this application has the following effects:

[0026] The preparation method provided in the present application can realize the preparation of AlY alloy target with high yttrium content (Y=40~80wt%). Compared with the conventional AlY alloy target preparation method, the present application adopts a powder metallurgy method, and replaces pure Y powder with AlY13 / 87wt% alloy powder and adds it to the AlY target. Through vacuum hot pressing and sintering process control, it realizes the preparation of high yttrium content aluminum-yttrium alloy target with high density, low content of impurity elements N, O, and H, and uniform composition without segregation. At the same time, the composite target structure is designed, and the AlSi alloy bottom material with excellent comprehensive mechanical properties is configured on the bottom surface of the AlY alloy, which solves the problem that the threads and steps cannot be machined due to the intrinsic brittleness of the AlY alloy target as the Y content increases.

[0027] The preparation method provided in the present application effectively prevents the temperature runaway caused by the heat release of the violent alloying reaction of aluminum and yttrium by setting a heat preservation step and controlling the heating rate during the hot pressing sintering process, thereby ensuring the stable quality or performance of the target material. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1This is the metallographic structure diagram of the aluminum-yttrium alloy substrate target layer in Example 3 of the present application.

[0029] Figure 2 This is a scanning electron microscope image of the aluminum-yttrium alloy substrate target layer in Example 3 of the present application.

[0030] Figure 3 This is a picture of the finished product of the aluminum-yttrium alloy composite target material in Example 3 of the present application.

[0031] Figure 4 This is a picture of the finished product of the aluminum-yttrium alloy composite target material in Comparative Example 1 of the present application. DETAILED DESCRIPTION

[0032] The present application is further described in detail below in conjunction with examples, comparative examples and performance testing experiments. These examples should not be construed as limiting the scope of protection claimed in the present application.

[0033] Example

[0034] Examples 1-5

[0035] Examples 1-5 respectively provide an aluminum-yttrium alloy composite target material and a preparation method thereof.

[0036] The difference between the above embodiments is that the composition of the AlY alloy target layer in the aluminum-yttrium alloy composite target is specifically shown in Table 1.

[0037] The method for preparing the aluminum-yttrium alloy target in the above embodiment comprises the following steps:

[0038] Powder mixing: Al powder and AlY13 / 87wt% alloy powder are weighed in proportion and mixed evenly to obtain AlY alloy target layer powder; at the same time, Al powder and AlSi10 alloy powder are weighed in proportion and mixed evenly to obtain AlSi alloy bottom layer powder (Al(AlSi10) 50 / 50wt% is converted into atomic percentage as AlSi95 / 5at%); wherein, Al powder is 2N8-200 mesh air atomized aluminum powder, AlY13 / 87wt% alloy powder is 2N8-300 mesh, and AlSi10 alloy powder is 2N8-200 mesh; the parameter conditions for uniform powder mixing are: mixing in a three-dimensional mixer, the speed is 700r / min, the mixing time is 6h, and no stirring ball is added during powder mixing.

[0039] Compression molding: The AlSi alloy bottom layer powder is pressed to obtain an AlSi alloy bottom layer cold pressed blank with a density of 85%; the pressed blank is round according to the required target shape; the pressing pressure is 500 tons, and the holding time is 2s; the diameter of the AlSi alloy cold pressed blank is D120mm and the thickness is 12mm;

[0040] The AlSi alloy bottom cold pressed billet is placed into a graphite mold, and the AlY alloy target layer powder is evenly filled on top (the powder layer thickness is about 47 mm).

[0041] Hot pressing sintering: in 10 -2 The hot pressing sintering treatment was carried out under the vacuum condition of 1.50 MPa, and after slow cooling, the composite target blank was demolded; the parameter conditions of the hot pressing sintering treatment were as follows: after loading the powder, a pressure of 5 MPa was applied, and the temperature was kept at 200 ° C for 2 hours; then the temperature was increased to 550 ° C at a heating rate of 3 ° C / min, and the pressure was linearly increased to the set value of 35 MPa, and the temperature was kept at this temperature for 2 hours; then the temperature was increased to 620 ° C at a heating rate of 1 ° C / min, and the temperature was kept for 1.5 hours; the specific parameters of the slow cooling were as follows: the hot pressing sintering temperature of 620 ° C was cooled down to 400 ° C at a cooling rate of 2 ° C / min, and then the pressure was released and the furnace was cooled to room temperature;

[0042] Post-processing: The composite target blank is machined to obtain a target product that meets the requirements of the drawings and has a good surface quality. Table 1 Composition of the aluminum-yttrium alloy composite target in Examples 1-5

[0043]

[0044]

[0045] Examples 6-10

[0046] Examples 6-10 respectively provide an aluminum-yttrium alloy composite target material and a preparation method thereof.

[0047] The difference between the above embodiment and embodiment 3 is that the hot pressing parameter conditions of the hot pressing sintering process are different, as shown in Table 2.

[0048] Table 2 Hot pressing parameters of hot pressing sintering in Examples 3, 6-10 and Comparative Examples 6-8

[0049]

[0050] The composition and other process parameters of the aluminum-yttrium alloy target in the above embodiment are the same as those in embodiment 3.

[0051] Examples 11-13

[0052] Examples 11-13 respectively provide an aluminum-yttrium alloy composite target material and a preparation method thereof.

[0053] The difference between the above embodiment and embodiment 3 is that the parameter conditions of slow cooling during hot pressing sintering are different, as shown below.

[0054] In Example 11, the specific parameters of cooling are: cooling the hot pressing sintering temperature of 620°C to 400°C at a cooling rate of 5°C / min, then releasing the pressure and cooling to room temperature in the furnace.

[0055] In Example 12, the specific cooling parameters are: cooling the hot pressing sintering temperature of 620°C to 400°C at a cooling rate of 0.5°C / min, then releasing the pressure and cooling to room temperature in the furnace.

[0056] In Example 13, the specific parameters of cooling are: cooling the hot pressing sintering temperature of 620°C to 500°C at a cooling rate of 2°C / min, then releasing the pressure and cooling to room temperature in the furnace.

[0057] The composition and other process parameters of the aluminum-yttrium alloy target in the above embodiment are the same as those in embodiment 3.

[0058] Comparative Example

[0059] Comparative Example 1

[0060] This comparative example provides an aluminum-yttrium alloy composite target material and a preparation method thereof.

[0061] The difference between this comparative example and Example 3 is that: the form of adding AlY powder is different, specifically, the mixed powder is mixed evenly with element powders: Al powder and Y powder are weighed in proportion and mixed evenly to obtain AlY40 / 60wt% alloy matrix powder; at the same time, Al powder and AlSi10 alloy powder are weighed in proportion and mixed evenly to obtain aluminum silicon alloy base powder; wherein, Al powder is 2N8-200 mesh air atomized aluminum powder, Y powder is 2N8-300 mesh, and AlSi10 alloy powder is 2N8-200 mesh; the parameter conditions for uniform powder mixing are: mixing in a three-dimensional mixer, a speed of 700r / min, a mixing time of 6h, and no stirring ball is added to the mixed powder.

[0062] The composition and other process parameters of the aluminum-yttrium alloy target in this comparative example are the same as those in Example 3.

[0063] Comparative Example 2

[0064] This comparative example provides an aluminum-yttrium alloy composite target material and a preparation method thereof.

[0065] The difference between this comparative example and Example 3 is that the AlSi base powder is added in a different form, specifically: Al powder and AlY13 / 87wt% alloy powder are weighed in proportion and mixed evenly to obtain AlY40 / 60wt% alloy matrix powder; at the same time, Al powder and pure Si powder are weighed in proportion and mixed evenly to obtain aluminum silicon alloy base powder (AlSi95 / 5at% alloy base powder); wherein, Al powder is 2N8-200 mesh air atomized aluminum powder, AlY13 / 87wt% alloy powder is 2N8-300 mesh, and Si powder particle size is 3N6-200 mesh; the parameter conditions for uniform powder mixing are: mixing in a three-dimensional mixer, a rotation speed of 700r / min, a mixing time of 6h, and no stirring ball is added to the mixed powder.

[0066] The composition and other process parameters of the aluminum-yttrium alloy target in this comparative example are the same as those in Example 3.

[0067] Comparative Example 3

[0068] This comparative example provides an aluminum-yttrium alloy composite target material and a preparation method thereof.

[0069] The difference between this comparative example and Example 3 is that the compression molding is different, specifically: the AlSi alloy bottom layer powder is compression molded to obtain an AlSi alloy bottom layer cold pressed blank with a density of 75%; the pressed blank is round according to the required target shape; the compression pressure is 500 tons, and the holding time is 2s; the diameter of the AlSi alloy cold pressed blank is D120mm and the thickness is 12mm; the AlSi alloy bottom layer cold pressed blank is loaded into a graphite mold, and the AlY alloy target layer powder is evenly filled on the top (the target layer packing density is about 45%, and the thickness is about 47mm). The composition and other process parameters of the aluminum-yttrium alloy target material of this comparative example are the same as those of Example 3.

[0070] Comparative Example 4

[0071] This comparative example provides an aluminum-yttrium alloy composite target material and a preparation method thereof.

[0072] The difference between this comparative example and Example 3 is that the compression molding is different, specifically: the AlY alloy target layer powder and the AlSi alloy bottom layer powder are respectively compression molded to obtain an AlY alloy matrix cold pressed billet with a density of 85% and an AlSi alloy bottom layer cold pressed billet with a density of 75%; according to the required target material shape, the pressed billet is round; the compression pressure is 500 tons, and the holding time is 2s; the diameter of the AlY target layer cold pressed billet is D120mm and the thickness is 20mm; the diameter of the AlSi cold pressed billet is D120mm and the thickness is 10mm; the AlSi bottom layer cold pressed billet is loaded into a graphite mold, and the target layer cold pressed billet is stacked on top.

[0073] The composition and other process parameters of the aluminum-yttrium alloy target in this comparative example are the same as those in Example 3.

[0074] Comparative Example 5

[0075] This comparative example provides an aluminum-yttrium alloy composite target material and a preparation method thereof.

[0076] The difference between this comparative example and Example 3 is that the sintering process is different, and hot isostatic pressing is used instead of hot pressing sintering. Specifically, the AlSi alloy bottom cold pressed billet is placed in a stainless steel sleeve, and AlY alloy target layer powder (filling density 45%, thickness of about 47mm) is evenly filled on the top, and degassed at 400℃, and the degassing vacuum degree is 2×10 -2 Pa, degassing and holding time is 3h, hot isostatic pressing sintering parameters are 450℃ holding time and 2h, cooling with the furnace, and the ingot is peeled to obtain the aluminum-yttrium alloy composite target.

[0077] The composition and other process parameters of the aluminum-yttrium alloy target in this comparative example are the same as those in Example 3.

[0078] Comparative Examples 6-8

[0079] Comparative Examples 6-8 provide an aluminum-yttrium alloy composite target and a preparation method thereof.

[0080] The difference between Comparative Examples 6-8 and Example 3 is that the parameter conditions of the hot pressing sintering process are different, as shown in Table 2.

[0081] The composition and other process parameters of the aluminum-yttrium alloy target of the comparative example are the same as those of Example 3.

[0082] Comparative Example 9

[0083] This comparative example provides an aluminum-yttrium alloy composite target material and a preparation method thereof.

[0084] The difference between this comparative example and Example 3 is that slow cooling is not adopted when cooling the high temperature section of hot pressing sintering, but directly cooling with the furnace (cooling rate ≥ 10°C / min) to room temperature.

[0085] The composition and other process parameters of the aluminum-yttrium alloy target in this comparative example are the same as those in Example 3.

[0086] Performance testing

[0087] (1) Relative density of AlY alloy target layer: The measured density is measured by the Archimedean drainage method. The relative density is equal to the measured density divided by the theoretical density.

[0088] (2) Non-metallic impurity element content of AlY alloy matrix target: N / O / H content was measured by inert gas melting infrared thermal conductivity method.

[0089] (3) AlY alloy target layer bending strength test method: The bending strength is measured using a UTM5105X universal material testing machine in accordance with the industry standard YB / T 5349-2014 “Methods for testing bending mechanical properties of metallic materials”.

[0090] (4) AlSi alloy bottom layer strength test method: The bottom layer strength is measured using a UTM5105X universal material testing machine in accordance with the national standard GB / T 228.1-2010 "Metallic materials tensile test Part 1: Room temperature test method".

[0091] (5) Thermal conductivity test method of AlSi alloy bottom layer: The thermal conductivity coefficient is measured by LFA-457 laser thermal conductivity meter. The thermal diffusion coefficient of the bottom layer material is tested according to the national standard GB / T22588-2008 "Flash method for measuring thermal diffusion coefficient or thermal conductivity".

[0092] Test results: as shown in Table 3.

[0093] Table 3 Performance test results of AlY targets in Examples 1-13 and Comparative Examples 1-9

[0094]

[0095]

[0096] Combined with the test results in Table 3, Figure 1 This is the metallographic structure diagram of the AlY alloy target layer in Example 3 of the present application; Figure 2 This is a scanning electron microscope image of the AlY alloy target layer in Example 3 of the present application; Figure 3 This is a finished product of the aluminum-yttrium alloy composite target material in Example 3 of the present application. The AlY alloy target layer (Y=40-80wt%) in the aluminum-yttrium alloy composite target material prepared in the present application has a relative density of ≥101.3%, a low impurity content, wherein the N content is ≤115ppm, the O content is ≤1812ppm, and the H content is ≤81ppm, and the bending strength mechanical properties are excellent, and the organization is uniform and has no segregation.

[0097] Comparative Example 1: Al powder and Y powder are mixed evenly to prepare AlY alloy target layer. The impurity elements N, O and H in the AlY alloy target layer are high, and segregation occurs in the target material. Figure 4 : Picture of the finished product of aluminum-yttrium alloy target in Comparative Example 1.

[0098] In Comparative Example 2, Al powder and Si powder were uniformly mixed to prepare an AlSi95 / 5at% alloy bottom layer, and the mechanical properties and thermal conductivity of the bottom layer were poor.

[0099] Comparative Example 3 was set as AlY alloy target layer powder + AlSi alloy bottom layer cold pressed billet with a density of 75%. The results showed that the boundary between the target layer and the bottom layer bonding surface was not straight and had waves.

[0100] In comparative example 4, both the target layer and the bottom layer were molded to obtain cold pressed billets, and AlY alloy target layer cold pressed billets with a density of 85% and AlSi alloy bottom layer cold pressed billets with a density of 75% were obtained. The results showed that the boundary line of the bonding surface between the target layer and the bottom layer was not straight and had waves.

[0101] Comparative Example 5 uses the steps of degassing + hot isostatic pressing instead of hot pressing and sintering to prepare an aluminum-yttrium alloy composite target. The outer circle of the AlY alloy target has cracks, and the impurity contents of N, O, and H are relatively high. This is because Comparative Example 5 is degassed and sealed at a relatively low temperature of 400°C, and no vacuum is performed subsequently. Therefore, the non-metallic impurities desorbed or decomposed above 400°C cannot be fully removed, resulting in a relatively high content of impurities N, O, and H in the target.

[0102] Comparative Example 6 was directly heated to 630° C. at a heating rate of 9° C. / min. During the hot pressing sintering process, the temperature was out of control and reached above 650° C., and a liquid phase appeared.

[0103] In Comparative Example 7, the temperature was directly increased to 550° C. at a heating rate of 15° C. / min. The relative density of the AlY alloy target layer was low and the impurity content was high. The mechanical properties and thermal conductivity of the bottom layer were poor.

[0104] In Comparative Example 8, the temperature was directly increased to 450° C. at a heating rate of 9° C. / min, and then increased to 630° C. at a heating rate of 7° C. / min. During the hot pressing sintering process, the temperature was out of control and rushed to above 650° C., and a liquid phase appeared.

[0105] In Comparative Example 9, slow cooling was not used during the cooling of the high temperature section of hot pressing sintering, and cracks appeared on the outer circle and large surface of the target blank.

[0106] Although the present invention has been described in detail above with general descriptions and specific embodiments, it is obvious to those skilled in the art that some modifications or improvements may be made thereto based on the present invention. Therefore, these modifications or improvements made without departing from the spirit of the present invention all fall within the scope of protection claimed by the present invention.

Claims

1. A method for preparing an aluminum-yttrium alloy composite target, characterized in that: The specific steps include: Mixing powder: Al powder and AlY13 / 87wt% alloy powder are weighed and mixed evenly according to a proportion to obtain an AlY alloy target layer powder composed of Al=20-60wt% and Y=40-80wt%; at the same time, Al powder and AlSi10 alloy powder are weighed and mixed evenly according to a proportion to obtain an AlSi alloy bottom layer powder composed of Al=0-60wt% and AlSi10=40-100wt%; Compression molding: The AlSi alloy bottom layer powder is subjected to compression molding to obtain an AlSi alloy bottom layer cold pressed billet with a density of 80-95%; Mold loading: Load the AlSi alloy bottom cold pressed billet into the mold, and evenly fill the AlY alloy target layer powder on top; Hot pressing sintering: in 10 -1 -10 -3 The composite target blank is obtained by hot pressing and sintering under vacuum conditions of 1000 Pa and slowly cooling and demolding. The parameters of the hot pressing sintering treatment are as follows: after powder loading, a pressure of 3-8 MPa is applied, and the temperature is kept at 150-250°C for 1-4 hours; then the temperature is increased to 480-580°C at a heating rate of 3-10°C / min, and the temperature is kept for 1-3 hours, and the pressure is linearly increased to a set value of 20-50 MPa; then the temperature is increased to 600-650°C at a heating rate of 0.5-3°C / min, and the temperature is kept for 0.5-2 hours; The specific parameters of the slow cooling are: cooling the hot pressing sintering temperature of 600-650°C to 350-450°C at a cooling rate of 0.5-5°C / min, then unloading the pressure and cooling to room temperature with the furnace; Post-processing: machining the composite target blank to obtain a target product.

2. The method for preparing an aluminum-yttrium alloy composite target according to claim 1, characterized in that: The Al powder is -200 mesh air atomized aluminum powder, the AlY13 / 87wt% alloy powder has a particle size of -300 mesh; the AlSi10 alloy powder has a particle size of -150 mesh.

3. The method for preparing an aluminum-yttrium alloy composite target according to claim 1, characterized in that: The parameters of the powder mixing are: mixing with a three-dimensional mixer, a rotation speed of 500-900 r / min, and a mixing time of 3-8 h.

4. The method for preparing an aluminum-yttrium alloy composite target according to claim 1, characterized in that: The AlSi alloy bottom cold-pressed billet has a diameter of D60-D185 mm and a thickness of 10-30 mm.

5. The method for preparing an aluminum-yttrium alloy composite target according to claim 1, characterized in that: The parameters of the compression molding are as follows: the compression pressure is 150-800 tons, and the holding time is 0-10s and is not 0.

6. The method for preparing an aluminum-yttrium alloy composite target according to claim 1, characterized in that: The parameters of the hot pressing sintering treatment are as follows: after powder loading, a pressure of 3-8 MPa is applied, and the temperature is kept at 150-250° C. for 1-4 hours; then the temperature is increased to 500-580° C. at a heating rate of 3-9° C. / min, and the temperature is kept for 1-3 hours, and the pressure is linearly increased to a set value of 20-50 MPa; then the temperature is increased to 600-640° C. at a heating rate of 0.5-2° C. / min, and the temperature is kept for 0.5-2 hours.

7. The method for preparing an aluminum-yttrium alloy composite target according to claim 1, characterized in that: The specific parameters of the slow cooling are: cooling the hot pressing sintering temperature of 600-650°C to 350-400°C at a cooling rate of 0.5-3°C / min, then unloading the pressure and cooling to room temperature along with the furnace.

8. An aluminum-yttrium alloy composite target, characterized in that: The composite target is obtained by using the preparation method of the aluminum-yttrium alloy composite target described in any one of claims 1 to 7.

Citation Information

Patent Citations

  • Composite target material and manufacturing method thereof

    CN113981389A