Mo-ti-ta-ce alloy target material, preparation method and application thereof

Abstract

The application discloses a Mo-Ti-Ta-Ce alloy target material and a preparation method and application thereof, and belongs to the technical field of alloy sputtering targets and powder metallurgy. The preparation method of the alloy target material is as follows: titanium, tantalum, cerium and molybdenum are weighed according to the atomic percentage of each element; under the protection of inert gas, tantalum powder, cerium dioxide powder and molybdenum powder are weighed and subjected to first ball milling treatment to obtain Mo-Ta-CeO2 pre-alloy powder; TiH2 powder and the remaining Mo powder are weighed and subjected to second ball milling treatment to obtain Mo-Ti pre-alloy powder; the two kinds of pre-alloy powders are uniformly mixed, then cold isostatic pressing is carried out to obtain a cold-pressed compact; the cold-pressed compact is sintered to obtain a sintered compact; the sintered compact is subjected to rolling treatment to obtain a rolled target material; and the rolled target material is subjected to annealing treatment to obtain the Mo-Ti-Ta-Ce alloy target material. The thin film prepared by the alloy target material has excellent corrosion resistance, oxidation resistance and electrical conductivity.

Description

Technical Field

[0001] This invention relates to the fields of alloy sputtering targets and powder metallurgy technology, and more specifically to a Mo-Ti-Ta-Ce alloy target, its preparation method, and its application. Background Technology

[0002] With the continuous upgrading of flat panel displays such as Liquid Crystal Displays (LCDs), Thin Film Transistor Liquid Crystal Displays (TFT-LCDs), and Plasma Display Panels (PDPs), their sizes are becoming larger and their application scenarios are becoming more diverse. The continuous advancement of smart interconnection technologies is increasing the demand for flat panel displays in different scenarios. Displays used in various fields, including industry, are facing more complex service conditions, placing more stringent demands on the performance of sputtering targets and barrier layer films in the displays.

[0003] Low-resistance Al or Cu are typically chosen as wiring materials in flat panel displays or other semiconductor devices. However, the fabrication process of wiring layers in electronic devices involves a heating process. Direct contact between the Al or Cu conductive layer and the Si semiconductor film at high temperatures can cause Al or Cu to diffuse extensively in Si. Therefore, a molybdenum alloy film is required as a barrier layer between the two.

[0004] Currently, thin films sputtered from alloy targets based on MoTi / MoNiTi systems are mainly used as barrier layers. However, barrier layers sputtered from targets with this composition suffer from insufficient corrosion resistance, oxidation resistance, and high-temperature performance. For example, in some flat panel displays used in industrial environments with high humidity, acid / alkalinity, and high temperatures, the internal barrier layer is highly susceptible to the effects of moisture, acid / alkaline atmospheres, or temperature. Furthermore, during signal cable cabling for flat panel displays, the internal structure is exposed to high-temperature, oxygen-rich environments for extended periods, requiring the barrier layer to possess higher corrosion resistance and oxidation resistance. Simultaneously, the corrosion resistance and oxidation resistance of the barrier layer should be improved without compromising, or even increasing, its electrical conductivity. Summary of the Invention

[0005] To address the above problems, this invention provides a Mo-Ti-Ta-Ce alloy target, its preparation method, and its application. When the Mo-Ti-Ta-Ce alloy target obtained by this invention is used to prepare thin films, the prepared films exhibit excellent corrosion resistance, oxidation resistance, and electrical conductivity.

[0006] The first objective of this invention is to provide a method for preparing a Mo-Ti-Ta-Ce alloy target, comprising the following steps:

[0007] Weigh each raw material according to the atomic percentage of each element in the Mo-Ti-Ta-Ce alloy target: 20%~40%Ti, 5%~12%Ta and 0.05%~0.12%Ce, with the balance being Mo and unavoidable impurities, Mo≥45%, totaling 100%.

[0008] Under inert gas protection, Ta powder, CeO2 powder and Mo powder are weighed according to 5%~10%Ta, 0.05%~0.12%Ce and 15%~21%Mo, and mixed evenly to obtain a first mixed powder. The first mixed powder is subjected to a first ball milling treatment to obtain Mo-Ta-CeO2 pre-alloyed powder.

[0009] Under inert gas protection, TiH2 powder with 20%~40% Ti was weighed and mixed evenly with the remaining Mo powder to obtain a second mixed powder. The second mixed powder was then subjected to a second ball milling process to obtain Mo-Ti pre-alloyed powder.

[0010] Mo-Ta-CeO2 pre-alloyed powder and Mo-Ti pre-alloyed powder were mixed in batches and then subjected to cold isostatic pressing to obtain a cold-pressed billet.

[0011] The cold-pressed green body is sintered in a reducing atmosphere to obtain a sintered green body.

[0012] The sintered billet is rolled to obtain the rolled target material; the rolled target material is annealed at 900℃~1050℃ in a reducing atmosphere to obtain the Mo-Ti-Ta-Ce alloy target material.

[0013] In a preferred embodiment of the present invention, in the first ball milling process, the ball-to-material ratio is 5~10:1, and the ball milling time is 1.5h~3h.

[0014] In a preferred embodiment of the present invention, in the second ball milling process, the ball-to-material ratio is 2~6:1, and the ball milling time is 2h~4h.

[0015] In a preferred embodiment of the present invention, when mixing Mo-Ta-CeO2 pre-alloyed powder and Mo-Ti pre-alloyed powder, a three-dimensional mixer is used, and the mixing time is 4h~5h.

[0016] In a preferred embodiment of the present invention, the pressure in the cold isostatic pressing process is 150MPa~250MPa, and the holding time is 6min~20min.

[0017] In a preferred embodiment of the present invention, during the sintering process, the first stage heating rate is set to 10℃ / min, and the temperature is raised to 950℃~1100℃ and held for 3.5h~5h; the second stage heating rate is set to 10℃ / min, and the temperature is raised to 1290℃~1310℃ and held for 1h~2h; the third stage heating rate is set to 5℃~8℃ / min, and the temperature is raised to 1350℃~1450℃ and held for 4h~6h.

[0018] In a preferred embodiment of the present invention, during the rolling process, the initial rolling temperature is 1150℃~1400℃, and the final rolling temperature is 1000℃~1200℃; the total rolling deformation in the rolling process is controlled at about 45%, and the single-pass rolling deformation is controlled at 15%~25%; the hot rolling process is preheated to 1050℃~1100℃ before each pass, and the preheating time is 0.5h~1h.

[0019] In a preferred embodiment of the present invention, the annealing time is 1 hour to 2 hours.

[0020] The second objective of this invention is to provide a Mo-Ti-Ta-Ce alloy target material prepared by the above-described preparation method.

[0021] A third objective of this invention is to provide the application of the aforementioned Mo-Ti-Ta-Ce alloy target in the preparation of thin films by magnetron sputtering.

[0022] Compared with the prior art, the present invention has the following beneficial effects:

[0023] The molybdenum alloy target matrix of this invention is Mo-Ti, with Ta and Ce added. When the sintering temperature reaches above 880°C, Ti undergoes a phase transformation, changing from α-Ti to β-Ti. β-Ti then forms an infinite solid solution (β-Ti, Mo) with Mo. This allows the alloy to exhibit the advantages of Mo, such as corrosion resistance and good electrical conductivity, while also showcasing the excellent properties of Ta and Ce. In addition to forming a solid solution to slow down the softening trend of Mo at high temperatures, Ti and Mo also precipitate TiMo, Ti3Mo, and other second phases, which have a dispersion strengthening effect on the alloy and improve the high-temperature strength of the target. Furthermore, Ti's standard electrode potential is higher than that of Mo. When subjected to corrosion, the passivation film formed by Ti increases the overall potential of the alloy, improving its corrosion resistance. Adding Ta to the Mo-Ti matrix allows it to form a crystalline solid solution, refining the alloy grain size and densifying the microstructure, thus giving the target material good plasticity. It also improves the sputtering rate of the target material and enhances the homogenization of the film composition and microstructure. During sintering, when Ta and Mo coexist, Ta, in addition to forming a solid solution, preferentially combines with O to form a Ta₂O₅ layer, improving the oxidation resistance of the target material and film. Furthermore, during high-temperature sintering, ordered phases such as TaMo₂ or Ta₂Mo are formed in certain regions. These highly chemically inert phases can act as corrosion-resistant islands, hindering the spread of localized corrosion and improving the corrosion resistance of the target material and film. Ta alloying promotes the formation of smooth, ordered island structures on the surface of the target material or film, improving the conductivity of the film. This invention also adds the rare earth element Ce to the Mo-Ti based alloy. This element is mainly distributed uniformly in the Mo-Ti matrix in the form of fine CeO₂ particles, purifying grain boundaries and reducing the resistivity of the film.

[0024] In the preparation process, the main process of this invention is premixing-ball milling-mixing. First, two types of pre-alloy powders, Mo-Ti pre-alloy powder and Mo-Ta-Ce pre-alloy powder, are prepared. The pre-alloy powders are prepared using a high-energy ball milling process. Then, the two pre-alloy powders are mixed to obtain the final alloy powder. This process can maximize the uniform mixing of each alloying element. The energy state of Mo-TiH2 powder is improved during the high-energy ball milling process, and the subsequent sintering process can more easily form a molybdenum-titanium solid solution. Attached Figure Description

[0025] Figure 1 The image shows the metallographic structure of the alloy target material prepared in Example 1 of this invention in its sintered state at a scale bar of 50 μm.

[0026] Figure 2 The image shows the metallographic structure of the alloy target material prepared in Example 1 of this invention in its sintered state at a scale bar of 100 μm.

[0027] Figure 3 This is a scanning electron microscope image of the sintered alloy target material prepared in Example 1 of the present invention, with a scale bar of 2 μm.

[0028] Figure 4 This is a scanning electron microscope image of the alloy target material prepared in Example 1 of the present invention in its sintered state with a scale bar of 5 μm. Detailed Implementation

[0029] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0030] This invention utilizes elements such as Mo, Ti, Ta, and Ce to prepare a molybdenum-titanium-based multi-element alloy target, and optimizes its composition and preparation process. Results show that the target and the sputtered film prepared using the composition and process employed in this invention exhibit improved corrosion resistance, oxidation resistance, and high-temperature performance compared to traditional MoTi / MoNiTi targets. Furthermore, the observed microstructure shows fine grains with uniform size distribution, and the target's plasticity is also improved to some extent. Moreover, when the film prepared from this target is used as a barrier layer between a conductive layer and a silicon semiconductor film, the device exhibits good conductivity with a slight improvement. It should be noted that the film sputtered using the target of this invention is an alloy film, primarily used as a barrier layer between an Al / Cu conductive layer and a silicon semiconductor film in flat panel displays or semiconductor devices.

[0031] It is important to note that the amount of Ce added must be strictly controlled within the range of 0.05~0.12 at%. This will maximize the purification of grain boundaries, reduce the resistivity of the film, and improve its conductivity. If the Ce addition is below this range, the CeO2 particles will mainly act as electron scatterers, increasing the resistivity of the film. If the Ce addition is above this range, the strong grain-refining effect of rare earth elements will lead to excessively high grain boundary density in both the target material and the film, increasing the probability of electron scattering and weakening its conductivity.

[0032] The specific preparation steps are as follows:

[0033] Weigh each raw material according to the atomic percentage of each element in the Mo-Ti-Ta-Ce alloy target, wherein 20%~40%Ti, 5%~12%Ta and 0.05%~0.12%Ce, with the balance being Mo and unavoidable impurities, Mo≥45%, totaling 100%.

[0034] Under inert gas protection, Ta powder, CeO2 powder and Mo powder are weighed according to 5%~10%Ta, 0.05%~0.12%Ce and 15%~21%Mo, and mixed evenly to obtain a first mixed powder. The first mixed powder is subjected to a first ball milling treatment to obtain Mo-Ta-CeO2 pre-alloyed powder.

[0035] Under inert gas protection, TiH2 powder with 20%~40% Ti was weighed and mixed evenly with the remaining Mo powder to obtain a second mixed powder. The second mixed powder was then subjected to a second ball milling process to obtain Mo-Ti pre-alloyed powder.

[0036] Under inert gas protection, Mo-Ti pre-alloy powder and Mo-Ta-CeO2 pre-alloy powder are mixed evenly and then subjected to cold isostatic pressing to obtain a cold-pressed billet. The pre-alloy powder is prepared by high-energy ball milling, and then the two pre-alloy powders are mixed to obtain the final alloy powder. This process can maximize the uniform mixing of each alloying element. The energy state of Mo-TiH2 powder is improved during high-energy ball milling, and the subsequent sintering process can promote the formation of molybdenum-titanium solid solution.

[0037] The cold-pressed billet is loaded into an intermediate frequency furnace and sintered under a reducing atmosphere to obtain a sintered billet. Vacuuming the ball mill jar before preparing the pre-alloyed powder removes some of the oxygen from the powder. During the multi-gradient hydrogen reduction sintering process, residual oxygen in the target billet is consumed and removed. The multi-gradient hydrogen reduction sintering process used in this step is mainly based on the considerations of the easy oxidation of molybdenum alloys and promoting the precipitation of beneficial second phases in the alloy target. According to the phase diagram and production requirements, the sintering process is set as follows: the first stage heating rate is set to 10℃ / min, heating to 950℃~1100℃ and holding for 3.5h~5h; the second stage heating rate is set to 10℃ / min, heating to 1290℃~1310℃ and holding for 1h~2h; the third stage heating rate is set to 5℃~8℃ / min, heating to 1350℃~1450℃ and holding for 4h~6h.

[0038] The sintered billet is rolled to obtain the rolled target material.

[0039] The rolled target material was annealed at 900℃~1050℃ in a reducing atmosphere, with H2 as the reducing atmosphere during annealing, to obtain a Mo-Ti-Ta-Ce alloy target material.

[0040] During the preparation process according to the preparation steps of this invention, different sizes and specifications of target materials can be used according to actual needs.

[0041] Example 1

[0042] This embodiment provides a Mo-Ti-Ta-Ce alloy target and its preparation process. The composition of the alloy target, in atomic percentage, includes Mo 63.94at%, Ti 30at%, Ta 6at%, and Ce 0.06at.

[0043] Step 1: Weigh 15 at% Mo powder, 6 at% Ta powder, and 0.06 at% CeO2 powder, and mix them in a three-dimensional mixer purged with argon gas for 2.5 hours. Then, perform high-energy ball milling on the mixed powder, using 6mm diameter tungsten carbide grinding balls at a ball-to-powder ratio of 5:1. Before ball milling, evacuate the grinding jar to 10°C. -1 Pa was introduced and argon gas was introduced. Finally, the mixture was ball-milled at 300 r / min for 2.5 h to obtain Mo-Ta-CeO2 pre-alloyed powder.

[0044] Step 2: 30 at% TiH2 powder and 48.94 at% Mo powder were loaded into a three-dimensional mixer filled with argon gas and mixed for 2 hours. The mixed powder was then subjected to high-energy ball milling using 6mm diameter tungsten carbide grinding balls at a ball-to-powder ratio of 3.5:1. The grinding jar was evacuated for 10 minutes before ball milling. -1 Pa was introduced and argon gas was introduced. Finally, the mixture was ball-milled at 300 r / min for 2.5 h to obtain Mo-Ti pre-alloyed powder.

[0045] Step 3: Mix the Mo-Ta-Ce2O pre-alloy powder obtained in Step 1 with the Mo-Ti pre-alloy powder obtained in Step 2 under an argon atmosphere for 5 hours at a rotation speed of 28 r / min to obtain a homogeneous alloy powder.

[0046] Step 4: Pour the mixed alloy powder into the rubber sleeve and vibrate it to compact it. Then, seal the rubber sleeve tightly with a rubber stopper and place it into an isostatic pressing device. The holding pressure is 180 MPa and the holding time is 8 minutes to obtain a cold-pressed billet.

[0047] Step 5: Shape the cold-pressed blank, remove the burrs and flash from the surface, and obtain a regular geometric shape.

[0048] Step 6: Place the shaped cold-pressed billet into an intermediate frequency furnace. Then, perform multi-gradient reduction sintering on the cold-pressed billet. In the first stage, the temperature is increased to 960℃ at 10℃ / min and held for 4 hours. In the second stage, the temperature is increased to 1295℃ at 10℃ / min and held for 1.5 hours. In the third stage, the temperature is increased to 1370℃ at 6℃ / min and held for 5 hours. The entire sintering process is carried out in a hydrogen atmosphere with a hydrogen input rate of 200 ml / min. Finally, the sintered billet is obtained.

[0049] Step 7: Heat the sintered billet to 1300℃ to begin the first rolling pass. The second rolling pass temperature is controlled at 1200℃, and the final rolling pass temperature is 1100℃. The total rolling deformation is controlled at 45%, and the deformation per single pass is controlled at 15%. Three rolling passes are performed. Before each rolling pass, the billet is held at 1050℃ for 1 hour to obtain the rolled piece.

[0050] Step 8: Machining the rolled piece. First, use a leveling machine and polishing equipment to level and polish the rolled plate, and then use a cutting machine to trim the dimensions of the rolled piece to obtain the rolled target material.

[0051] Step 9: Anneal the rolled target material under hydrogen atmosphere at a temperature of 900℃ for 1 hour to obtain the Mo-Ti-Ta-Ce alloy target material.

[0052] Figures 1-2 The image shows the metallographic structure of the alloy target material in the sintered state prepared in this embodiment. It should be noted that the sintered state is the state after sintering in the furnace (before rolling), that is, the product after hydrogen reduction sintering of the cold-pressed billet in step 6.

[0053] from Figures 1-2 The grain boundaries of the alloy grains can be clearly seen, and the grain size in the microstructure is relatively uniform; dark-colored second-phase particles precipitate inside the grains and are dispersed in the matrix. Figures 3-4 These are scanning electron microscope images of the same location at different magnifications in the sintered state of the alloy target prepared in this example, mainly characterizing the precipitation location of the second phase particles in the alloy and local magnified images. Figure 3 The smaller black particles on the left are the second phase in the alloy, and they are located inside the grains and are very small.

[0054] The alloy target material prepared in this embodiment has an average grain size of approximately 51 μm and exhibits good plastic deformation capability.

[0055] Example 2

[0056] This embodiment provides a Mo-Ti-Ta-Ce alloy target and its preparation process. The composition of the alloy target, by atomic percentage, includes Mo 56.92 at%, Ti 35 at%, Ta 8 at%, and Ce 0.08 at%.

[0057] Step 1: Weigh 17 at% Mo powder, 8 at% Ta powder, and 0.06 at% CeO2 powder, and mix them in a three-dimensional mixer purged with argon gas for 2.5 hours. Then, perform high-energy ball milling on the mixed powder, using 6mm diameter tungsten carbide grinding balls at a ball-to-powder ratio of 6:1. Before ball milling, evacuate the grinding jar to 10°C. -1 Pa was introduced and argon gas was introduced. Finally, the mixture was ball-milled at 350 r / min for 2 h to obtain Mo-Ta-CeO2 pre-alloyed powder.

[0058] Step 2: 35 at% TiH2 powder and 41.92 at% Mo powder were loaded into a three-dimensional mixer filled with argon gas and mixed for 2 hours. The mixed powder was then subjected to high-energy ball milling using 6mm diameter tungsten carbide grinding balls at a ball-to-powder ratio of 4.5:1. The grinding jar was evacuated for 10 minutes before ball milling. -1 Pa was introduced and argon gas was introduced. Finally, the mixture was ball-milled at 350 r / min for 2 h to obtain Mo-Ti pre-alloyed powder.

[0059] Step 3: Mix the Mo-Ta-CeO2 pre-alloy powder obtained in Step 1 with the Mo-Ti pre-alloy powder obtained in Step 2 under an argon atmosphere for 5 hours to obtain a homogeneous alloy powder.

[0060] Step 4: Pour the mixed alloy powder into the rubber sleeve and vibrate it to compact it. Then, seal the rubber sleeve tightly with a rubber stopper and place it into an isostatic pressing device. The holding pressure is 190 MPa and the holding time is 10 min to obtain a cold-pressed billet.

[0061] Step 5: Shape the cold-pressed blank, remove the burrs and flash from the surface, and obtain a regular geometric shape.

[0062] Step 6: Place the shaped cold-pressed billet into an intermediate frequency furnace and then perform multi-gradient reduction sintering on the cold-pressed billet. In the first stage, the temperature is increased to 990℃ at 10℃ / min and held for 4.5h. In the second stage, the temperature is increased to 1300℃ at 10℃ / min and held for 1.5h. In the third stage, the temperature is increased to 1390℃ at 6℃ / min and held for 5.5h. The entire sintering process is carried out in a hydrogen atmosphere with a hydrogen input rate of 200ml / min. Finally, the sintered billet is obtained.

[0063] Step 7: Heat the sintered billet to 1200℃ to begin the first rolling pass. The second rolling pass temperature is controlled at 1200℃, and the final rolling pass temperature is 1050℃. The total rolling deformation is controlled at 45%, and the deformation per pass is controlled at 15%. Three rolling passes are performed. Before each rolling pass, the billet is held at 1050℃ for 1 hour to obtain the rolled piece.

[0064] Step 8: Machining the rolled piece, including leveling, surface polishing and dimensional adjustment, to obtain the rolled target material.

[0065] Step 9: Anneal the rolled target material at a temperature of 950℃, in an annealing atmosphere of H2, for 1.5 hours to obtain a Mo-Ti-Ta-Ce alloy target material.

[0066] The alloy target material prepared in this embodiment has an average grain size of approximately 53 μm and good deformation capability.

[0067] Example 3

[0068] This embodiment provides a Mo-Ti-Ta-Ce alloy target and its preparation process. The composition of the alloy target, in atomic percentage, includes Mo 49.9at%, Ti 40at%, Ta 10at%, and Ce 0.1at.

[0069] Step 1: Weigh 19 at% Mo powder, 10 at% Ta powder, and 0.1 at% CeO2 powder, and mix them in a three-dimensional mixer purged with argon gas for 3 hours; then, perform high-energy ball milling on the mixed powder, using 6mm diameter tungsten carbide grinding balls at a ball-to-powder ratio of 7.5:1. Before ball milling, evacuate the grinding jar to 100°C. -1 Pa was introduced and argon gas was introduced. Finally, the mixture was ball-milled at 400 r / min for 1.5 h to obtain Mo-Ta-CeO2 pre-alloyed powder.

[0070] Step 2: 40 at% TiH2 powder and 30.9 at% Mo powder were loaded into a three-dimensional mixer filled with argon gas and mixed for 2 hours. The mixed powder was then subjected to high-energy ball milling using 6mm diameter tungsten carbide grinding balls at a ball-to-powder ratio of 5:1. The grinding jar was evacuated for 10 minutes before ball milling. -1 Pa was introduced and argon gas was introduced. Finally, the mixture was ball-milled at 350 r / min for 2 h to obtain Mo-Ti pre-alloyed powder.

[0071] Step 3: Mix the Mo-Ta-Ce2O pre-alloy powder obtained in Step 1 with the Mo-Ti pre-alloy powder obtained in Step 2 under an argon atmosphere for 5 hours to obtain a homogeneous alloy powder.

[0072] Step 4: Pour the mixed alloy powder into the rubber sleeve and vibrate it to compact it. Then, seal the rubber sleeve tightly with a rubber stopper and place it into an isostatic pressing device. The holding pressure is 200 MPa and the holding time is 15 minutes to obtain a cold-pressed billet.

[0073] Step 5: Shape the cold-pressed blank, remove the burrs and flash from the surface, and obtain a regular geometric shape.

[0074] Step 6: Place the shaped cold-pressed billet into an intermediate frequency furnace and then perform multi-gradient reduction sintering on the cold-pressed billet. In the first stage, the temperature is increased to 1000℃ at 10℃ / min and held for 5 hours. In the second stage, the temperature is increased to 1310℃ at 10℃ / min and held for 2 hours. In the third stage, the temperature is increased to 1450℃ at 6℃ / min and held for 6 hours. The entire sintering process is carried out in a hydrogen atmosphere with a hydrogen input rate of 200 ml / min. Finally, the sintered billet is obtained.

[0075] Step 7: Heat the sintered billet to 1200℃ to begin the first rolling pass. The second rolling pass temperature is controlled at 1200℃, and the final rolling pass temperature is 1050℃. The total rolling deformation is controlled at 45%, and the deformation per pass is controlled at 15%. Three rolling passes are performed. Before each rolling pass, the billet is held at 1050℃ for 1 hour to obtain the rolled piece.

[0076] Step 8: Machining the rolled piece, including leveling, surface polishing and dimensional adjustment, to obtain the rolled target material.

[0077] Step 9: Anneal the rolled target material at a temperature of 1050℃, in an annealing atmosphere of H2, for 2 hours to obtain a Mo-Ti-Ta-Ce alloy target material.

[0078] The high sintering and annealing temperatures in this embodiment resulted in coarse grains in the prepared alloy target material, with an average grain size of approximately 66 μm and moderate deformation capability.

[0079] Example 4

[0080] This embodiment provides a Mo-Ti-Ta-Ce alloy target and its preparation process. The composition of the alloy target, in atomic percentage, includes Mo 47.88at%, Ti 40at%, Ta 12at%, and Ce 0.12at.

[0081] Step 1: Weigh 21 at% Mo powder, 12 at% Ta powder, and 0.12 at% CeO2 powder, and mix them in a three-dimensional mixer purged with argon gas for 3 hours; then, perform high-energy ball milling on the mixed powder, using 6mm diameter tungsten carbide grinding balls at a ball-to-powder ratio of 9:1. Before ball milling, evacuate the grinding jar to 100°C. -1 Pa was introduced and argon gas was introduced. Finally, the mixture was ball-milled at 400 r / min for 1.5 h to obtain Mo-Ta-CeO2 pre-alloyed powder.

[0082] Step 2: 40 at% TiH2 powder and 26.88 at% Mo powder were loaded into a three-dimensional mixer purged with argon gas and mixed for 2 hours. The mixed powder was then subjected to high-energy ball milling using 6mm diameter tungsten carbide grinding balls at a ball-to-powder ratio of 6:1. The grinding jar was evacuated for 10 minutes before ball milling. -1 Pa was introduced and argon gas was introduced. Finally, the mixture was ball-milled at 350 r / min for 2 h to obtain Mo-Ti pre-alloyed powder.

[0083] Step 3: Mix the Mo-Ta-Ce2O pre-alloy powder obtained in Step 1 with the Mo-Ti pre-alloy powder obtained in Step 2 under an argon atmosphere for 5 hours to obtain a homogeneous alloy powder.

[0084] Step 4: Pour the mixed alloy powder into the rubber sleeve and vibrate it to compact it. Then, seal the rubber sleeve tightly with a rubber stopper and place it into an isostatic pressing device. The holding pressure is 230 MPa and the holding time is 20 min to obtain a cold-pressed billet.

[0085] Step 5: Shape the cold-pressed blank, remove the burrs and flash from the surface, and obtain a regular geometric shape.

[0086] Step 6: Place the shaped cold-pressed billet into an intermediate frequency furnace and then perform multi-gradient reduction sintering on the cold-pressed billet. In the first stage, the temperature is increased to 960℃ at 10℃ / min and held for 5 hours. In the second stage, the temperature is increased to 1300℃ at 10℃ / min and held for 2 hours. In the third stage, the temperature is increased to 1390℃ at 6℃ / min and held for 6 hours. The entire sintering process is carried out in a hydrogen atmosphere with a hydrogen input rate of 200 ml / min. Finally, the sintered billet is obtained.

[0087] Step 7: Heat the sintered billet to 1200℃ to begin the first rolling pass. The second rolling pass temperature is controlled at 1200℃, and the final rolling pass temperature is 1050℃. The total rolling deformation is controlled at 45%, and the deformation per pass is controlled at 15%. Three rolling passes are performed. Before each rolling pass, the billet is held at 1050℃ for 1 hour to obtain the rolled piece.

[0088] Step 8: Machining the rolled piece, including leveling, surface polishing and dimensional adjustment, to obtain the rolled target material.

[0089] Step 9: Anneal the rolled target material at a temperature of 900℃, in an annealing atmosphere of H2, for 1 hour to obtain a Mo-Ti-Ta-Ce alloy target material.

[0090] The alloy target material prepared in this embodiment has high Ta and Ce content, an average grain size of about 42 μm, and good plastic deformation ability.

[0091] Comparative Example 1

[0092] This comparative example provides a Mo-Ti-Ta-Ce alloy target and its preparation process. The composition of the alloy target, in atomic percentage, includes Mo 63.94at%, Ti 30at%, Ta 6at%, and Ce 0.06at%.

[0093] Step 1: Weigh 15 at% Mo powder, 6 at% Ta powder, and 0.06 at% CeO2 powder, and mix them in a three-dimensional mixer purged with argon gas for 2.5 hours. Then, perform high-energy ball milling on the mixed powder, using 6mm diameter tungsten carbide grinding balls at a ball-to-powder ratio of 3:1. Before ball milling, evacuate the grinding jar to 10°C. -1Pa was introduced and argon gas was introduced. Finally, the mixture was ball-milled at 300 r / min for 2.5 h to obtain Mo-Ta-CeO2 pre-alloyed powder.

[0094] Step 2: 30 at% TiH2 powder and 48.94 at% Mo powder were loaded into a three-dimensional mixer purged with argon gas and mixed for 2 hours. The mixed powder was then subjected to high-energy ball milling using 6mm diameter tungsten carbide grinding balls at a ball-to-powder ratio of 1:1. The grinding jar was evacuated for 10 minutes before ball milling. -1 Pa was introduced and argon gas was introduced. Finally, the mixture was ball-milled at 300 r / min for 2.5 h to obtain Mo-Ti pre-alloyed powder.

[0095] Step 3: The Mo-Ta-CeO2 pre-alloy powder obtained in Step 1 and the Mo-Ti pre-alloy powder obtained in Step 2 are mixed under an argon atmosphere for 5 hours at a rotation speed of 28 r / min to obtain a homogeneous alloy powder.

[0096] Step 4: Pour the mixed alloy powder into the rubber sleeve and vibrate it to compact it. Then, seal the rubber sleeve tightly with a rubber stopper and place it into an isostatic pressing device. The holding pressure is 180 MPa and the holding time is 8 minutes to obtain a cold-pressed billet.

[0097] Step 5: Shape the cold-pressed blank, remove the burrs and flash from the surface, and obtain a regular geometric shape.

[0098] Step 6: Place the shaped cold-pressed billet into an intermediate frequency furnace and then perform multi-gradient reduction sintering on the cold-pressed billet. The first stage is held at 960℃ for 4 hours, the second stage is held at 1295℃ for 1.5 hours, and the third stage is held at 1370℃ for 5 hours. The entire sintering process is carried out in a hydrogen atmosphere with a hydrogen input rate of 200 ml / min. Finally, the sintered billet is obtained.

[0099] Step 7: Heat the sintered billet to 1300℃ to begin the first rolling pass. The second rolling pass temperature is controlled at 1200℃, and the final rolling pass temperature is 1100℃. The total rolling deformation is controlled at 45%, and the deformation per single pass is controlled at 15%. Three rolling passes are performed. Before each rolling pass, the billet is held at 1050℃ for 1 hour to obtain the rolled piece.

[0100] Step 8: Machining the rolled piece. First, use a leveling machine and polishing equipment to level and polish the rolled plate, and then use a cutting machine to trim the dimensions of the rolled piece to obtain the rolled target material.

[0101] Step 9: Anneal the rolled target material in H2 at a temperature of 900℃ and an annealing atmosphere of H2 for 1 hour to obtain the Mo-Ti-Ta-Ce alloy target material.

[0102] In the preparation of Mo-Ta-Ce pre-alloyed powder and Mo-Ti pre-alloyed powder using the alloy target provided in Comparative Example 1, the ball-to-material ratio in the ball milling process was reduced to 3:1 and 1:1, respectively; the rest was performed in accordance with Example 1.

[0103] In this comparative example, during the high-energy ball milling process for preparing the two pre-alloyed powders, the ball-to-material ratio was extremely low, and Ta and CeO2 could not be evenly distributed in the Mo powder, resulting in compositional segregation in many areas of the target material. The extremely low ball-to-material ratio provided insufficient energy during the ball milling process to allow Mo and Ti to combine, which was not conducive to the formation of Mo-Ti solid solution during sintering.

[0104] The average grain size of the alloy target prepared in this comparative example is approximately 67 μm.

[0105] Comparative Example 2

[0106] This comparative example provides a Mo-Ti-Ta-Ce alloy target and its preparation process. The composition of the alloy target, in atomic percentage, includes Mo 63.94at%, Ti 30at%, Ta 6at%, and Ce 0.06at%.

[0107] Step 1: Mix Mo powder, Ta powder, TiH2 powder and CeO2 under an argon atmosphere for 5 hours to obtain Mo-Ti-Ta-Ce powder.

[0108] Step 2: Pour Mo-Ti-Ta-Ce powder into the rubber sleeve and vibrate it to compact it. Then, seal the rubber sleeve tightly with a rubber stopper and place it into an isostatic pressing device. The holding pressure is 180 MPa and the holding time is 8 minutes to obtain a cold-pressed blank.

[0109] Step 3: Shape the cold-pressed blank to remove surface burrs and flash, and obtain a regular geometric shape.

[0110] Step 4: Place the shaped cold-pressed billet into an intermediate frequency furnace and then perform multi-gradient reduction sintering on the cold-pressed billet. The first stage is held at 960℃ for 4 hours, the second stage is held at 1295℃ for 1.5 hours, and the third stage is held at 1370℃ for 5 hours. The entire sintering process is carried out in a hydrogen atmosphere with a hydrogen input rate of 200 ml / min. Finally, the sintered billet is obtained.

[0111] Step 5: Heat the sintered billet to 1300℃ to begin the first rolling pass. The second rolling pass temperature is controlled at 1200℃, and the final rolling pass temperature is 1100℃. The total rolling deformation is controlled at 45%, and the deformation per pass is controlled at 15%. Three rolling passes are performed. Before each rolling pass, the billet is held at 1050℃ for 1 hour to obtain the rolled piece.

[0112] Step 6: Machining the rolled piece. First, use a leveling machine and polishing equipment to level and polish the rolled plate, and then use a cutting machine to trim the dimensions of the rolled piece to obtain the rolled target material.

[0113] Step 7: Anneal the rolled target material in H2 at a temperature of 900℃ and an annealing atmosphere of H2 for 1 hour to obtain the Mo-Ti-Ta-Ce alloy target material.

[0114] Comparative Example 3

[0115] This embodiment provides a Mo-Ti-Ta-Ce alloy target and its preparation process. The composition of the alloy target, in atomic percentage, includes Mo 63.94at%, Ti 30at%, Ta 6at%, and Ce 0.06at.

[0116] Step 1: 30 at% TiH2 powder and 48.94 at% Mo powder were loaded into a three-dimensional mixer purged with argon gas and mixed for 2 hours. The mixed powder was then subjected to high-energy ball milling using 6mm diameter tungsten carbide grinding balls at a ball-to-powder ratio of 3.5:1. The grinding jar was evacuated for 10 minutes before ball milling. -1 Pa was introduced and argon gas was introduced. Finally, the mixture was ball-milled at 300 r / min for 2.5 h to obtain Mo-Ti pre-alloyed powder.

[0117] Step 2: The Mo-Ti pre-alloy powder, Ta powder, CeO2 powder and the remaining Mo powder obtained in Step 1 are mixed under an argon atmosphere for 5 hours at a speed of 28 r / min to obtain a uniformly mixed alloy powder.

[0118] Step 3: Pour the mixed alloy powder into the rubber sleeve and vibrate it to compact it. Then, seal the rubber sleeve tightly with a rubber stopper and place it into an isostatic pressing device. The holding pressure is 180 MPa and the holding time is 8 minutes to obtain a cold-pressed billet.

[0119] Step 4: Shape the cold-pressed blank to remove surface burrs and flash, and obtain a regular geometric shape.

[0120] Step 5: Place the shaped cold-pressed billet into an intermediate frequency furnace and then perform multi-gradient reduction sintering on the cold-pressed billet. The first stage is held at 960℃ for 4 hours, the second stage is held at 1295℃ for 1.5 hours, and the third stage is held at 1370℃ for 5 hours. The entire sintering process is carried out in a hydrogen atmosphere with a hydrogen input rate of 200 ml / min. Finally, the sintered billet is obtained.

[0121] Step 6: Heat the sintered billet to 1300℃ to begin the first rolling pass. The second rolling pass temperature is controlled at 1200℃, and the final rolling pass temperature is 1100℃. The total rolling deformation is controlled at 45%, and the deformation per single pass is controlled at 15%. Three rolling passes are performed. Before each rolling pass, the billet is held at 1050℃ for 1 hour to obtain the rolled piece.

[0122] Step 7: Machining the rolled piece. First, use a leveling machine and polishing equipment to level and polish the rolled plate, and then use a cutting machine to trim the dimensions of the rolled piece to obtain the rolled target material.

[0123] Step 8: Anneal the rolled target material in H2 at a temperature of 900℃ for 1 hour to obtain the Mo-Ti-Ta-Ce alloy target material.

[0124] The average grain size of the alloy target prepared in this comparative example is approximately 66 μm.

[0125] Comparative Example 4

[0126] This comparative example provides a Mo-Ti-Ta-Ce alloy target and its preparation process. The composition of the alloy target, in atomic percentage, includes Mo 41.75at%, Ti 43at%, Ta 15at%, and Ce 0.25at%.

[0127] Step 1: Weigh 15 at% Mo powder, 6 at% Ta powder, and 0.06 at% CeO2 powder, and mix them in a three-dimensional mixer purged with argon gas for 2.5 hours. Then, perform high-energy ball milling on the mixed powder, using 6mm diameter tungsten carbide grinding balls at a ball-to-powder ratio of 5:1. Before ball milling, evacuate the grinding jar to 10°C. -1 Pa was introduced and argon gas was introduced. Finally, the mixture was ball-milled at 300 r / min for 2.5 h to obtain Mo-Ta-Ce2O pre-alloyed powder.

[0128] Step 2: 30 at% TiH2 powder and 48.94 at% Mo powder were loaded into a three-dimensional mixer filled with argon gas and mixed for 2 hours. The mixed powder was then subjected to high-energy ball milling using 6mm diameter tungsten carbide grinding balls at a ball-to-powder ratio of 3.5:1. The grinding jar was evacuated for 10 minutes before ball milling. -1 Pa was introduced and argon gas was introduced. Finally, the mixture was ball-milled at 300 r / min for 2.5 h to obtain Mo-Ti pre-alloyed powder.

[0129] Step 3: The Mo-Ta-Ce2O pre-alloy powder obtained in Step 1 and the Mo-Ti pre-alloy powder obtained in Step 2 are mixed under an argon atmosphere for 1.5 hours at a rotation speed of 28 r / min to obtain a homogeneous alloy powder.

[0130] Step 4: Pour the mixed alloy powder into the rubber sleeve and vibrate it to compact it. Then, seal the rubber sleeve tightly with a rubber stopper and place it into an isostatic pressing device. The holding pressure is 180 MPa and the holding time is 8 minutes to obtain a cold-pressed billet.

[0131] Step 5: Shape the cold-pressed blank, remove the burrs and flash from the surface, and obtain a regular geometric shape.

[0132] Step 6: Place the shaped cold-pressed billet into an intermediate frequency furnace and then perform multi-gradient reduction sintering on the cold-pressed billet. The first stage is held at 960℃ for 4 hours, the second stage is held at 1295℃ for 1.5 hours, and the third stage is held at 1370℃ for 5 hours. The entire sintering process is carried out in a hydrogen atmosphere with a hydrogen input rate of 200 ml / min. Finally, the sintered billet is obtained.

[0133] Step 7: Heat the sintered billet to 1300℃ to begin the first rolling pass. The second rolling pass temperature is controlled at 1200℃, and the final rolling pass temperature is 1100℃. The total rolling deformation is controlled at 45%, and the deformation per single pass is controlled at 15%. Three rolling passes are performed. Before each rolling pass, the billet is held at 1050℃ for 1 hour to obtain the rolled piece.

[0134] Step 8: Machining the rolled piece. First, use a leveling machine and polishing equipment to level and polish the rolled plate, and then use a cutting machine to trim the dimensions of the rolled piece to obtain the rolled target material.

[0135] Step 9: Anneal the rolled target material in H2 at a temperature of 900℃ for 1 hour to obtain the Mo-Ti-Ta-Ce alloy target material.

[0136] The average grain size of the alloy target prepared in this comparative example is approximately 29 μm.

[0137] The alloy targets prepared in the examples and comparative cases are used to perform film deposition using magnetron sputtering. The specific process is as follows:

[0138] Take a sample with an upper surface area of ​​2500 mm² from the finished target material. 2 Square samples were prepared; an alloy film was deposited on a 60mm × 60mm alkali-free glass substrate using a DC magnetron sputtering system. Before sputtering, the glass substrate was cleaned in an ultrasonic cleaner containing detergent for 15 minutes, followed by rinsing with acetone and anhydrous ethanol. Furthermore, the sputtering chamber was kept dry and cleaned before each sputtering operation, with a 0.1A magnetron current applied to the alloy target for 10 minutes under baffle protection. After cleaning, the glass substrate was heated to 120°C, argon gas was introduced into the sputtering chamber (maintaining an argon pressure of approximately 0.5 Pa), and then a vacuum of 5 × 10⁻⁶ Pa was applied. -3Pa; During film deposition, a rotary substrate holder (rotation speed of 25 rpm) was used with an incident angle of 30°, a deposition power of 100 W, and a deposition time of 15 min. The resistivity of the film was measured using a four-point probe resistivity meter to reflect its conductivity. The sample film was immersed in a 0.9% NaCl aqueous solution at room temperature, and the polarization (CV) curve was tested using an electrochemical analyzer to reflect its corrosion resistance. The sample film was placed in an environment of 85°C and 85% relative humidity, and the changes on the film surface caused by high temperature and high humidity were visually evaluated to reflect its oxidation resistance.

[0139] The thin film produced using the target material prepared in Example 1 has a resistivity of approximately 1.44 × 10⁻⁶. -7 Ω·cm; corrosion potential -0.2V; no oxidation corrosion after 540h exposure at 85℃ and 85%RH (relative humidity).

[0140] The thin film produced using the target material prepared in Example 2 has a resistivity of approximately 1.52 × 10⁻⁶. -7 Ω·cm; corrosion potential -0.3V; no oxidation corrosion after 530h exposure at 85℃ and 85%RH (relative humidity).

[0141] The thin film produced using the target material prepared in Example 3 has a resistivity of approximately 1.60 × 10⁻⁶. -7 Ω·cm; corrosion potential -0.33V; no oxidation corrosion after 500h exposure at 85℃ and 85%RH (relative humidity).

[0142] The thin film produced using the target material prepared in Example 4 has a resistivity of 1.88 × 10⁻⁶. -7 Ω·cm; corrosion potential -0.28V; no oxidation corrosion after 550h exposure at 85℃ and 85%RH (relative humidity).

[0143] The thin film produced using the target material prepared in Comparative Example 1 has a resistivity of 1.79 × 10⁻⁶. -7 Ω·cm; corrosion potential -0.23V; no oxidation corrosion after 520h exposure at 85℃ and 85%RH (relative humidity). Compared with the alloy target material prepared in Example 1, the alloy target material prepared in Comparative Example 1 has uneven composition and properties of sputtered alloy films due to multi-regional compositional segregation, resulting in a higher overall resistivity of the film; the lower ball-to-material ratio means that the energy generated by the grinding balls cannot achieve the effect of powder mechanical alloying, resulting in insufficient bonding of Mo and Ti, and also insufficient bonding of Mo, Ta, and Ce; in addition, the compositional and property segregation leads to a lower overall corrosion resistance and oxidation resistance of the alloy film.

[0144] Comparative Example 2 did not pre-prepare Mo-Ta-Ce and Mo-Ti pre-alloyed powders. Due to the large differences in specific gravity between the elements and their raw materials, this method cannot form alloy powders with uniform distribution of each element, and it affects the bonding of the MoTi matrix. Moreover, Ta and Ce cannot be tightly bonded with Mo and Ti during ball milling, resulting in severe micro-region segregation in the microstructure and composition of the produced alloy target material. Furthermore, the prepared target material has low density and a large number of pores in the matrix microstructure, making it impossible to use it for sputtering deposition of barrier layer films.

[0145] The thin film produced using the target material prepared in Comparative Example 3 has a resistivity of 1.86 × 10⁻⁶. -7 Ω·cm; corrosion potential -0.31V; no oxidation corrosion after 440h exposure at 85℃ and 85%RH (relative humidity). Compared with the alloy target prepared in Example 1, Comparative Example 3 did not prepare Mo-Ta-Ce pre-alloy powder, which resulted in the Ta powder and CeO2 powder not being uniformly distributed in the mixed powder. That is, Ta and Ce would aggregate and segregate in specific areas of the Mo-Ti matrix, which would prevent the synergistic effect mechanism of several alloying elements from being fully utilized. As a result, the conductivity, corrosion resistance and oxidation resistance of the target and its sputtered film could not be effectively improved.

[0146] The thin film produced using the target material prepared in Comparative Example 4 has a resistivity of 2.91 × 10⁻⁶. -7 Ω·cm; corrosion potential -0.23V; no oxidation corrosion after 520h exposure at 85℃ and 85%RH (relative humidity). Comparative Example 4 investigated the effects of excessive alloying elements on the target and film. Due to the excessive addition of Ta and CeO2, the grains of the alloy target were refined to an extremely strong degree, resulting in a grain boundary density exceeding the normal range, which led to excessively high resistivity of the target and its sputtered film. In addition, the excessively fine grains affected the sputtering efficiency of the target, resulting in a slow film deposition rate.

[0147] Although preferred embodiments of the invention have been described, those skilled in the art, upon learning the basic inventive concept, can make other changes and modifications to these embodiments. Therefore, the appended claims are intended to be interpreted as including both the preferred embodiments and all changes and modifications falling within the scope of the invention.

[0148] Obviously, those skilled in the art can make various modifications and variations to this invention without departing from its spirit and scope. Therefore, if these modifications and variations fall within the scope of the claims of this invention and their equivalents, this invention also intends to include these modifications and variations.

Claims

1. A method for preparing a Mo-Ti-Ta-Ce alloy target, characterized in that, Includes the following steps: According to the atomic percentage of each element in the Mo-Ti-Ta-Ce alloy target, the raw materials are weighed as follows: 20%~40%Ti, 5%~12%Ta and 0.05%~0.12%Ce, with the balance being Mo and unavoidable impurities, Mo≥45%, totaling 100%. Under inert gas protection, Ta powder, CeO2 powder, and Mo powder are weighed according to 5%~12%Ta, 0.05%~0.12%Ce, and 15%~21%Mo, and mixed evenly to obtain a first mixed powder. The first mixed powder is then subjected to a first ball milling treatment to obtain Mo-Ta-CeO2 pre-alloyed powder. In the first ball milling treatment, the ball-to-material ratio is 5~10:

1. Under inert gas protection, TiH2 powder with 20%~40% Ti was weighed and mixed evenly with the remaining Mo powder to obtain a second mixed powder. The second mixed powder was then subjected to a second ball milling process to obtain Mo-Ti pre-alloyed powder. In the second ball milling process, the ball-to-material ratio was 2~6:

1. Under inert gas protection, Mo-Ta-CeO2 pre-alloy powder and Mo-Ti pre-alloy powder are mixed in batches. After being mixed evenly, they are cold isostatically pressed to obtain a cold-pressed billet. The cold-pressed green body is sintered in a reducing atmosphere to obtain a sintered green body. The sintered billet is rolled to obtain the rolled target material; the rolled target material is annealed at 900℃~1050℃ in a reducing atmosphere to obtain the Mo-Ti-Ta-Ce alloy target material.

2. The method for preparing a Mo-Ti-Ta-Ce alloy target according to claim 1, characterized in that, In the first ball milling process, the ball milling time is 1.5h to 3h.

3. The method for preparing a Mo-Ti-Ta-Ce alloy target according to claim 1, characterized in that, In the second ball milling process, the ball milling time is 2h~4h.

4. The method for preparing a Mo-Ti-Ta-Ce alloy target according to claim 1, characterized in that, When mixing Mo-Ta-CeO2 pre-alloyed powder and Mo-Ti pre-alloyed powder, a three-dimensional mixer is used, and the mixing time is 4h~5h.

5. The method for preparing a Mo-Ti-Ta-Ce alloy target according to claim 1, characterized in that, In cold isostatic pressing, the pressure is 150MPa~250MPa and the holding time is 6min~20min.

6. The method for preparing a Mo-Ti-Ta-Ce alloy target according to claim 1, characterized in that, During the sintering process, the first stage heating rate was set to 10℃ / min, and the temperature was raised to 950℃~1100℃ and held for 3.5~5h; the second stage heating rate was set to 10℃ / min, and the temperature was raised to 1290℃~1310℃ and held for 1h~2h; the third stage heating rate was set to 5℃~8℃ / min, and the temperature was raised to 1350℃~1450℃ and held for 4h~6h.

7. The method for preparing a Mo-Ti-Ta-Ce alloy target according to claim 1, characterized in that, During the rolling process, the initial rolling temperature is 1150℃~1400℃, and the final rolling temperature is 1000℃~1200℃; the total rolling deformation is controlled at 45%, and the single-pass rolling deformation is controlled at 15%~25%; the hot rolling process is preheated to 1050℃~1100℃ before each pass, and the preheating time is 0.5h~1h.

8. The method for preparing a Mo-Ti-Ta-Ce alloy target according to claim 1, characterized in that, Annealing time is 1 to 2 hours.

9. A Mo-Ti-Ta-Ce alloy target prepared by the preparation method according to any one of claims 1 to 8.

10. The application of the Mo-Ti-Ta-Ce alloy target as described in claim 9 in the preparation of thin films by magnetron sputtering.

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