A film layer structure with same reflectivity in visible light band and a coating process thereof

Abstract

The application discloses a film layer structure with same reflectivity in a visible light band and a film coating process, the film layer structure comprises, in sequence, a PET substrate layer, a single crystal silicon film layer, a silicon nitride film layer, a silicon oxide film layer, and a niobium pentoxide layer is further coated outside the silicon oxide film layer, and the silicon nitride film layer is composed of three silicon nitride layers; the application further discloses a preparation method for preparing the film layer structure with same reflectivity in the visible light band, and the preparation method comprises the following steps: S1, single crystal silicon deposition; S2, deposition of a first silicon nitride layer; S3, deposition of a second silicon nitride layer; S4, deposition of a third silicon nitride layer; and S5, deposition of a silicon oxide film layer; the film layer structure provided by the application has the same reflectivity in the visible light band, the color index approaches 0, the film layer structure looks transparent and colorless, when the film material is pasted to a back cover, the film material structure cannot be obviously distinguished by naked eyes; the visual beauty of glass is maintained, and the effects of scratch prevention and drop prevention are achieved.

Description

Technical Field

[0001] This invention relates to the field of low-temperature coating technology, specifically to a film structure with the same reflectivity in the visible light band and its coating process. Background Technology

[0002] With the popularization of smartphones, people have begun to pursue differentiation in phone appearance, seeking more unique looks and colors, leading to the development of phone back cover decoration. Back cover glass surface decoration shares similarities with ordinary glass surface decoration, but the decoration methods must be simple in process, low in cost, and easy to mechanize production. Some complex, manually operated surface decoration methods that cause significant pollution are not suitable for phone back cover production. There are two main types of phone back cover glass surface decoration methods: one is to directly decorate the surface of the glass back cover, and the other is to adhere a decorative film to the back cover glass.

[0003] However, in the existing technology, although surface decoration directly on the glass back cover can achieve an aesthetic effect, due to the characteristics of the glass substrate, the surface is easily scratched and broken, which may cause injury to people. On the other hand, attaching a decorative film to the back cover glass can also achieve a decorative effect, but due to the transmission and reflection characteristics of the film material, there are defects that are easily noticed by the human eye.

[0004] Therefore, providing a novel film structure with the same reflectivity in the visible light band and its coating process to solve the aforementioned defects in mobile phone back cover decoration is a major problem that needs to be solved. Summary of the Invention

[0005] To address the shortcomings of existing technologies, the present invention aims to provide a film structure and coating process with the same reflectivity in the visible light band. The technical solution provided by the present invention produces a film material that maintains the same transmittance in the visible light band. While achieving this characteristic, the color index of the film material approaches 0, meaning it appears transparent and colorless. Thus, when the film material is adhered to the back cover, its structure is not clearly discernible to the naked eye. This maintains the visual aesthetics of glass while also providing scratch and drop protection. Furthermore, due to its reflectivity, the film material can also be used as a mirror.

[0006] To achieve the above objectives, the present invention provides the following technical solution:

[0007] A coating process for preparing a film structure with the same reflectivity in the visible light band includes the following steps:

[0008] S1. Monocrystalline silicon deposition: Monocrystalline silicon is bombarded on the surface of a PET substrate by magnetron sputtering to form a monocrystalline silicon film layer and deposit it on the surface of the PET substrate.

[0009] S2. Deposition of the first silicon nitride layer:

[0010] S201. Deposition of the first silicon nitride layer: A first silicon nitride layer with a thickness of 14-16 nm is formed on the surface of a single-crystal silicon film by magnetron sputtering; the process parameters of the magnetron sputtering are: a flow rate of 1.5 m-3 m / min, a power of 10-24 kW, and the rare gas introduced is a mixture of argon and nitrogen in a mass ratio of 1:1, with an argon flow rate of 90-120 sccm and a nitrogen flow rate of 90-120 sccm.

[0011] S202. Argon ion irradiation: The first silicon nitride layer is irradiated with a voltage of 20-300 kV, an irradiation energy of 40-300 keV, and an irradiation dose of 10. 10 -10 15 ions / cm 2 Argon ion irradiation for 5-10 minutes;

[0012] S203. Niobium pentoxide film deposition: Adjust argon ion irradiation parameters to a voltage of 300-400 kV, an irradiation energy of 300-500 keV, and an irradiation dose of 10... 11 -10 16 ions / cm 2 Under irradiation, a 3-5 nm thick niobium pentoxide film is formed on the surface of the first silicon nitride layer by magnetron sputtering and left to stand at room temperature for 1-2 hours.

[0013] S204. Niobium pentoxide film modification: The surface of the niobium pentoxide film is cleaned with Plasma. Argon gas is introduced to generate high-energy plasma to bombard the surface of the niobium pentoxide film, removing the niobium pentoxide layer on the surface of the first silicon nitride layer. The argon gas is introduced at 80-150 sccm, the radio frequency power is 1-3 kW, and the cleaning time is 5-10 seconds.

[0014] S3. Deposition of the second silicon nitride layer:

[0015] S301. Deposition of the second silicon nitride layer: A second silicon nitride layer with a thickness of 8-10 nm is formed on the surface of the first silicon nitride layer by magnetron sputtering; the process parameters of the magnetron sputtering are: a flow rate of 1.5 m-3 m / min, a power of 8-18 kW, and the rare gas introduced is a mixture of argon and nitrogen in a mass ratio of 1:1, with an argon flow rate of 90-120 sccm and a nitrogen flow rate of 90-120 sccm.

[0016] S302. Niobium pentoxide film deposition: at a voltage of 300-400 kV, an irradiation energy of 300-500 keV, and an irradiation dose of 10... 11 -10 16 ions / cm 2Under irradiation, a 2-3 nm thick niobium pentoxide layer is formed on the surface of the second silicon nitride layer by magnetron sputtering and left to stand at room temperature for 1-1.5 h.

[0017] S303. Niobium pentoxide film modification: The surface of the niobium pentoxide film is cleaned with Plasma. Argon gas is introduced to generate high-energy plasma to bombard the surface of the niobium pentoxide film, removing the niobium pentoxide layer on the surface of the second silicon nitride layer. The argon gas is introduced at 80-150 sccm, the radio frequency power is 1-3 kW, and the cleaning time is 4-7 seconds.

[0018] S4. Deposition of the third silicon nitride layer:

[0019] S401. Deposition of the third silicon nitride layer: A third silicon nitride layer with a thickness of 8-14 nm is formed on the surface of the second silicon nitride layer by magnetron sputtering; the process parameters of the magnetron sputtering are: a flow rate of 1.5 m-3 m / min, a power of 12-20 kW, and the rare gas introduced is a mixture of argon and nitrogen in a mass ratio of 1:1, with an argon flow rate of 90-120 sccm and a nitrogen flow rate of 90-120 sccm.

[0020] S402. Niobium pentoxide film deposition: at a voltage of 300-400 kV, an irradiation energy of 300-500 keV, and an irradiation dose of 10... 11 -10 16 ions / cm 2 Under irradiation, a 2-3 nm thick niobium pentoxide layer is formed on the surface of the third silicon nitride layer by magnetron sputtering and left to stand at room temperature for 1-2 hours;

[0021] S403. Niobium pentoxide film modification: The surface of the niobium pentoxide film is cleaned with Plasma. Argon gas is introduced to generate high-energy plasma to bombard the surface of the niobium pentoxide film, removing the niobium pentoxide layer on the surface of the third silicon nitride layer. The argon gas is introduced at 80-150 sccm, the radio frequency power is 1-3 kW, and the cleaning time is 5-7 seconds.

[0022] S5. Deposition of silicon oxide film: A 20-30 nm thick silicon oxide film is formed on the surface of the third silicon nitride layer by magnetron sputtering, thus obtaining a film structure with the same reflectivity in the visible light band.

[0023] Preferably, in S1, the process parameters for magnetron sputtering are: a travel speed of 0.5-1.5 m / min, a power of 5-15 kW, and the rare gas introduced is argon with a purity of ≥99.99% and a flow rate of 100-200 sccm.

[0024] Preferably, in S203, S302 and S402, the magnetron sputtering coating process parameters for the niobium pentoxide film are: a travel speed of 1.5m-3m / min, a power of 15-30kw, and the rare gas introduced is a mixture of argon and nitrogen in a mass ratio of 1:1, with an argon flow rate of 100-120sccm and a nitrogen flow rate of 100-120sccm.

[0025] Preferably, in S5, the process parameters for magnetron sputtering are: a travel speed of 1.5m-3m / min, a power of 16-24kw, and the rare gas introduced is a mixture of argon and oxygen in a mass ratio of 1:1, with an argon flow rate of 90-120sccm and an oxygen flow rate of 90-120sccm.

[0026] Preferably, after step S5, pure oxygen needs to be introduced to ensure the complete reaction of silicon dioxide. The purity of the pure oxygen is ≥99.99%, the flow rate is 150-200 sccm, and the time for introducing pure oxygen is 1-2 hours.

[0027] Preferably, after step S5, a niobium pentoxide layer is deposited on the outside of the silicon oxide film by magnetron sputtering at a speed of 1.5m-3m / min and a power of 15-30kw. The rare gas introduced is a mixture of argon and nitrogen in a mass ratio of 1:1, with an argon flow rate of 100-120sccm and a nitrogen flow rate of 100-120sccm.

[0028] A film structure with the same reflectivity in the visible light band, prepared based on the aforementioned coating process, comprises a monocrystalline silicon film layer, a silicon nitride film layer, and a silicon oxide film layer sequentially deposited on a PET substrate layer.

[0029] The silicon nitride film includes a first silicon nitride layer, a second silicon nitride layer, and a third silicon nitride layer deposited sequentially.

[0030] The thickness of the first silicon nitride layer is 14-16 nm, the thickness of the second silicon nitride layer is 8-10 nm, and the thickness of the third silicon nitride layer is 8-14 nm;

[0031] The thickness of the silicon oxide film is 20-30 nm.

[0032] Preferably, a niobium pentoxide layer is sputtered outside the silicon oxide film; the thickness of the niobium pentoxide layer is 1-2 nm.

[0033] Preferably, the thickness of the silicon nitride film is controlled to be 36 nm, and the thickness of the silicon oxide film is controlled to be 25 nm.

[0034] Compared with the prior art, the beneficial effects of the present invention are:

[0035] 1. Compared with direct decoration on the back cover glass, the technical solution of the present invention improves the adhesion of the film by bombarding the surface of the film material with monocrystalline silicon. The resulting film material can effectively prevent the risk of scratches on the back cover glass. At the same time, the film material attached to the glass also has an explosion-proof effect. Even if the glass breaks due to excessive force, the broken glass will adhere to the surface of the film material to prevent it from causing harm to the human body.

[0036] 2. Compared with traditional decorative films, this invention improves the reflectivity of the film material by using silicon nitride and niobium pentoxide, absorbing yellow light and effectively adjusting color indicators. Without affecting the thickness of the silicon nitride and silicon oxide film layers, the residual use of niobium pentoxide can remove various dazzling colors. In the visible light band, the transmittance is around 80%, the reflectivity is around 20%, and the product's color b-value is <1, approaching 0, thus removing various dazzling colors. While maintaining the various visual characteristics of the glass, the film structure covering the back of the glass is difficult for the naked eye to distinguish, improving the aesthetics and practicality of the glass. At the same time, because the film material has a certain reflectivity, it can also be used as a mirror. Attached Figure Description

[0037] Figure 1 This is a flowchart illustrating the fabrication process of the film structure with the same reflectivity in the visible light band according to the present invention.

[0038] Figure 2 This is a flowchart of the process for preparing the first silicon nitride layer of the present invention;

[0039] Figure 3 This is a flowchart of the process for preparing the second silicon nitride layer of the present invention;

[0040] Figure 4 This is a flowchart of the process for preparing the third silicon nitride layer of the present invention;

[0041] Figure 5 This is a schematic diagram of the film structure with the same reflectivity in the visible light band of the present invention.

[0042] In the figure: 1. PET substrate layer; 2. Monocrystalline silicon film layer; 31. First silicon nitride layer; 32. Second silicon nitride layer; 33. Third silicon nitride layer; 4. Silicon oxide layer; 5. Niobium pentoxide layer. Detailed Implementation

[0043] The present invention will now be clearly and completely described in conjunction with embodiments thereof. Obviously, the described embodiments are merely some, not all, of the embodiments of the present invention. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without creative effort are within the scope of protection of the present invention.

[0044] Please see Figure 1-5The present invention provides a technical solution:

[0045] Example 1

[0046] S1. Single crystal silicon deposition: By magnetron sputtering, and setting specific process parameters as follows: speed 0.5m / min, power 5kw, 99.99% pure argon gas, and argon gas flow rate controlled at 100sccm, single crystal silicon is bombarded on the surface of PET substrate and deposited on the surface of PET substrate. The thickness of single crystal silicon film is 1-2nm.

[0047] S2. Deposition of the first silicon nitride layer:

[0048] S201. Deposition of the first silicon nitride layer: By magnetron sputtering, and setting the specific process parameters as follows: speed 1.5m / min, power 10kw, argon and nitrogen gas in a 1:1 ratio, argon gas flow rate controlled at 90sccm, nitrogen gas flow rate controlled at 90sccm, a 14nm thick first silicon nitride layer is formed on the surface of the single crystal silicon film.

[0049] S202. Argon ion irradiation: The first silicon nitride layer is subjected to a voltage of 90 kV; the irradiation energy is 100 keV, and the irradiation dose is 10. 10 ions / cm 2 Argon ion irradiation for 5 minutes; because the first silicon nitride layer is at the bottom of the film structure, a separate argon ion irradiation is required after the first silicon nitride layer is deposited to obtain a first silicon nitride layer with better performance, while a separate argon ion irradiation is not required when depositing the second and third silicon nitride layers.

[0050] S203. Niobium pentoxide film deposition: Adjust argon ion irradiation parameters to a voltage of 300 kV, irradiation energy of 300 keV, and irradiation dose of 10. 11 ions / cm 2 Under irradiation, a 3 nm thick niobium pentoxide layer was formed on the surface of the first silicon nitride layer by magnetron sputtering. After standing at room temperature for 1 hour, the magnetron sputtering process parameters were set as follows: speed 1.5 m / min, power 15 kW, and the rare gas introduced was a mixture of argon and nitrogen in a mass ratio of 1:1, with an argon flow rate of 100 sccm and a nitrogen flow rate of 100 sccm.

[0051] S204. Niobium pentoxide film modification: The surface of the niobium pentoxide layer is cleaned by using plasma cleaning. Argon gas is introduced to generate high-energy plasma to bombard the surface of the niobium pentoxide layer, removing the niobium pentoxide layer on the surface of the first silicon nitride layer. The argon gas is introduced at 80 sccm, the radio frequency power is 1 kW, and the cleaning time is 5 seconds.

[0052] S205. Niobium pentoxide detection: After cleaning and modifying the niobium pentoxide film on the surface of the first silicon nitride layer, elemental diffraction is used to detect whether there is any niobium pentoxide residue on the surface of the first silicon nitride layer. Elemental diffraction for detecting chemical element residues is a conventional existing technology, and only the detection method for niobium pentoxide residues is described here without further details.

[0053] S3. Deposition of the second silicon nitride layer:

[0054] S301. Deposition of the second silicon nitride layer: By magnetron sputtering, and setting the specific process parameters as follows: speed 1.5m / min, power 8kw, argon and nitrogen gas in a 1:1 ratio, argon gas flow rate controlled at 90sccm, nitrogen gas flow rate controlled at 90sccm, an 8nm thick second silicon nitride layer is formed on the surface of the first silicon nitride layer.

[0055] S302. Niobium pentoxide film deposition: Adjust argon ion irradiation parameters to a voltage of 300 kV, irradiation energy of 300 keV, and irradiation dose of 10. 11 ions / cm 2 Under irradiation, a 2nm thick niobium pentoxide layer was formed on the surface of the second silicon nitride layer by magnetron sputtering. After standing at room temperature for 1 hour, the magnetron sputtering process parameters were set as follows: speed 1.5m / min, power 15kw, and the rare gas introduced was a mixture of argon and nitrogen in a mass ratio of 1:1, with an argon flow rate of 100sccm and a nitrogen flow rate of 100sccm.

[0056] S303. Niobium pentoxide film modification: The surface of the niobium pentoxide layer is cleaned by using plasma cleaning. Argon gas is introduced to generate high-energy plasma to bombard the surface of the niobium pentoxide layer, removing the niobium pentoxide layer on the surface of the second silicon nitride layer. The argon gas is introduced at 80 sccm, the radio frequency power is 1 kW, and the cleaning time is 4 seconds.

[0057] S304. Niobium pentoxide detection: After cleaning and modifying the niobium pentoxide film on the surface of the second silicon nitride layer, elemental diffraction is used to detect whether there is any niobium pentoxide residue on the surface of the second silicon nitride layer.

[0058] S4. Deposition of the third silicon nitride layer:

[0059] S401. Deposition of the third silicon nitride layer: By magnetron sputtering, with specific parameters set as follows: speed 1.5m / min, power 12kw, argon and nitrogen gas in a 1:1 ratio, argon gas flow rate controlled at 90sccm, and nitrogen gas flow rate controlled at 90sccm, an 8nm thick third silicon nitride layer is formed on the surface of the second silicon nitride layer.

[0060] S402. Niobium pentoxide film deposition: Adjust argon ion irradiation parameters to a voltage of 300 kV, irradiation energy of 300 keV, and irradiation dose of 10. 11 ions / cm 2 Under irradiation, a 2nm thick niobium pentoxide layer was formed on the surface of the second silicon nitride layer by magnetron sputtering. After standing at room temperature for 1 hour, the magnetron sputtering process parameters were set as follows: speed 1.5m / min, power 15kw, and the rare gas introduced was a mixture of argon and nitrogen in a mass ratio of 1:1, with an argon flow rate of 100sccm and a nitrogen flow rate of 100sccm.

[0061] S403. Niobium pentoxide film modification: The surface of the niobium pentoxide layer is cleaned by using plasma cleaning. Argon gas is introduced to generate high-energy plasma to bombard the surface of the niobium pentoxide layer, removing the niobium pentoxide layer on the surface of the second silicon nitride layer. The argon gas is introduced at 80 sccm, the radio frequency power is 1 kW, and the cleaning time is 5 seconds.

[0062] S404. Niobium pentoxide detection: After cleaning and modifying the niobium pentoxide film on the surface of the third silicon nitride layer, elemental diffraction is used to detect whether there is any niobium pentoxide residue on the surface of the third silicon nitride layer.

[0063] S5. Deposition of silicon oxide film: By magnetron sputtering, with specific parameters set as follows: speed 1.5m / min, power 16kw, argon and oxygen in a 1:1 ratio, argon flow rate controlled at 90sccm, oxygen flow rate controlled at 90sccm, a 20nm thick silicon oxide film is formed on the surface of the third silicon nitride layer.

[0064] S6. Purification of the silicon oxide film: Introduce 99.99% pure oxygen at a flow rate of 150 sccm for 1 hour to ensure complete reaction of the silicon oxide.

[0065] S7. Niobium pentoxide film deposition: A 3nm thick niobium pentoxide layer is formed on the surface of the silicon oxide film by magnetron sputtering. After standing at room temperature for 1 hour, a film structure with the same reflectivity in the visible light band is obtained. The magnetron sputtering process parameters are set as follows: speed 1.5m / min, power 15kw, and the rare gas introduced is a mixture of argon and nitrogen in a mass ratio of 1:1, with an argon flow rate of 100sccm and a nitrogen flow rate of 100sccm.

[0066] Example 2

[0067] S1. Single crystal silicon deposition: By magnetron sputtering, and setting specific process parameters as follows: speed 1.5m / min, power 15kw, 99.99% pure argon gas is introduced, and the argon gas flow rate is controlled at 200sccm, the single crystal silicon bombards the surface of the PET substrate and is deposited on the surface of the PET substrate.

[0068] S2. Deposition of the first silicon nitride layer:

[0069] S201. Deposition of the first silicon nitride layer: A 16nm thick first silicon nitride layer is formed on the surface of a single crystal silicon film by magnetron sputtering with specific process parameters set as follows: speed 3m / min, power 24kw, argon and nitrogen gas in a 1:1 ratio, argon gas flow rate controlled at 120sccm, and nitrogen gas flow rate controlled at 120sccm.

[0070] S202. Argon ion irradiation: The first silicon nitride layer is subjected to a voltage of 300 kV; the irradiation energy is 300 keV, and the irradiation dose is 10. 15 ions / cm 2 Argon ion irradiation for 10 minutes;

[0071] S203. Niobium pentoxide film deposition: Adjust argon ion irradiation parameters to a voltage of 400 kV, irradiation energy of 500 keV, and irradiation dose of 10. 16 ions / cm 2 Under irradiation, a 5 nm thick niobium pentoxide layer was formed on the surface of the first silicon nitride layer by magnetron sputtering. After standing at room temperature for 2 hours, the magnetron sputtering process parameters were set as follows: speed 3 m / min, power 28 kW, and the rare gas introduced was a mixture of argon and nitrogen in a mass ratio of 1:1, with an argon flow rate of 120 sccm and a nitrogen flow rate of 120 sccm.

[0072] S204. Niobium pentoxide film modification: The surface of the niobium pentoxide layer is cleaned by using plasma cleaning. Argon gas is introduced to generate high-energy plasma to bombard the surface of the niobium pentoxide layer, removing the niobium pentoxide layer on the surface of the first silicon nitride layer. The argon gas is introduced at 150 sccm, the radio frequency power is 3 kW, and the cleaning time is 10 seconds.

[0073] S205. Niobium pentoxide detection: After cleaning and modifying the niobium pentoxide film on the surface of the first silicon nitride layer, elemental diffraction is used to detect whether there is any niobium pentoxide residue on the surface of the first silicon nitride layer.

[0074] S3. Deposition of the second silicon nitride layer:

[0075] S301. Deposition of the second silicon nitride layer: By magnetron sputtering, and setting the specific process parameters as follows: speed 3m / min, power 18kw, argon and nitrogen gas in a 1:1 ratio, argon gas flow rate controlled at 120sccm, nitrogen gas flow rate controlled at 120sccm, a 10nm thick second silicon nitride layer is formed on the surface of the first silicon nitride layer.

[0076] S302. Niobium pentoxide film deposition: Adjust argon ion irradiation parameters to a voltage of 400 kV, irradiation energy of 500 keV, and irradiation dose of 10. 16 ions / cm 2 Under irradiation, a 3nm thick niobium pentoxide layer was formed on the surface of the second silicon nitride layer by magnetron sputtering. After standing at room temperature for 2 hours, the magnetron sputtering process parameters were set as follows: speed 3m / min, power 18kw, and the rare gas introduced was a mixture of argon and nitrogen in a mass ratio of 1:1, with an argon flow rate of 120sccm and a nitrogen flow rate of 120sccm.

[0077] S303. Niobium pentoxide film modification: The surface of the niobium pentoxide layer is cleaned by using plasma cleaning. Argon gas is introduced to generate high-energy plasma to bombard the surface of the niobium pentoxide layer, removing the niobium pentoxide layer on the surface of the second silicon nitride layer. The argon gas is introduced at 150 sccm, the radio frequency power is 3 kW, and the cleaning time is 7 seconds.

[0078] S304. Niobium pentoxide detection: After cleaning and modifying the niobium pentoxide film on the surface of the second silicon nitride layer, elemental diffraction is used to detect whether there is any niobium pentoxide residue on the surface of the second silicon nitride layer.

[0079] S4. Deposition of the third silicon nitride layer:

[0080] S401. Deposition of the third silicon nitride layer: A 14nm thick third silicon nitride layer is formed on the surface of the second silicon nitride layer by magnetron sputtering with specific parameters set as follows: speed 3m / min, power 20kw, argon and nitrogen gas in a 1:1 ratio, argon gas flow rate controlled at 120sccm, and nitrogen gas flow rate controlled at 120sccm.

[0081] S402. Niobium pentoxide film deposition: Adjust argon ion irradiation parameters to a voltage of 400 kV, irradiation energy of 500 keV, and irradiation dose of 10. 16 ions / cm 2Under irradiation, a 3nm thick niobium pentoxide layer was formed on the surface of the second silicon nitride layer by magnetron sputtering. After standing at room temperature for 2 hours, the magnetron sputtering process parameters were set as follows: speed 3m / min, power 30kw, and the rare gas introduced was a mixture of argon and nitrogen in a mass ratio of 1:1, with an argon flow rate of 120sccm and a nitrogen flow rate of 120sccm.

[0082] S403. Niobium pentoxide film modification: The surface of the niobium pentoxide layer is cleaned by using plasma cleaning. Argon gas is introduced to generate high-energy plasma to bombard the surface of the niobium pentoxide layer, removing the niobium pentoxide layer on the surface of the second silicon nitride layer. The argon gas is introduced at 150 sccm, the radio frequency power is 3 kW, and the cleaning time is 7 seconds.

[0083] S404. Niobium pentoxide detection: After cleaning and modifying the niobium pentoxide film on the surface of the third silicon nitride layer, elemental diffraction is used to detect whether there is any niobium pentoxide residue on the surface of the third silicon nitride layer.

[0084] S5. Deposition of silicon oxide film: By magnetron sputtering, with specific parameters set as follows: speed 3m / min, power 24kw, argon and oxygen in a 1:1 ratio, argon flow rate controlled at 120sccm, oxygen flow rate controlled at 120sccm, a 30nm thick silicon oxide film is formed on the surface of the third silicon nitride layer.

[0085] S6. Purification of the silicon oxide film: Introduce 99.99% pure oxygen at a flow rate of 200 sccm for 2 hours to ensure complete reaction of the silicon oxide.

[0086] S7. Niobium pentoxide film deposition: A 5nm thick niobium pentoxide layer is formed on the surface of the silicon oxide film by magnetron sputtering. After standing at room temperature for 2 hours, a film structure with the same reflectivity in the visible light band is obtained. The magnetron sputtering process parameters are set as follows: speed 3m / min, power 30kW, and the rare gas introduced is a mixture of argon and nitrogen in a mass ratio of 1:1, with an argon flow rate of 120sccm and a nitrogen flow rate of 120sccm.

[0087] Example 3

[0088] S1. Single crystal silicon deposition: By magnetron sputtering, and setting specific process parameters as follows: speed 1m / min, power 12kw, 99.99% pure argon gas, and argon gas flow rate controlled at 150sccm, single crystal silicon is bombarded on the surface of PET substrate and deposited on the surface of PET substrate.

[0089] S2. Deposition of the first silicon nitride layer:

[0090] S201. Deposition of the first silicon nitride layer: By magnetron sputtering, and setting the specific process parameters as follows: speed 2m / min, power 18kw, argon and nitrogen gas in a 1:1 ratio, argon gas flow rate controlled at 100sccm, nitrogen gas flow rate controlled at 100sccm, a 15nm thick first silicon nitride layer is formed on the surface of the single crystal silicon film.

[0091] S202. Argon ion irradiation: The first silicon nitride layer is subjected to a voltage of 200 kV; the irradiation energy is 200 keV, and the irradiation dose is 10. 12 ions / cm 2 Argon ion irradiation for 8 minutes;

[0092] S203. Niobium pentoxide film deposition: Adjust argon ion irradiation parameters to a voltage of 350 kV, irradiation energy of 400 keV, and irradiation dose of 10. 13 ions / cm 2 Under irradiation, a 4 nm thick niobium pentoxide layer was formed on the surface of the first silicon nitride layer by magnetron sputtering. After standing at room temperature for 1.5 h, the magnetron sputtering process parameters were set as follows: speed 2 m / min, power 22 kW, and the rare gas introduced was a mixture of argon and nitrogen in a mass ratio of 1:1, with an argon flow rate of 110 sccm and a nitrogen flow rate of 110 sccm.

[0093] S204. Niobium pentoxide film modification: The surface of the niobium pentoxide layer is cleaned by using plasma cleaning. Argon gas is introduced to generate high-energy plasma to bombard the surface of the niobium pentoxide layer, removing the niobium pentoxide layer on the surface of the first silicon nitride layer. The argon gas is introduced at 130 sccm, the radio frequency power is 2 kW, and the cleaning time is 8 seconds.

[0094] S205. Niobium pentoxide detection: After cleaning and modifying the niobium pentoxide film on the surface of the first silicon nitride layer, elemental diffraction is used to detect whether there is any niobium pentoxide residue on the surface of the first silicon nitride layer.

[0095] S3. Deposition of the second silicon nitride layer:

[0096] S301. Deposition of the second silicon nitride layer: By magnetron sputtering, and setting the specific process parameters as follows: speed 2m / min, power 14kw, argon and nitrogen gas in a 1:1 ratio, argon gas flow rate controlled at 110sccm, nitrogen gas flow rate controlled at 110sccm, a 19nm thick second silicon nitride layer is formed on the surface of the first silicon nitride layer.

[0097] S302. Niobium pentoxide film deposition: Adjust argon ion irradiation parameters to a voltage of 350 kV, irradiation energy of 400 keV, and irradiation dose of 10. 14 ions / cm2 Under irradiation, a 2nm thick niobium pentoxide layer was formed on the surface of the second silicon nitride layer by magnetron sputtering. After standing at room temperature for 1.5h, the magnetron sputtering process parameters were set as follows: speed 2m / min, power 14kw, and the rare gas introduced was a mixture of argon and nitrogen in a mass ratio of 1:1, with an argon flow rate of 110sccm and a nitrogen flow rate of 110sccm.

[0098] S303. Niobium pentoxide film modification: The surface of the niobium pentoxide layer is cleaned by using plasma cleaning. Argon gas is introduced to generate high-energy plasma to bombard the surface of the niobium pentoxide layer, removing the niobium pentoxide layer on the surface of the second silicon nitride layer. The argon gas is introduced at 130 sccm, the radio frequency power is 2 kW, and the cleaning time is 6 seconds.

[0099] S304. Niobium pentoxide detection: After cleaning and modifying the niobium pentoxide film on the surface of the second silicon nitride layer, elemental diffraction is used to detect whether there is any niobium pentoxide residue on the surface of the second silicon nitride layer.

[0100] S4. Deposition of the third silicon nitride layer:

[0101] S401. Deposition of the third silicon nitride layer: A 10nm thick third silicon nitride layer is formed on the surface of the second silicon nitride layer by magnetron sputtering with specific parameters set as follows: speed 2m / min, power 16kw, argon and nitrogen gas in a 1:1 ratio, argon gas flow rate controlled at 110sccm, and nitrogen gas flow rate controlled at 110sccm.

[0102] S402. Niobium pentoxide film deposition: Adjust argon ion irradiation parameters to a voltage of 350 kV, irradiation energy of 400 keV, and irradiation dose of 10. 14 ions / cm 2 Under irradiation, a 2nm thick niobium pentoxide layer was formed on the surface of the second silicon nitride layer by magnetron sputtering. After standing at room temperature for 1.5h, the magnetron sputtering process parameters were set as follows: speed 2m / min, power 25kw, and the rare gas introduced was a mixture of argon and nitrogen in a mass ratio of 1:1, with an argon flow rate of 110sccm and a nitrogen flow rate of 110sccm.

[0103] S403. Niobium pentoxide film modification: The surface of the niobium pentoxide layer is cleaned by using plasma cleaning. Argon gas is introduced to generate high-energy plasma to bombard the surface of the niobium pentoxide layer, removing the niobium pentoxide layer on the surface of the second silicon nitride layer. The argon gas is introduced at 130 sccm, the radio frequency power is 2 kW, and the cleaning time is 5 seconds.

[0104] S404. Niobium pentoxide detection: After cleaning and modifying the niobium pentoxide film on the surface of the third silicon nitride layer, elemental diffraction is used to detect whether there is any niobium pentoxide residue on the surface of the third silicon nitride layer.

[0105] S5. Deposition of silicon oxide film: By magnetron sputtering, with specific parameters set as follows: speed 2m / min, power 18kw, argon and oxygen in a 1:1 ratio, argon flow rate controlled at 110sccm, oxygen flow rate controlled at 110sccm, a 25nm thick silicon oxide film is formed on the surface of the third silicon nitride layer.

[0106] S6. Purification of the silicon oxide film: Introduce 99.99% pure oxygen at a flow rate of 170 sccm for 1.5 h to ensure complete reaction of the silicon oxide.

[0107] S7. Niobium pentoxide film deposition: A 4nm thick niobium pentoxide layer is formed on the surface of the silicon oxide film by magnetron sputtering. After standing at room temperature for 1.5h, a film structure with the same reflectivity in the visible light band is obtained. The magnetron sputtering process parameters are set as follows: speed 2m / min, power 25kw, and the rare gas introduced is a mixture of argon and nitrogen in a mass ratio of 1:1, with an argon flow rate of 110sccm and a nitrogen flow rate of 110sccm.

[0108] Comparative Example

[0109] Comparative Example 1:

[0110] The difference between Comparative Example 1 and Example 1 is that in Comparative Example 1, steps S2, S3, and S4, which originally existed in Example 1, were omitted, thereby eliminating the steps of "deposition of the first silicon nitride layer", "deposition of the second silicon nitride layer", "deposition of the third silicon nitride layer", "deposition of the niobium pentoxide layer", and "modification of the niobium pentoxide layer". In Comparative Example 1, a 20 nm silicon nitride layer is formed by a single deposition, and the silicon oxide film layer is deposited with a thickness of 10 nm in step S5. The remaining steps are exactly the same as those in Example 1.

[0111] Comparative Example 2:

[0112] The difference between Comparative Example 2 and Example 1 is that steps S2, S3, and S4, which were originally present in Example 1, were omitted in Comparative Example 2, thereby eliminating the steps of "deposition of the first silicon nitride layer", "deposition of the second silicon nitride layer", "deposition of the third silicon nitride layer", "deposition of the niobium pentoxide layer", and "modification of the niobium pentoxide layer". In Comparative Example 2, a 30 nm silicon nitride layer is formed by a single deposition, and the silicon oxide film layer is deposited with a thickness of 20 nm in step S5. The remaining steps are exactly the same as those in Example 1.

[0113] Comparative Example 3:

[0114] The difference between Comparative Example 3 and Example 1 is that steps S2, S3, and S4, which were originally present in Example 1, were omitted in Comparative Example 3, thereby eliminating the steps of "deposition of niobium pentoxide layer" and "modification of niobium pentoxide layer". A silicon nitride layer with a total thickness of 30 nm was formed by three depositions, and a silicon oxide film layer with a thickness of 20 nm was deposited in step S5. The remaining steps are exactly the same in Comparative Example 3 and Example 1.

[0115] Comparative Example 4:

[0116] The only difference between Comparative Example 4 and Example 1 is that steps S2, S3, and S4, which were originally present in Example 1, were omitted in Comparative Example 4, thereby eliminating the steps of "deposition of niobium pentoxide layer" and "modification of niobium pentoxide layer". In Comparative Example 4, the thickness of the silicon nitride film after three depositions is 20 nm, and the thickness of the silicon oxide film in step S5 is 10 nm. The remaining steps are exactly the same as those in Example 1.

[0117] The presence or absence of niobium pentoxide in Examples 1-3 and Comparative Examples 1-5, and the corresponding transmittance and reflectance at the 550nm wavelength were measured. The results are shown in the table below:

[0118]

[0119]

[0120] The test results in the table show that the color indicators of Examples 1-3 are significantly better than those of Comparative Examples 1-5. Taking the visible light band of 550nm as an example, the transmittance of 550nm is about 80%, the reflectance is about 20%, and the color B value is <1. Therefore, the film structure with the same reflectance in the visible light band provided by the present invention is reliable. At the same time, there are significant differences in the color indicators between Example 1 and Comparative Examples 1-5. This invention demonstrates that, based on the modification of silicon nitride film with niobium pentoxide, and with the silicon nitride film thickness between 30-40 nm and the silicon oxide film thickness between 20-30 nm, without affecting the overall thickness of the silicon nitride film, the method of first coating and then cleaning allows a residual portion of the niobium pentoxide film to remain on the surface of the silicon nitride film. Based on the inherent properties of niobium pentoxide, its combination with the silicon nitride film can effectively adjust color indicators. In the visible light band, the transmittance is around 80%, the reflectance is around 20%, and the product's color b-value is <1, approaching 0. This eliminates various dazzling colors, and while maintaining the various visual characteristics of the glass, the film structure covering the back of the glass is difficult for the naked eye to distinguish, improving the aesthetics and practicality of the glass.

[0121] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A coating process for preparing a film layer structure with the same reflectivity in the visible light band, characterized in that, Comprising the following steps: S1. Single crystal silicon deposition: The surface of the PET substrate is bombarded by single crystal silicon by the method of magnetron sputtering to form a single crystal silicon film layer and deposit on the surface of the PET substrate; S2. Deposition of the first silicon nitride layer: S201. First silicon nitride layer deposition: A 14-16 nm thick first silicon nitride layer is formed on the surface of the single crystal silicon film layer by magnetron sputtering; the process parameters of the magnetron sputtering are: walking speed 1.5-3 m / min, power 10-24 kw, the mixed gas of argon and nitrogen with a mass ratio of 1:1 is introduced, argon flow 90-120 sccm, nitrogen flow 90-120 sccm; S202. Argon ion irradiation: the formed first silicon nitride layer is irradiated with argon ions at a voltage of 20-300 kV, an irradiation energy of 40-300 keV, and an irradiation dose of 10 10 -10 15 ions / cm 2 for 5-10 min. S203. Depositing a niobium pentoxide film layer: adjust argon ion irradiation parameters, at a voltage of 300-400 kV, irradiation energy of 300-500 keV, irradiation dose of 10 11 -10 16 ions / cm 2 Under the irradiation conditions, a 3-5 nm thick niobium pentoxide film layer is formed on the surface of the first silicon nitride layer by magnetron sputtering, and is left at room temperature for 1-2 h. S204. Modification of the niobium pentoxide film layer: The surface of the niobium pentoxide film layer is cleaned by plasma, argon plasma is generated to bombard the surface of the niobium pentoxide film layer, and the first silicon nitride layer on the surface of the niobium pentoxide layer is removed, the argon flow is controlled at 80-150 sccm, the radio frequency power is 1-3 kw, and the cleaning time is 5-10 s; S3. Deposition of the second silicon nitride layer: S301. Second silicon nitride layer deposition: A 8-10 nm thick second silicon nitride layer is formed on the surface of the first silicon nitride layer by magnetron sputtering; the process parameters of the magnetron sputtering are: walking speed 1.5-3 m / min, power 8-18 kw, the mixed gas of argon and nitrogen with a mass ratio of 1:1 is introduced, argon flow 90-120 sccm, nitrogen flow 90-120 sccm; S302. Depositing a niobium pentoxide film layer: under the irradiation condition of voltage 300-400 kV, irradiation energy 300-500 keV, irradiation dose 10 11 -10 16 ions / cm 2 , a 2-3 nm thick niobium pentoxide layer is formed on the surface of the second silicon nitride layer by magnetron sputtering, and the sample is left at room temperature for 1-1.5 h; S303. Modification of the niobium pentoxide film layer: The surface of the niobium pentoxide film layer is cleaned by plasma, argon plasma is generated to bombard the surface of the niobium pentoxide film layer, and the second silicon nitride layer on the surface of the niobium pentoxide layer is removed, the argon flow is controlled at 80-150 sccm, the radio frequency power is 1-3 kw, and the cleaning time is 4-7 s; S4. Deposition of the third silicon nitride layer: S401. Third silicon nitride layer deposition: A 8-14 nm thick third silicon nitride layer is formed on the surface of the second silicon nitride layer by magnetron sputtering; the process parameters of the magnetron sputtering are: walking speed 1.5-3 m / min, power 12-20 kw, the mixed gas of argon and nitrogen with a mass ratio of 1:1 is introduced, argon flow 90-120 sccm, nitrogen flow 90-120 sccm; S402. Depositing a niobium pentoxide film layer: under the irradiation condition of voltage 300-400 kV, irradiation energy 300-500 keV, irradiation dose 10 11 -10 16 ions / cm 2 , a 2-3 nm thick niobium pentoxide layer is formed on the surface of the third silicon nitride layer by magnetron sputtering, and the sample is left at room temperature for 1-2 h. S403. Modification of the niobium pentoxide film layer: The surface of the niobium pentoxide film layer is cleaned by plasma, argon plasma is generated to bombard the surface of the niobium pentoxide film layer, and the third silicon nitride layer on the surface of the niobium pentoxide layer is removed, the argon flow is controlled at 80-150 sccm, the radio frequency power is 1-3 kw, and the cleaning time is 5-7 s; S5. Deposition of the silicon oxide film layer: A 20-30 nm thick silicon oxide film layer is formed on the surface of the third silicon nitride layer by magnetron sputtering, that is, a film layer structure with the same reflectivity in the visible light band is obtained.

2. The coating process of claim 1, wherein In S1, the process parameters of the magnetron sputtering are as follows: walking speed 0.5-1.5 m / min, power 5-15 kw, and argon gas with purity ≥99.99% and flow rate 100-200 sccm.

3. The coating process of claim 1, wherein In S203, S302 and S402, the process parameters of the magnetron sputtering of the niobium pentoxide film layer are as follows: walking speed 1.5-3 m / min, power 15-30 kw, and a mixture of argon and nitrogen with mass ratio 1:1, argon flow rate 100-120 sccm, and nitrogen flow rate 100-120 sccm.

4. The coating process of claim 1, wherein In S5, the process parameters of the magnetron sputtering are as follows: walking speed 1.5-3 m / min, power 16-24 kw, and a mixture of argon and oxygen with mass ratio 1:1, argon flow rate 90-120 sccm, and oxygen flow rate 90-120 sccm.

5. The coating process of claim 1, wherein After S5, pure oxygen with purity ≥99.99% and flow rate 150-200 sccm is introduced to make the silicon oxide reaction complete, and the pure oxygen is introduced for 1-2 h.

6. The coating process of claim 1, wherein After S5, a niobium pentoxide layer is sputtered outside the silicon oxide film layer by magnetron sputtering, with walking speed 1.5-3 m / min, power 15-30 kw, and a mixture of argon and nitrogen with mass ratio 1:1, argon flow rate 100-120 sccm, and nitrogen flow rate 100-120 sccm.

7. A film layer structure with the same reflectivity in the visible light band prepared based on the film coating process according to claims 1-6, characterized in that, The single crystal silicon film layer, the silicon nitride film layer and the silicon oxide film layer are sequentially deposited on the PET substrate layer. The silicon nitride film layer comprises a first silicon nitride layer, a second silicon nitride layer and a third silicon nitride layer sequentially deposited. The thickness of the first silicon nitride layer is 14-16 nm, the thickness of the second silicon nitride layer is 8-10 nm, and the thickness of the third silicon nitride layer is 8-14 nm. The thickness of the silicon oxide film layer is 20-30 nm.

8. The film layer structure of claim 7, wherein the film layer structure has a reflectivity of 50% or more in a visible light wavelength band. The silicon oxide film layer is further sputtered with a niobium pentoxide layer, and the thickness of the niobium pentoxide layer is 1-2 nm.

9. The film layer structure of claim 7, wherein the film layer structure has a reflectivity of 50% or more in a visible light wavelength band. The thickness of the silicon nitride film layer is controlled to be 36 nm, and the thickness of the silicon oxide film layer is controlled to be 25 nm.

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