Vacuum magnetron sputtering produced temperable mirror and preparation method thereof

Abstract

The invention discloses a temperable mirror produced by vacuum magnetron sputtering and a preparation method, the temperable mirror comprises a glass base layer, the surface of the glass base layer is sequentially provided with a transition layer, a dielectric layer, a functional layer and a protective layer from bottom to top, the protective layer is sputtered and plated on the outer surface of the functional layer, and the functional layer is sputtered and plated on the outer surface of the dielectric layer. The dielectric layer is sputtered and plated on the outer surface of the transition layer, and the transition layer is sputtered and plated on the outer surface of the glass base layer. According to the temperable mirror produced through vacuum magnetron sputtering and the preparation method, the transition layer, the dielectric layer, the functional layer and the protective layer are sequentially formed on the surface of the glass base layer through sputtering, so that the high-temperature resistance of tempered coated glass is effectively improved, and the problems of demolding, oxidation and the like in the tempering process of traditional coated glass are solved; the high-temperature-resistant optical glass has the advantages of being good in high-temperature resistance, high in scratch resistance, excellent in optical performance, low in production cost, small in environmental influence, high in production efficiency, wide in application range and the like.

Description

Technical Field

[0001] The invention relates to the technical field of vacuum magnetron sputtering coated glass, in particular to a vacuum magnetron sputtering produced tempered mirror and a preparation method thereof. Background Art

[0002] With the acceleration of urbanization and the improvement of people's living standards, the appearance and functional requirements of buildings are getting higher and higher. Coated glass, as a building material with special optical properties, has been widely used in modern buildings. Coated glass can not only provide good visual effects, but also effectively control the entry and reflection of light, reduce energy consumption, and improve living comfort. However, coated glass faces some challenges in practical applications. On the one hand, in order to meet the requirements of buildings for strength and weather resistance, coated glass needs to be tempered. On the other hand, during the tempering process of traditional coated glass, due to the influence of high temperature, the film layer is prone to oxidation and crystal change, resulting in problems such as film removal and oxidation, which affects the stability and service life of the coated glass. In addition, the traditional coated glass production process often requires the use of high-temperature furnaces or chemical vapor deposition (CVD) and other methods, which not only have high production costs but also have certain impacts on the environment. Therefore, developing a new type of coated glass and its preparation method that can meet the tempering requirements and maintain the stability of the coating is of great significance to improving the performance and application range of coated glass. In order to solve the above problems, the present invention provides a vacuum magnetron sputtering production of tempered mirrors and a preparation method, which effectively improves the scratch resistance and oxidation resistance of the glass by sequentially sputtering a transition layer, a dielectric layer, a functional layer and a protective layer on the surface of a glass base layer, and prepares a high-reflectivity tempered coated glass that is resistant to processing, easy to store and easy to transport. This method can not only meet the requirements of tempering treatment, but also protect the film layer from the influence of high temperature, thereby maintaining the stability and optical properties of the coating. Summary of the invention

[0003] The object of the present invention is to provide a vacuum magnetron sputtering temperable mirror and a preparation method thereof, so as to solve the problems raised in the above background technology.

[0004] To achieve the above-mentioned purpose, the present invention provides the following technical solutions: a vacuum magnetron sputtering production toughened mirror, comprising a glass substrate, the surface of the glass substrate is provided with a transition layer, a dielectric layer, a functional layer and a protective layer from bottom to top, the protective layer is sputtered on the outer surface of the functional layer, the functional layer is sputtered on the outer surface of the dielectric layer, the dielectric layer is sputtered on the outer surface of the transition layer, and the transition layer is sputtered on the outer surface of the glass substrate; The sputtering forming step includes the following steps: Step 1, sputtering to form a first SixNy layer; Step 2, sputtering the outer side of the first SixNy layer to form a TiO2 layer; Step 3, sputtering the outer side of TiO2 to form a functional Al layer; Step 4, sputtering the outer side of the functional layer Al layer to form SixNy; Step 5: The thickness of the first transition layer is 35nm to 50nm; Step 6: The thickness of the second dielectric layer is 25 nm to 110 nm; Step 7: The thickness of the third functional layer is 20 nm to 55 nm; Step 8: The thickness of the fourth protective layer is 45 nm to 110 nm; Step 9: The functional layer is an Al or Ag layer.

[0005] Preferably, power control is used during magnetron sputtering. To ensure stable sputtering and not damage the target material, the power of the silicon aluminum target and silicon aluminum target is 0-65Kw, and the ratio of high-purity argon and high-purity nitrogen in the sputtering process gas is 1:1.2.

[0006] Preferably, the titanium target power is 0-55Kw, and the ratio of high-purity argon and high-purity oxygen in the sputtering process gas is 1:0.8.

[0007] Preferably, the power of the aluminum target is 0-45Kw, and the sputtering process gas is high-purity argon.

[0008] Preferably, the thickness of the protective layer is 40 nm to 100 nm.

[0009] To achieve the above object, the present invention provides the following technical solution: a method for preparing a temperable mirror by vacuum magnetron sputtering, comprising the following steps: Step 1, vacuum magnetron sputtering is performed on the surface of the glass substrate using target materials respectively, and the first transition layer, the second dielectric layer, the functional layer and the protective layer are sputtered in sequence; Step 2, sputtering to form a first SixNy layer; Step 3, sputtering to form a TiO2 layer outside the first SixNy layer; Step 4, sputtering to form an Al or Ag layer outside the second layer; Step 5: Sputtering forms SixNy on the outside of the third layer. The sputtering forms have stronger hardness and smoothness.

[0010] Preferably, during magnetron sputtering, the target material used at the cathode position includes but is not limited to a silicon aluminum target, a titanium target, a titanium aluminum target, and a silver target. The corresponding target material can be selected according to the material to be sputtered.

[0011] Preferably, the silicon-aluminum target is a silicon-aluminum alloy target with a silicon-aluminum weight ratio of 94:6, the silver target has a silver purity of 4N, and the aluminum target has a purity of 4N. The silicon-aluminum alloy target and the titanium target are rotary targets.

[0012] Step 1, sputtering to form a first SixNy layer; Step 2, sputtering the outer side of the first SixNy layer to form a TiO2 layer; Step 3, sputtering the outer side of TiO2 to form a functional Al layer; Step 4, sputtering the outer side of the functional layer Al layer to form SixNy; Step 5: The thickness of the first transition layer is 35nm to 50nm; Step 6: The thickness of the second dielectric layer is 25 nm to 110 nm; Step 7: The thickness of the third functional layer is 20 nm to 55 nm; Step 8: The thickness of the fourth protective layer is 45 nm to 110 nm; Step 9: The functional layer is an Al or Ag layer.

[0013] As a preferred technical solution of the present invention, a vacuum magnetron sputtering method for producing a temperable mirror comprises the following steps: Step 1, vacuum magnetron sputtering is performed on the surface of the glass substrate using target materials respectively, and the first transition layer, the second dielectric layer, the functional layer and the protective layer are sputtered in sequence; Step 2, sputtering to form a first SixNy layer; Step 3, sputtering to form a TiO2 layer outside the first SixNy layer; Step 4, sputtering to form an Al or Ag layer outside the second layer; Step 5: Sputtering forms SixNy on the outside of the third layer. The sputtering forms have stronger hardness and smoothness.

[0014] It can effectively increase the scratch resistance and oxidation resistance of glass. According to this scheme, high-reflective tempered coated glass that is resistant to processing, easy to store and easy to transport can be produced.

[0015] As a preferred technical solution of the present invention, during magnetron sputtering, the target material used at the cathode position includes but is not limited to silicon aluminum target, titanium target, titanium aluminum target, silver target, and the corresponding target material can be selected according to the material to be sputtered.

[0016] As a preferred technical solution of the present invention, the silicon-aluminum target is a silicon-aluminum alloy target with a silicon-aluminum weight ratio of 94:6, the silver target has a purity of 4N, and the aluminum target has a purity of 4N. The silicon-aluminum alloy target and the titanium target are rotating targets.

[0017] As a preferred technical solution of the present invention, power control is used during magnetron sputtering. To ensure stable sputtering and not damage the target material, the power of the silicon aluminum target and silicon aluminum target is 0-65Kw, and the ratio of high-purity argon and high-purity nitrogen in the sputtering process gas is 1:1.2.

[0018] As a preferred technical solution of the present invention, the titanium target power is 0-55Kw, and the ratio of high-purity argon and high-purity oxygen in the sputtering process gas is 1:0.8.

[0019] As a preferred technical solution of the present invention, the power of the aluminum target is 0-45Kw, and the sputtering process gas is high-purity argon.

[0020] As a preferred technical solution of the present invention, the thickness of the protective layer is 40nm to 100nm.

[0021] The appearance color of the processing-resistant, highly reflective, tempered coated glass is silver-white.

[0022] A method for using a vacuum magnetron sputtering process to produce a temperable mirror: S1. Prepare the glass substrate: select a suitable glass substrate according to the type of glass substrate to be coated, and place it on the substrate holder; S2. Install the target: Install the target to be sputtered in the equipment, ensuring that the target and the substrate are kept at an appropriate distance; S3. Vacuuming: Turn on the vacuum pump in the equipment to extract the gas in the vacuum chamber to achieve a high vacuum state. Usually, the pressure in the vacuum chamber needs to be reduced to below 10-5Pa; S4, sputtering to form the first SixNy layer: Turn on the magnetron sputtering power supply to ionize the sputtering gas (such as argon) to form plasma. The charged particles in the plasma are accelerated under the action of the magnetic field and collide with the target material, sputtering the target atoms or molecules onto the surface of the glass substrate to form the first SixNy layer; S5, sputtering to form a TiO2 layer: sputtering to form a TiO2 layer outside the first SixNy layer. This step can be performed using a titanium target or a titanium aluminum target; S6. Sputtering to form a functional Al layer: Sputtering to form a functional Al layer outside the TiO2 layer. The functional layer can be made of aluminum (Al) or silver (Ag) targets; S7, sputtering to form a SixNy layer: sputtering to form a SixNy layer outside the functional Al layer; S8. Control sputtering parameters: according to the coating characteristics and requirements to be prepared, adjust the sputtering power, sputtering gas flow, sputtering time and substrate temperature and other parameters to control the growth rate and quality of the film; S9. Check the coating quality: During the sputtering process, the growth of the coating can be observed in real time through the observation window or monitoring equipment. If necessary, the coating can be inspected and evaluated using optical microscopes, scanning electron microscopes (SEM) and other equipment after sputtering is completed; S10, shut down the equipment: after the sputtering is completed, turn off the magnetron sputtering power supply, turn off the vacuum pump, wait for the pressure in the vacuum chamber to return to atmospheric pressure, take out the glass substrate, and shut down the equipment.

[0023] Through the above steps, magnetron sputtering equipment can be used to prepare high-reflectivity tempered coated glass with high reflectivity, processing resistance, easy storage and good transportation. During use, attention should be paid to the safe operation and maintenance of the equipment to ensure stable operation of the equipment and reliability of the coating quality.

[0024] Compared with the prior art, the beneficial effects of the present invention are: the vacuum magnetron sputtering production of temperable mirror and preparation method: Improve the high temperature resistance of tempered coated glass: By sputtering the transition layer, dielectric layer, functional layer and protective layer on the surface of the glass substrate in sequence, the high temperature resistance of the tempered coated glass is effectively improved, avoiding the problems of film stripping and oxidation in the tempering process of traditional coated glass, and enhancing the scratch resistance and oxidation resistance of tempered coated glass: using vacuum magnetron sputtering technology, a functional layer with strong hardness and smoothness is formed on the surface of the glass substrate, which improves the scratch resistance and oxidation resistance of the tempered coated glass, extends the service life of the coated glass, and improves the optical properties of the tempered coated glass: by controlling the sputtering parameters and selecting the appropriate target material, a high-reflectivity tempered coated glass with high reflectivity, processing resistance, easy storage and good transportation is prepared Glass meets the requirements of modern architecture for optical properties and reduces production costs and environmental impact: Compared with traditional high-temperature furnaces or chemical vapor deposition (CVD) and other methods, the use of vacuum magnetron sputtering technology to produce tempered coated glass has the advantages of low production cost and small environmental impact, which is conducive to achieving green production and sustainable development, and improving production efficiency and equipment utilization: The preparation method provided by the present invention is simple and easy, with high equipment utilization, which is conducive to improving production efficiency and equipment utilization, suitable for large-scale production, and broadening the application scope of tempered coated glass: The high-reflection tempered coated glass provided by the present invention is not only suitable for the construction field, but also can be widely used in automobiles, ships, solar energy and other fields, and has broad application prospects. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 It is a schematic diagram of the internal structure of the processing-resistant, highly reflective, tempered coated glass of the present invention.

[0026] In the figure: 1. Glass base layer; 2. Transition layer; 3. Dielectric layer; 4. Functional layer; 5. Protective layer. DETAILED DESCRIPTION

[0027] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0028] See also Figure 1 The present invention provides a technical solution: a vacuum magnetron sputtering temperable mirror and a preparation method, comprising a glass substrate 1, a transition layer 2, a dielectric layer 3, a functional layer 4 and a protective layer 5 are sequentially arranged on the surface of the glass substrate 1 from bottom to top, the protective layer 5 is sputter-plated on the outer surface of the functional layer 4, the functional layer 4 is sputter-plated on the outer surface of the dielectric layer 3, the dielectric layer 3 is sputter-plated on the outer surface of the transition layer 2, and the transition layer 2 is sputter-plated on the outer surface of the glass substrate 1; The sputtering forming step includes the following steps: Step 1, sputtering to form a first SixNy layer; Step 2: Sputtering is performed on the outside of the first SixNy layer to form a TiO2 layer.

[0029] Step 3, sputtering the outer side of TiO2 to form a functional Al layer; Step 4, sputtering the outer side of the functional layer Al layer to form SixNy; Step 5: The thickness of the first transition layer is 35nm to 50nm; Step 6: The thickness of the second dielectric layer is 25 nm to 110 nm; Step 7: The thickness of the third functional layer is 20 nm to 55 nm; Step 8: The thickness of the fourth protective layer is 45 nm to 110 nm; Step 9: The functional layer is an Al or Ag layer.

[0030] A vacuum magnetron sputtering method for producing a temperable mirror comprises the following steps: Step 1, vacuum magnetron sputtering is performed on the surface of the glass substrate using target materials respectively, and the first transition layer, the second dielectric layer, the functional layer and the protective layer are sputtered in sequence; Step 2, sputtering to form a first SixNy layer; Step 3, sputtering to form a TiO2 layer outside the first SixNy layer; Step 4, sputtering to form an Al or Ag layer outside the second layer; Step 5: Sputtering forms SixNy on the outside of the third layer. The sputtering forms have stronger hardness and smoothness.

[0031] It can effectively increase the scratch resistance and oxidation resistance of glass. According to this scheme, high-reflective tempered coated glass that is resistant to processing, easy to store and easy to transport can be produced.

[0032] During magnetron sputtering, the target material used at the cathode position includes but is not limited to a silicon aluminum target, a titanium target, a titanium aluminum target, and a silver target. The corresponding target material can be selected according to the material to be sputtered.

[0033] The silicon-aluminum target is a silicon-aluminum alloy target with a silicon-aluminum weight ratio of 94:6, the silver target has a purity of 4N, and the aluminum target has a purity of 4N. The silicon-aluminum alloy target and the titanium target are rotary targets.

[0034] During magnetron sputtering, power control is used. To ensure stable sputtering and not damage the target material, the power of the silicon-aluminum target and silicon-aluminum target is 0-65Kw, and the ratio of high-purity argon and high-purity nitrogen in the sputtering process gas is 1:1.2.

[0035] The power of the titanium target is 0-55Kw, and the ratio of high-purity argon and high-purity oxygen in the sputtering process gas is 1:0.8.

[0036] The aluminum target power is 0~45Kw, and the sputtering process gas is high-purity argon.

[0037] The thickness of the protective layer 5 is 40 nm to 100 nm.

[0038] The appearance color of the processing-resistant, highly reflective, tempered coated glass is silver-white.

[0039] A method for using a vacuum magnetron sputtering process to produce a temperable mirror: S1. Prepare the glass substrate: select a suitable glass substrate according to the type of glass substrate to be coated, and place it on the substrate holder; S2. Install the target: Install the target to be sputtered in the equipment, ensuring that the target and the substrate are kept at an appropriate distance; S3. Vacuuming: Turn on the vacuum pump in the equipment to extract the gas in the vacuum chamber to achieve a high vacuum state. Usually, the pressure in the vacuum chamber needs to be reduced to below 10-5Pa; S4, sputtering to form the first SixNy layer: Turn on the magnetron sputtering power supply to ionize the sputtering gas (such as nitrogen) to form plasma. The charged particles in the plasma are accelerated under the action of the magnetic field and collide with the target material, sputtering the target atoms onto the surface of the glass substrate to form the first SixNy layer; S5, sputtering to form a TiO2 layer: sputtering to form a TiO2 layer outside the first SixNy layer. This step can be performed using a titanium target or a titanium aluminum target; S6. Sputtering to form a functional Al layer: Sputtering to form a functional Al layer outside the TiO2 layer. The functional layer can be made of aluminum (Al) or silver (Ag) targets; S7, sputtering to form a SixNy layer: sputtering to form a SixNy layer outside the functional Al layer; S8. Control sputtering parameters: according to the coating characteristics and requirements to be prepared, adjust the sputtering power, sputtering gas flow, sputtering time and substrate temperature and other parameters to control the growth rate and quality of the film; S9. Check the coating quality: During the sputtering process, the growth of the coating can be observed in real time through the observation window or monitoring equipment. If necessary, the coating can be inspected and evaluated using optical microscopes, scanning electron microscopes (SEM) and other equipment after sputtering is completed; S10, shut down the equipment: after the sputtering is completed, turn off the magnetron sputtering power supply, turn off the vacuum pump, wait for the pressure in the vacuum chamber to return to atmospheric pressure, take out the glass substrate, and shut down the equipment.

[0040] Through the above steps, magnetron sputtering equipment can be used to prepare high-reflectivity tempered coated glass with high reflectivity, processing resistance, easy storage and good transportation. During use, attention should be paid to the safe operation and maintenance of the equipment to ensure stable operation of the equipment and reliability of the coating quality.

[0041] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A vacuum magnetron sputtering method for producing a temperable mirror, comprising a glass substrate (1), characterized in that: The surface of the glass substrate (1) is provided with a transition layer (2), a dielectric layer (3), a functional layer (4) and a protective layer (5) in order from bottom to top, the protective layer (5) is sputter-coated on the outer surface of the functional layer (4), the functional layer (4) is sputter-coated on the outer surface of the dielectric layer (3), the dielectric layer (3) is sputter-coated on the outer surface of the transition layer (2), and the transition layer (2) is sputter-coated on the outer surface of the glass substrate (1); The sputtering forming step includes the following steps: Step 1, sputtering to form a first SixNy layer; Step 2, sputtering the outer side of the first SixNy layer to form a TiO2 layer; Step 3, sputtering the outer side of TiO2 to form a functional Al layer; Step 4, sputtering the outer side of the functional layer Al layer to form SixNy; Step 5: The thickness of the first transition layer is 35nm to 50nm; Step 6: The thickness of the second dielectric layer is 25 nm to 110 nm; Step 7: The thickness of the third functional layer is 20 nm to 55 nm; Step 8: The thickness of the fourth protective layer is 45 nm to 110 nm; Step 9: The functional layer is an Al or Ag layer.

2. The method for producing a toughened mirror by vacuum magnetron sputtering according to claim 1, characterized in that: During magnetron sputtering, power control is used. To ensure stable sputtering and not damage the target material, the power of the silicon-aluminum target and silicon-aluminum target is 0-65Kw, and the ratio of high-purity argon and high-purity nitrogen in the sputtering process gas is 1:1.

2.

3. The method for producing a toughened mirror by vacuum magnetron sputtering according to claim 2, characterized in that: The power of the titanium target is 0-55Kw, and the ratio of high-purity argon and high-purity oxygen in the sputtering process gas is 1:0.

8.

4. The method for producing a toughened mirror by vacuum magnetron sputtering according to claim 2, characterized in that: The aluminum target power is 0~45Kw, and the sputtering process gas is high-purity argon.

5. The method for producing a toughened mirror by vacuum magnetron sputtering according to claim 1, characterized in that: The thickness of the protective layer (5) is 40 nm to 100 nm.

6. The method for preparing a toughened mirror by vacuum magnetron sputtering according to claim 1, comprising the following steps: Step 1, vacuum magnetron sputtering is performed on the surface of the glass substrate using target materials respectively, and the first transition layer, the second dielectric layer, the functional layer and the protective layer are sputtered in sequence; Step 2, sputtering to form a first SixNy layer; Step 3, sputtering to form a TiO2 layer outside the first SixNy layer; Step 4, sputtering to form an Al or Ag layer outside the second layer; Step 5: Sputtering forms SixNy on the outside of the third layer. The sputtering forms have stronger hardness and smoothness.

7. The method for preparing a toughened mirror by vacuum magnetron sputtering according to claim 6, characterized in that: During magnetron sputtering, the target material used at the cathode position includes but is not limited to a silicon aluminum target, a titanium target, a titanium aluminum target, and a silver target. The corresponding target material can be selected according to the material to be sputtered.

8. The method for preparing a toughened mirror by vacuum magnetron sputtering according to claim 7, characterized in that: The silicon-aluminum target is a silicon-aluminum alloy target with a silicon-aluminum weight ratio of 94:6, the silver target has a purity of 4N, and the aluminum target has a purity of 4N. The silicon-aluminum alloy target and the titanium target are rotary targets.

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