A fine-grained titanium-silicon sputtering target and its preparation method

Abstract

This invention provides a fine-grained titanium-silicon target and its preparation method. The method uses pure Ti powder and Ti5Si3 alloy powder as raw materials. The raw material powders are pre-treated by ball milling and then encapsulated for vacuum hot degassing. The degassed encapsulated material is then subjected to hot isostatic pressing densification. Finally, heat treatment is used to stabilize the microstructure and reduce internal stress. The titanium-silicon target prepared by this invention has the following advantages: (1) The titanium-silicon target contains only two phases, Ti phase and Ti5Si3 phase, without other phases such as TiSi and TiSi2; (2) The microstructure of the titanium-silicon target is fine and uniform, with an average grain size <50μm; (3) The titanium-silicon target has high density, with a relative density >99%; (4) The Ti phase and Ti5Si3 phase are uniformly distributed without segregation; (5) The silicon content is high, reaching up to 35 at%.

Description

Technical Field

[0001] This application relates to the technical field of metal and alloy target preparation, and in particular to a fine-grained titanium-silicon target and its preparation method. Background Technology

[0002] TiN coatings possess excellent wear and corrosion resistance, making them one of the most widely used tool coatings. However, TiN coatings exhibit low hardness and poor resistance to high-temperature oxidation. Incorporating Si into TiN coatings to form an amorphous Si3N4-encapsulated nanocrystalline TiN TiN nanocomposite structure coating can significantly improve the performance of TiN coatings.

[0003] Titanium-silicon sputtering targets, as a key consumable material, are crucial for the preparation of high-performance TiSiN hard coatings. Currently, the main methods for preparing titanium-silicon sputtering targets include melting and casting, hot pressing and sintering, and hot isostatic pressing. Titanium-silicon sputtering targets prepared by melting and casting suffer from problems such as component segregation, coarse grains, and susceptibility to cracking, significantly limiting their practical applications. Titanium-silicon sputtering targets prepared by hot pressing and sintering suffer from low density, uneven density distribution, small size, and difficulty in large-scale production. Hot isostatic pressing is the optimal method for large-scale production of titanium-silicon sputtering targets with uniform microstructure, uniform density, and large size. Currently, most silicon in titanium-silicon sputtering targets comes from raw silicon powder. This results in residual pure silicon phase and low alloying degree, leading to large and numerous particles on the film, affecting the film composition and roughness, and ultimately degrading film performance.

[0004] Existing titanium-silicon sputtering targets are made from Ti+TiSi2 alloy powder, obtained through hot isostatic pressing at 800–1100℃. These targets contain four phases: Ti, TiSi, Ti5Si3, and TiSi2. However, when using these targets for film deposition, the differences in melting point, work function, and other properties among these four phases lead to compositional deviations and numerous large-particle defects in the film, negatively impacting film performance. Summary of the Invention

[0005] This application provides a fine-grained titanium-silicon target and its preparation method. The titanium-silicon target prepared by this invention has the following advantages: (1) The titanium-silicon target contains only two phases, Ti phase and Ti5Si3 phase, and no other phases such as TiSi and TiSi2; (2) The microstructure of the titanium-silicon target is fine and uniform, with an average grain size of <50μm; (3) The titanium-silicon target has a high density, with a relative density >99%; (4) The Ti phase and Ti5Si3 phase are uniformly distributed without segregation; (5) The silicon content is high, with the highest silicon content reaching 35 at%.

[0006] In a first aspect, a fine-grained titanium-silicon target material is provided, wherein the titanium-silicon target material is a two-phase material composed of Ti phase and Ti5Si3 phase.

[0007] In conjunction with the first aspect, in some implementations of the first aspect, the proportion of Ti element in the titanium-silicon target is 65-95%, and the proportion of Si element is 5-35%.

[0008] In conjunction with the first aspect, in some implementations of the first aspect, the raw materials of the titanium-silicon target are pure Ti powder and Ti5Si3 alloy powder, which are prepared by hot isostatic pressing, wherein the hot isostatic pressing temperature is 700-799℃.

[0009] In conjunction with the first aspect, in some implementations of the first aspect, the average grain size of the titanium-silicon target is <50 μm.

[0010] Secondly, a method for preparing a fine-grained titanium-silicon target is provided, comprising:

[0011] The raw material powders were pretreated by ball milling and mixing. The raw material powders included pure Ti powder and Ti5Si3 alloy powder.

[0012] The pre-treated powder after ball milling is packed into a sleeve, and then sealed after vacuum thermal degassing.

[0013] Perform hot isostatic pressing densification treatment;

[0014] The target material after hot isostatic pressing densification is then subjected to heat treatment.

[0015] In conjunction with the second aspect, in some implementations of the second aspect, the proportion of Ti element in the raw material powder is 65-95%, and the proportion of Si element is 5-35%.

[0016] In conjunction with the second aspect, in some implementations of the second aspect, the hot isostatic pressing densification treatment satisfies the following conditions: temperature 700–799℃, pressure 140–150MPa, and holding time 4–5h.

[0017] In conjunction with the second aspect, in some implementations of the second aspect, the heat treatment satisfies the following conditions: temperature 500–600°C, holding time 60–90 min, and furnace cooling.

[0018] In conjunction with the second aspect, in certain implementations of the second aspect, the raw material powder satisfies at least one of the following:

[0019] The purity of the Ti powder is 99.9%, the laser particle size is D10 = 5-10μm, D50 = 25-35μm, D90 = 40-60μm, the tap density is 2.6-2.8g / cm3, and the oxygen content is <2000ppm;

[0020] The purity of Ti5Si3 alloy powder is 99.8%, the laser particle size is D10 = 3-8μm, D50 = 20-30μm, D90 = 35-55μm, the tap density is 2.3-2.5g / cm3, and the oxygen content is <2000ppm.

[0021] In conjunction with the second aspect, in certain implementations of the second aspect, the method satisfies at least one of the following:

[0022] The ball milling pretreatment meets the requirements of a ball milling time of 5-12 hours and a ball-to-material weight ratio of (0.5-5):1.

[0023] The relative density of the powder reaches over 60%;

[0024] The vacuum thermal degassing process is performed at room temperature under a vacuum of less than 2*10. -3 The temperature is raised to 650–750°C, and the vacuum is below 1*10⁻⁶. -3 Pa and keep warm for 180–300 minutes.

[0025] Thirdly, a fine-grained titanium-silicon sputtering target is provided, which is prepared by the method described in any of the implementations of the second aspect above.

[0026] Compared with the prior art, the solution provided in this application has at least the following beneficial technical effects:

[0027] (1) The titanium-silicon target material prepared by this invention contains only two phases, Ti phase and Ti5Si3 phase, and no other phases such as TiSi and TiSi2. This satisfies the requirements for hard coatings in continuous cutting, dry cutting or cutting of difficult-to-machine materials.

[0028] (2) By controlling the particle size and tap density of the raw material powder, the titanium-silicon mixed powder can achieve a high powder density while ensuring the uniformity of mixing. In this invention, the relative powder density of the titanium-silicon mixed powder can reach more than 60%. Thus, the titanium-silicon mixed powder can reduce the shrinkage deformation during hot isostatic pressing without the need for cumbersome cold isostatic pressing, improve the regularity of the encapsulation after hot isostatic pressing, reduce processing allowance, and improve powder utilization.

[0029] (3) The hot isostatic pressing densification temperature of the titanium-silicon mixed powder in this invention is relatively low, which can achieve fine grains with an average grain size of <50μm on the basis of ensuring densification. At the same time, it can also reduce the degree of interdiffusion between titanium and silicon elements, weaken the alloy brittleness, and avoid target cracking.

[0030] (4) In this invention, the titanium silicon target material is heat-treated after hot isostatic pressing, which can effectively buffer the stress of the hot isostatic pressing process and prevent the target material from cracking during processing. Attached Figure Description

[0031] Figure 1 This is a metallographic diagram of the titanium-silicon target material prepared in Example 1 of the present invention.

[0032] Figure 2 This is the XRD pattern of the titanium-silicon target material prepared in Example 1 of this invention.

[0033] Figure 3 These are microscopic images of the TiSiN film coating on the titanium-silicon target prepared in Example 1 of this invention.

[0034] Figure 4 This is the XRD pattern of the titanium-silicon target material prepared in Example 5 of the present invention.

[0035] Figure 5 These are microscopic images of the TiSiN film coating on the titanium-silicon target prepared in Example 5 of this invention. Detailed Implementation

[0036] The present application will now be described in further detail with reference to the accompanying drawings and specific embodiments.

[0037] Figure 1 The metallographic structure of a fine-grained titanium-silicon target provided in an embodiment of this application is shown.

[0038] Figure 1 The titanium-silicon target shown is a two-phase material composed of Ti phase and Ti5Si3 phase. That is to say, the titanium-silicon target does not include other titanium-silicon phases, such as TiSi phase, TiSi2 phase, etc.

[0039] In some embodiments, the proportion of Ti in the titanium-silicon target is 65-95%, and the proportion of Si is 5-35%. For example, the proportion of Ti is 70%, and the proportion of Si is 30%; or the proportion of Ti is 75%, and the proportion of Si is 25%; or the proportion of Ti is 80%, and the proportion of Si is 20%; or the proportion of Ti is 85%, and the proportion of Si is 15%; or the proportion of Ti is 93%, and the proportion of Si is 7%. It should be understood that since the target does not contain other phases, the mass ratio of the Ti phase to the Ti5Si3 phase can be calculated based on the atomic ratio of Ti and Si. The atomic ratio of Ti and Si can be set, for example, according to the material of the workpiece to be coated.

[0040] In some embodiments, to obtain a relatively pure dual-phase structure, the titanium-silicon target can be prepared by pure Ti powder and Ti5Si3 alloy powder, and during the hot isostatic pressing process, the diffusion of Si element is reduced by medium-temperature treatment to avoid the formation of other titanium-silicon phases besides Ti5Si3 phase.

[0041] In one embodiment, the Ti powder has a purity of 99.9%, a laser particle size of D10 = 5-10 μm, D50 = 25-35 μm, D90 = 40-60 μm, a tap density of 2.6-2.8 g / cm3, and an oxygen content of <2000 ppm.

[0042] In one embodiment, the purity of the Ti5Si3 alloy powder is 99.8%, the laser particle size is D10 = 3-8 μm, D50 = 20-30 μm, D90 = 35-55 μm, the tap density is 2.3-2.5 g / cm3, and the oxygen content is <2000 ppm.

[0043] The following describes a method for preparing a fine-grained titanium-silicon target according to an embodiment of this application.

[0044] (1) Selection of raw material powder.

[0045] The titanium-silicon target raw material powder prepared by this invention is pure Ti powder and Ti5Si3 alloy powder. The Ti powder has a purity of 99.9%, with laser particle sizes of D10 = 5–10 μm, D50 = 25–35 μm, and D90 = 40–60 μm, a tap density of 2.6–2.8 g / cm³, and an oxygen content <2000 ppm. The Ti5Si3 alloy powder has a purity of 99.8%, with laser particle sizes of D10 = 3–8 μm, D50 = 20–30 μm, and D90 = 35–55 μm, a tap density of 2.3–2.5 g / cm³, and an oxygen content <2000 ppm. By selecting the material, particle size, and impurity content of the raw material powder, a foundation is laid for the densification and phase control of the titanium-silicon alloy target.

[0046] (2) Pretreatment of raw material powder by ball milling and mixing.

[0047] The ball milling and mixing pretreatment process for the raw material powder of the titanium-silicon target in this invention involves ball milling the raw material powder in a three-dimensional mixer under argon protection according to the required component ratio. Specifically, the ball milling time is 5–12 hours, and the ball-to-powder weight ratio is (0.5–5):1. This ball milling and mixing pretreatment achieves uniform mixing of the raw Ti powder and Ti5Si3 alloy powder, laying the foundation for controlling the microstructure uniformity of the titanium-silicon alloy target.

[0048] (3) The powder after ball milling and pretreatment is packed into a bag.

[0049] In this invention, the powder after ball milling and pretreatment is loaded into a package, and the relative density of the powder needs to reach more than 60%.

[0050] (4) Vacuum thermal degassing treatment.

[0051] The vacuum thermal degassing process in this invention is performed at room temperature with a vacuum level below 2*10.-3 The temperature is raised to 650–750°C, and the vacuum is below 1*10⁻⁶. -3 After holding at a pressure of 180–300 min, the power is cut off and the material is sealed. Vacuum thermal degassing is a crucial step in the hot isostatic pressing (HIP) process. If the vacuum thermal degassing temperature is too low, adsorbed gases cannot be extracted, directly affecting the final shape and density of the target material. Conversely, if the vacuum thermal degassing temperature is too high, it increases energy consumption and production costs.

[0052] (5) Hot isostatic pressing densification treatment.

[0053] In this invention, the hot isostatic pressing (HIP) densification process is carried out at 700–799°C, a pressure of 140–150 MPa, and a holding time of 4–5 hours. HIP is a special powder sintering method where the activity of the powder is greatly enhanced under high temperature and pressure, allowing for material densification at a lower temperature than atmospheric pressure sintering. The HIP temperature is the core parameter of the HIP process. If the HIP temperature is too low, densification of the raw material powder cannot be achieved. If the HIP temperature is too high, the interdiffusion distance between titanium and silicon elements increases, increasing alloy brittleness and causing cracking of the titanium-silicon alloy target. It also results in coarse grains, affecting the film performance.

[0054] (6) Heat treatment.

[0055] In this invention, the target material after hot isostatic pressing densification is subjected to heat treatment. The heat treatment process involves holding at 500–600°C for 60–90 minutes, followed by furnace cooling. The purpose of heat treatment is to stabilize the microstructure of the titanium-silicon target material, reduce internal stress, prevent cracking, and facilitate subsequent machining.

[0056] It should be understood that the titanium-silicon sputtering targets prepared in existing technologies have a high degree of alloying. With the interdiffusion of titanium and silicon, multiple titanium-silicon phases exist within these targets, such as TiSi and TiSi2 phases. Unlike the Ti5Si3 phase, the presence of TiSi and TiSi2 phases can easily lead to problems such as large droplets and large particles during coating, resulting in coating defects. Furthermore, when multiple titanium-silicon phases exist within the sputtering target, the differences in the physicochemical properties of these phases can also easily lead to more defects in the film layer during the coating process, affecting the film performance.

[0057] In this embodiment, the titanium-silicon target is a two-phase material composed of Ti and Ti5Si3 phases. Firstly, because the melting point of the Ti5Si3 phase is relatively high, it is less prone to forming large droplets or particles during the coating process, thus resulting in fewer defects in the coating. Secondly, the densification temperature required for the Ti phase is relatively low; hot isostatic pressing at 700°C is sufficient to densify the Ti phase. Thirdly, the relatively low hot isostatic pressing temperature can also suppress the diffusion of Si elements, preventing the formation of other phase components in the titanium-silicon target. Fourthly, the low hot isostatic pressing temperature also helps to produce a fine and uniform microstructure in the target, with an average grain size of <50μm.

[0058] Example 1

[0059] The titanium-silicon target material prepared in this embodiment has a composition ratio of Ti85Si15at%. The preparation method includes the following steps:

[0060] (1) Weigh out the raw material powders: pure Ti powder and Ti5Si3 alloy powder. The weight ratio of Ti powder to Ti5Si3 alloy powder is 64.01:35.99. The purity of the Ti powder is 99.9%, the laser particle size is D10 = 6μm, D50 = 29μm, D90 = 55μm, and the tap density is 2.75g / cm³. 3 The oxygen content is 1600 ppm; the purity of the Ti5Si3 alloy powder is 99.8%, the laser-cut particle size is D10 = 4 μm, D50 = 28 μm, D90 = 50 μm, and the tap density is 2.42 g / cm³. 3 The oxygen content is 1760 ppm.

[0061] (2) The weighed raw material powder was placed into a three-dimensional mixer under argon protection for ball milling to enhance mixing. The ball milling time was 8 hours, and the ball-to-material weight ratio was 1:1.

[0062] (3) The mixed powder is loaded into a package with a relative density of 62.4%.

[0063] (4) The packaged powder is then subjected to vacuum thermal degassing. The degassing process is carried out at room temperature under a vacuum of less than 2*10. -3 The temperature is raised to 680℃, and the vacuum is below 1*10. -3 After applying pressure and maintaining the temperature for 200 minutes, the power was cut off and the sample was sealed with a weld.

[0064] (5) The degassed cladding is subjected to hot isostatic pressing (HIP) densification treatment. The HIP process is 750℃, 150MPa, and 4.5h.

[0065] (6) The hot isostatically pressed titanium-silicon target material is heat-treated. The heat treatment process is to hold at 550℃ for 60 minutes and then cool it with the furnace.

[0066] The titanium-silicon target material prepared in Example 1 of this invention was subjected to density, XRD and metallographic analysis. Figure 1 and Figure 2 The images show the metallographic structure and XRD pattern of the titanium-silicon target material prepared in Example 1 of this invention. The results show that the titanium-silicon target material has a high density, with a relative density of 99.3%; it contains only two phases, Ti phase and Ti5Si3 phase, and no other phases such as TiSi and TiSi2; the microstructure is dense, fine and uniform, with an average grain size of 39 μm.

[0067] The titanium-silicon target material prepared in Example 1 of this invention was coated with nitrogen gas to prepare a TiSiN film. Figure 3 These are microscopic images of the TiSiN film coated on the titanium-silicon target prepared in Example 1 of this invention. The results show that the film surface is uniform and dense, and the size and number of "large particle" defects are small.

[0068] Example 2

[0069] The titanium-silicon target material prepared in this embodiment has a composition ratio of Ti 80Si 20 at%. The preparation method includes the following steps:

[0070] (1) Weigh out the raw material powders: pure Ti powder and Ti5Si3 alloy powder. The weight ratio of Ti powder to Ti5Si3 alloy powder is 50.91:49.09. The purity of the Ti powder is 99.9%, the laser particle size is D10 = 8 μm, D50 = 33 μm, D90 = 57 μm, and the tap density is 2.69 g / cm³. 3 The oxygen content is 1520 ppm; the purity of the Ti5Si3 alloy powder is 99.8%, the laser-etched particle size is D10 = 5 μm, D50 = 22 μm, D90 = 43 μm, and the tap density is 2.39 g / cm³. 3 The oxygen content is 1830 ppm.

[0071] (2) The weighed raw material powder was placed into a three-dimensional mixer under argon protection for ball milling to enhance mixing. The ball milling time was 6 hours, and the ball-to-material weight ratio was 2:1.

[0072] (3) The mixed powder is loaded into a package with a relative density of 63.2%.

[0073] (4) The packaged powder is then subjected to vacuum thermal degassing. The degassing process is carried out at room temperature under a vacuum of less than 2*10. -3 The temperature is raised to 650℃, and the vacuum is below 1*10. -3 After applying pressure and maintaining the temperature for 180 minutes, the power was cut off and the device was sealed with a welding torch.

[0074] (5) The degassed cladding is subjected to hot isostatic pressing (HIP) densification treatment. The HIP process is 730℃, 140MPa, and 5h.

[0075] (6) The hot isostatically pressed titanium-silicon target material is heat-treated. The heat treatment process is to hold at 580℃ for 70 minutes and then cool it with the furnace.

[0076] The titanium-silicon target material prepared in Example 2 of this invention was subjected to density, XRD, and metallographic analysis. The results showed that the titanium-silicon target material had a high density, with a relative density of 99.5%; it contained only two phases, Ti and Ti5Si3, and no other phases such as TiSi and TiSi2; the microstructure was dense, fine, and uniform, with an average grain size of 42 μm.

[0077] Example 3

[0078] The titanium-silicon target material prepared in this embodiment has a composition ratio of Ti 75Si 25 at%. The preparation method includes the following steps:

[0079] (1) Weigh out the raw material powders: pure Ti powder and Ti5Si3 alloy powder. The weight ratio of Ti powder to Ti5Si3 alloy powder is 37.21:62.79. The purity of the Ti powder is 99.9%, the laser particle size is D10 = 9 μm, D50 = 28 μm, D90 = 43 μm, and the tap density is 2.61 g / cm³. 3 The oxygen content is 1730 ppm; the purity of the Ti5Si3 alloy powder is 99.8%, the laser-etched particle size is D10 = 3 μm, D50 = 24 μm, D90 = 36 μm, and the tap density is 2.35 g / cm³. 3 The oxygen content is 1690 ppm.

[0080] (2) The weighed raw material powder was placed into a three-dimensional mixer under argon protection for ball milling and enhanced mixing. The ball milling time was 10 hours, and the ball-to-material weight ratio was 3:1.

[0081] (3) The mixed powder is loaded into a package with a relative density of 61.9%.

[0082] (4) The packaged powder is then subjected to vacuum thermal degassing. The degassing process is carried out at room temperature under a vacuum of less than 2*10. -3 The temperature is raised to 750℃, and the vacuum is below 1*10. -3 After applying pressure and maintaining the temperature for 280 minutes, the power was cut off and the sample was sealed with solder.

[0083] (5) The degassed cladding is then subjected to hot isostatic pressing (HIP) densification. The HIP process is performed at 799℃, pressure 150MPa, and holding time 5h.

[0084] (6) The hot isostatically pressed titanium-silicon target material is heat-treated. The heat treatment process is to hold at 500℃ for 90 minutes and then cool it with the furnace.

[0085] The titanium-silicon target material prepared in Example 3 of this invention was subjected to density, XRD, and metallographic analysis. The results showed that the titanium-silicon target material had a high density, with a relative density of 99.4%; it contained only two phases, Ti and Ti5Si3, and no other phases such as TiSi and TiSi2; the microstructure was dense, fine, and uniform, with an average grain size of 45 μm.

[0086] Example 4

[0087] The titanium-silicon target material prepared in this embodiment has a composition ratio of Ti 70Si 30 at%. The preparation method includes the following steps:

[0088] (1) Weigh out the raw material powders: pure Ti powder and Ti5Si3 alloy powder. The weight ratio of Ti powder to Ti5Si3 alloy powder is 22.86:77.14. The purity of the Ti powder is 99.9%, the laser particle size is D10 = 5μm, D50 = 35μm, D90 = 50μm, and the tap density is 2.73g / cm³. 3 The oxygen content is 1860 ppm; the purity of the Ti5Si3 alloy powder is 99.8%, the laser-etched particle size is D10 = 7 μm, D50 = 28 μm, D90 = 53 μm, and the tap density is 2.46 g / cm³. 3 The oxygen content is 1810 ppm.

[0089] (2) The weighed raw material powder was placed into a three-dimensional mixer under argon protection for ball milling and enhanced mixing. The ball milling time was 12 hours, and the ball-to-material weight ratio was 5:1.

[0090] (3) The mixed powder is loaded into a package with a relative density of 62.8%.

[0091] (4) The packaged powder is then subjected to vacuum thermal degassing. The degassing process is carried out at room temperature under a vacuum of less than 2*10. -3 The temperature is raised to 720℃, and the vacuum is below 1*10. -3 After applying pressure and maintaining the temperature for 300 minutes, the power was cut off and the sample was sealed with a weld.

[0092] (5) The degassed cladding is subjected to hot isostatic pressing (HIP) densification treatment. The HIP process is 790℃, 150MPa, and 4.5h.

[0093] (6) The hot isostatically pressed titanium-silicon target material is heat-treated. The heat treatment process is 520℃, held for 80 minutes and then cooled in the furnace.

[0094] The titanium-silicon target material prepared in Example 4 of this invention was subjected to density, XRD, and metallographic analysis. The results showed that the titanium-silicon target material had a high density, with a relative density of 99.5%; it contained only two phases, Ti and Ti5Si3, and no other phases such as TiSi and TiSi2; the microstructure was dense, fine, and uniform, with an average grain size of 46 μm.

[0095] Example 5

[0096] In this embodiment, except that the Ti5Si3 alloy powder in the raw material powder is replaced with TiSi2 alloy powder, the other steps and process conditions are the same as in Embodiment 1 of the present invention.

[0097] Figure 4 This is the XRD pattern of the titanium-silicon target material prepared in Example 5 of the present invention. The results show that the titanium-silicon target material prepared in Example 5 of the present invention contains not only Ti phase and Ti5Si3 phase, but also TiSi and TiSi2 phases, indicating a low degree of alloying.

[0098] The titanium-silicon target material prepared in Example 5 of this invention was coated with nitrogen gas to prepare a TiSiN film. Figure 5 These are microscopic images of the TiSiN film coated on the titanium-silicon target prepared in Example 5 of this invention. The results show that the surface structure of the film is not uniform and dense, and the "large particle" defects are large in size and numerous.

[0099] As can be seen from the above embodiments, the present invention uses pure Ti powder and Ti5Si3 alloy powder as raw materials. After ball milling and mixing pretreatment, the raw material powder is packaged and vacuum hot degassing treatment is performed. The degassing package is then subjected to hot isostatic pressing densification treatment. Finally, heat treatment is used to stabilize the microstructure and reduce internal stress, thereby obtaining a titanium silicon target material containing only two phases, Ti phase and Ti5Si3 phase, with a uniform and fine microstructure.

[0100] Although the present invention has been disclosed above with reference to preferred embodiments, it is not intended to limit the present invention. Any person skilled in the art can make possible changes and modifications without departing from the spirit and scope of the present invention. Therefore, the scope of protection of the present invention should be determined by the scope defined in the claims of the present invention.

Claims

1. A fine-grained titanium-silicon sputtering target, characterized in that, The titanium-silicon target is a two-phase material composed of Ti phase and Ti5Si3 phase; in the titanium-silicon target, the proportion of Ti element is 80~95%, and the proportion of Si element is 5~20%; The raw materials of the titanium-silicon target are pure Ti powder and Ti5Si3 alloy powder, which are prepared by hot isostatic pressing (HIP). The HIP temperature is 700-799℃, the pressure is 140-150MPa, and the holding time is 4-5h. The raw material powder satisfies: The purity of the Ti powder is 99.9%, the laser particle size is D10=5~10μm, D50=25~35μm, D90=40~60μm, the tap density is 2.6~2.8g / cm3, and the oxygen content is <2000ppm; The purity of Ti5Si3 alloy powder is 99.8%, the laser particle size is D10=3~8μm, D50=20~30μm, D90=35~55μm, the tap density is 2.3~2.5g / cm3, and the oxygen content is <2000ppm.

2. The fine-grained titanium-silicon sputtering target according to claim 1, characterized in that, The average grain size of the titanium-silicon target is <50μm.

3. A method for preparing a fine-grained titanium-silicon target as described in claim 1 or 2, characterized in that, include: The raw material powders, including pure Ti powder and Ti5Si3 alloy powder, are subjected to ball milling and mixing pretreatment. The pre-treated powder after ball milling is packed into a sleeve, and then sealed after vacuum thermal degassing. Perform hot isostatic pressing densification treatment; The target material after hot isostatic pressing densification is then subjected to heat treatment.

4. The method according to claim 3, characterized in that, The heat treatment meets the following requirements: temperature 500-600℃, holding time 60-90 min, and cooling in the furnace.

5. The method according to claim 3, characterized in that, The method satisfies at least one of the following: The ball milling pretreatment meets the requirements of a ball milling time of 5-12 hours and a ball-to-material weight ratio of (0.5-5):

1. The relative density of the powder reaches over 60%; The vacuum thermal degassing process is performed at room temperature under a vacuum of less than 2*10. -3 The temperature is raised to 650–750°C, and the vacuum is below 1*10⁻⁶. -3 Pa and keep warm for 180–300 minutes.

6. A fine-grained titanium-silicon sputtering target, characterized in that, The fine-grained titanium-silicon target is prepared by the method described in any one of claims 3 to 5.

Images