Technological method for preparing light gold by using planar target sputtering coating machine

Abstract

The invention discloses a process method for preparing light gold by a planar target sputtering coating machine, which relates to the technical field of coating, and comprises the following steps: ultrasonically cleaning a substrate, sealing and drying, conveying the dried substrate to vacuum coating planar magnetron sputtering equipment, and starting ion bombardment when the vacuum degree of a cavity is less than or equal to 6 * 10 <-3 > Pa; plane Cr target direct current sputtering is carried out; n2 is introduced into the cavity, and the Cr target current is controlled to be 6-10 A; continuously feeding N2, and synchronously starting a Cr target and a Ti target; n2 is continuously fed, the current of a Cr target is controlled to be 10-0.5 A, and the current of a Ti target is controlled to be 6-10 A; annealing under the protection of N2, wherein the Lab value of the film layer is L: 80-84; a3 to 5; and b: 8-14. Therefore, according to the process method for preparing the light golden color through the planar target sputtering coating machine, the brightness of a film layer is improved through planar target direct-current sputtering power supply deposition, meanwhile, the hardness and wear resistance of a metal product are improved through CrN deposition, and the light golden color is obtained through TiCrN process reaction.

Description

Technical Field

[0001] The present invention relates to the field of coating technologies, and in particular, to a process method for preparing a light golden color by a planar target sputtering coating machine. Background Art

[0002] PVD is a technology that, in a vacuum environment, converts solid or liquid materials into gaseous atoms, molecules, or ions through physical means and deposits a thin film on the surface of a substrate. The physical vapor deposition technology has a simple process, a great effect on environmental improvement, no pollution, less consumables, a uniform and dense film formation, and a strong bonding force with the substrate. In the PVD industry, the light golden color system is widely used in metal products, showing wealth and luxury on the surface, and is therefore very popular. In the prior art, PVD treatment is performed on the surface in the field of metal smart wearables to achieve the color system, and among them, the light golden film layer occupies a large proportion in the 3C smart wearables field.

[0003] However, in the prior art, there is a problem that large particles are sputtered by a multi-arc ion coating machine, resulting in a dull product color and a large color deviation value. Summary of the Invention

[0004] Aiming at the above defects, the purpose of the present invention is to provide a process method for preparing a light golden color by a planar target sputtering coating machine, aiming to solve the problem that large particles are sputtered by a multi-arc ion coating machine in the prior art, resulting in a dull product.

[0005] To solve the above technical problems, the technical solution of the present invention is as follows: A process method for preparing a light golden color by a planar target sputtering coating machine includes the following steps: Step 1, substrate pretreatment; After the substrate is ultrasonically cleaned and sealed and dried, the dried substrate is sent to a vacuum coating planar magnetron sputtering device. When the chamber vacuum degree of the vacuum coating planar magnetron sputtering device ≤ 6×10 -3 Pa, ion bombardment is started, the bias voltage is controlled at 100 - 300v, the sputtering current is 0.5A ± 0.1A, and the time is 10 - 20min; Step 2, preparation of a Cr bottom layer; Direct current sputtering of a planar Cr target, the Cr target current is controlled at 6 - 10A, the bias voltage is controlled at 100 - 200v, and the time is 10 - 20min; Step 3, preparation of a CrN intermediate layer; N2 is introduced into the chamber, the Cr target current is controlled at 6 - 10A, the direct current bias voltage is controlled at 50 - 100v, and the time is 30 - 90min; Step 4, preparation of a CrTiN transition layer; Continuously feed N2, synchronously turn on the Cr target and the Ti target, control the Cr target current at 6 - 10 A, the Ti target current at 6 - 10 A, the DC bias voltage at 50 - 100 v, and the time for 30 - 80 min; Step Five, preparation of the TiCrN color layer; Continuously feed N2, control the Cr target current at 10 - 0.5 A, the Ti target current at 6 - 10 A, the bias voltage at 50 - 100 v, and the deposition time at 20 - 60 min; Step Six, post - treatment; Anneal under the protection of N2, and the Lab values of the film layer are L: 80 - 84; a: 3 - 5; b: 8 - 14.

[0006] Among them, in Step One, the substrate is stainless steel or titanium alloy. The substrate is ultrasonically cleaned with acetone for 3 - 4 h, and the cavity of the vacuum coating planar magnetron sputtering equipment is pre - heated to 150 - 200 °C.

[0007] Among them, in Step Two, during the operation of the planar Cr target, Ar needs to be fed into the cavity, and the gas flow rate of Ar is 50 - 60 sccm; the deposition rate is 0.8 nm / s, and the thickness of the bottom layer is 0.2 - 0.4 μm.

[0008] Among them, in Step Three, the gas flow rate of N2 linearly increases from 30 sccm to 60 sccm, with a slope of 0.5 sccm / s.

[0009] Among them, in Step Three, the thickness of the intermediate layer is 0.6 - 0.8 μm.

[0010] Among them, in Step Four, the gas flow rate of N2 linearly increases from 10 sccm to 60 sccm.

[0011] Among them, in Step Four, the thickness of the transition layer is 0.8 - 1.2 μm.

[0012] Among them, in Step Five, the Cr target current linearly decreases from 10 A to 0.5 A, with a linear slope of - 0.2 A / min.

[0013] Among them, in Step Five, the gas flow rate of N2 is 10 - 60 sccm.

[0014] Among them, in Step Five, the thickness of the color layer is 0.5 - 1 μm.

[0015] After adopting the above - mentioned technical solution, the beneficial effects of the present invention are: First, this solution consists of a substrate layer - a primer layer - an intermediate layer - a transition layer - a color layer. By combining the interlayer properties such as toughness, rigidity, toughness-rigidity transition, and high surface hardness, a composite system with impact resistance and wear resistance is formed, achieving multi-layer anti-corrosion. Second, the primer layer has high reflectivity properties, the intermediate layer has properties of gradually changing refractive index, the transition layer has properties of interference color display, and coupled with the relatively low color difference of the color layer, this ensures that the Lab value of the final product in light gold color is precisely controllable. Third, a process method for preparing light gold color using a planar target sputtering vacuum coating machine is adopted. The deposition of the planar target DC sputtering power supply improves the brightness of the film layer. At the same time, CrN deposition also enhances the hardness and wear resistance of the metal product. The light gold color is obtained due to the TiCrN process reaction. Detailed implementation manners

[0016] It should be understood that the specific embodiments described herein are merely used to explain the present invention and are not used to limit the present invention.

[0017] Embodiment: A process method for preparing light gold color using a planar target sputtering coating machine includes the following steps: Step 1, substrate pretreatment; The substrate is ultrasonically cleaned and then sealed and dried. The dried substrate is sent to a vacuum coating planar magnetron sputtering device. When the chamber vacuum degree of the vacuum coating planar magnetron sputtering device is ≤6×10 -3 Pa, ion bombardment is started, the bias voltage is controlled at 100 - 300v, the sputtering current is 0.5A ± 0.1A, and the time is 10 - 20min.

[0018] The purpose of substrate pretreatment is to remove the oxide layer on the substrate surface, thereby ensuring the quality of the subsequent coating and reducing quality problems.

[0019] Step 2, preparation of the Cr primer layer; Planar DC sputtering of a Cr target, the Cr target current is controlled at 6 - 10A, the bias voltage is controlled at 100 - 200v, and the time is 10 - 20min.

[0020] The function of the primer layer is to improve the adhesion between the substrate and the film layer, effectively blocking the diffusion of metal elements of the substrate into the film layer, thereby avoiding the problem of excessive color difference in the final product.

[0021] Step 3, preparation of the CrN intermediate layer; N2 is introduced into the chamber, the Cr target current is controlled at 6 - 10A, the DC bias voltage is controlled at 50 - 100v, and the time is 30 - 90min.

[0022] Chromium nitride is a hard coating with high wear resistance and excellent oxidation resistance due to its excellent adhesion to steel and titanium. The intermediate layer provides rigid support for the subsequent film layers, reducing the problem of film layer collapse caused by external forces and inhibiting the propagation of interlayer cracks. Moreover, the intermediate layer has high chemical inertness, which delays the corrosion rate and ensures the overall lifespan.

[0023] Step 4: Preparation of the CrTiN transition layer; Continuously feed N2, simultaneously turn on the Cr target and the Ti target. The current of the Cr target is controlled at 6 - 10 A, the current of the Ti target is controlled at 6 - 10 A, the DC bias voltage is controlled at 50 - 100 v, and the time is 30 - 80 min.

[0024] The role of the transition layer is to avoid the problem of interface peeling caused by lattice mismatch, that is, to reduce the problem of color layer peeling. The CrTiN layer provides a smooth transition for the optical interference color display of the color layer by adjusting the Ti content. The nano - composite structure of CrTiN provides multiple interface dislocation slip paths, releasing the internal stress in the film layer and enabling the film layer to remain intact during bending deformation.

[0025] Step 5: Preparation of the TiCrN color layer; Continuously feed N2, the current of the Cr target is controlled at 10 - 0.5 A, the current of the Ti target is controlled at 6 - 10 A, the bias voltage is controlled at 50 - 100 v, and the deposition time is 20 - 60 min.

[0026] The color layer is mainly responsible for providing an aesthetic appearance and a specific color effect. The color layer can be directly coated on the transition layer, and the desired color can be obtained by controlling the parameters during the deposition process.

[0027] Step 6: Post - treatment; Anneal under the protection of N2, and the Lab values of the film layer are L: 80 - 84; a: 3 - 5; b: 8 - 14.

[0028] In Step 1, the substrate is stainless steel or titanium alloy. The substrate is ultrasonically cleaned with acetone for 3 - 4 h, and the cavity of the vacuum coating planar magnetron sputtering equipment is pre - heated to 150 - 200 °C.

[0029] In Step 2, during the operation of the planar Cr target, Ar needs to be fed into the cavity. The gas flow rate of Ar is 50 - 60 sccm; the deposition rate is 0.8 nm / s, and the thickness of the bottom layer is 0.2 - 0.4 um.

[0030] In Step 3, the gas flow rate of N2 linearly increases from 30 sccm to 60 sccm with a slope of 0.5 sccm / s.

[0031] The gas flow rate of N2 in Step 3 is divided into three stages, namely: Stage 1 (0 - 20 min): The N2 flow rate is 30 → 45 sccm, the Cr target current is 10 A, forming a high Cr content layer (Cr:N = 65:35); Stage 2 (20 - 40 min): The N2 flow rate is 45 → 55 sccm, the Cr target current is 8 A, forming a transition layer (Cr:N = 55:45); Stage 3 (40 - 60 min): The N2 flow rate is 55 → 60 sccm, the Cr target current is 6 A, forming a surface N-rich layer (Cr:N = 48:52).

[0032] In step three, the thickness of the intermediate layer is 0.6 - 0.8 um.

[0033] In step four, the gas flow rate of N2 linearly increases from 10 sccm to 60 sccm. In this solution, the N2 flow rate of the CrTiN transition layer is regulated according to a piecewise function: The first 10 minutes: The N2 flow rate is 10 → 30 sccm (slope 2 sccm / min); The middle 30 minutes: The N2 flow rate is 30 → 50 sccm (slope 0.67 sccm / min); The last 10 minutes: The N2 flow rate is 50 → 60 sccm (slope 1 sccm / min).

[0034] The dynamic slope of the Cr target current in the TiCrN color layer satisfies the equation: , (0 ≤ t ≤ 40 min), where t is the time (min), and the current control accuracy is ±0.1 A.

[0035] In step four, the thickness of the transition layer is 0.8 - 1.2 um.

[0036] In step five, the Cr target current linearly decreases from 10 A to 0.5 A, with a linear slope of -0.2 A / min.

[0037] In step five, the gas flow rate of N2 is 10 - 60 sccm.

[0038] In step five, the thickness of the color layer is 0.5 - 1.0 um.

[0039] Example 1: Using the above solution for coating, where: In step one, the bias voltage is controlled at 100 v, the sputtering current is 0.4 A, and the time is 10 min. The substrate is ultrasonically cleaned with acetone for 3 h, and the cavity of the vacuum coating planar magnetron sputtering equipment is preheated to 150 °C.

[0040] In Step 2, the Cr target current is controlled at 6 A, the bias voltage is controlled at 100 V, and the time is 10 min. The gas flow rate of Ar is 50 sccm; the thickness of the bottom layer is 0.2 μm.

[0041] In Step 3, the Cr target current is controlled at 6 A, the DC bias voltage is controlled at 50 V, and the time is 30 min. The thickness of the intermediate layer is 0.6 μm.

[0042] In Step 4, the Cr target current is controlled at 6 A, the Ti target current is controlled at 6 A, the DC bias voltage is controlled at 50 V, and the time is 30 min. In Step 4, the thickness of the transition layer is 0.8 μm.

[0043] In Step 5, the Cr target current is controlled at 10 A, the Ti target current is controlled at 6 A, the bias voltage is controlled at 50 V, and the deposition time is 20 min. In Step 5, the gas flow rate of N2 is 10 sccm. In Step 5, the thickness of the color layer is 0.5 μm.

[0044] Example 2: The difference between this example and Example 1 is: In Step 1, the bias voltage is controlled at 150 V, the sputtering current is 0.5 A, and the time is 15 min. The substrate is ultrasonically cleaned with acetone for 3.5 h, and the cavity of the vacuum coating planar magnetron sputtering equipment is vacuum preheated to 160 °C.

[0045] In Step 2, the Cr target current is controlled at 8 A, the bias voltage is controlled at 150 V, and the time is 15 min. The gas flow rate of Ar is 55 sccm; the thickness of the bottom layer is 0.3 μm.

[0046] In Step 3, the Cr target current is controlled at 8 A, the DC bias voltage is controlled at 80 V, and the time is 70 min. The thickness of the intermediate layer is 0.7 μm.

[0047] In Step 4, the Cr target current is controlled at 8 A, the Ti target current is controlled at 8 A, the DC bias voltage is controlled at 82 V, and the time is 50 min. In Step 4, the thickness of the transition layer is 0.9 μm.

[0048] In Step 5, the Cr target current is controlled at 5 A, the Ti target current is controlled at 8 A, the bias voltage is controlled at 80 V, and the deposition time is 40 min. In Step 5, the gas flow rate of N2 is 40 sccm. In Step 5, the thickness of the color layer is 0.6 μm.

[0049] Example 3: The difference between this example and Example 1 is: In Step 1, the bias voltage is controlled at 300 V, the sputtering current is 0.4 A, and the time is 20 min. The substrate is ultrasonically cleaned with acetone for 4 h, and the cavity of the vacuum coating planar magnetron sputtering equipment is vacuum preheated to 200 °C.

[0050] In Step 2, the Cr target current is controlled at 10 A, the bias voltage is controlled at 200 V, the time is 20 min, the gas flow rate of Ar is 60 sccm, and the thickness of the bottom layer is 0.4 μm.

[0051] In Step 3, the Cr target current is controlled at 10 A, the DC bias voltage is controlled at 100 V, the time is 90 min, and the thickness of the intermediate layer is 0.8 μm.

[0052] In Step 4, the Cr target current is controlled at 10 A, the Ti target current is controlled at 10 A, the DC bias voltage is controlled at 100 V, the time is 80 min, and the thickness of the transition layer in Step 4 is 1.2 μm.

[0053] In Step 5, the Cr target current is controlled at 0.5 A, the Ti target current is controlled at 10 A, the bias voltage is controlled at 100 V, the deposition time is 60 min, the gas flow rate of N2 is 60 sccm in Step 5, and the thickness of the color layer is 1 μm.

[0054] Take the coated products in Examples 1 - 3 and inspect their Lab values. The results are as follows:

[0055] In summary, the advantages of this solution are as follows: First, this solution consists of a substrate - bottom layer - intermediate layer - transition layer - color layer, which combines the interlayer properties such as toughness, rigidity, toughness - rigidity transition, and high surface hardness to form an impact - resistant and wear - resistant composite system, achieving multi - layer anti - corrosion. Second, the bottom layer has high - reflection properties, the intermediate layer has a gradually changing refractive index property, the transition layer has an interference color - showing property, and coupled with the relatively low color difference of the color layer, this ensures that the light - golden Lab value of the final product is precisely controllable. Third, a process method for preparing light - golden using a planar target sputtering vacuum coating machine is adopted, and the planar target DC sputtering power supply deposition improves the brightness of the film layer. At the same time, CrN deposition also improves the hardness and wear resistance of metal products, and the light - golden color is obtained due to the TiCrN process reaction.

[0056] The present invention is not limited to the above - mentioned specific embodiments. Those of ordinary skill in the art, starting from the above - mentioned concept and without creative labor, can make various transformations, all of which fall within the protection scope of the present invention.

Claims

1. A process method for preparing a light golden color by a planar target sputtering coating machine, characterized in that, It includes the following steps: Step 1, substrate pretreatment; After ultrasonic cleaning, the substrate is sealed and dried, and the dried substrate is sent to a vacuum coating planar magnetron sputtering equipment. When the chamber vacuum degree of the vacuum coating planar magnetron sputtering equipment is ≤ 6×10 -3 Pa, ion bombardment is started, the bias voltage is controlled at 100 - 300V, the sputtering current is 0.5A ± 0.1A, and the time is 10 - 20min; Step 2, preparation of Cr underlayer; Direct current sputtering of planar Cr target, with the Cr target current controlled at 6 - 10 A, the bias voltage controlled at 100 - 200 V, and the time being 10 - 20 min; Step 3, preparation of CrN intermediate layer; Introduce N2 into the cavity, with the Cr target current controlled at 6 - 10 A, the direct current bias voltage controlled at 50 - 100 V, and the time being 30 - 90 min; Step 4, preparation of CrTiN transition layer; Continuously feed N2, simultaneously turn on the Cr target and Ti target, with the Cr target current controlled at 6 - 10 A, the Ti target current controlled at 6 - 10 A, the direct current bias voltage controlled at 50 - 100 V, and the time being 30 - 80 min; Step 5, preparation of TiCrN color layer; Continuously feed N2, with the Cr target current controlled at 10 - 0.5 A, the Ti target current controlled at 6 - 10 A, the bias voltage controlled at 50 - 100 V, and the deposition time being 20 - 60 min; Step 6, post - treatment; Anneal under the protection of N2, with the Lab value of the film layer being L: 80 - 84; a 3 - 5; b：8-14。 2. The method for preparing a light gold process of a planar target sputtering coating machine according to claim 1, characterized in that, In Step 1, the substrate is stainless steel or titanium alloy. The substrate is ultrasonically cleaned with acetone for 3 - 4 h, and the cavity of the vacuum coating planar magnetron sputtering equipment is pre - heated to 150 - 200 °C.

3. The preparation process of the light gold color by the planar target sputtering coating machine according to claim 1, characterized in that In Step 2, Ar needs to be introduced into the cavity during the operation of the planar Cr target. The gas flow rate of Ar is 50 - 60 sccm; the deposition rate is 0.8 nm / s, and the thickness of the underlayer is 0.2 - 0.4 μm.

4. The process method for preparing a light gold color by means of the planar target sputtering coating machine according to claim 1, characterized in that, In Step 3, the gas flow rate of N2 linearly increases from 30 sccm to 60 sccm, with a slope of 0.5 sccm / s.

5. The process method for preparing a light gold color by using the planar target sputtering coating machine according to claim 1, characterized in that, In Step 3, the thickness of the intermediate layer is 0.6 - 0.8 μm.

6. The process method for preparing a light gold color by using the planar target sputtering coating machine according to claim 1, characterized in that, In Step 4, the gas flow rate of N2 linearly increases from 10 sccm to 60 sccm.

7. The process method for preparing a light golden color by the planar target sputtering coating machine according to claim 1, characterized in that, In Step 4, the thickness of the transition layer is 0.8 - 1.2 μm.

8. The process method for preparing a light golden color by means of the planar target sputtering coating machine according to claim 1, characterized in that, In Step 5, the Cr target current linearly decreases from 10 A to 0.5 A, with a linear slope of - 0.2 A / min.

9. The process method for preparing a light gold color by the planar target sputtering coating machine according to claim 1, characterized in that, In Step 5, the gas flow rate of N2 is 10 - 60 sccm.

10. The process method for preparing a light gold color by using the planar target sputtering coating machine according to claim 1, characterized in that, In Step 5, the thickness of the color layer is 0.5 - 1 μm.

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