A silver-gray process method prepared by a planar target sputtering coating machine
By preparing a multilayer silver-gray PVD film on a substrate, the problem of easy damage to the film was solved, achieving high-performance adhesion and wear resistance while maintaining the product's gloss.
Patent Information
- Application Number
- CN202510968596.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-07-15
- Publication Date
- 2025-11-11
- Estimated Expiration
- 2045-07-15
AI Technical Summary
The films prepared by existing coating technologies are easily scratched, have insufficient adhesion and wear resistance, resulting in a loss of gloss.
A planar target sputtering coating machine was used to prepare a silver-gray process. Through multi-layer film structure design, including an underlayer, intermediate layer and color layer, combined with precise process parameter control, a multi-phase composite structure of Cr, SiCrN and Si target was formed, which optimized the adhesion and wear resistance of the film layer.
It improves the adhesion and wear resistance of the film layer, ensuring that the film layer is not easily damaged during use and maintains its gloss.
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Abstract
Description
Technical Field
[0001] This invention relates to the field of PVD coating technology, specifically a method for preparing silver-gray coating using a planar target sputtering coating machine. Background Technology
[0002] Physical vapor deposition (PVD) is a technique that uses physical means in a vacuum environment to convert solid or liquid materials into gaseous atoms, molecules or ions and deposit them on the surface of a substrate to form a thin film.
[0003] With the widespread application of PVD technology in surface coating, especially in the field of smart wearables where PVD treatment is used to achieve different color schemes and enhance aesthetics, many electronic product components and workpieces now utilize coating processes for their exterior decoration, which are highly favored by consumers.
[0004] However, the film layer prepared by existing coating technology is easily scratched when in contact with external objects, and the film layer is easy to peel off from the damaged area, resulting in a loss of gloss. Summary of the Invention
[0005] To address the problems existing in the prior art, this invention provides a method for preparing silver-gray coatings using a planar target sputtering coating machine, aiming to improve the adhesion and wear resistance of the film. To achieve the above objective, this invention provides a method for preparing silver-gray coatings using a planar target sputtering coating machine, comprising the following steps:
[0006] S1. Place the substrate in the vacuum chamber of the vacuum coating magnetron sputtering equipment and evacuate to a chamber vacuum level of 6.0 × 10⁻⁶. -3 Pa, argon gas is continuously introduced, the argon gas flow rate is adjusted to make the gas pressure reach the predetermined value, the bias power supply is turned on, and the ion beam is used to bombard the surface of the substrate to complete the pretreatment.
[0007] 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.
[0008] S3. Introduce nitrogen gas, turn on the Si target, adjust its current to 6-10A, control the current of the Cr target to 6-10A, and control the negative bias voltage to 100-200V to form an intermediate layer on the surface of the substrate.
[0009] S4. Adjust the nitrogen flow rate, control the negative bias voltage at 30-100V, control the Cr target current at 6-10A, adjust the Si target current to 6-10A, and form a transition layer on the surface of the intermediate layer.
[0010] S5. Turn off the nitrogen gas, adjust the Cr target current to 0.5-1A, adjust the Si target current to 8-10A, and control the negative bias voltage at 30-100V to form a silver-gray color layer on the surface of the transition layer.
[0011] 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.
[0012] 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.
[0013] 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.
[0014] Preferably, the thickness of the underlayer is 0.3 to 0.5 μm.
[0015] Preferably, the thickness of the intermediate layer is 0.8 to 1.2 μm.
[0016] Preferably, the thickness of the transition layer is 0.5 to 1 μm.
[0017] Preferably, the thickness of the color layer is 0.5 to 1 μm.
[0018] After adopting the above technical solution, the beneficial effects of the present invention are:
[0019] The silver-gray process of preparing a planar target sputtering coating machine involves sequentially depositing an underlayer, intermediate layer, transition layer, and color layer on the substrate surface. Through multilayer film structure design and precise process parameter control, a high-performance silver-gray PVD film is prepared, improving the adhesion and wear resistance of the PVD film. Detailed Implementation
[0020] The features and exemplary embodiments of various aspects of the present invention will now be described in detail. To make the objectives, technical solutions, and advantages of the present invention clearer, the present invention will be further described in detail below with reference to 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 practiced without 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 invention.
[0021] Example 1
[0022] This embodiment employs a planar target sputtering coating method to prepare a silver-gray film, sequentially depositing an underlayer, intermediate layer, transition layer, and color layer onto a substrate. Through multilayer film structure design and precise process parameter control, a high-performance silver-gray PVD film is successfully prepared. The following is a detailed analysis of this method and its key technical points.
[0023] Step 1: Ion bombardment pretreatment
[0024] Prepare the vacuum coating magnetron sputtering equipment, and fix the cleaned and dried substrate onto the workpiece holder inside the vacuum chamber. Start the vacuum pump and evacuate the vacuum chamber pressure to 6.0 × 10⁻⁶. -3 To reduce collisions between residual gas molecules and sputtered particles, argon gas is introduced into the vacuum chamber at a flow rate of 30 sccm. The vacuum pump speed must be matched with the gas flow rate to maintain a dynamic equilibrium pressure of 0.5 Pa. The sputtering current is controlled at 0.5 A, switched to pulsed bias, with a duty cycle of 60% (60% of the time applying a negative bias of 300V, and 40% of the time the voltage returns to zero), continuously bombarding the substrate for 20 minutes to remove surface contaminants or oxide layers.
[0025] Step 2: Drilling the bottom layer of sediment
[0026] 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, and the negative bias voltage was controlled at 200 V, resulting in a Cr underlayer with a film thickness of 0.3 μm.
[0027] Step 3: Intermediate layer deposition
[0028] Nitrogen gas is introduced, with the flow rate controlled at 30 sccm, and the vacuum chamber pressure is maintained at 0.25 Pa. The Si target is turned on and the current is adjusted to 6 A. The current of the Cr target is controlled at 6 A, and the negative bias voltage is controlled at 100 V. A CrSiN intermediate layer with a thickness of 1.2 μm is formed on the surface of the Cr substrate.
[0029] Step 4: Transition Layer Deposition
[0030] 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, and the negative bias voltage was controlled at 30 V. A SiCrN transition layer with a film thickness of 1 μm was formed on the CrSiN intermediate layer.
[0031] The SiCrN transition layer, through the synergistic reaction of Cr / Si target sputtering and nitrogen gas, forms a multiphase composite structure, playing a crucial role in bridging the gap between the upper and lower layers in terms of mechanical properties and thermal stability. It primarily addresses 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 and simultaneously minimizing interface defects and stress concentration.
[0032] Step 5: Color layer deposition
[0033] 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 with a thickness of 1 μm.
[0034] The high refractive index of Si combined with the metallic reflective properties of Cr enhances the balanced reflection of visible light across the entire wavelength range through interference effects, avoiding the dominance of a single wavelength and presenting a stable silver-gray tone.
[0035] Example 2
[0036] Step 1: Ion bombardment pretreatment
[0037] Prepare the vacuum coating magnetron sputtering equipment, and fix the cleaned and dried substrate onto the workpiece holder inside the vacuum chamber. Start the vacuum pump and evacuate the vacuum chamber pressure to 6.0 × 10⁻⁶. -3 To reduce collisions between residual gas molecules and sputtered particles, argon gas is introduced into the vacuum chamber at a flow rate of 45 sccm. The vacuum pump speed must be matched with the gas flow rate to maintain a dynamic equilibrium pressure of 0.8 Pa. The sputtering current is controlled at 1 A, switched to pulse bias, with a duty cycle of 60% (300V negative bias applied for 60% of the time, and the voltage returned to zero for 40% of the time), and the substrate is continuously bombarded for 15 minutes to remove surface contaminants or oxide layers.
[0038] Step 2: Drilling the bottom layer of sediment
[0039] 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, and the negative bias voltage was controlled at 100 V, resulting in a Cr underlayer with a film thickness of 0.35 μm.
[0040] Step 3: Intermediate layer deposition
[0041] Nitrogen gas is introduced, with the flow rate controlled at 35 sccm, and the vacuum chamber pressure is maintained at 0.3 Pa. The Si target is turned on and the current is adjusted to 8 A. The current of the Cr target is controlled at 8 A, and the negative bias voltage is controlled at 120 V. A CrSiN intermediate layer with a thickness of 1 μm is formed on the surface of the Cr substrate.
[0042] Step 4: Transition Layer Deposition
[0043] 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, and the negative bias voltage was controlled at 50 V. A SiCrN transition layer with a film thickness of 0.8 μm was formed on the CrSiN intermediate layer.
[0044] Step 5: Color layer deposition
[0045] Nitrogen gas was shut 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, forming a silver-gray film with a thickness of 0.8 μm.
[0046] Example 3
[0047] Step 1: Ion bombardment pretreatment
[0048] Prepare the vacuum coating magnetron sputtering equipment, and fix the cleaned and dried substrate onto the workpiece holder inside the vacuum chamber. Start the vacuum pump and evacuate the vacuum chamber pressure to 6.0 × 10⁻⁶. -3 To reduce collisions between residual gas molecules and sputtered particles, argon gas is introduced into the vacuum chamber at a flow rate of 50 sccm. The vacuum pump speed must be matched with the gas flow rate to maintain a dynamic equilibrium pressure of 1 Pa. The sputtering current is controlled at 1.5 A, switched to pulsed bias, with a duty cycle of 60% (300V negative bias applied for 60% of the time, and the voltage returned to zero for 40% of the time), and the substrate is continuously bombarded for 10 minutes to remove surface contaminants or oxide layers.
[0049] Step 2: Drilling the bottom layer of sediment
[0050] 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, and the negative bias voltage was controlled at 150 V, resulting in a Cr underlayer with a film thickness of 0.5 μm.
[0051] Step 3: Intermediate layer deposition
[0052] Nitrogen gas is introduced, with the flow rate controlled at 50 sccm, and the vacuum chamber pressure is maintained at 0.5 Pa. The Si target is turned on and the current is adjusted to 10 A. The current of the Cr target is controlled at 10 A, and the bias voltage is controlled at 200 V. A CrSiN intermediate layer with a thickness of 0.8 μm is formed on the surface of the Cr substrate.
[0053] Step 4: Transition Layer Deposition
[0054] 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, and the bias voltage was controlled at 100 V. A SiCrN transition layer with a film thickness of 0.5 μm was formed on the CrSiN intermediate layer.
[0055] Step 5: Color layer deposition
[0056] Nitrogen gas was turned off, and 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. A silver-gray film with a thickness of 0.5 μm was formed, and a substrate with a high-performance silver-gray PVD film was obtained.
[0057] Example 4
[0058] The difference between this embodiment and Embodiment 1 is that:
[0059] Step 2: Drilling the bottom layer of sediment
[0060] The Cr target was activated, and the argon flow rate was adjusted to 40 sccm. The vacuum chamber pressure was maintained at 0.5 Pa, and Cr underlayer deposition was continuously performed to form a Cr underlayer with a thickness of 0.3 μm. The Cr underlayer was deposited in stages to reduce internal stress gradients. The first stage involved high-speed deposition, with the Cr target current adjusted to 10 A and the negative bias voltage controlled at 200 V, forming an underlayer with a thickness of 0.1 μm. The final stage involved low-speed optimization, with the Cr target current adjusted to 6 A and the negative bias voltage controlled at 100 V, forming a surface layer with a thickness of 0.2 μm.
[0061] Step 3: Intermediate layer deposition
[0062] Maintaining a vacuum chamber pressure of 0.25 Pa, adjusting the current and bias voltage, and continuing deposition, an intermediate layer with a film thickness of 0.8 μm was formed.
[0063] The intermediate layer adopts a sandwich structure, through the synergistic effect of the base layer, alternating layers and the top cap layer, to achieve component gradient transition, stress buffering and performance enhancement.
[0064] Turn on the Si target and Cr target, set the Si target current to 2.5A and the Cr target current to 6A, and control the negative bias voltage at 50V to form a Cr-rich base layer (Cr-Si solid solution) with a thickness of 0.2μm. This achieves a compositional gradient transition with the Cr underlayer and reduces interface abrupt changes.
[0065] The alternating layers are a CrSiN / Si3N4 periodic structure, with each cycle consisting of a CrSiN sublayer and a Si3N4 sublayer, with a total thickness of 0.2 μm, for a total of 40 cycles. Nitrogen gas is introduced at a flow rate of 45 sccm, the Si target current is adjusted to 6 A, the Cr target current is adjusted to 6 A, and the negative bias voltage is 180 V, forming a CrSiN sublayer with a thickness of 0.003 μm. The Cr target is then turned off, the Si target current is increased to 8 A, and the negative bias voltage is 150 V, forming a Si3N4 sublayer with a thickness of 0.002 μm.
[0066] During the deposition of the capping layer, the nitrogen flow rate was adjusted to 60 sccm, the Si target current was adjusted to 6A, the Cr target current was adjusted to 8A, and the negative bias voltage was controlled at 100V to form a CrSiN layer with a thickness of 0.4μm.
[0067] Step 5: Color layer deposition
[0068] 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 with a thickness of 0.5 μm.
[0069] Example 5
[0070] The difference between this embodiment and embodiment 4 is that:
[0071] Step 2: Drilling the bottom layer of sediment
[0072] 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.
[0073] Step 3: Intermediate layer deposition
[0074] Turn on the Si target and Cr target, set the Si target current to 2.5A and the Cr target current to 6A, and control the negative bias voltage at 50V to form a Cr-rich base layer (Cr-Si solid solution) with a thickness of 0.3μm. This achieves a compositional gradient transition with the Cr underlayer and reduces interface abrupt changes.
[0075] The alternating layers are a CrSiN / Si3N4 periodic structure, with each cycle consisting of a CrSiN sublayer and a Si3N4 sublayer, with a total thickness of 0.2 μm, for a total of 40 cycles. Nitrogen gas is introduced at a flow rate of 45 sccm, the Si target current is adjusted to 6 A, the Cr target current is adjusted to 6 A, and the negative bias voltage is 180 V, forming a CrSiN sublayer with a thickness of 0.003 μm. The Cr target is then turned off, the Si target current is increased to 8 A, and the negative bias voltage is 150 V, forming a Si3N4 sublayer with a thickness of 0.002 μm.
[0076] During the deposition of the capping layer, the nitrogen flow rate was adjusted to 60 sccm, the Si target current was adjusted to 6A, the Cr target current was adjusted to 8A, and the negative bias voltage was controlled at 100V to form a CrSiN layer with a thickness of 0.2μm.
[0077] Step 5: Color layer deposition
[0078] 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 with a thickness of 0.5 μm.
[0079] Example 6
[0080] The difference between this embodiment and embodiment 4 is that:
[0081] Step 2: Drilling the bottom layer of sediment
[0082] 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.
[0083] Step 3: Intermediate layer deposition
[0084] Turn on the Si target and Cr target, set the Si target current to 5A and the Cr target current to 8A, and control the negative bias voltage at 100V to form a Cr-rich base layer (Cr-Si solid solution) with a thickness of 0.2μm. This achieves a compositional gradient transition with the Cr base layer and reduces interface abrupt changes.
[0085] The alternating layers are a periodic CrSiN / Si3N4 structure, with each cycle consisting of a CrSiN sublayer and a Si3N4 sublayer, with a total thickness of 0.2 μm, for a total of 20 cycles. Nitrogen gas is introduced at a flow rate of 45 sccm, the Si target current is adjusted to 6 A, the Cr target current is adjusted to 6 A, and the negative bias voltage is 180 V, forming a CrSiN sublayer with a thickness of 0.003 μm. The Cr target is then turned off, the Si target current is increased to 8 A, and the negative bias voltage is 150 V, forming a Si3N4 sublayer with a thickness of 0.002 μm.
[0086] During the deposition of the capping layer, the nitrogen flow rate was adjusted to 60 sccm, the Si target current was adjusted to 8A, the Cr target current was adjusted to 6A, and the negative bias voltage was controlled at 100V to form a CrSiN layer with a thickness of 0.1μm.
[0087] Step 5: Color layer deposition
[0088] 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 with a thickness of 0.5 μm.
[0089] The coated products obtained in the above embodiments were tested, and the test results are shown in the table below.
[0090]
[0091] Abrasion resistance test
[0092] 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 5 N / cm. 2 The grinding head reciprocated against the substrate at a sliding speed of 0.2 m / s, with a unidirectional stroke of 50 mm. Water was added during friction observation, and the wear level was rated after 4 hours. The wear level judgment criteria are shown in the table below.
[0093]
[0094] The embodiments described above are not exhaustive and do not limit the invention to specific implementations. Clearly, many modifications and variations can be made based on the above description. These embodiments are selected and specifically described in this specification to better explain the principles and practical applications of the invention, thereby enabling those skilled in the art to effectively utilize the invention and its modifications. Any modifications, equivalent substitutions, or improvements made within the spirit and principles of the invention should be included within the scope of protection of the invention.
Claims
1. A method for preparing silver-gray coating using a planar target sputtering coating machine, characterized in that, Includes the following steps: S1. Place the substrate in the vacuum chamber of the vacuum coating magnetron sputtering equipment and evacuate to a chamber vacuum level of 6.0 × 10⁻⁶. -3 Pa, adjust the argon gas flow rate to reach the predetermined pressure, turn on the bias power supply, and use the ion beam to bombard the substrate surface 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. Introduce nitrogen gas to deposit an intermediate layer on the surface of the bottom layer using a gradient deposition method. Specific steps include: S31. Set the Si target current to 2.5A, the Cr target current to 6A, and the negative bias voltage to 50V to form a Cr-rich base layer on the upper surface of the substrate. S32. Periodic deposition: The Si target current is adjusted to 6A, the Cr target current is adjusted to 6A, and the negative bias voltage is 180V to form a CrSiN sublayer on the base layer; the Cr target is turned off and the Si target current is adjusted to 8A, and the negative bias voltage is adjusted to 150V to form a Si3N4 sublayer on the CrSiN sublayer, completing one cycle of deposition; the operation is repeated to perform 40 cycles of nano-stacked process to form alternating layers of hierarchical structure; The S33 and Si target currents are adjusted to 6A, the Cr target current is adjusted to 8A, and the negative bias voltage is controlled at 100V to form a capping layer on the outer layer of the alternating layers. S4. Adjust the nitrogen flow rate, control the negative bias voltage at 30-100V, control the Cr target current at 6-10A, adjust the Si target current to 6-10A, and form a transition layer on the surface of the intermediate layer. S5. Turn off the nitrogen gas, adjust the Cr target current to 0.5-1A, adjust the Si target current to 8-10A, and control the negative bias voltage at 30-100V to form a silver-gray color layer on the surface of the capping layer.
2. The method for preparing silver-gray coating using 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 method for preparing silver-gray coating using 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 method for preparing silver-gray coating using 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 method for preparing silver-gray coating using a planar target sputtering coating machine according to claim 1, characterized in that: The thickness of the base layer is 0.3 to 0.5 μm.
6. The method for preparing silver-gray coating using 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 method for preparing silver-gray coating using 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 method for preparing silver-gray coating using a planar target sputtering coating machine according to claim 1, characterized in that: The thickness of the color layer is 0.5–1 μm.
Citation Information
Patent Citations
Film layer and preparation method of film layer
CN116815135A