Alpha phase tungsten-molybdenum alloy thin film and method of making same

Abstract

The application discloses a preparation method of an alpha-phase tungsten-molybdenum alloy film, and specific steps are as follows: step 1: depositing W x Mo 1‑x alloy layers on a substrate by a magnetron sputtering method simultaneously, wherein 0.2<=x<=0.8; step 2: annealing: annealing the sample after the deposition of the W x Mo 1‑x alloy layers is finished. The application further discloses the alpha-phase tungsten-molybdenum alloy film prepared by the method, which is in an alpha phase and has good thermal stability.

Description

Technical Field

[0001] This invention belongs to the technical field of tungsten-molybdenum alloy thin film materials, specifically relating to alpha-phase tungsten-molybdenum alloy thin films, and also to a method for preparing alpha-phase tungsten-molybdenum alloy thin films. Background Technology

[0002] Tungsten-molybdenum alloys are important high-temperature materials with excellent high-temperature strength, oxidation resistance, and wear resistance, as well as good corrosion resistance. Therefore, they are widely used in aerospace, defense, and high-temperature industrial fields. With the miniaturization of devices, the demand for high-quality tungsten-molybdenum alloy thin films is becoming increasingly urgent. Furthermore, to meet the needs of different fields, it is necessary to adjust the tungsten-molybdenum ratio and optimize its performance. Due to the complex phase structure of tungsten, which includes alpha and beta phases, and the fact that beta tungsten is a metastable phase with poor thermal stability, it will transform into alpha tungsten under certain film thicknesses and temperatures. Therefore, high-quality tungsten-molybdenum alloys with tunable alpha phase composition are more valuable for applications. Summary of the Invention

[0003] The first objective of this invention is to provide a method for preparing alpha-phase tungsten-molybdenum alloy thin films. This invention achieves the preparation of alpha-phase tungsten-molybdenum alloy thin films by co-sputtering tungsten and molybdenum and then by vacuum annealing.

[0004] A second objective of this invention is to provide an alpha-phase tungsten-molybdenum alloy thin film, which is in the alpha phase and has good thermal stability.

[0005] The first technical solution adopted in this invention is a method for preparing alpha-phase tungsten-molybdenum alloy thin films, the specific steps of which are as follows: Step 1: Simultaneously deposit W on the substrate using magnetron sputtering x Mo 1-x Alloy layer, where 0.2 ≤ x ≤ 0.8; Step 2: Annealing: In W x Mo 1-x After the alloy layer deposition is completed, the sample is annealed.

[0006] The invention is further characterized in that: In step 1, the substrate is a Si substrate, a SiO2 substrate, or a Si substrate with a pre-printed pattern.

[0007] In step 1, W in the alpha phase tungsten-molybdenum alloy thin film x Mo 1-x The alloy layer was deposited using a magnetron sputtering system with an argon atmosphere and an argon flow rate of 18 sccm-36 sccm.

[0008] In step 1, a magnetron sputtering system is used to simultaneously deposit W and Mo on the substrate; the sputtering power of the W target is 20W-60W, and the sputtering power of the Mo target is 13W-60W; the sputtering time is 128s-300s.

[0009] The substrate rotation speed in the magnetron sputtering system is 5 rpm to 20 rpm.

[0010] In step 2, the annealing temperature is 500℃-700℃. In step 2, the annealing time is 0.5h-2h.

[0011] The second technical solution adopted in this invention is an alpha phase tungsten-molybdenum alloy thin film, which is prepared by the above method.

[0012] The beneficial effects of this invention are: Since beta-phase tungsten-molybdenum alloys experience significantly increased stress accumulation at high temperatures, leading to increased thermodynamic instability, the method of this invention restructures the tungsten-molybdenum alloy into a stable alpha-phase tungsten-molybdenum alloy, resulting in an alpha-phase tungsten-molybdenum alloy film with good thermal stability. Attached Figure Description

[0013] Figure 1 This is a schematic diagram of the structure of the alpha phase tungsten-molybdenum alloy thin film of the present invention; Figure 2 The [W] obtained in Example 1 was annealed at 600°C for 1 hour. 0.8 Mo 0.2 XRD of alloy thin films; Figure 3 The [W] obtained in Example 2 after annealing at 600°C for 1 hour 0.6 Mo 0.4 XRD of alloy thin films; Figure 4 The [W] obtained in Example 3 after annealing at 600°C for 1 hour 0.5 Mo 0.5 XRD of alloy thin films; Figure 5 The [W] obtained in Example 4 after annealing at 600°C for 1 hour 0.4 Mo 0.6 XRD of alloy thin films; Figure 6 The [W] obtained in Example 5 after annealing at 600°C for 1 hour 0.2 Mo 0.8 XRD of alloy thin films; Figure 7 The [W] obtained in Example 6 after annealing at 500°C for 1 hour 0.5 Mo 0.5 XRD of alloy thin films; Figure 8 The [W] obtained in Example 7 after annealing at 700°C for 1 hour 0.5 Mo 0.5 XRD of alloy thin films.

[0014] In the figure, 1. substrate, 2. W x Mo 1-x Alloy layer. Detailed Implementation

[0015] The present invention will now be described in detail with reference to the accompanying drawings and specific embodiments.

[0016] This invention provides a method for preparing alpha-phase tungsten-molybdenum alloy thin films, the specific steps of which are as follows: Step 1: Simultaneously deposit W on substrate 1 using magnetron sputtering x Mo 1-x Alloy layer 2, where 0.2 ≤ x ≤ 0.8; In step 1, substrate 1 is a Si substrate, a SiO2 substrate, or a Si substrate with a pre-printed pattern.

[0017] In step 1, W in the alpha phase tungsten-molybdenum alloy thin film x Mo 1-x The deposition of alloy layer 2 was prepared using a magnetron sputtering system with an argon atmosphere and an argon flow rate of 18 sccm-36 sccm.

[0018] In step 1, a magnetron sputtering system is used to simultaneously deposit W and Mo on the substrate; the sputtering power of the W target is 20W-60W, and the sputtering power of the Mo target is 13W-60W. Sputtering time is 128s-300s.

[0019] The substrate rotation speed in the magnetron sputtering system is 5 rpm-20 rpm.

[0020] Step 2: Annealing: In W x Mo 1-x After the deposition of alloy layer 2 is completed, the sample is annealed.

[0021] In step 2, the annealing temperature is 500℃-700℃. In step 2, the annealing time is 0.5h-2h.

[0022] This invention also provides alpha-phase tungsten-molybdenum alloy thin films, such as... Figure 1 As shown, W is arranged sequentially from top to bottom. x Mo 1-x Alloy layer 2 and substrate 1 were prepared using the method described above.

[0023] The specifications of the instruments used in all the following embodiments are as follows: Magnetron sputtering system: Brand: Kurt J.Lesker, Model: PVD 75 Proline.

[0024] Vacuum annealing furnace: Brand: Dongfang Chenjing; Model: High-temperature magnetic field heating furnace.

[0025] Multifunctional X-ray diffractometer: Brand: Rigaku, Japan; Model: Smartlab SE.

[0026] Example 1: A method for preparing tungsten-molybdenum alloy thin films with alpha phase, W x Mo 1-x In alloy layer 2, the content of W is 80% and the content of Mo is 20% by atomic percentage. W and Mo are deposited simultaneously on substrate 1 (substrate 1 is a Si substrate) using DC magnetron sputtering to obtain W. x Mo 1-x Alloy layer 2.

[0027] W in alpha phase tungsten-molybdenum alloy thin films x Mo 1-x The deposition of alloy layer 2 was prepared using a magnetron sputtering system with an argon atmosphere and an argon flow rate of 18 sccm.

[0028] W and Mo were deposited simultaneously on a substrate using a magnetron sputtering system. In this embodiment, the sputtering power of the W target was 60 W, and the sputtering power of the Mo target was 13 W. The sputtering time was 300 s, and the substrate rotation speed of the magnetron sputtering system was 10 rpm.

[0029] After deposition, the sample was placed in a vacuum annealing furnace for in-situ annealing at a temperature of 600℃ for 1 hour. The alloy layer was 16 nm thick, with a W content of 80% and a Mo content of 20%.

[0030] XRD is used to measure the crystal structure of a sample, such as... Figure 2 As shown, the sample annealed at 600℃ exhibits a tungsten-molybdenum alloy with an alpha phase structure.

[0031] Example 2: A method for preparing tungsten-molybdenum alloy thin films with alpha phase, W x Mo 1-x In alloy layer 2, the content of W is 60% and the content of Mo is 40% by atomic percentage. W and Mo are deposited simultaneously on substrate 1 (substrate 1 is a Si substrate) using DC magnetron sputtering to obtain W. x Mo 1-x Alloy layer 2.

[0032] W in alpha phase tungsten-molybdenum alloy thin films x Mo 1-x The deposition of alloy layer 2 was prepared using a magnetron sputtering system with an argon atmosphere and an argon flow rate of 36 sccm.

[0033] W and Mo were deposited simultaneously on a substrate using a magnetron sputtering system. In this embodiment, the sputtering power of the W target was 60 W, and the sputtering power of the Mo target was 19 W. The sputtering time was 226 s, the sputtering pressure was 23 sccm, and the substrate rotation speed of the magnetron sputtering system was 10 rpm.

[0034] After deposition, the sample was placed in a vacuum annealing furnace for in-situ annealing at a temperature of 600℃ for 1 hour. The alloy layer was 16 nm thick, with a W content of 60% and a Mo content of 40%.

[0035] XRD is used to measure the crystal structure of a sample, such as... Figure 3 As shown, the sample annealed at 600℃ exhibits a tungsten-molybdenum alloy with an alpha phase structure.

[0036] Example 3: A method for preparing tungsten-molybdenum alloy thin films with alpha phase, W x Mo 1-x In alloy layer 2, the content of W is 50% and the content of Mo is 50% by atomic percentage. W and Mo are deposited simultaneously on substrate 1 (substrate 1 is a Si substrate) using DC magnetron sputtering to obtain W. x Mo 1-x Alloy layer 2.

[0037] W in alpha phase tungsten-molybdenum alloy thin films x Mo 1-x The deposition of alloy layer 2 was prepared using a magnetron sputtering system with an argon atmosphere and an argon flow rate of 30 sccm.

[0038] W and Mo were deposited simultaneously on a substrate using a magnetron sputtering system. In this embodiment, the sputtering power of the W target was 60 W, and the sputtering power of the Mo target was 40 W. The sputtering time was 158 s, and the substrate rotation speed of the magnetron sputtering system was 10 rpm.

[0039] After deposition, the sample was placed in a vacuum annealing furnace for in-situ annealing at a temperature of 600℃ for 1 hour. The alloy layer was 16 nm thick with 50% W and 50% Mo.

[0040] XRD is used to measure the crystal structure of a sample, such as... Figure 4 As shown, the sample annealed at 600℃ exhibits a tungsten-molybdenum alloy with an alpha phase structure.

[0041] Example 4: A method for preparing tungsten-molybdenum alloy thin films with alpha phase, W x Mo 1-x In alloy layer 2, the content of W is 40% and the content of Mo is 60% by atomic percentage. W and Mo are deposited simultaneously on substrate 1 (substrate 1 is a Si substrate) using DC magnetron sputtering to obtain W. x Mo 1-x Alloy layer 2.

[0042] W in alpha phase tungsten-molybdenum alloy thin films x Mo 1-x The deposition of alloy layer 2 was prepared using a magnetron sputtering system with an argon atmosphere and an argon flow rate of 25 sccm.

[0043] W and Mo were deposited simultaneously on a substrate using a magnetron sputtering system. In this embodiment, the sputtering power of the W target was 65 W, and the sputtering power of the Mo target was 60 W. The sputtering time was 128 s, and the substrate rotation speed of the magnetron sputtering system was 10 rpm.

[0044] After deposition, the sample was placed in a vacuum annealing furnace for in-situ annealing at a temperature of 600℃ for 1 hour. The alloy layer was 16 nm thick, with a W content of 40% and a Mo content of 60%.

[0045] XRD is used to measure the crystal structure of a sample, such as... Figure 5 As shown, the sample annealed at 600℃ exhibits a tungsten-molybdenum alloy with an alpha phase structure.

[0046] Example 5: A method for preparing tungsten-molybdenum alloy thin films with alpha phase, W x Mo 1-x In alloy layer 2, the content of W is 20% and the content of Mo is 80% by atomic percentage. W and Mo are deposited simultaneously on substrate 1 (substrate 1 is a Si substrate) using DC magnetron sputtering to obtain W. x Mo 1-x Alloy layer 2.

[0047] W in alpha phase tungsten-molybdenum alloy thin films x Mo 1-x The deposition of alloy layer 2 was prepared using a magnetron sputtering system with an argon atmosphere and an argon flow rate of 20 sccm.

[0048] W and Mo were deposited simultaneously on a substrate using a magnetron sputtering system. In this embodiment, the sputtering power of the W target was 20 W, and the sputtering power of the Mo target was 60 W. The sputtering time was 172 s, and the substrate rotation speed of the magnetron sputtering system was 10 rpm.

[0049] After deposition, the sample was placed in a vacuum annealing furnace for in-situ annealing at a temperature of 600℃ for 1 hour. The alloy layer was 16 nm thick, with a W content of 20% and a Mo content of 80%.

[0050] XRD is used to measure the crystal structure of a sample, such as... Figure 6 As shown, the sample annealed at 600℃ exhibits a tungsten-molybdenum alloy with an alpha phase structure.

[0051] Example 6: A method for preparing tungsten-molybdenum alloy thin films with alpha phase, W x Mo 1-x In alloy layer 2, the content of W is 50% and the content of Mo is 50% by atomic percentage. W and Mo are deposited simultaneously on substrate 1 (substrate 1 is a SiO2 substrate) using DC magnetron sputtering to obtain W. x Mo 1-x Alloy layer 2.

[0052] In this embodiment, the sputtering power of the W target is 60W, and the sputtering power of the Mo target is 40W. The sputtering time is 158s, and the substrate rotation speed of the magnetron sputtering system is 10rpm.

[0053] W in alpha phase tungsten-molybdenum alloy thin films x Mo 1-x Alloy layer 2 was deposited using a magnetron sputtering system with an argon atmosphere and a flow rate of 19 sccm. W and Mo were simultaneously deposited on the substrate using a magnetron sputtering system. After deposition, the sample was placed in a vacuum annealing furnace for in-situ annealing at a temperature of 500°C for 1 hour. The alloy layer was 16 nm thick and contained 50% W and 50% Mo.

[0054] XRD is used to measure the crystal structure of a sample, such as... Figure 7 As shown, the sample annealed at 500℃ exhibits a tungsten-molybdenum alloy with an alpha phase structure.

[0055] Example 7: A method for preparing tungsten-molybdenum alloy thin films with alpha phase, W x Mo 1-x In alloy layer 2, the content of W is 50% and the content of Mo is 50% by atomic percentage. W and Mo are deposited simultaneously on substrate 1 (substrate 1 is a SiO2 substrate) using DC magnetron sputtering to obtain W. x Mo 1-x Alloy layer 2.

[0056] W in alpha phase tungsten-molybdenum alloy thin films x Mo1-x The deposition of alloy layer 2 was prepared using a magnetron sputtering system with an argon atmosphere and an argon flow rate of 33 sccm.

[0057] W and Mo were deposited simultaneously on a substrate using a magnetron sputtering system. In this embodiment, the sputtering power of the W target was 60 W, and the sputtering power of the Mo target was 40 W. The sputtering time was 158 s, and the substrate rotation speed of the magnetron sputtering system was 10 rpm.

[0058] After deposition, the sample was placed in a vacuum annealing furnace for in-situ annealing at 700℃ for 1 hour. The alloy layer had a thickness of 16 nm, a W content of 50%, and a Mo content of 50%.

[0059] XRD is used to measure the crystal structure of a sample, such as... Figure 8 As shown, the sample annealed at 700℃ exhibits a tungsten-molybdenum alloy with an alpha phase structure.

Claims

1. A method for preparing alpha-phase tungsten-molybdenum alloy thin films, characterized in that, The specific steps are as follows: Step 1: Simultaneously deposit W on substrate (1) by magnetron sputtering x Mo 1-x Alloy layer (2), where 0.2≤x≤0.8; In step 1, W and Mo are deposited simultaneously on substrate (1) using a magnetron sputtering system; the sputtering power of the W target is 20W-65W, and the sputtering power of the Mo target is 13W-60W; the sputtering time is 128s-300s; the substrate rotation speed in the magnetron sputtering system is 5rpm-20rpm. Step 2: Annealing: In W x Mo 1-x After the alloy layer (2) is deposited, the sample is annealed. In step 2, the annealing temperature is 500℃-700℃; In step 2, the annealing time is 0.5h-2h; In step 2, the annealing environment is annealing under vacuum conditions.

2. The method for preparing alpha-phase tungsten-molybdenum alloy thin films according to claim 1, characterized in that, In step 1, the substrate (1) is a Si substrate, a SiO2 substrate, or a Si substrate with a pre-printed pattern.

3. The method for preparing alpha-phase tungsten-molybdenum alloy thin films according to claim 2, characterized in that, In step 1, W in the alpha phase tungsten-molybdenum alloy thin film x Mo 1-x The deposition of the alloy layer (2) was prepared by a magnetron sputtering system with argon gas in the sputtering atmosphere and an argon gas flow rate of 18 sccm-36 sccm.

4. An alpha-phase tungsten-molybdenum alloy thin film, characterized in that, It is prepared by the method described in any one of claims 1-3.

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