A blue light absorbing composite rare earth coating material and preparation method thereof

Abstract

The present invention discloses a blue light-absorbing composite rare earth coating material and a preparation method thereof, belonging to the field of vacuum optical coating technology. In the present invention, high-purity micron-grade inorganic raw material powders of different components are uniformly mixed in a high-energy ball mill, and then the mixture is granulated using a high-pressure molding machine. Finally, the granules are placed in a vacuum sintering furnace for high-temperature sintering. Under high temperature and oxygen-deficient conditions, oxygen loss and oxygen abstraction reactions occur between the component materials, and finally, a dense granular blue light-absorbing coating material is formed through sintering. A blue light-absorbing nanofilm is formed on the surface of a resin or glass substrate by vacuum coating. The blue light-absorbing coating material can adjust the blue light absorption ratio by regulating the ratio of the components to meet the needs of different products and different application scenarios. The product has a low reflectivity and is soft and non-glaring, thereby improving the comfort and user experience during use.

Description

Technical Field

[0001] The present invention belongs to the technical field of vacuum optical coating, and specifically relates to a blue light absorbing composite rare earth coating material and a preparation method thereof. Background Art

[0002] Long-term exposure to blue light can easily cause eye damage, particularly macular degeneration. Blue light can penetrate the lens and reach the retina, causing damage there. This accelerates the oxidation of eye cells, produces a large number of free radicals, and leads to macular degeneration. Blue light can also cause blurred vision and visual fatigue. It can also inhibit melatonin secretion, disrupt sleep, and increase the risk of major illnesses. An investigation revealed that most current products, such as blue light-blocking tempered glass for mobile phones and blue light-blocking glasses, utilize optical designs based on the varying refractive indices of the coating material. This blue light-reflecting layer is formed on the substrate surface through vacuum coating to achieve the desired blue light-blocking effect.

[0003] However, this method has the defect of large reflection. When the light intensity is high, the surface of the product will reflect glaring blue light, seriously affecting the user experience. Summary of the Invention

[0004] The purpose of the present invention is to provide a blue light absorbing composite rare earth coating material and a preparation method thereof in order to solve the above-mentioned problems.

[0005] The technical solution adopted by the present invention is as follows: a blue light absorbing composite rare earth coating material and a preparation method thereof, comprising the following steps:

[0006] S1: Use a high-energy ball mill to evenly mix different proportions of micron-sized silicon monoxide, lanthanum titanate, holmium oxide, praseodymium oxide, lutetium oxide, cerium oxide and other inorganic oxide powder raw materials;

[0007] The ratio is:

[0008] 50.36 parts by weight of silicon monoxide, 30.95 g of lanthanum titanate, 28.55 to 108.55 parts by weight of holmium oxide, 10.37 to 30.37 parts by weight of praseodymium oxide, 9.58 to 49.58 parts by weight of lutetium oxide, and 20.19 to 80.19 parts by weight of cerium oxide;

[0009] S2: Using a high-pressure molding machine to shape and granulate the mixed material to obtain a granular material with a particle size range of 3-5 mm;

[0010] S3: placing the granular material in a vacuum sintering furnace and sintering it for 4 hours at a vacuum degree of 1.0×10-2Pa and a temperature of 1400°C to fully react and further improve the density of the granular material;

[0011] S4: vacuum-seal the sintered coating material and store it for later use;

[0012] S5: Place the eyeglass substrate on a special fixture and perform ultrasonic cleaning using a cleaning machine and deionized water respectively; and use a blast dryer to dry the cleaned substrate at a temperature of 50°C;

[0013] S6: Place the dried substrate on the umbrella stand of the vacuum coating machine and fix it with a special clamp, and add the sintered blue light absorbing coating material and silica particles into the crucible;

[0014] S7: Close the hatch, set the deposition rate and film thickness of the coating material and other parameters, and run the vacuum coating machine to perform the vacuum coating process;

[0015] S8: After the coating is completed, use a spectrophotometer and a reflectometer to test the product's performance such as light transmittance and reflectivity to verify the product's blue light absorption performance, thus completing the entire blue light absorbing composite rare earth coating material and its preparation process.

[0016] In a preferred embodiment, in step S1, the ball mill speed is controlled at 300-500 rpm and the milling time is set to 2-4 hours to ensure uniform mixing of the powdered raw materials. Furthermore, the milling jar is filled with zirconia balls with a diameter of 3-10 mm, with a ball-to-material ratio of 10:1, to enhance mixing.

[0017] In a preferred embodiment, in step S2, the molding pressure should be controlled at 30-50 MPa and the holding time should be 5-10 minutes. During the granulation process, the particle size distribution of the particles should be as uniform as possible to ensure that the particle size of the granular material is within the range of 3-5 mm.

[0018] In a preferred embodiment, in step S3, the vacuum level is maintained at 1.0×10^-2 Pa, the sintering temperature is 1400°C, the heating rate is controlled at 5-10°C / minute, and the holding time is 4 hours. During the sintering process, the temperature should be uniformly distributed to avoid cracks in the material.

[0019] In a preferred embodiment, in step S4, when the coating material is stored in a vacuum sealed manner, a vacuum packaging bag with good sealing performance should be used, and the coating material should be stored in a dry, light-proof environment at room temperature to prevent moisture and oxidation.

[0020] In a preferred embodiment, during ultrasonic cleaning in step S5, the cleaning solution temperature is controlled at 40-60°C, the ultrasonic frequency is 40 kHz, and the cleaning time is 10-15 minutes. The resistivity of the deionized water should be greater than 10 MΩ·cm to ensure the cleanliness of the substrate surface.

[0021] In a preferred embodiment, in step S6, when the substrate is fixed on the umbrella stand of the vacuum coating machine, the distance between the substrate and the coating material should be controlled to be 80-120 mm. The materials in the crucible should be fully mixed to ensure uniform coating.

[0022] In a preferred embodiment, in step S7, during the vacuum coating process, the deposition rate of the coating material is set to 0.1-0.5 nm / s, and the film thickness is controlled to 50-200 nm according to actual needs. The vacuum degree of the vacuum coating machine should be maintained below 1.0×10^-3 Pa.

[0023] In a preferred embodiment, in step S8, when testing light transmittance and reflectance, the spectrophotometer wavelength range should be set to 380-780 nm, and the reflectometer detection angles should be set to 0°, 45°, and 90°. The test data can be used to evaluate the product's blue light absorption performance.

[0024] In a preferred embodiment, in step S8, after completing the performance test, if the product passes the test, it is packaged, labeled, and stored. During the packaging process, the product surface should be free of scratches and stains, and anti-static and moisture-proof packaging materials should be used. Furthermore, the product is batch labeled to facilitate traceability and management.

[0025] In summary, due to the adoption of the above technical solution, the beneficial effects of the present invention are:

[0026] In the present invention, high-purity micron-sized inorganic raw material powders of different components are mixed evenly in a high-energy ball mill, and then the mixture is granulated using a high-pressure molding machine. Finally, the granules are placed in a vacuum sintering furnace for high-temperature sintering. Under high temperature and oxygen-deficient conditions, oxygen loss and oxygen abstraction reactions occur between the component materials, and finally a dense granular blue light absorbing coating material is formed by sintering. A blue light absorbing nanofilm is formed on the surface of a resin or glass substrate by vacuum coating. The blue light absorbing coating material can adjust the blue light absorption ratio by regulating the ratio of the components to meet the needs of different products and different application scenarios. The product has a low reflectivity and is soft and non-glaring, thereby improving the comfort and experience during use. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Figure 1 It is a schematic diagram of the process principle of the present invention. DETAILED DESCRIPTION

[0028] In order to make the purpose, technical solutions and advantages of the present invention more clearly understood, the present invention will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not intended to limit the present invention.

[0029] Reference Figure 1 ,

[0030] A blue light absorbing composite rare earth coating material and a preparation method thereof, comprising the following steps:

[0031] S1: Use a high-energy ball mill to evenly mix different proportions of micron-sized silicon monoxide, lanthanum titanate, holmium oxide, praseodymium oxide, lutetium oxide, cerium oxide and other inorganic oxide powder raw materials;

[0032] The ratio is:

[0033] 50.36 parts by weight of silicon monoxide, 30.95 g of lanthanum titanate, 28.55 to 108.55 parts by weight of holmium oxide, 10.37 to 30.37 parts by weight of praseodymium oxide, 9.58 to 49.58 parts by weight of lutetium oxide, and 20.19 to 80.19 parts by weight of cerium oxide;

[0034] S2: Using a high-pressure molding machine to shape and granulate the mixed material to obtain a granular material with a particle size range of 3-5 mm;

[0035] S3: placing the granular material in a vacuum sintering furnace and sintering it for 4 hours at a vacuum degree of 1.0×10-2Pa and a temperature of 1400°C to fully react and further improve the density of the granular material;

[0036] S4: vacuum-seal the sintered coating material and store it for later use;

[0037] S5: Place the lens substrate (resin) on a special fixture and perform ultrasonic cleaning using a cleaning machine and deionized water respectively; and use a blast dryer to dry the cleaned lens substrate at a temperature of 50°C;

[0038] S6: Place the dried substrate on the umbrella stand of the vacuum coating machine and fix it with a special clamp, and add the sintered blue light absorbing coating material and silica particles into the crucible;

[0039] S7: Close the hatch, set the deposition rate and film thickness of the coating material and other parameters, and run the vacuum coating machine to perform the vacuum coating process;

[0040] S8: After the coating is completed, use a spectrophotometer and a reflectometer to test the product's performance such as light transmittance and reflectivity to verify the product's blue light absorption performance, thus completing the entire blue light absorbing composite rare earth coating material and its preparation process.

[0041] In step S1, the ball mill speed should be controlled at 300-500 rpm and the milling time should be set to 2-4 hours to ensure uniform mixing of the powder raw materials. At the same time, the ball mill should be filled with zirconia balls with a diameter of 3-10 mm, with a ball-to-material ratio of 10:1 to enhance the mixing effect.

[0042] In step S2, the molding pressure should be controlled at 30-50 MPa and the holding time should be 5-10 minutes. During the granulation process, the particle size distribution of the particles should be as uniform as possible to ensure that the particle size of the granular material is within the range of 3-5 mm.

[0043] In step S3, the vacuum level should be maintained at 1.0 × 10-2 Pa, the sintering temperature should be 1400°C, the heating rate should be controlled at 5-10°C / minute, and the holding time should be 4 hours. During the sintering process, the temperature should be evenly distributed to avoid cracks in the material.

[0044] In step S4, when the coating material is stored in a vacuum sealed manner, a vacuum packaging bag with good sealing performance should be used and the coating material should be stored in a dry, light-proof environment at room temperature to prevent moisture and oxidation of the coating material.

[0045] In step S5, during ultrasonic cleaning, the temperature of the cleaning solution is controlled at 40-60°C, the ultrasonic frequency is 40kHz, and the cleaning time is 10-15 minutes. The resistivity of the deionized water should be greater than 10MΩ·cm to ensure the cleanliness of the substrate surface.

[0046] In step S6, when the substrate is fixed on the umbrella stand of the vacuum coating machine, the distance between the substrate and the coating material should be controlled at 80-120 mm. The materials in the crucible should be fully mixed to ensure uniform coating.

[0047] In step S7, during the vacuum coating process, the deposition rate of the coating material is set to 0.1-0.5 nm / s, and the film thickness is controlled to 50-200 nm according to actual needs. The vacuum degree of the vacuum coating machine should be maintained below 1.0×10^-3 Pa.

[0048] In step S8, when testing light transmittance and reflectance, the spectrophotometer's wavelength range should be set to 380-780 nm, and the reflectometer's detection angles should be set to 0°, 45°, and 90°. The test data can be used to evaluate the product's blue light absorption performance.

[0049] In step S8, after completing the performance test, if the product is qualified, it will be packaged, labeled and put into storage. During the packaging process, it should be ensured that there are no scratches or stains on the surface of the product, and anti-static and moisture-proof packaging materials should be used. At the same time, the product is batch-labeled for easy traceability and management.

[0050] Example 1

[0051] (1) using a high-energy ball mill, 50.36 parts by weight of silicon monoxide, 30.95 parts by weight of lanthanum titanate, 28.55 parts by weight of holmium oxide, 10.37 parts by weight of praseodymium oxide, 9.58 parts by weight of lutetium oxide, and 20.19 parts by weight of cerium oxide, etc., were uniformly mixed;

[0052] (2) using a high-pressure molding machine to shape and granulate the mixed material to obtain a granular material with a particle size range of 3-5 mm;

[0053] (3) Place the granular material in a vacuum sintering furnace at a vacuum degree of 1.0×10- 2 Pa, sintered at 1400 ° C for 4 hours to fully react and further improve the density of the pellets;

[0054] (4) vacuum sealing the sintered coating material for future use;

[0055] (5) Place the lens substrate (resin) on a special fixture and perform ultrasonic cleaning using a cleaning machine and deionized water respectively; and use a blast dryer to dry the cleaned lens substrate at a temperature of 50°C;

[0056] (6) Place the dried substrate on the umbrella stand of the vacuum coating machine and fix it with a special clamp, and add the sintered blue light absorbing coating material and silica particles into the crucible;

[0057] (7) Close the hatch, set the deposition rate and film thickness of the coating material and other parameters.

[0058] Run the vacuum coating machine to carry out the vacuum coating process;

[0059] (8) After the coating is completed, use a spectrophotometer and a reflectometer to test the product's light transmittance and reflectivity to verify the product's blue light absorption performance.

[0060] The prepared eyeglass lens product covered with blue light absorbing nano-film is light yellow in color, with an average light transmittance of 85%, a reflectivity of 4%, and a blue light absorption of 25% at a wavelength of 450nm. The product has a good blue light absorption effect, and also solves the problem of high reflectivity, greatly improving the product's performance and user experience to meet the needs of different groups of people.

[0061] Example 2

[0062] (1) using a high-energy ball mill, 50.36 parts by weight of silicon monoxide, 30.95 parts by weight of lanthanum titanate, 68.55 parts by weight of holmium oxide, 20.37 parts by weight of praseodymium oxide, 29.58 parts by weight of lutetium oxide, and 50.19 parts by weight of cerium oxide, etc., were uniformly mixed;

[0063] (2) using a high-pressure molding machine to shape and granulate the mixed material to obtain a granular material with a particle size range of 3-5 mm;

[0064] (3) Place the granular material in a vacuum sintering furnace at a vacuum degree of 1.0×10- 2Pa, sintered at 1400 ° C for 4 hours to fully react and further improve the density of the pellets;

[0065] (4) vacuum sealing the sintered coating material for future use;

[0066] (5) Place the tempered film substrate (glass) of the mobile phone on a special fixture and use a cleaning machine and deionized water for ultrasonic cleaning respectively; and use a blast dryer to dry the cleaned substrate at a temperature of 80°C;

[0067] (6) Place the dried substrate on the umbrella stand of the vacuum coating machine and fix it with a special clamp, and add the sintered blue light absorbing coating material and silica particles into the crucible;

[0068] (7) Close the hatch, set the deposition rate and film thickness of the coating material and other parameters.

[0069] Run the vacuum coating machine to carry out the vacuum coating process;

[0070] (8) After the coating is completed, use a spectrophotometer and a reflectometer to test the product's light transmittance and reflectivity to verify the product's blue light absorption performance.

[0071] The mobile phone tempered film product covered with blue light absorbing nano-film is light yellow in color, with an average light transmittance of 75%, a reflectivity of 5%, and a blue light absorption of 40% at a wavelength of 450nm. The product has better blue light absorption effect and also solves the problem of high reflectivity, meeting the needs of different groups of people and improving the user experience of the product.

[0072] Example 3

[0073] (1) using a high-energy ball mill, 50.36 parts by weight of silicon monoxide, 30.95 parts by weight of lanthanum titanate, 108.55 parts by weight of holmium oxide, 30.37 parts by weight of praseodymium oxide, 49.58 parts by weight of lutetium oxide, 80.19 parts by weight of cerium oxide and other micron-sized inorganic oxide powder raw materials were mixed uniformly;

[0074] (2) using a high-pressure molding machine to shape and granulate the mixed material to obtain a granular material with a particle size range of 3-5 mm;

[0075] (3) Place the granular material in a vacuum sintering furnace at a vacuum degree of 1.0×10- 2 Pa, sintered at 1400 ° C for 4 hours to fully react and further improve the density of the pellets;

[0076] (4) vacuum sealing the sintered coating material for future use;

[0077] (5) Place the tempered film substrate (glass) of the mobile phone on a special fixture and use a cleaning machine and deionized water for ultrasonic cleaning respectively; and use a blast dryer to dry the cleaned substrate at a temperature of 80°C;

[0078] (6) Place the dried substrate on the umbrella stand of the vacuum coating machine and fix it with a special clamp, and add the sintered blue light absorbing coating material and silica particles into the crucible;

[0079] (7) Close the hatch, set the deposition rate and film thickness of the coating material and other parameters.

[0080] Run the vacuum coating machine to carry out the vacuum coating process;

[0081] (8) After the coating is completed, use a spectrophotometer and a reflectometer to test the product's light transmittance and reflectivity to verify the product's blue light absorption performance.

[0082] The mobile phone tempered film product covered with blue light absorbing nano-film is brown in color, with an average light transmittance of 65%, a reflectivity of 5%, and a blue light absorption of 55% at a wavelength of 450nm. The product has a higher blue light absorption effect, and the surface reflection is small, soft and not dazzling, meeting the needs of different groups of people.

[0083] Example Data Sheet

[0084]

[0085] Based on the above, it can be known that in the present invention, high-purity micron-sized inorganic raw material powders of different components are mixed evenly by a high-energy ball mill, and then the mixture is granulated using a high-pressure molding machine. Finally, the granular material is placed in a vacuum sintering furnace for high-temperature sintering. Under high temperature and oxygen-deficient conditions, oxygen loss and oxygen-absorption reactions occur between the component materials, and finally a dense granular blue light absorbing coating material is formed by sintering. A blue light absorbing nanofilm is formed on the surface of a resin or glass substrate by vacuum coating. The blue light absorbing coating material can adjust the blue light absorption ratio by regulating the ratio of the components to meet the needs of different products and different application scenarios. The product has a low reflectivity, is soft and non-glaring, thereby improving the comfort and experience during use.

[0086] It should be noted that, in this document, relational terms such as first and second, etc., are used only to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any actual relationship or order between these entities or operations. Moreover, the term "comprises" or any other variant thereof is intended to cover non-exclusive inclusion, so that a process, method, article or device that includes a series of elements includes not only those elements, but also other elements that are not explicitly listed, or also includes elements that are inherent to such process, method, article or device. In the absence of further restrictions, an element defined by the sentence "comprises a ..." does not exclude the presence of other identical elements in the process, method, article or device that includes the element.

[0087] The above description is intended to enable one skilled in the art to implement or use the present invention. Various modifications to these embodiments will be readily apparent to one skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention is not limited to the embodiments shown herein but is intended to conform to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A method for preparing a blue light absorbing composite rare earth coating material, characterized in that: The following steps are involved: S1: Using a high-energy ball mill, micron-sized silicon monoxide, lanthanum titanate, holmium oxide, praseodymium oxide, lutetium oxide, and cerium oxide inorganic oxide powder raw materials of different proportions are mixed uniformly; The ratio is: 50.36 parts by weight of silicon monoxide, 30.95 parts by weight of lanthanum titanate, 28.55 to 108.55 parts by weight of holmium oxide, 10.37 to 30.37 parts by weight of praseodymium oxide, 9.58 to 49.58 parts by weight of lutetium oxide, and 20.19 to 80.19 parts by weight of cerium oxide; S2: Using a high-pressure molding machine to shape and granulate the mixed material to obtain a granular material with a particle size range of 3-5 mm; S3: Place the granular material in a vacuum sintering furnace at a vacuum degree of 1.0×10 —2 Pa, sintered at 1400 ° C for 4 hours to fully react and further improve the density of the pellets; S4: vacuum-seal the sintered coating material and store it for later use; S5: Place the substrate on a special fixture and perform ultrasonic cleaning using a cleaning machine and deionized water respectively; and use a blast dryer to dry the cleaned substrate at a temperature of 50°C. S6: Place the dried substrate on the umbrella stand of the vacuum coating machine and fix it with a special clamp, and add the sintered blue light absorbing coating material and silica particles into the crucible; S7: Close the hatch, set the deposition rate and film thickness parameters of the coating material, and run the vacuum coating machine to perform the vacuum coating process; S8: After the coating is completed, use a spectrophotometer and a reflectometer to test the light transmittance and reflectivity of the product to verify the blue light absorption performance of the product, thus completing the preparation process of the entire blue light absorption composite rare earth coating material.

2. The method for preparing a blue light absorbing composite rare earth coating material according to claim 1, wherein: In step S1, the speed of the ball mill is controlled at 300-500 rpm, and the ball milling time is set to 2-4 hours to ensure that the powder raw materials are evenly mixed; at the same time, the ball mill jar is filled with zirconia balls with a diameter of 3-10 mm, and the ball-to-material ratio is 10:

1.

3. The method for preparing a blue light absorbing composite rare earth coating material according to claim 1, wherein: In step S2, the molding pressure is controlled at 30-50 MPa, and the holding time is 5-10 minutes; the particle size of the granular material is in the range of 3-5 mm.

4. The method for preparing a blue light absorbing composite rare earth coating material according to claim 1, wherein: In step S3, the vacuum degree is maintained at 1.0×10 -2 Pa, the sintering temperature is 1400℃, the heating rate is controlled at 5-10℃ / min, and the holding time is 4 hours.

5. The method for preparing a blue light absorbing composite rare earth coating material according to claim 1, wherein: In step S4, when the product is stored in a vacuum sealed state, a vacuum packaging bag with good sealing performance is used and the product is stored in a dry, light-proof environment at room temperature.

6. The method for preparing a blue light absorbing composite rare earth coating material according to claim 1, wherein: In step S5, during ultrasonic cleaning, the temperature of the cleaning liquid is controlled at 40-60° C., the ultrasonic frequency is 40 kHz, and the cleaning time is 10-15 minutes; the resistivity of the deionized water is greater than 10 MΩ·cm to ensure the cleanliness of the substrate surface.

7. The method for preparing a blue light absorbing composite rare earth coating material according to claim 1, wherein: In step S6, when the substrate on the umbrella stand of the vacuum coating machine is fixed, the distance between the substrate and the coating material is controlled to be 80-120 mm.

8. The method for preparing a blue light absorbing composite rare earth coating material according to claim 1, wherein: In the step S7, during the vacuum coating process, the deposition rate of the coating material is set to 0.1-0.5 nm / s, and the film thickness is controlled to 50-200 nm according to actual needs; the vacuum degree of the vacuum coating machine is maintained at 1.0×10 -3 Below Pa.

9. The method for preparing a blue light absorbing composite rare earth coating material according to claim 1, wherein: In step S8, when testing the light transmittance and reflectance, the wavelength range of the spectrophotometer is set to 380-780 nm, and the detection angles of the reflectometer are set to 0°, 45°, and 90°; the blue light absorption performance of the product is evaluated based on the test data.

10. The method for preparing a blue light absorbing composite rare earth coating material according to claim 1, wherein: In step S8, after completing the performance test, if the product is qualified, it will be packaged, labeled and put into storage; during the packaging process, ensure that there are no scratches or stains on the product surface, and use anti-static and moisture-proof packaging materials; at the same time, the product is batch-labeled for easy traceability and management.

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