Process method for preparing silver gray by using planar target sputtering coating machine

Abstract

The invention relates to the technical field of PVD (Physical Vapor Deposition) coating, in particular to a process method for preparing silver gray by a planar target sputtering coating machine, which comprises the following steps of: placing a base material in a vacuum chamber, introducing argon, and bombarding the surface of the base material by using an ion beam; starting the Cr target, adjusting the current and bias voltage of the Cr target, and forming a base layer on the surface of the substrate; introducing nitrogen, opening the Si target, and forming an intermediate layer on the surface of the base layer; the nitrogen flow is adjusted, the current and bias voltage of the Cr target and the Si target are adjusted, and a transition layer is formed on the surface of the middle layer; and closing the nitrogen, adjusting the current and bias voltage of the Cr target and the Si target, and forming a silver gray color layer on the surface of the transition layer. According to the process method for preparing the silver gray through the planar target sputtering coating machine, the bottom layer, the middle layer, the transition layer and the color layer are sequentially plated on the surface of the base material, through the structural design of the multi-layer film and accurate process parameter control, preparation of the high-performance silver gray PVD film layer is achieved, and the binding force and the abrasion resistance of the PVD film layer are improved.

Description

Technical Field

[0001] The invention relates to the technical field of PVD coating, in particular to a process method for preparing silver-gray film using a planar target sputtering coating machine. Background Art

[0002] Physical vapor deposition (PVD) technology is a technology that converts solid or liquid materials into gaseous atoms, molecules or ions through physical means in a vacuum environment and deposits them on the surface of the substrate to form a thin film.

[0003] With the widespread application of PVD technology in the field of surface coating, especially in the field of smart wearables, PVD treatment is used on the surface to achieve different colors to enhance the aesthetics. Nowadays, many electronic product components and workpieces are coated with coating technology, which is very popular among consumers.

[0004] However, the film layer prepared by the existing coating technology is easily scratched when it comes into contact with external objects, and the film layer is easily peeled off from the damaged area, resulting in loss of gloss. Summary of the Invention

[0005] In order to solve the problems existing in the prior art, the present invention provides a process method for preparing silver-gray film using a planar target sputtering coating machine, aiming to improve the bonding strength and wear resistance of the film layer. To achieve the above-mentioned purpose, the present invention provides a process method for preparing silver-gray film using a planar target sputtering coating machine, comprising the following steps: S1. Place the substrate in the vacuum chamber of the vacuum coating magnetron sputtering equipment and evacuate the chamber to a vacuum degree of 6.0×10 -3 Pa, continue to introduce argon gas, adjust the argon gas flow rate to make the gas pressure reach the predetermined value, turn on the bias power supply, and bombard the substrate surface with ion beam to complete the pretreatment; S2. Adjust the argon flow rate to maintain the vacuum chamber pressure at 0.3-0.5 Pa, turn on the Cr target, adjust the Cr target current to 6-10 A, and control the negative bias voltage at 100-200 V to form a base layer on the substrate surface; S3. Nitrogen is introduced, the Si target is turned on, and its current is adjusted to 6-10A. The current of the Cr target is controlled at 6-10A, and the negative bias voltage is controlled at 100-200V to form an intermediate layer on the surface of the base layer; S4. Adjust the nitrogen flow rate, control the negative bias voltage at 30-100 V, control the Cr target current at 6-10 A, and adjust the Si target current to 6-10 A to form a transition layer on the surface of the intermediate layer; S5. Turn off the nitrogen, adjust the Cr target current to 0.5-1A, adjust the Si target current to 8-10A, control the negative bias voltage to 30-100V, and form a silver-gray color layer on the surface of the transition layer.

[0006] Preferably, in step S1, the argon flow rate is set to 30-50 sccm, and the dynamic equilibrium pressure is maintained at 0.5-1 Pa.

[0007] Preferably, in step S3, the nitrogen flow rate is set to 30-50 sccm and the vacuum chamber pressure is maintained at 0.25-0.5 Pa.

[0008] Preferably, in step S4, the nitrogen flow rate is set to 55-65 sccm, and the vacuum chamber pressure is maintained at 0.3-0.5 Pa.

[0009] Preferably, the thickness of the primer layer is 0.3 to 0.5 μm.

[0010] Preferably, the thickness of the intermediate layer is 0.8 to 1.2 μm.

[0011] Preferably, the thickness of the transition layer is 0.5-1 μm.

[0012] Preferably, the thickness of the color layer is 0.5-1 μm.

[0013] After adopting the above technical solution, the beneficial effects of the present invention are: The flat target sputtering coating machine is used to prepare the silver-gray process method, and the base layer, intermediate layer, transition layer and color layer are plated on the surface of the substrate in sequence. Through the multi-layer film structure design and precise process parameter control, the preparation of high-performance silver-gray PVD film layer is achieved, and the bonding strength and wear resistance of the PVD film layer are improved. DETAILED DESCRIPTION

[0014] The features and exemplary embodiments of various aspects of the present invention will be described in detail below. In order to make the objects, technical solutions and advantages of the present invention clearer, the present invention will be further described in detail below in conjunction with specific embodiments. It should be understood that the specific embodiments described herein are only configured to explain the present invention and are not configured to limit the present invention. For those skilled in the art, the present invention can be implemented without the need for some of these specific details. The following description of the embodiments is merely to provide a better understanding of the present invention by illustrating examples of the present invention.

[0015] Example 1 This example utilizes a planar target sputtering coating machine to produce a silver-gray coating. A base layer, intermediate layer, transition layer, and color layer are sequentially deposited onto a substrate. Through multilayer film structure design and precise process parameter control, a high-performance silver-gray PVD film is produced. The following is a detailed analysis and key technical points of this method.

[0016] Step 1: Ion bombardment pretreatment Prepare the vacuum coating magnetron sputtering equipment and fix the cleaned and dried substrate on the workpiece holder in the vacuum chamber. Start the vacuum pump and pump the vacuum chamber pressure to 6.0×10 -3 Pa, reducing collisions between residual gas molecules and sputtered particles. Argon gas was introduced into the vacuum chamber at a flow rate of 30 sccm. The vacuum pump speed was matched to the gas flow rate to maintain a dynamic equilibrium pressure of 0.5 Pa. The sputtering current was controlled at 0.5 A, and a pulsed bias was switched to a 60% duty cycle (300 V negative bias applied 60% of the time, zero voltage applied 40% of the time). The substrate was bombarded continuously for 20 minutes to remove surface contaminants or oxide layers.

[0017] Step 2: Base deposition The argon flow rate was set to 40 sccm, the vacuum chamber pressure was maintained at 0.3 Pa, the Cr target was turned on, the Cr target current was controlled at 10 A, the negative bias voltage was controlled at 200 V, and a Cr base layer with a film thickness of 0.3 μm was obtained.

[0018] Step 3: Intermediate layer deposition Nitrogen gas was introduced with a nitrogen flow rate controlled at 30 sccm, the vacuum chamber pressure was maintained at 0.25 Pa, the Si target was turned on and the current was adjusted to 6 A, the current of the Cr target was controlled at 6 A, the negative bias voltage was controlled at 100 V, and a CrSiN intermediate layer with a thickness of 1.2 μm was formed on the surface of the Cr base layer.

[0019] Step 4: Transition layer deposition The nitrogen flow rate was set to 55 sccm, the vacuum chamber pressure was maintained at 0.3 Pa, the Cr target current was set to 6 A, the Si target current was adjusted to 6 A, the negative bias voltage was controlled at 30 V, and a SiCrN transition layer with a film thickness of 1 μm was formed on the CrSiN intermediate layer.

[0020] The SiCrN transition layer, formed through the synergistic reaction of Cr / Si target sputtering and nitrogen gas, forms a multiphase composite structure. This plays a key role in connecting the upper and lower layers in terms of mechanical properties and thermal stability, primarily addressing the chemical and physical compatibility issues between adjacent layers. By adjusting the Si / Cr ratio, a gradient nitride structure is formed, reducing the lattice mismatch with the intermediate layer while also minimizing interface defects and stress concentration.

[0021] Step 5: Color layer deposition The nitrogen gas was turned off, the vacuum chamber pressure was maintained at 0.3 Pa, the Cr target current was adjusted to 0.5 A, the Si target current was adjusted to 8 A, and the negative bias voltage was controlled at 30 V to form a silver-gray film layer with a thickness of 1 μm.

[0022] The high refractive index of Si combined with the metallic reflective properties of Cr enhances the balanced reflection of visible light across the entire band through the interference effect, avoiding the dominance of a single wavelength and presenting a stable silver-gray tone.

[0023] Example 2 Step 1: Ion bombardment pretreatment Prepare the vacuum coating magnetron sputtering equipment and fix the cleaned and dried substrate on the workpiece holder in the vacuum chamber. Start the vacuum pump and pump the vacuum chamber pressure to 6.0×10 -3 Pa, reducing collisions between residual gas molecules and sputtered particles. Argon gas was introduced into the vacuum chamber at a flow rate of 45 sccm. The vacuum pump speed was matched to the gas flow rate to maintain a dynamic equilibrium pressure of 0.8 Pa. The sputtering current was controlled at 1 A, and a pulsed bias was switched to a 60% duty cycle (300 V negative bias applied 60% of the time, zero voltage applied 40% of the time). The substrate was bombarded continuously for 15 minutes to remove surface contaminants or oxide layers.

[0024] Step 2: Base deposition The argon flow rate was set to 45 sccm, the vacuum chamber pressure was maintained at 0.4 Pa, the Cr target was turned on, the Cr target current was controlled at 6 A, the negative bias voltage was controlled at 100 V, and a Cr base layer with a film thickness of 0.35 μm was obtained.

[0025] Step 3: Intermediate layer deposition Nitrogen gas was introduced with a nitrogen flow rate controlled at 35 sccm, the vacuum chamber pressure was maintained at 0.3 Pa, the Si target was turned on and the current was adjusted to 8 A, the current of the Cr target was controlled at 8 A, the negative bias voltage was controlled at 120 V, and a CrSiN intermediate layer with a thickness of 1 μm was formed on the surface of the Cr base layer.

[0026] Step 4: Transition layer deposition The nitrogen flow rate was set to 60 sccm, the vacuum chamber pressure was maintained at 0.35 Pa, the Cr target current was set to 8 A, the Si target current was adjusted to 8 A, the negative bias voltage was controlled at 50 V, and a SiCrN transition layer with a film thickness of 0.8 μm was formed on the CrSiN intermediate layer.

[0027] Step 5: Color layer deposition The nitrogen gas was turned off, the vacuum chamber pressure was maintained at 0.35 Pa, the Cr target current was adjusted to 0.55 A, the Si target current was adjusted to 8.5 A, and the negative bias voltage was controlled at 50 V to form a silver-gray film layer with a thickness of 0.8 μm.

[0028] Example 3 Step 1: Ion bombardment pretreatment Prepare the vacuum coating magnetron sputtering equipment and fix the cleaned and dried substrate on the workpiece holder in the vacuum chamber. Start the vacuum pump and pump the vacuum chamber pressure to 6.0×10 -3Pa, reducing collisions between residual gas molecules and sputtered particles. Argon gas was introduced into the vacuum chamber at a flow rate of 50 sccm. The vacuum pump speed must match the gas flow rate to maintain a dynamic equilibrium pressure of 1 Pa. The sputtering current was controlled at 1.5 A, and a pulsed bias was switched to a 60% duty cycle (300 V negative bias applied 60% of the time, zero voltage applied 40% of the time). The substrate was bombarded continuously for 10 minutes to remove surface contaminants or oxide layers.

[0029] Step 2: Base deposition The argon flow rate was set to 50 sccm, the vacuum chamber pressure was maintained at 0.5 Pa, the Cr target was turned on, the Cr target current was controlled at 8 A, the negative bias voltage was controlled at 150 V, and a Cr base layer with a film thickness of 0.5 μm was obtained.

[0030] Step 3: Intermediate layer deposition Nitrogen gas was introduced with a nitrogen flow rate controlled at 50 sccm, the vacuum chamber pressure was maintained at 0.5 Pa, the Si target was turned on and the current was adjusted to 10 A, the current of the Cr target was controlled at 10 A, the bias voltage was controlled at 200 V, and a CrSiN intermediate layer with a thickness of 0.8 μm was formed on the surface of the Cr base layer.

[0031] Step 4: Transition layer deposition The nitrogen flow rate was set to 65 sccm, the vacuum chamber pressure was maintained at 0.5 Pa, the Cr target current was set to 10 A, the Si target current was adjusted to 10 A, the bias voltage was controlled at 100 V, and a SiCrN transition layer with a film thickness of 0.5 μm was formed on the CrSiN intermediate layer.

[0032] Step 5: Color layer deposition The nitrogen gas was turned off, the vacuum chamber pressure was maintained at 0.5 Pa, the Cr target current was adjusted to 1 A, the Si target current was adjusted to 10 A, and the bias voltage was controlled at 100 V to form a silver-gray film layer with a thickness of 0.5 μm, thereby obtaining a substrate with a high-performance silver-gray PVD film layer.

[0033] Example 4 The difference between this embodiment and embodiment 1 is that: Step 2: Base deposition The Cr target was activated, the argon flow rate was adjusted to 40 sccm, and the vacuum chamber pressure was maintained at 0.5 Pa. Deposition continued to form a Cr base layer with a thickness of 0.3 μm. The Cr base layer was deposited in stages to reduce internal stress gradients. The first stage was a high-speed deposition stage with a Cr target current of 10 A and a negative bias voltage of 200 V, resulting in a base layer with a thickness of 0.1 μm. The final stage was a low-speed optimization stage with a Cr target current of 6 A and a negative bias voltage of 100 V, resulting in a surface layer with a thickness of 0.2 μm.

[0034] Step 3: Intermediate layer deposition The vacuum chamber pressure was maintained at 0.25 Pa, the current and bias voltage were adjusted, and deposition was continued to form an intermediate layer with a film thickness of 0.8 μm.

[0035] The middle layer adopts a sandwich structure, and through the synergistic effect of the base layer, alternating layer and capping layer, it achieves composition gradient transition, stress buffering and performance enhancement.

[0036] Turn on the Si target and Cr target, set the Si target current to 2.5A, the Cr target current to 6A, and the negative bias voltage to 50V to form a 0.2μm thick Cr-rich base layer (Cr-Si solid solution), which realizes a composition gradient transition with the Cr base layer and reduces interface mutations.

[0037] The alternating layers formed a periodic CrSiN / Si3N4 structure, with each period consisting of a CrSiN sublayer and a Si3N4 sublayer, with a total thickness of 0.2μm. A total of 40 periods were formed. Nitrogen gas was introduced at a flow rate of 45sccm. The Si target current was adjusted to 6A, the Cr target current was adjusted to 6A, and a negative bias voltage of 180V was applied, forming a CrSiN sublayer with a thickness of 0.003μm. The Cr target was turned off, the Si target current was increased to 8A, and a negative bias voltage of 150V was applied, forming a Si3N4 sublayer with a thickness of 0.002μm.

[0038] When depositing the capping layer, the nitrogen flow rate was adjusted to 60 sccm, the Si target current was adjusted to 6 A, the Cr target current was adjusted to 8 A, and the negative bias voltage was controlled at 100 V to form a CrSiN layer with a thickness of 0.4 μm.

[0039] Step 5: Color layer deposition The nitrogen gas was turned off, the vacuum chamber pressure was maintained at 0.3 Pa, the Cr target current was adjusted to 0.6 A, the Si target current was adjusted to 7.5 A, and the bias voltage was controlled at 45 V to form a silver-gray film layer with a thickness of 0.5 μm.

[0040] Example 5 The difference between this embodiment and embodiment 4 is that: Step 2: Base deposition In the first stage of high-speed deposition, the Cr target current was adjusted to 10A and the negative bias voltage was controlled at 200V to form a bottom layer with a thickness of 0.2μm. In the final stage of low-speed optimization, the Cr target current was adjusted to 6A and the negative bias voltage was controlled at 100V to form a surface layer with a thickness of 0.1μm.

[0041] Step 3: Intermediate layer deposition Turn on the Si target and Cr target, set the Si target current to 2.5A, the Cr target current to 6A, and the negative bias voltage to 50V to form a 0.3μm thick Cr-rich base layer (Cr-Si solid solution), which realizes a composition gradient transition with the Cr base layer and reduces interface mutations.

[0042] The alternating layers formed a periodic CrSiN / Si3N4 structure, with each period consisting of a CrSiN sublayer and a Si3N4 sublayer, with a total thickness of 0.2μm. A total of 40 periods were formed. Nitrogen gas was introduced at a flow rate of 45sccm. The Si target current was adjusted to 6A, the Cr target current was adjusted to 6A, and a negative bias voltage of 180V was applied, forming a CrSiN sublayer with a thickness of 0.003μm. The Cr target was turned off, the Si target current was increased to 8A, and a negative bias voltage of 150V was applied, forming a Si3N4 sublayer with a thickness of 0.002μm.

[0043] When depositing the capping layer, the nitrogen flow rate was adjusted to 60 sccm, the Si target current was adjusted to 6 A, the Cr target current was adjusted to 8 A, and the negative bias voltage was controlled at 100 V to form a CrSiN layer with a thickness of 0.2 μm.

[0044] Step 5: Color layer deposition The nitrogen gas was turned off, the vacuum chamber pressure was maintained at 0.5 Pa, the Cr target current was adjusted to 0.8 A, the Si target current was adjusted to 7.5 A, and the negative bias voltage was controlled at 50 V to form a silver-gray film layer with a thickness of 0.5 μm.

[0045] Example 6 The difference between this embodiment and embodiment 4 is that: Step 2: Base deposition In the first stage of high-speed deposition, the Cr target current was adjusted to 6A, and the negative bias voltage was controlled at 200V to form a bottom layer with a thickness of 0.1μm; in the final stage of low-speed optimization, the Cr target current was adjusted to 8A, and the negative bias voltage was controlled at 100V to form a surface layer with a thickness of 0.2μm.

[0046] Step 3: Intermediate layer deposition Turn on the Si target and Cr target, set the Si target current to 5A, the Cr target current to 8A, and the negative bias voltage to 100V to form a 0.2μm thick Cr-rich base layer (Cr-Si solid solution), which realizes a composition gradient transition with the Cr base layer and reduces interface mutations.

[0047] The alternating layers formed a periodic CrSiN / Si3N4 structure, with each period consisting of a CrSiN sublayer and a Si3N4 sublayer, with a total thickness of 0.2μm. A total of 20 periods were formed. Nitrogen gas was introduced at a flow rate of 45sccm. The Si target current was adjusted to 6A, the Cr target current was adjusted to 6A, and a negative bias voltage of 180V was applied, forming a CrSiN sublayer with a thickness of 0.003μm. The Cr target was turned off, the Si target current was increased to 8A, and a negative bias voltage of 150V was applied, forming a Si3N4 sublayer with a thickness of 0.002μm.

[0048] When depositing the capping layer, the nitrogen flow rate was adjusted to 60 sccm, the Si target current was adjusted to 8 A, the Cr target current was adjusted to 6 A, and the negative bias voltage was controlled at 100 V to form a CrSiN layer with a thickness of 0.1 μm.

[0049] Step 5: Color layer deposition The nitrogen gas was turned off, the vacuum chamber pressure was maintained at 0.5 Pa, the Cr target current was adjusted to 1 A, the Si target current was adjusted to 8 A, and the negative bias voltage was controlled at 100 V to form a silver-gray film layer with a thickness of 0.5 μm.

[0050] The coating products obtained in the above embodiments were tested, and the test results are shown in the following table.

[0051]

[0052] Wear resistance test The substrate coated with the deposited layer is mounted on the fixture of the friction tester in a water lubricated environment. The contact pressure between the spherical silicon carbide grinding head and the substrate is set to 5N / cm 2 The grinding head rubs the substrate back and forth at a sliding speed of 0.2 m / s, with a one-way stroke of 50 mm. Water is added during the friction observation, and the wear degree is rated after 4 hours. The wear degree judgment criteria are shown in the following table.

[0053]

[0054] While the embodiments of the present invention are described above, these embodiments do not exhaustively describe all details, nor do they limit the present invention to specific embodiments. Clearly, many modifications and variations can be made based on the above description. This specification selects and specifically describes these embodiments in order to better explain the principles and practical applications of the present invention, thereby enabling those skilled in the art to make good use of the present invention and its modifications and uses. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention shall be included within the scope of protection of the present invention.

Claims

1. A process for preparing silver-gray color by a planar target sputtering coating machine, characterized in that: The steps include: S1. Place the substrate in the vacuum chamber of the vacuum coating magnetron sputtering equipment and evacuate the chamber to a vacuum degree of 6.0×10 -3 Pa, adjust the argon flow rate to make the gas pressure reach the predetermined value, turn on the bias power supply, and bombard the substrate surface with an ion beam to complete the pretreatment; S2. Adjust the argon flow rate to maintain the vacuum chamber pressure at 0.3-0.5 Pa, turn on the Cr target, adjust the Cr target current to 6-10 A, and control the negative bias voltage at 100-200 V to form a base layer on the substrate surface; S3. Nitrogen is introduced, the Si target is turned on, and its current is adjusted to 6-10A. The current of the Cr target is controlled at 6-10A, and the negative bias voltage is controlled at 100-200V to form an intermediate layer on the surface of the base layer; S4. Adjust the nitrogen flow rate, control the negative bias voltage at 30-100 V, control the Cr target current at 6-10 A, and adjust the Si target current to 6-10 A to form a transition layer on the surface of the intermediate layer; S5. Turn off the nitrogen, adjust the Cr target current to 0.5-1A, adjust the Si target current to 8-10A, control the negative bias voltage to 30-100V, and form a silver-gray color layer on the surface of the transition layer.

2. The process for preparing silver-gray color by a planar target sputtering coating machine according to claim 1, characterized in that: In step S1 , the argon flow rate is set to 30-50 sccm, and the dynamic equilibrium pressure is maintained at 0.5-1 Pa.

3. The process for preparing silver-gray color by a planar target sputtering coating machine according to claim 1, characterized in that: In step S3, the nitrogen flow rate is set to 30-50 sccm and the vacuum chamber pressure is maintained at 0.25-0.5 Pa.

4. The process for preparing silver-gray color by a planar target sputtering coating machine according to claim 1, characterized in that: In step S4, the nitrogen flow rate is set to 55-65 sccm, and the vacuum chamber pressure is maintained at 0.3-0.5 Pa.

5. The process for preparing silver-gray color by a planar target sputtering coating machine according to claim 1, characterized in that: The thickness of the primer layer is 0.3-0.5 μm.

6. The process for preparing silver-gray color by a planar target sputtering coating machine according to claim 1, characterized in that: The thickness of the intermediate layer is 0.8-1.2 μm.

7. The process for preparing silver-gray color by a planar target sputtering coating machine according to claim 1, characterized in that: The thickness of the transition layer is 0.5-1 μm.

8. The process for preparing silver-gray color by a planar target sputtering coating machine according to claim 1, characterized in that: The thickness of the color layer is 0.5-1 μm.

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