AlTi target material without combined phase as well as preparation method and application of AlTi target material

Abstract

The invention discloses a combined phase-free AlTi target material as well as a preparation method and application thereof. The preparation method comprises the following steps: carrying out pre-oxidation treatment on Ti powder; the Al powder and the pre-oxidized Ti powder are subjected to ball milling and mixing; carrying out compression molding on the obtained mixed powder to obtain a biscuit; and the biscuit is subjected to hot isostatic pressing, and the non-combined-phase AlTi target material is obtained. According to the target material prepared through the method, high density and high purity are kept, meanwhile, generation of an AlxTiy compound phase can be avoided, the coating performance of the target material is improved, and the stability of the target material in industrial application is improved. The hard alloy coating prepared from the target material is uniform in component, high in hardness and good in film-substrate binding force.

Description

Technical Field

[0001] The present invention relates to the technical field of powder metallurgy, and in particular to an AlTi target material without a chemical combination phase, a preparation method thereof, and an application thereof. Background Art

[0002] Carbide cutting tools, due to their high hardness, high wear resistance, and excellent cutting performance, are widely used in aerospace, automotive manufacturing, mold manufacturing, and other fields. However, under the extreme mechanical and thermal conditions caused by high-speed cutting, excessive wear affects the tool life and processing quality of carbide tools. Due to its high hardness, wear resistance, and excellent high-temperature oxidation resistance, AlTiN hard coatings can significantly extend the cutting life of carbide tools and have attracted the attention of tool researchers. AlTi targets are the key raw material for depositing AlTiN coatings. Therefore, the high performance of AlTiN coatings is limited by the microstructure and properties of the target material.

[0003] Traditional AlTi target preparation methods mainly include smelting method and powder metallurgy method. The smelting method is to melt aluminum and titanium in a certain proportion and then cast them into targets. Due to the high smelting temperature, AlTi is easily formed. x Ti compound phase. Powder metallurgy involves mixing aluminum powder and titanium powder in a specific ratio and then preparing an aluminum-titanium target using methods such as hot pressing or hot isostatic pressing. The above aluminum-titanium target preparation techniques inevitably form intermetallic compounds such as TiAl3, TiAl, and Ti3Al. Due to their high melting points, the ionization rate of intermetallic compounds during the PVD coating process is lower than that of metallic Al and Ti, seriously affecting the composition of the coating or film, and thus the coating's performance. Furthermore, the electrical conductivity of the intermetallic compounds differs from that of the metallic phase in the target, leading to localized abnormal discharges. This not only shortens the target's service life but also creates numerous defects in the coating or film, thereby reducing its overall performance. Therefore, AlTi targets free of intermetallic phases are crucial for the preparation of high-quality AlTiN hard coatings.

[0004] Because the smelting method requires a temperature above the metal's melting point, molten metals are prone to forming intermetallic compounds. Therefore, powder metallurgy is a reliable method for producing intermetallic phase-free aluminum-titanium targets. Adjusting powder metallurgy process parameters (lowering the sintering temperature) or adding antioxidant additives can produce aluminum-titanium targets with few or no intermetallic phases. However, lowering the sintering temperature may result in insufficient target density, affecting the target's coating behavior and the overall performance of the coating / thin film. Adding antioxidant additives may also affect the target's purity, ultimately affecting the overall performance of the coating / thin film. Summary of the Invention

[0005] To address the shortcomings of the prior art, the first objective of the present invention is to provide a method for preparing an AlTi target material free of intermetallic phases. This method is simple and controllable, avoiding the formation of intermetallic phases without lowering the sintering temperature or adding antioxidant additives. This method results in a target material with high purity and density, reduces uncertainty during the deposition process, and thus improves the performance and application reliability of coatings / thin films.

[0006] The second object of the present invention is to provide a non-compound phase AlTi target prepared by the above preparation method. The non-compound phase AlTi target provided by the present invention has high density and good strength. The coating prepared by using it as a raw material for cemented carbide tool coating has high hardness and good wear resistance.

[0007] The third object of the present invention is to provide an application of the AlTi target material without a chemical combination phase prepared by the above preparation method.

[0008] In order to achieve the above object, the present invention adopts the following technical solutions:

[0009] The present invention discloses a method for preparing a non-compound phase AlTi target material, comprising the steps of: subjecting Ti powder to oxidation treatment to obtain TiO2@Ti powder; mixing the TiO2@Ti powder with Al powder to obtain a mixed powder; molding the mixed powder to obtain a green embryo; and hot isostatically pressing the green embryo to obtain the non-compound phase AlTi target material.

[0010] The preparation method of the present invention first forms an oxide film on the surface of the Ti powder by oxidizing the Ti powder. The oxide film can effectively block the Al powder and the Ti powder, avoiding the generation of AlTi compounds during the hot isostatic pressing sintering process. In the AlTi target material formed by sintering, a small amount of TiO2 particles has a dispersion strengthening effect on the aluminum-titanium target material, thereby making the AlTi target material of the present invention have the performance characteristics of high density and high strength.

[0011] In a preferred embodiment, the Ti powder has a purity of ≥99.5% and a particle size range of 55 to 200 μm, preferably 100 to 200 μm. Using Ti powder within this range ensures a moderate oxide layer thickness and optimal performance. Ti powder with excessively large particle sizes can affect the composition ratio of the target after coating and also affect the target's compositional uniformity. Ti powder with excessively small particle sizes can make it difficult to control the oxide film thickness, resulting in excessive oxidation and, in turn, affecting the performance of the target and coating / film.

[0012] In a preferred embodiment, the Al powder has a purity of ≥99.9% and a particle size range of 2 to 200 μm, preferably 2 to 100 μm. Excessive Al powder can impair the uniformity of the mixed powder, affecting the compositional uniformity of the target material and, in turn, the performance of the coating. Excessively small Al powders tend to agglomerate, hindering gas discharge during sintering and limiting target densification.

[0013] In the present invention, there is no restriction on the shapes of Ti powder and Al powder. Both low-cost non-spherical powder and spherical powder can be sintered densely. Therefore, based on cost considerations, the shapes of Ti powder and Al powder are preferably non-spherical.

[0014] In a preferred embodiment, in the mixed powder, the atomic ratio of Al to Ti is 4-7:3-6.

[0015] In a preferred embodiment, the temperature of the oxidation treatment is 400-650° C., preferably 400-600° C., and the holding time is 0.5-3 h, preferably 2-3 h.

[0016] In the present invention, the temperature of the oxidation treatment needs to be effectively controlled. If the oxidation temperature is too low, the TiO2 layer on the surface of the Ti powder will be relatively thin and uneven, and will not be able to effectively block the Al powder and Ti powder. AlTi compounds will still be generated during the hot isostatic pressing process, which will ultimately affect the quality of the target material. If the oxidation temperature is too high, the TiO2 layer formed on the surface of the titanium powder will be too thick, and excessive oxygen content will be introduced, resulting in loose structure and decreased density of the target material after sintering, and a large amount of TiO2 will enter the hard coating, increasing the defects of the coating and reducing the overall performance of the coating.

[0017] In a preferred embodiment, the mixing method is dry ball milling, the rotation speed of the dry ball milling is 100-500 r / min, preferably 400-500 r / min, and the time of the dry ball milling is 5-24 h, preferably 16-24 h.

[0018] Further preferably, the grinding balls for dry ball milling are zirconia balls, and during dry ball milling, the mass ratio of the mixed powder to the grinding balls is 1:1-10.

[0019] TiO2@Ti powder and Al powder are fully mixed and evenly mixed by dry ball milling, and hot isostatic pressing is combined to ensure the high density and excellent mechanical properties of the target material.

[0020] Preferably, the compression molding method is to place the mixed powder in a stainless steel mold for hydraulic molding, the compression molding pressure is 10-40 MPa, and the holding time is 30-600 s.

[0021] In practice, the mixed powder is weighed, bagged, placed in a stainless steel mold, and compression-molded to produce a green blank. Compression molding before hot isostatic pressing (HIP) improves powder utilization and avoids the significant deformation and low yield associated with direct HIP sintering of the mixed powder. Furthermore, multiple layers can be stacked to adjust the target thickness.

[0022] In a preferred embodiment, the hot isostatic pressing sintering is performed at a temperature of 450-600° C., a pressure of 100-200 MPa, and a heat and pressure holding time of 2-10 hours.

[0023] In the actual operation process, the obtained blanks are stacked in multiple layers and loaded into a metal sheath. After welding, sealing and degassing, they are placed in a hot isostatic pressing equipment and sintered according to the set process. After cooling, they are demolded to obtain the AlTi target material. Finally, the AlTi target material is mechanically processed to remove the sheath, and the finished aluminum-titanium alloy target material is obtained according to the drawing.

[0024] The present invention also provides an AlTi target material free of chemical combination phase prepared by the above preparation method.

[0025] In a preferred embodiment, in the AlTi target material without a combined phase, the atomic percentage of Al is 40 to 70%, and the atomic percentage of Ti is 30 to 60%.

[0026] In a preferred embodiment, the AlTi target material without a compound phase does not contain an aluminum-titanium compound phase, and the relative density of the AlTi target material is ≥98%.

[0027] The present invention also provides an application of a combined phase-free AlTi target prepared by the above-described preparation method, wherein the combined phase-free AlTi target is used as a target source to deposit a hard nitride coating via cathodic arc evaporation. In the present invention, using the combined phase-free AlTi target as a target source via cathodic arc evaporation can produce a hard nitride coating with uniform composition, high hardness, and good film-substrate bonding.

[0028] The target material prepared by the preparation method of the present invention can avoid the formation of AlTi compound phase while maintaining high density and high purity, thereby improving the sputtering performance of the target material and its reliability in practical applications. The cemented carbide coating prepared using the target material has uniform composition, high hardness and excellent cutting performance.

[0029] Beneficial effects

[0030] (1) By precisely controlling the oxidation treatment temperature, oxidation time, and powder particle size of the Ti powder, a dense, ultra-thin oxide film can be formed on the surface of the titanium powder particles, effectively inhibiting the formation of compound phases. This eliminates the need to lower the sintering temperature to avoid the formation of intermetallic compounds, ensuring the sintering temperature and increasing the density of the target. Furthermore, the oxygen content and purity of the target are guaranteed without the need to introduce antioxidant additives.

[0031] (2) The process of combining dry hydraulic forming and hot isostatic pressing sintering is adopted to reduce the shrinkage deformation of the target blank, avoid the occurrence of anisotropic deformation, ensure the high density and excellent mechanical properties of the target material, and improve the target material yield rate.

[0032] (3) The suppression of the intermetallic phase improves the coating behavior of the target material, avoids abnormal discharge, significantly increases the service life of the target material, and can also greatly improve the overall performance of the coating / thin film.

[0033] The technical solution of the present invention is further described in detail below through the accompanying drawings and embodiments. BRIEF DESCRIPTION OF THE DRAWINGS

[0034] Figure 1 This is a process flow chart of a method for preparing an aluminum-titanium target material without a compound phase and an application example of the present invention;

[0035] Figure 2 This is a finished image of the aluminum-titanium target material without AlTi compound phase prepared in Example 1 of the present invention;

[0036] Figure 3 This is a backscattered photograph of the fracture of the aluminum-titanium target prepared in Example 1 of the present invention;

[0037] Figure 4 This is a backscattered photograph of the fracture of the aluminum-titanium target prepared in Example 2 of the present invention;

[0038] Figure 5 This is a backscattered photograph of the fracture of the aluminum-titanium target prepared in Example 3 of the present invention;

[0039] Figure 6 These are the XRD patterns of the aluminum-titanium target prepared in Example 1 of the present invention and the XRD patterns of the coating prepared from the target: (a) XRD pattern of the aluminum-titanium target; (b) XRD pattern of the coating prepared from the aluminum-titanium target. DETAILED DESCRIPTION

[0040] The present invention will be described in further detail below with reference to the embodiments and drawings, but the embodiments of the present invention are not limited thereto.

[0041] Example 1

[0042] The AlTi target prepared in this embodiment consists of 70 at.% Al+30 at.% Ti.

[0043] (1) Weigh the corresponding Al powder and Ti powder according to the ratio, wherein the purity of Al powder is 99.9%, the particle size range is 2 μm~100 μm, and the purity of Ti powder is above 99.5%, the particle size range is 100 μm~200 μm, and both powders are non-spherical powders;

[0044] (2) The Ti powder was oxidized at a temperature of 500 °C and kept at this temperature for 3 h to obtain TiO2@Ti powder.

[0045] (3) Dry milling the Al powder and TiO2@Ti powder in a ball mill for 20 h to obtain a mixed powder. The dry milling process employed a powder-to-ball ratio of 1:1.5, with zirconia balls as the grinding balls and a high-speed milling speed of 500 r / min.

[0046] (4) The mixed powder obtained by ball milling in step (3) is placed in a stainless steel mold, vibrated evenly, and molded at a molding pressure of 20 MPa. The pressure is maintained for 60 seconds to obtain an AlTi blank.

[0047] (5) The green blanks obtained in step (4) are stacked in multiple layers and placed in a metal sheath. After welding, sealing, and degassing, hot isostatic pressing and sintering are performed. After cooling, the AlTi target is demolded. The hot isostatic pressing temperature is 600°C and the pressure is 150 MPa. The temperature and pressure are then maintained for 5 hours. After cooling, the AlTi target is demolded.

[0048] (6) The AlTi target material obtained in step (5) is mechanically processed to remove the sheath, and processed according to the drawing to obtain a finished AlTi target material without a chemical phase.

[0049] Example 2

[0050] The AlTi target prepared in this embodiment consists of 60 at.% Al+40 at.% Ti.

[0051] (1) Weigh the corresponding Al powder and Ti powder according to the ratio, wherein the purity of Al powder is 99.9%, the particle size range is 2 μm~100 μm, and the purity of Ti powder is above 99.5%, the particle size range is 100 μm~200 μm, and both powders are non-spherical powders;

[0052] (2) The Ti powder was oxidized at a temperature of 500 °C and kept at this temperature for 3 h to obtain TiO2@Ti powder.

[0053] (3) Dry milling the Al powder and TiO2@Ti powder in a ball mill for 20 h to obtain a mixed powder. The dry milling process employed a powder-to-ball ratio of 1:1.5, with zirconia balls as the grinding balls and a high-speed milling speed of 500 r / min.

[0054] (4) The mixed powder obtained by ball milling in step (3) is placed in a stainless steel mold, vibrated evenly, and molded at a molding pressure of 20 MPa. The pressure is maintained for 60 seconds to obtain an AlTi blank.

[0055] (5) The green blanks obtained in step (4) are stacked in multiple layers and placed in a metal sheath. After welding, sealing, and degassing, hot isostatic pressing and sintering are performed. After cooling, the AlTi target is demolded. The hot isostatic pressing temperature is 600°C and the pressure is 150 MPa. The temperature and pressure are then maintained for 5 hours. After cooling, the AlTi target is demolded.

[0056] (6) The AlTi target material obtained in step (5) is mechanically processed to remove the sheath, and processed according to the drawing to obtain a finished AlTi target material without a chemical phase.

[0057] Example 3

[0058] The AlTi target prepared in this embodiment consists of 40 at.% Al+60 at.% Ti.

[0059] (1) Weigh the corresponding Al powder and Ti powder according to the ratio, wherein the purity of Al powder is 99.9%, the particle size range is 2 μm~100 μm, and the purity of Ti powder is above 99.5%, the particle size range is 100 μm~200 μm, and both powders are non-spherical powders;

[0060] (2) The Ti powder was oxidized at a temperature of 500 °C and kept at this temperature for 3 h to obtain TiO2@Ti powder.

[0061] (3) Dry milling the Al powder and TiO2@Ti powder in a ball mill for 20 h to obtain a mixed powder. The dry milling process employed a powder-to-ball ratio of 1:1.5, with zirconia balls as the grinding balls and a high-speed milling speed of 500 r / min.

[0062] (4) The mixed powder obtained by ball milling in step (3) is placed in a stainless steel mold, vibrated evenly, and molded at a molding pressure of 20 MPa. The pressure is maintained for 60 seconds to obtain an AlTi blank.

[0063] (5) The green blanks obtained in step (4) are stacked in multiple layers and placed in a metal sheath. After welding, sealing, and degassing, hot isostatic pressing and sintering are performed. After cooling, the AlTi target is demolded. The hot isostatic pressing temperature is 600°C and the pressure is 150 MPa. The temperature and pressure are then maintained for 5 hours. After cooling, the AlTi target is demolded.

[0064] (6) The AlTi target material obtained in step (5) is mechanically processed to remove the sheath, and processed according to the drawing to obtain a finished AlTi target material without a chemical phase.

[0065] Comparative Example 1

[0066] The AlTi target prepared in this comparative example consists of 70 at.% Al + 30 at.% Ti, wherein the Ti powder is not subjected to oxidation treatment.

[0067] (1) Weigh the corresponding Al powder and Ti powder according to the ratio, wherein the purity of Al powder is 99.9%, the particle size range is 2 μm~100 μm, and the purity of Ti powder is above 99.5%, the particle size range is 100 μm~200 μm, and both powders are non-spherical powders;

[0068] (2) Dry milling the Al and Ti powders in a ball mill for 20 h to obtain a mixed powder. The dry milling process employed a powder-to-ball ratio of 1:1.5, using zirconia balls as the grinding balls, and a high-speed milling speed of 500 r / min.

[0069] (3) The mixed powder obtained by ball milling in step (2) was loaded into a stainless steel mold, vibrated evenly, and compression molded at a pressing pressure of 20 MPa for 60 seconds to obtain an AlTi blank;

[0070] (4) The blank obtained in step (3) is placed in a metal sheath, welded and sealed, degassed, and then hot isostatically pressed and sintered. After cooling, the blank is demolded to obtain an AlTi target. The hot isostatic pressing temperature is 600°C and the pressure is 150 MPa, and then the temperature and pressure are maintained for 5 hours. After cooling, the blank is demolded to obtain an AlTi target.

[0071] (5) The AlTi target material obtained in step (4) is mechanically processed to remove the sheath, and the AlTi target material is processed according to the drawing to obtain a finished product.

[0072] Comparative Example 2

[0073] The AlTi target prepared in this comparative example consists of 70 at.% Al + 30 at.% Ti, wherein the Ti powder is oxidized at 200°C.

[0074] (1) Weigh the corresponding Al powder and Ti powder according to the ratio, wherein the purity of Al powder is 99.9%, the particle size range is 2 μm~100 μm, and the purity of Ti powder is above 99.5%, the particle size range is 100 μm~200 μm, and both powders are non-spherical powders;

[0075] (2) The Ti powder was oxidized at 200°C for 3 h to obtain TiO2@Ti powder.

[0076] (3) Dry milling the Al powder and TiO2@Ti powder in a ball mill for 20 h to obtain a mixed powder. The dry milling process employed a powder-to-ball ratio of 1:1.5, with zirconia balls as the grinding balls and a high-speed milling speed of 500 r / min.

[0077] (4) The mixed powder obtained by ball milling in step (3) was loaded into a stainless steel mold, vibrated evenly, and compression molded at a pressing pressure of 20 MPa for 60 seconds to obtain an AlTi blank;

[0078] (5) The green blanks obtained in step (4) are stacked in multiple layers and placed in a metal sheath, welded, sealed, degassed, and then hot isostatically pressed and sintered. After cooling, the blanks are demolded to obtain an AlTi target. The hot isostatic pressing temperature is 600°C and the pressure is 150 MPa, and then the temperature and pressure are maintained for 5 hours. After cooling, the blanks are demolded to obtain an AlTi target.

[0079] (6) The AlTi target obtained in step (5) is mechanically processed to remove the sheath, and the AlTi target finished product is obtained according to the drawing.

[0080] Comparative Example 3

[0081] The AlTi target prepared in this comparative example consists of 70 at.% Al + 30 at.% Ti, wherein the Ti powder is oxidized at 700°C.

[0082] (1) Weigh the corresponding Al powder and Ti powder according to the ratio, wherein the purity of Al powder is 99.9%, the particle size range is 2 μm~100 μm, and the purity of Ti powder is above 99.5%, the particle size range is 100 μm~200 μm, and both powders are non-spherical powders;

[0083] (2) The Ti powder was oxidized at 700 °C for 3 h to obtain TiO2@Ti powder.

[0084] (3) Dry milling the Al powder and TiO2@Ti powder in a ball mill for 20 h to obtain a mixed powder. The dry milling process employed a powder-to-ball ratio of 1:1.5, with zirconia balls as the grinding balls and a high-speed milling speed of 500 r / min.

[0085] (4) The mixed powder obtained by ball milling in step (3) was loaded into a stainless steel mold, vibrated evenly, and compression molded at a pressing pressure of 20 MPa for 60 seconds to obtain an AlTi blank;

[0086] (5) The green blanks obtained in step (4) are stacked in multiple layers and placed in a metal sheath, welded, sealed, degassed, and then hot isostatically pressed and sintered. After cooling, the blanks are demolded to obtain an AlTi target. The hot isostatic pressing temperature is 600°C and the pressure is 150 MPa, and then the temperature and pressure are maintained for 5 hours. After cooling, the blanks are demolded to obtain an AlTi target.

[0087] (6) The AlTi target material obtained in step (5) is mechanically processed to remove the sheath, and the AlTi target material is processed according to the drawing to obtain a finished product.

[0088] Comparative Example 4

[0089] The AlTi target prepared in this embodiment consists of 70 at.% Al+30 at.% Ti.

[0090] (1) Weigh the corresponding Al powder and Ti powder according to the proportion, wherein the purity of Al powder is 99.9%, the particle size range is 2μm~100μm, and the purity of Ti powder is above 99.5%, the particle size range is 250μm~300μm, and both powders are non-spherical powders;

[0091] (2) The Ti powder was oxidized at 500°C for 3 h to obtain TiO2@Ti powder.

[0092] (3) Dry milling the Al powder and TiO2@Ti powder in a ball mill for 20 h to obtain a mixed powder. The dry milling process employed a powder-to-ball ratio of 1:1.5, with zirconia balls as the grinding balls and a high-speed milling speed of 500 r / min.

[0093] (4) The mixed powder obtained by ball milling in step (3) was loaded into a stainless steel mold, vibrated evenly, and compression molded at a pressing pressure of 20 MPa for 60 seconds to obtain an AlTi blank;

[0094] (5) The green blanks obtained in step (4) are stacked in multiple layers and placed in a metal sheath, welded, sealed, degassed, and then hot isostatically pressed and sintered. After cooling, the blanks are demolded to obtain an AlTi target. The hot isostatic pressing temperature is 600°C and the pressure is 150 MPa, and then the temperature and pressure are maintained for 5 hours. After cooling, the blanks are demolded to obtain an AlTi target.

[0095] (6) The AlTi target material obtained in step (5) is mechanically processed to remove the sheath, and the AlTi target material is processed according to the drawing to obtain a finished product.

[0096] Comparative Example 5

[0097] The AlTi target prepared in this embodiment consists of 70 at.% Al+30 at.% Ti.

[0098] (1) Weighing the corresponding Al powder and Ti powder according to the proportion, wherein the purity of Al powder is 99.9%, the particle size range is 2 μm~100 μm, the purity of Ti powder is above 99.5%, the particle size range is less than 50 μm, and both powders are non-spherical powders;

[0099] (2) The Ti powder was oxidized at 500°C for 3 h to obtain TiO2@Ti powder.

[0100] (3) Dry milling the Al powder and TiO2@Ti powder in a ball mill for 20 h to obtain a mixed powder. The dry milling process employed a powder-to-ball ratio of 1:1.5, with zirconia balls as the grinding balls and a high-speed milling speed of 500 r / min.

[0101] (4) The mixed powder obtained by ball milling in step (3) was loaded into a stainless steel mold, vibrated evenly, and compression molded at a pressing pressure of 20 MPa for 60 seconds to obtain an AlTi blank;

[0102] (5) The green blanks obtained in step (4) are stacked in multiple layers and placed in a metal sheath, welded, sealed, degassed, and then hot isostatically pressed and sintered. After cooling, the blanks are demolded to obtain an AlTi target. The hot isostatic pressing temperature is 600°C and the pressure is 150 MPa, and then the temperature and pressure are maintained for 5 hours. After cooling, the blanks are demolded to obtain an AlTi target.

[0103] (6) The AlTi target material obtained in step (5) is mechanically processed to remove the sheath, and the AlTi target material is processed according to the drawing to obtain a finished product.

[0104] Result analysis:

[0105] 1. It can be concluded from Examples 1-3 that by properly adjusting the ratio of aluminum to titanium, the AlTi targets prepared by the above method have the same phase composition and no Al x Ti y The AlTiN coatings sputtered using Examples 1-3 achieved hardnesses of 37.7 GPa, 39 GPa, and 38.5 GPa, respectively, demonstrating high hardness. Furthermore, the appropriate oxidation temperature and Ti powder particle size range effectively inhibited the formation of combined phases, maintaining high sintering density and target strength, making them suitable for sputtering applications.

[0106] 2. It can be seen from Example 1 and Comparative Example 1 that unoxidized Ti powder will lead to the presence of Al x Ti y The compound phase causes the target material to become more brittle and the density to decrease, which in turn affects the wear resistance and adhesion of the sputtering coating.

[0107] 3. As can be seen from Example 1 and Comparative Examples 2 and 3, if the oxidation temperature is too low, the TiO2 layer on the surface of the Ti powder is relatively thin and uneven, which cannot effectively block the Al powder and Ti powder. AlTi compounds are generated during the hot isostatic pressing process, ultimately affecting the quality of the target. If the oxidation temperature is too high, the TiO2 layer formed on the surface is too thick, which reduces the activity of Ti and deteriorates the diffusion ability between powders during sintering, resulting in a loose structure and reduced bonding strength of the sintered target. If the oxidation temperature is too high, a large amount of TiO2 is generated during the sintering process, resulting in a large amount of oxygen-rich phase in the target. The coating may contain trace oxide inclusions, which affect the bonding strength and wear resistance of the coating and make the coating more likely to peel under conditions such as high-speed cutting.

[0108] 4. As can be seen from Example 1 and Comparative Examples 4 and 5, oversized Ti particles are difficult to distribute evenly during the ball milling process, and the degree of mixing with Al powder is low, which makes it difficult for Ti particles to effectively combine during the sintering process, resulting in an increase in pores inside the target material; oversized Ti particles will lead to incomplete oxidation, uneven internal structure during sintering, and reduced relative density, affecting the performance of the target material and, in turn, the performance of the prepared coating. If the Ti powder particle size is too fine, it will lead to excessive oxidation of the Ti powder, resulting in a thicker TiO2 layer formed on its surface, which is easy to form an oxygen-rich phase during the sintering process, causing microcracks inside the target material and reducing mechanical properties; if the Ti powder is too small, it will easily agglomerate during the ball milling process, resulting in uneven mixing of Ti and Al, uneven distribution of the microstructure inside the target material, and affecting the performance stability of the target material.

[0109] By comparison, it can be seen that the present invention can effectively inhibit the formation of compounds by pre-oxidizing Ti powder and optimizing the oxidation temperature and particle size of Ti powder, thereby ensuring that the AlTi target has higher density and excellent performance.

[0110]

[0111] Finally, it should be noted that the above embodiments are preferred implementations of the present invention, but the implementations of the present invention are not limited to the above embodiments. Any changes or replacements made by those skilled in the art within the technical scope disclosed in the present invention should be covered within the scope of protection of the present invention.

Claims

1. A method for preparing a non-combination phase AlTi target, characterized by: Ti powder is oxidized to obtain TiO2@Ti powder, TiO2@Ti powder is mixed with Al powder to obtain mixed powder, the mixed powder is molded to obtain a green embryo, and the green embryo is hot isostatically pressed to obtain a chemical phase-free AlTi target.

2. The method for preparing a non-combination phase AlTi target according to claim 1, characterized in that: The purity of the Ti powder is ≥99.5%, and the particle size range is 55-200 μm; The purity of the Al powder is ≥99.5%, and the particle size range is 2 to 200 μm.

3. The method for preparing a composite phase-free AlTi target according to claim 1 or 2, characterized in that: In the mixed powder, the atomic ratio of Al to Ti is 4-7:3-6.

4. The method for preparing a composite phase-free AlTi target according to claim 1 or 2, wherein: The temperature of the oxidation treatment is 400-650° C., and the holding time is 0.5-3 hours.

5. The method for preparing a composite phase-free AlTi target according to claim 1 or 2, characterized in that: The mixing method is dry ball milling, the rotation speed of the dry ball milling is 100-500 r / min, and the dry ball milling time is 5-24 hours.

6. The method for preparing a non-combination phase AlTi target according to claim 5, characterized in that: The grinding balls for the dry ball milling are zirconia balls. During the dry ball milling, the mass ratio of the mixed powder to the grinding balls is 1:1-10.

7. The method for preparing a composite phase-free AlTi target according to claim 1 or 2, characterized in that: The compression molding method is to place the mixed powder in a stainless steel mold for hydraulic molding. The compression molding pressure is 10-40 MPa, and the holding time is 30-600 seconds.

8. The method for preparing a composite phase-free AlTi target according to claim 1 or 2, characterized in that: The hot isostatic pressing sintering temperature is 450-600° C., the pressure is 100-200 MPa, and the heat and pressure holding time is 2-10 hours.

9. An AlTi target material free of combined phases prepared by the preparation method according to any one of claims 1 to 8, characterized in that: In the AlTi target material without a combined phase, the atomic percentage of Al is 40 to 70%, and the atomic percentage of Ti is 30 to 60%; The AlTi target material without a combined phase does not contain an aluminum-titanium combined phase, and the relative density of the AlTi target material without a combined phase is ≥98%.

10. Use of a composite phase-free AlTi target prepared by the preparation method according to any one of claims 1 to 8, characterized in that: The AlTi target material without a combined phase is used as a target source to deposit a hard nitride coating through cathode arc evaporation.

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