Plating film resistant to strong alkaline cleaning and plating processing method

Abstract

To provide a thin film capable of guaranteeing the strength and density of a thin film to improve acid and alkali resistance, and a method for forming the same.SOLUTION: There is provided a strong alkali cleaning resistant plating film including a glass substrate 1 including a silica dioxide plating layer 2, tri-titanium pentoxide 3, a silica dioxide plating layer, tri-titanium pentoxide, a silica dioxide plating layer, tri-titanium pentoxide, silica dioxide, a lanthanoid material plating layer 4, silica dioxide, and a lanthanoid material plating layer provided in this order. A plating method comprises S1: providing a glass substrate, S2: evacuating a plating sputtering apparatus to 5.00*10-3 PA and S3: preliminarily melting the material; namely, heating a tri-titanium pentoxide solid by fixing three sets of cathode targets in a cavity and setting the current intensity of the apparatus to 440 MA to preliminarily melt it into a liquid; and mixing a lanthanoid material having a solid powder form with a titanium dioxide target and the tantalum pentoxide.SELECTED DRAWING: Figure 3

Description

[Technical field]

[0001] The present invention relates to the field of lens plating, and more particularly to a plating film resistant to strong alkaline cleaning and a plating method. [Background technology]

[0002] The vacuum coating process generally consists of a vacuum cavity, an air extraction system, a heating system, a coating material heating system and a monitoring system, and the coating products are widely used in mobile phones, cameras, projectors, security cameras and so on.

[0003] At present, the most commonly used method in China is thermal deposition using TI3O5 / SiO2, which has a layered structure and low density (Figure 1), so its service life in subsequent environmental tests is relatively short, and it can only be used as an internal accessory of the equipment in practice, and its alkali resistance during cleaning (PH ≥ 12, temperature: 70 degrees, time: 5 minutes) is also low, which causes problems in the product manufacturing process. Manual wiping work requires more effort. Summary of the Invention

[0004] In order to solve the above technical problems, the present invention provides a plating film that is resistant to strong alkali cleaning, which includes a glass substrate having a silicon dioxide plating layer, a titanium dioxide plating layer, a titanium dioxide plating layer, a silicon dioxide plating layer, a titanium dioxide plating layer, a silicon dioxide plating layer, a titanium dioxide plating layer, a lanthanide material plating layer, and a silicon dioxide plating layer formed in this order.

[0005] Preferably, the lanthanide material plating layer comprises a mixture of one or more of the following: lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, and lutetium.

[0006] Preferably, the lanthanide material further contains tantalum and titanium elements mixed therein.

[0007] A plating method for producing a plating film resistant to strong alkaline cleaning, comprising the steps of: S1: Provide a glass substrate; S2: Plating sputtering equipment 5.00 × 10 -3 Vacuum to Pa, S3: Pre-melt the material, i.e. fix three sets of cathode targets in the cavity, and set the current strength of the device to 440M. A By setting the temperature, the titanium dioxide solid is heated and pre-melted into a liquid. This causes the first set of cathode targets to be formed after the temperature is lowered. The lanthanide material in solid powder form was then mixed with titanium dioxide. And and tantalum pentoxide, and pre-melt it into a liquid by heating it by setting the intensity of the device current to 480 MA, so that the lanthanide material is mixed with titanium element and tantalum element; This allows After cooling The second set Solid Cathode Target is formed ,Silicon dioxide is used as the third set of cathode targets. S4: The material is evaporated and plated, that is, oxygen gas and argon gas are injected in a ratio of 1:3-5, the argon gas is ionized by a sputtering device, and the cathode target of the cathode is bombarded by ion bombardment; the third set of silicon dioxide targets, the first set of titanium dioxide targets, the third set of silicon dioxide targets, the first set of titanium dioxide targets, the third set of silicon dioxide targets, the first set of titanium dioxide targets, the third set of silicon dioxide targets, the second set of lanthanide material targets, the third set of silicon dioxide targets, and the second set of lanthanide material targets The thickness of the resulting titanium pentoxide plating film was 450 nm, and the current used was 420 m A, the speed was 3.5 Å / sec, the thickness of the silicon dioxide plating film was 418 nm, and the current was 180 m A, the speed was 8.0 Å / sec, the thickness of the lanthanide material mixture plating film was 53 nm, and the current was 460 m A, the speed is 2.5 Å / sec; S5: Maintain pressure for 30 minutes; S6: Execute gas relief; S7: Inspect the product by measuring the alkaline cleaning resistance spectrum, pack it, and proceed to the next step.

[0008] Preferably, in the vapor deposition plating process, the ratio and amount of argon gas and oxygen gas are adjusted so that when plating silicon dioxide and titanium pentoxide, the total injection amount is 1% and 0.8% of the cavity, and the injection ratio of oxygen gas and argon gas is 1:3 and 2:5; when plating a lanthanide material plating layer, the total injection amount is 0.4% of the cavity, and the injection ratio of oxygen gas and argon gas is 1:5.

[0009] Preferably, the premelting temperature is 1800°C to 2000°C.

[0010] The plating film resistant to strong alkali cleaning provided by the present invention has the following beneficial effects: the present invention uses Ti3O5 / SiO2 to form a film through an ion source film formation process, and at the same time adds an appropriate amount of lanthanide material to process the film, which has a columnar structure (Figure 2) and is more dense. In addition, the plating process can adjust the ratio of oxygen gas and argon gas to ensure the strength and density of the film, and improve the acid and alkali resistance. [Brief description of the drawings]

[0011] In order to describe the technical solutions in the embodiments of the present invention more clearly, the following briefly describes the drawings which need to be used in the description of the embodiments. [Figure 1] FIG. 1 is a microscopic view of a typical silicon dioxide and titanium pentoxide plating film in the prior art. [Diagram 2] FIG. 2 is a diagram showing the configuration of a plating film according to the present invention. [Diagram 3] [Table 1] A microscopic view of a plating film according to the present invention. [Table 1] A summary table of a reliability test report test method according to the present invention. [Table 2] A plating processing spectroscopy test table according to the present invention. [Table 3] A cleaning spectroscopy test table according to the present invention. [Table 4] A high temperature and high humidity storage test table according to the present invention. [Table 5] A thermal shock test table according to the present invention. [Table 6] A high temperature storage test table according to the present invention. [Table 7] A low temperature storage test table according to the present invention. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0012] DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS The technical solutions in the embodiments of the present invention will be described clearly and completely below in conjunction with the drawings in the embodiments of the present invention.

[0013] Example 1 The plating film is resistant to strong alkaline cleaning and includes a glass substrate having a silicon dioxide plating layer, a titanium dioxide plating layer, a titanium dioxide plating layer, a silicon dioxide plating layer, a titanium dioxide plating layer, a titanium dioxide plating layer, a cerium-tantalum-titanium mixed layer, silicon dioxide, and a lanthanide material plating layer formed in this order.

[0014] Example 2 The plating film is resistant to strong alkaline cleaning and includes a glass substrate having a silicon dioxide plating layer, a titanium dioxide plating layer, a titanium dioxide plating layer, a silicon dioxide plating layer, a titanium dioxide plating layer, a titanium dioxide plating layer, a lanthanum-tantalum-titanium mixed layer, silicon dioxide, and a lanthanide material plating layer formed in this order.

[0015] Example 3 The plating film is resistant to strong alkaline cleaning and includes a glass substrate having a silicon dioxide plating layer, a titanium dioxide plating layer, a titanium dioxide plating layer, a silicon dioxide plating layer, a titanium dioxide plating layer, a titanium dioxide plating layer, a praseodymium-tantalum-titanium mixed layer, silicon dioxide, and a lanthanide material plating layer formed in this order.

[0016] Example 4 The plating film is resistant to strong alkaline cleaning and includes a glass substrate having a silicon dioxide plating layer, a titanium dioxide plating layer, a titanium dioxide plating layer, a silicon dioxide plating layer, a titanium dioxide plating layer, a titanium dioxide plating layer, a europium-tantalum-titanium mixed layer, silicon dioxide, and a lanthanide material plating layer formed in this order.

[0017] Example 5 A plating method for producing a plating film resistant to strong alkaline cleaning, comprising the steps of: S1: Provide a glass substrate; S2: Plating sputtering equipment 5.00 × 10 -3 Vacuum to Pa, S3: Pre-melting the material, i.e., fixing three sets of cathode targets in the cavity, and setting the current strength of the device to 440MA to heat the titanium dioxide solid to pre-melt it into liquid, the pre-melting temperature is 1800°C; This causes the first set of cathode targets to be formed after the temperature is lowered. The lanthanide material in solid powder form was then mixed with titanium dioxide. And and tantalum pentoxide, and the lanthanide metal material, titanium dioxide and tantalum pentoxide are also melted and mixed at this temperature, and the current strength of the device is set to 480 MA to heat and pre-melt into a liquid, and the lanthanide material is mixed with titanium element and tantalum element; This allows After cooling The second set Solid Cathode Target is formed ,Silicon dioxide is used as the third set of cathode targets. S4: The material is evaporated and plated, that is, oxygen gas and argon gas are injected into the cavity at 1% and 0.8% injection amount and 1:3 and 2:5 ratio, and the argon gas is ionized by the sputtering device, and the cathode target of the cathode is bombarded by the ion bombardment, and the cathode target is rotated by the turntable inside the sputtering device, and the position of the cathode target can be adjusted. the third set of silicon dioxide targets, the first set of titanium dioxide targets, the third set of silicon dioxide targets, the first set of titanium dioxide targets, the third set of silicon dioxide targets, the first set of titanium dioxide targets, the third set of silicon dioxide targets, the second set of lanthanide material targets, the third set of silicon dioxide targets, and the second set of lanthanide material targets When sputtering the lanthanide material mixed plating layer, the gas injection amount is 0.4%, the thickness of the obtained titanium pentoxide plating film is 450 nm, and the current used is 420 m A, the speed was 3.5 Å / sec, the thickness of the silicon dioxide plating film was 418 nm, and the current was 180 m A, the speed was 8.0 Å / sec, the thickness of the lanthanide material mixture plating film was 53 nm, and the current was 460 m A, the speed is 2.5 Å / sec; S5: Maintain pressure for 30 minutes; S6: Execute gas relief; S7: Inspect the product by measuring the alkaline cleaning resistance spectrum, pack it, and proceed to the next step.

[0018] By adjusting the ratio of argon gas to oxygen gas, the ratio of argon gas increases, the particle kinetics increases, and the plating film can be made denser, and therefore the acid, alkali, and weather resistance is also improved. In addition, by increasing the amount of gas, the film thickness can be increased, and by adjusting the amount of gas injected between different layers, the ratio of oxygen gas also changes, and as the film thickness changes, the stress inside the film decreases due to the change in the amount of oxygen gas, improving the strength of the film.

[0019] Comparative Example A glass substrate is plated in the following order: a silicon dioxide plating layer, a titanium pentoxide plating layer, a silicon dioxide plating layer, a titanium pentoxide plating layer, a silicon dioxide plating layer, a titanium pentoxide plating layer, and silicon dioxide.

[0020] The plating process is as follows: S1: Provide a glass substrate; S2: Plating sputtering equipment 5.00*10 -3 Vacuum to Pa, S3: Pre-melting the material, i.e., fixing two sets of cathode targets in the cavity, and heating the titanium dioxide solid to liquid by setting the current strength of the device to 440MA, the pre-melting temperature is 1800℃, and silicon dioxide is used as the cathode target, and each forms a solid cathode target after cooling; S4: The material is evaporated and plated, that is, oxygen gas and argon gas are injected into the cavity at an injection amount of 1% and a ratio of 1:3, the argon gas is ionized by the sputtering device, and the cathode target of the cathode is bombarded by ion bombardment, the cathode target is rotated by the turntable inside the sputtering device, and the position of the cathode target can be adjusted, and the sputtering is performed in the following order: silicon dioxide, titanium dioxide, silicon dioxide, titanium dioxide, silicon dioxide, titanium dioxide, silicon dioxide; S5: Maintain pressure for 30 minutes; S6: Execute gas relief; S7: Inspect the product by measuring the alkaline cleaning resistance spectrum, pack it, and proceed to the next step.

[0021] The following tests were carried out on the products in the above examples and the plating films produced in the comparative examples.

[0022] Plating spectroscopic test: After plating, the product was subjected to spectroscopic test, the spectrum curve was output, and it was judged whether the spectrum met the specification requirements. The detailed results are shown in Table 2.

[0023] Washing spectroscopy test: After washing with high pH solution, the product was subjected to spectroscopy test, and the spectrum curve was output, and the spectrum met the specification requirements. The detailed results are shown in Table 3.

[0024] High temperature and humidity storage: 1) The temperature of the incubator was set to 85°C ± 3°C, and the relative humidity was set to 85% ± 5%, 2) The test sample was left in the incubator for 1000 hours (hours; the same applies below), 3) The sample was allowed to recover at room temperature (25°C ± 5°C) for 24 hours, and then tested for spectroscopy, appearance, and film strength. The detailed results are shown in Table 4.

[0025] Thermal shock: 1) The samples were stored in a cycle of -40°C±2°C (30 minutes) and 85°C±3°C (30 minutes) for 1000 hours with a temperature change time of 5 minutes. 2) The samples were allowed to recover at room temperature (25°C±5°C) for 24 hours, and then tested for spectroscopy, appearance, and film strength. The detailed results are shown in Table 5.

[0026] High temperature storage: 1) The temperature of the incubator was set to 105°C ± 3°C, and the sample was left in the incubator for 1000 hours. 2) The sample was allowed to recover at room temperature (25°C ± 5°C) for 24 hours, and then the spectroscopy, appearance, and film strength tests were performed. The detailed results are shown in Table 6.

[0027] Low temperature storage: 1) The temperature of the incubator was set to -40℃±3℃, and the sample was left in the incubator for 1000 hours. 2) The sample was allowed to recover at room temperature (25℃±5℃) for 24 hours, and then the spectroscopy, appearance, and film strength tests were performed. The detailed results are shown in Table 7.

[0028] In the above tests, all of the products of Examples 1 to 4 met the requirements, and all of the products manufactured by the method of Example 5 met the requirements. On the other hand, when the comparative example was immersed in a high pH solution and then subjected to the above tests, obvious defects occurred on the surface, making it unsuitable for use.

[0029] This product adds lanthanide materials to the plating film layer, and mixes tantalum and titanium elements to separate the sizes of different ions, thereby reducing the gaps in the film layer after plating. Referring to Figures 1 and 2, it can be seen from the microscopic view after plating in this embodiment that the density of the plating film is greatly increased, and the corrosion resistance is further improved. In addition, another factor that increases the density of the plating film is the plating process. In the plating process, the ratio of argon gas and oxygen gas is adjusted, and after the amount of argon gas is increased, the ion power is increased, and the density of the plating film is further increased. At the same time, the deposition plating of different plating layers is performed in the same cavity, and different amounts of oxygen gas are injected, so that the stress of the plating film between different layers is reduced due to the change in the amount of oxygen gas, and the strength of the plating film is improved.

[0030] [Table 1] JPEG0007607964000001.jpg120170

[0031] [Table 2] JPEG0007607964000002.jpg197170

[0032] [Table 3] JPEG0007607964000003.jpg215170

[0033] [Table 4] JPEG0007607964000004.jpg220170

[0034] [Table 5] JPEG0007607964000005.jpg216170

[0035] [Table 6] JPEG0007607964000006.jpg216170

[0036] [Table 7] JPEG0007607964000007.jpg216170 [Explanation of symbols]

[0037] 1. Glass substrate 2. Silicon dioxide plating layer 3.Titanium pentoxide 4. Lanthanide material plating layer

Claims

1. A plating method for producing a plating film resistant to strong alkaline cleaning, comprising the steps of: S1: Providing a glass substrate; S2: Plating sputtering device 5.00 x 10 -3 Pulling a vacuum on the PA; S3: pre-melting the material, i.e. fixing three sets of cathode targets in the cavity, heating and pre-melting the solid titanium trioxide into liquid by setting the current intensity of the device to 440 MA, thus forming the first set of cathode targets after cooling; mixing the lanthanide material in solid powder form with titanium dioxide and tantalum pentoxide, heating and pre-melting the liquid by setting the current intensity of the device to 480 MA, thus mixing the lanthanide material with titanium element and tantalum element, thus forming the second set of solid cathode targets after cooling; and using silicon dioxide as the third set of cathode targets; S4: The material is vapor-deposited and plated, that is, oxygen gas and argon gas are injected in a ratio of 1:3 to 5, the argon gas is ionized by a sputtering device, and the cathode target of the cathode is bombarded by ion bombardment, so that the silicon dioxide target of the third set, the titanium pentoxide target of the first set, the silicon dioxide target of the third set, the titanium pentoxide target of the first set, the silicon dioxide target of the third set, the titanium pentoxide target of the first set, the silicon dioxide target of the third set, the titanium pentoxide target of the first set, the silicon dioxide target of the third set, sputtering the first set of lanthanide material targets, the second set of lanthanide material targets, the third set of silicon dioxide targets, and the second set of lanthanide material targets in that order, so that the resulting titanium dioxide plating film has a thickness of 450 nm, a current of 420 mA, and a sputtering speed of 3.5 Å / sec; the resulting silicon dioxide plating film has a thickness of 418 nm, a current of 180 mA, and a sputtering speed of 8.0 Å / sec; and the resulting lanthanide material mixture plating film has a thickness of 53 nm, a current of 460 mA, and a sputtering speed of 2.5 Å / sec. S5: Maintaining the pressure for 30 minutes; S6: A step of performing gas relief; S7: inspecting the plating film by the alkaline cleaning resistance measurement spectrum, packaging, and proceeding to the next step.

2. The method for processing a plating film resistant to strong alkali cleaning according to claim 1, characterized in that in the deposition plating process, the ratio and amount of argon gas and oxygen gas are adjusted, and when plating silicon dioxide and titanium pentoxide, the total injection amount is 1% and 0.8% of the cavity, and the injection ratio of oxygen gas and argon gas is 1:3 and 2:5, respectively; when plating a lanthanide material plating layer, the total injection amount is 0.4% of the cavity, and the injection ratio of oxygen gas and argon gas is 1:

5.

3. 2. The method for processing a plating film resistant to strong alkali cleaning according to claim 1, wherein the temperature of pre-melting is 1800°C to 2000°C.

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