WO2023185179A1 - Dispositif électronique - Google Patents

Dispositif électronique Download PDF

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Publication number
WO2023185179A1
WO2023185179A1 PCT/CN2023/070076 CN2023070076W WO2023185179A1 WO 2023185179 A1 WO2023185179 A1 WO 2023185179A1 CN 2023070076 W CN2023070076 W CN 2023070076W WO 2023185179 A1 WO2023185179 A1 WO 2023185179A1
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Prior art keywords
glass
glass substrate
reflective
refractive index
micro
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PCT/CN2023/070076
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English (en)
Chinese (zh)
Inventor
缪灯奎
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荣耀终端有限公司
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Publication of WO2023185179A1 publication Critical patent/WO2023185179A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C15/00—Surface treatment of glass, not in the form of fibres or filaments, by etching
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
    • G02B1/11—Anti-reflection coatings
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
    • G02B1/11—Anti-reflection coatings
    • G02B1/113—Anti-reflection coatings using inorganic layer materials only
    • G02B1/115—Multilayers
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
    • G02B1/11—Anti-reflection coatings
    • G02B1/118—Anti-reflection coatings having sub-optical wavelength surface structures designed to provide an enhanced transmittance, e.g. moth-eye structures
    • G—PHYSICS
    • G09—EDUCATION; CRYPTOGRAPHY; DISPLAY; ADVERTISING; SEALS
    • G09F—DISPLAYING; ADVERTISING; SIGNS; LABELS OR NAME-PLATES; SEALS
    • G09F9/00—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements

Definitions

  • the present application relates to the technical field of electronic equipment, and in particular to an anti-reflective glass, its preparation method, a display screen of an electronic equipment, and an electronic equipment.
  • an AR film layer is formed on the glass substrate, which can reduce the reflectivity of the glass and increase the transmittance of the glass.
  • the AR film layer is generally thin and easily punctured, causing the glass to be easily scratched and visible scratches to the naked eye.
  • scratched will destroy the stress balance of the glass, resulting in a decrease in the impact resistance of the glass.
  • a dense high-hardness material coating can be plated on the surface of the glass substrate.
  • the dense high-hardness material coatings will generate repulsive forces and produce compressive stress, causing the glass substrate to The deformation of the material makes it unable to be used on larger-sized structures such as mobile phone covers, but can only be used on small-sized structures such as camera lenses and watch covers.
  • This application provides an anti-reflective glass, a preparation method thereof, a display screen of an electronic device, and an electronic device, which solves the problems of the anti-reflective glass being easily scratched, the impact resistance being reduced, and the glass substrate being easily deformed.
  • An anti-reflective glass including a glass substrate, the first surface of the glass substrate having a micro-nano structure; a first anti-reflective film layer superimposed on the first surface of the glass substrate, the first anti-reflective film is made of high The refractive index layer and the low refractive index layer are alternately superimposed.
  • a micro-nano structure is provided on the surface of the glass substrate.
  • the micro-nano structure is a surface structure of micron or nanometer size, which can ensure the dense accumulation of film atoms in short distances, improve the hardness of the film, thereby improving the scratch resistance of the coated glass surface.
  • the long-range undulating structure allows the film lamination stress to be released locally, reducing the stress deformation of the glass substrate. When stacking a thicker anti-reflection film layer, no large stress deformation will occur, so it can be used in electronics. In larger structures such as device displays. .
  • the micro-nano structure is composed of a plurality of micron-sized and/or nano-sized protrusions; or is composed of a plurality of micron-sized and/or nano-sized grooves or depressions.
  • the plurality of protrusions, grooves or depressions may be arranged irregularly or regularly, for example, in an array structure.
  • the height of the protrusions is 50-1000nm, the bottom size is 100-3000nm, and the spacing between adjacent protrusions is 100-1000nm.
  • the micro-nano structure is formed by multiple ravines or multiple depressions, the depth and length of the ravines and the distance between adjacent ravines also meet the above dimensions or relationships.
  • the thickness of the first anti-reflection film layer is 500-3000 nm.
  • a glass substrate with a micro-nano structure on the surface is superposed with an anti-reflection film layer with a thickness of more than 500 nm, it can reduce the stress of the film layer and the stress deformation of the glass substrate, making it applicable to large-size structures of more than 50 mm.
  • the material of the low refractive index layer is Al 2 O 3 ; and the material of the high refractive index layer is AlN or AlON.
  • Al 2 O 3 has a high hardness, with a Mohs hardness of about 9, which can further improve the scratch resistance of anti-reflective glass.
  • the Mohs hardness of the anti-reflective glass surface under a force of 500g is above 7.
  • the deformation amount is less than 0.20 mm when the thickness is 0.55 mm.
  • the Vickers hardness of the anti-reflective glass is above 1100HV.
  • the anti-reflection glass has a reflectivity of ⁇ 2% and a transmittance of >93% in the light wavelength region of 380 to 780 nm.
  • the embodiments of the present application also provide a method for preparing anti-reflective glass, which is characterized by including:
  • Step S1 forming a micro-nano structure on at least one surface of the glass substrate
  • Step S2 Superimpose a first anti-reflective film layer on the surface of the glass substrate with a micro-nano structure.
  • the first anti-reflective film is formed by alternately superposing a high refractive index layer and a low refractive index layer.
  • a micro-nano structure can be formed on at least one surface of the glass substrate through a metal mask method, a diamond flying knife, an acid etching method, etc., and a first anti-reflection layer can be superimposed on the surface of the glass substrate with a micro-nano structure using a vacuum deposition method. film layer.
  • Embodiments of the present application also provide an electronic device display screen and electronic device, including the anti-reflective glass described in the above technical solution or the anti-reflective glass prepared by the preparation method described in the above technical solution.
  • the above-mentioned anti-reflective glass has small stress deformation, low reflectivity, high transmittance, good scratch resistance and high hardness, and can be used as a display screen for electronic devices, such as small-sized displays such as watches or Large-size displays such as mobile phones.
  • the anti-reflective glass can be used as an outer screen of a display screen of an electronic device.
  • Electronic devices using the above-mentioned anti-reflective glass as a display screen will not cause glare under strong sunlight, making it easier for users to see the content displayed on the screen clearly and improving the product use experience.
  • electronic equipment display screens have good scratch resistance and are not prone to scratches visible to the naked eye. They do not affect the appearance of electronic equipment and do not reduce the impact resistance of glass.
  • Figure 1 is a schematic diagram of the stacked structure of AR coated glass
  • Figure 2 is a schematic diagram of the laminated structure of hard AR coated glass
  • Figure 3 is a schematic diagram of the laminated structure of the anti-reflective glass provided by the embodiment of the present application.
  • Figure 4 is a schematic diagram of the first micro-nano structure on the surface of the glass substrate provided by this application;
  • Figure 5 is a schematic diagram of the second micro-nano structure on the surface of the glass substrate provided by this application.
  • Figure 6 is a schematic diagram of the third micro-nano structure on the surface of the glass substrate provided by this application.
  • Figure 7 is a schematic diagram of the first alternating structure of the first anti-reflection film layer provided by this application.
  • Figure 8 is a schematic diagram of the second alternating structure of the first anti-reflection film layer provided by this application.
  • Figure 9 is a schematic diagram of the third alternating structure of the first anti-reflection film layer provided by this application.
  • Figure 10 is a schematic diagram of the preparation process of anti-reflective glass provided by the embodiment of the present application.
  • Figure 11 is a schematic flow chart of forming a surface micro-nano structure using a metal mask method according to an embodiment of the present application
  • Figure 12 is a scanning electron microscope photograph of the glass substrate prepared in Example 1 of the present invention.
  • Figure 13 is the CAV scanning result of the anti-reflective glass of Example 1 of the present application.
  • Figure 14 is a scanning electron microscope photograph of the glass substrate prepared in Example 2 of the present invention.
  • Figure 15 is the CAV scanning result of the anti-reflective glass of Example 2 of the present application.
  • Figure 16 is a schematic structural diagram of a mobile phone.
  • the cover is part of the display screen of the electronic device, and can also be called the outer screen of the display screen, and is used to protect the inner screen with the display function in the display screen.
  • high refractive index and low refractive index refer to the relative values of the refractive indexes to each other, for example, high refractive index > low refractive index.
  • high refractive index materials and low refractive index materials refer to the relative values of the refractive index of different materials.
  • the low refractive index is about 1.3 to 1.7 or 1.3 to 1.75
  • the low refractive index material includes a material with a refractive index of about 1.3 to 1.7 or 1.3 to 1.75
  • the high refractive index is about 1.7 to 2.5
  • High refractive index materials include materials with a refractive index of about 1.7 to 2.5.
  • the transmission of glass refers to the property of light passing through the glass, expressed as transmittance; the reflection of glass refers to the light blocked by the glass and reflected at a certain angle, expressed as reflectivity; the refractive index of glass It refers to the ratio of the propagation speed of light in vacuum to the propagation speed of light in glass.
  • the glass substrate refers to glass without anti-reflection treatment, including ordinary glass, tempered glass, etc., wherein tempered glass is chemically strengthened glass obtained by chemical strengthening treatment such as ion exchange of ordinary glass.
  • Glass is a light-dense medium with a refractive index of 1.54. In a strong light environment, about 4.2% of the reflected light from each surface is reflected into the human eye, causing glare and making it difficult for the eyes to see clearly the display content on the screen. Use of electronic products.
  • high refractive index materials high refractive index 1
  • low refractive index materials low refractive index 1
  • Figure 1 is a schematic diagram of the stacked structure of AR coated glass.
  • the reflectivity of the glass substrate is 8.4%, the reflectivity after double-sided coating is ⁇ 1%; when the transmittance of the glass substrate is 93%, the transmittance after double-sided coating is >98%; and the thickness of the film layer is generally less than 300nm, the deformation of the glass substrate caused by the stress of the film layer can be ignored, and it does not affect the application of glass in larger structures, such as being used as cover glass for mobile phones.
  • the film layer is thin and easily punctured, and the coated glass is more susceptible to scratches than the glass substrate.
  • a hard film layer can be inserted into the AR film layer to form a hard AR film layer. See Figure 2.
  • Figure 2 is a schematic diagram of the stacked structure of hard AR coated glass. Using high refractive index materials (high refractive index 1) and low refractive index materials (low refractive index 1), they are alternately stacked on the glass substrate (substrate) according to the optical film design, and a hard film layer is inserted as an anti-scratch layer to form Hard AR coated glass. On the one hand, the hard AR film layer can reduce the reflectivity of the glass.
  • the reflectance of the glass substrate is 8.4%
  • the reflectivity after double-sided coating is ⁇ 1%; on the other hand, it can increase the transmittance of the glass.
  • the transmittance of the glass substrate is 93%
  • the transmittance after double-sided coating is >98%; on the other hand, it can improve the scratch resistance of the glass.
  • the thickness of the hard film layer is generally 500-5000nm, making the thickness of the entire hard AR film layer greater than 800nm, and the glass substrate deformation caused by the stress of the film layer is large.
  • the 0.55mm thick tempered glass used as a mobile phone cover has a deformation ratio of 0.4mm, exceeding the standard tolerance of 0.2mm. This kind of glass cannot be used in larger-sized structures and can only be used in small-sized structures smaller than 50mm such as camera lenses and watch covers.
  • the anti-reflective glass includes: a glass substrate 1, the first surface of the glass substrate has a micro-nano structure 11; a first anti-reflective film layer 2 superimposed on the first surface of the glass substrate 1, the first anti-reflective film layer 2 is superimposed on the first surface of the glass substrate 1.
  • the reflective film layer is formed by alternately stacking high refractive index layers 21 and low refractive index layers 22 .
  • the glass substrate 1 only needs to have a high transmittance.
  • the transmittance of the glass substrate 1 is greater than or equal to 85% in a light wavelength region ranging from 380 to 780 nm. In other embodiments, the transmittance of the glass substrate 1 in the light wavelength range of 380 to 780 nm is greater than or equal to 90%, or even greater than or equal to 92%.
  • the reflectivity of the glass substrate 1 in the light wavelength region ranging from 380 to 780 nm is ⁇ 15%. In other embodiments, the reflectivity of the glass substrate 1 in the light wavelength region ranging from 380 to 780 nm is ⁇ 10%.
  • the glass substrate 1 may be ordinary glass, or may be tempered glass obtained by ion exchange treatment of ordinary glass.
  • a typical chemical composition of the glass substrate 1 includes SiO 2 , B 2 O 3 , Al 2 O 3 , alkali metal oxides and alkaline earth metal oxides.
  • the glass substrate 1 may also include other chemical compositions as needed. , such as rare earth oxides or other divalent metal oxides.
  • the tempered glass can be prepared according to the following method: preheat ordinary glass and then perform ion exchange treatment, and then sequentially pickle and alkali wash to obtain tempered glass.
  • the ion exchange treatment is specifically: treatment in an ion exchange treatment agent, the ion exchange agent includes KNO 3 , NaNO 3 , H 2 SiO 3 , La 2 O 3 and KOH, and the temperature of the ion exchange treatment is 435 to 445 °C, the time is 1.8 ⁇ 22h.
  • the ion exchanger includes 165-185 parts by mass of KNO 3 , 14-18 parts by mass of NaNO 3 , 3-5 parts by mass of H 2 SiO 3 , 0.05-0.15 parts by mass of La 2 O 3 and 4 to 8 parts by mass of KOH.
  • the tempered glass prepared by the above method has good strength and impact resistance and is not easily broken.
  • the thickness of the glass substrate 1 is 0.4mm ⁇ 0.7mm. In other embodiments, the thickness of the glass substrate 1 is 0.45mm ⁇ 0.65mm.
  • the surface of the glass substrate 1 has a micro-nano structure 11.
  • the micro-nano structure 11 is a surface structure of micron and/or nanometer size, which can ensure the dense accumulation of atoms in the short-range upper film layer, improve the hardness of the film layer, thereby improving the scratch resistance of the coated glass surface.
  • the long-range undulating structure allows the film lamination stress to be released locally, reducing the stress deformation of the glass substrate 1, and will not produce large stress deformation when stacking a thicker anti-reflection film layer, so it can be used In larger structures such as electronic device displays.
  • the surface of the glass substrate 1 has a plurality of micron and/or nanometer-sized protrusions, and the plurality of protrusions constitute a micro-nano structure on the surface of the glass substrate 1 .
  • Figure 4 is a schematic diagram of the first micro-nano structure on the surface of a glass substrate provided by this application.
  • the bottom size of the protrusion 41 is larger than the top size, and may be truncated cone-shaped, pyramid-shaped or steamed bun-shaped. In other embodiments, the bottom size of the protrusion is the same as the top size, and may be rectangular, cylindrical, etc.
  • the height of the protrusions is 50 to 1000 nm.
  • the protrusions are The height can be 100 ⁇ 800nm, or it can be 150 ⁇ 700nm, or it can be 200 ⁇ 600nm, or it can be 250 ⁇ 500nm, or it can be 300 ⁇ 400nm. In one embodiment, the bottom size of the protrusions is 100 to 3000 nm.
  • the protrusions are The bottom size can be 150 ⁇ 2000nm, or it can be 200 ⁇ 1500nm, or it can be 250 ⁇ 1000nm, or it can be 300 ⁇ 800nm, or it can be 350 ⁇ 500nm. In one embodiment, the spacing between adjacent protrusions is 100 to 1000 nm.
  • adjacent protrusions are The spacing between the protrusions may be 150-800 nm, or may be 200-600 nm, or may be 250-500 nm, or may be 300-400 nm.
  • the plurality of protrusions can be arranged irregularly and dispersed on the surface of the glass substrate.
  • the plurality of protrusions may be arranged in a regular manner, for example, in an array, that is, the plurality of protrusions are arranged in an array or a quasi-array arrangement.
  • Using multiple protrusions as micro-nano structures on the surface of the glass substrate makes it easier to form regular structures, such as array structures, which is beneficial to the release of stress in the film layer and reduces the stress deformation of the glass substrate.
  • the glass substrate 1 with a micro-nano structure on the surface has high gloss and transmittance.
  • the glass substrate 1 with a micro-nano structure on the surface has a transmittance of greater than or equal to 380 nm in the light wavelength range of 380 to 780 nm. 85% is even greater than or equal to 90%, or greater than or equal to 92%.
  • the glossiness of the glass substrate 1 with micro-nano structures on the surface is greater than 85, or even greater than 90.
  • the surface of the glass substrate 1 has a plurality of micron and/or nanometer-sized grooves, and the plurality of grooves constitute a micro-nano structure on the surface of the glass substrate 1 .
  • Figure 5 is a schematic diagram of the second micro-nano structure on the surface of the glass substrate provided by this application.
  • the bottom size of the gully 51 is smaller than the top size, that is, its cross-section may be inverted truncated cone shape, inverted pyramid shape or inverted steamed bun shape.
  • the bottom size of the gully is the same as the top size, and its cross-section is rectangular, cylindrical, etc.
  • the depth of the groove is 50-1000 nm.
  • the depth of the groove is It can be 100 ⁇ 800nm, or it can be 150 ⁇ 700nm, or it can be 200 ⁇ 600nm, or it can be 250 ⁇ 500nm, or it can be 300 ⁇ 400nm. In one embodiment, the length of the groove is 100-3000 nm.
  • the length of the groove is It can be 150-2000nm, or it can be 200-1500nm, or it can be 250-1000nm, or it can be 300-800nm, or it can be 350-500nm.
  • the width of the groove top is 100-3000 nm.
  • the width of the groove top is The width can be 150 ⁇ 2000nm, or it can be 200 ⁇ 1500nm, or it can be 250 ⁇ 1000nm, or it can be 300 ⁇ 800nm, or it can be 350 ⁇ 500nm. In one embodiment, the distance between adjacent grooves is 100 to 1000 nm.
  • the adjacent grooves are The spacing between them can be 150 ⁇ 800nm, or it can be 200 ⁇ 600nm, or it can be 250 ⁇ 500nm, or it can be 300 ⁇ 400nm.
  • the plurality of grooves can be arranged irregularly and dispersed on the surface of the glass substrate.
  • the plurality of ravines may be arranged in a regular manner, for example, in a staggered manner or in an array.
  • Using multiple grooves as the surface micro-nano structure of the glass substrate can be formed in more diverse ways, such as using acid treatment to obtain multiple irregular grooves, or using a diamond flying knife to obtain regular grooves, etc.
  • the surface of the glass substrate 1 has a plurality of micron and/or nanometer-sized depressions, and the plurality of depressions constitute a micro-nano structure on the surface of the glass substrate 1 .
  • Figure 6 is a schematic diagram of the third micro-nano structure on the surface of the glass substrate provided by the present application.
  • the bottom size of the depression 61 is smaller than the top size, and may be in the shape of an inverted cone, an inverted pyramid or an inverted steamed bun. In other embodiments, the bottom size of the depression is the same as the top size, and may be rectangular, cylindrical, etc. In one embodiment, the depth of the recess is 50-1000 nm.
  • the depth of the recess is It can be 100 ⁇ 800nm, or it can be 150 ⁇ 700nm, or it can be 200 ⁇ 600nm, or it can be 250 ⁇ 500nm, or it can be 300 ⁇ 400nm.
  • the top size of the recess is 100 to 3000 nm. In other embodiments, in order to avoid affecting the optical performance of the anti-reflective glass, such as not increasing its reflectivity and not reducing its transmittance, the recessed top size is 100 to 3000 nm.
  • the top size can be 150-2000nm, or it can be 200-1500nm, or it can be 250-1000nm, or it can be 300-800nm, or it can be 350-500nm.
  • the spacing between adjacent recesses is 100 to 1000 nm.
  • the adjacent recesses are The spacing between them can be 150 ⁇ 800nm, or it can be 200 ⁇ 600nm, or it can be 250 ⁇ 500nm, or it can be 300 ⁇ 400nm.
  • the plurality of depressions can be arranged irregularly and dispersed on the surface of the glass substrate. In other embodiments, the plurality of depressions may be arranged regularly, for example, in an array. Using multiple depressions as the surface micro-nano structure of the glass substrate is beneficial to retaining the surface structure of the glass substrate, such as retaining the ion exchange layer on the surface of the tempered glass substrate, so that the glass substrate maintains good mechanical properties.
  • micro-nano structure on the surface of the glass substrate 1 can be obtained through surface processing methods well known to those skilled in the art such as metal masks, diamond flying knives, acid etching, etc. This application has no special restrictions on this.
  • a typical process of using a metal mask to obtain surface micro-nano structures is as follows: a metal film, such as an indium film, is coated on a glass substrate, and then heated to shrink the metal film, and the remaining metal film is deplated after plasma etching, i.e. Glass substrates with micro-nano structures on the surface can be obtained.
  • a metal film such as an indium film
  • a typical process of using a diamond flying knife to obtain surface micro-nano structures is: placing the glass substrate on the workbench, using a diamond tool to fly-cut it to form a micro-groove structure array, prism matrix, micro-structure linear layer and other surfaces. structure.
  • a typical process of using acid etching to obtain surface micro-nano structures is: soaking the glass substrate in a mixture of hydrofluoric acid and sulfuric acid for 5 to 30 minutes, cleaning and drying.
  • the anti-reflective glass also includes a first anti-reflective film layer 2 superimposed on the surface of the glass substrate 1.
  • the first anti-reflective film layer 2 is formed by alternately superposing a high refractive index layer 21 and a low refractive index layer 22, which can reduce the reflectivity of the glass. , increase the transmittance of glass.
  • the thickness of the first anti-reflection film layer 2 is 500-3000 nm. In other embodiments, the thickness of the first anti-reflection film layer 2 may be 600-2500 nm, or may be 700-2000 nm, or may be It is 800 ⁇ 1500nm, or it can be 900 ⁇ 1200nm.
  • the period of alternating superposition of the high refractive index layer 21 and the low refractive index layer 22 and the thickness of each layer can be designed according to the optical requirements through film layer design software, such as TFC, Macleod, etc.
  • film layer design software such as TFC, Macleod, etc.
  • the period in which the high refractive index layer 21 and the low refractive index layer 22 are alternately superposed may be an integer number of periods or a non-integer number of periods.
  • the stacked structure of the first anti-reflection film layer 2 can be: high refractive index layer 21/low refractive index layer 22/high refractive index layer 21/low refractive index layer 22.../high refractive index layer 21/low refractive index Index layer 22/high refractive index layer 21/low refractive index layer 22, as shown in Figure 7; it can also be: high refractive index layer 21/low refractive index layer 22/high refractive index layer 21/low refractive index layer 22...
  • the materials of each high refractive index layer in the first anti-reflection film layer 2 are the same, and the materials of each low refractive index layer are the same. In other embodiments, the materials of each high refractive index layer in the first anti-reflection film layer 2 are the same, and the materials of each low refractive index layer are different; or, the materials of each high refractive index layer in the first anti-reflection film layer 2 are different. , the materials of each low refractive index layer are the same; or, the materials of each high refractive index layer in the first anti-reflection film layer 2 are different, and the materials of each low refractive index layer are also different.
  • the refractive index of the high refractive index layer material is 1.9-2.3; the refractive index of the low refractive index layer material is 1.6-1.8.
  • the materials of the high refractive index layer include but are not limited to Nb 2 O 5 , TiO 2 , Ta 2 O 5 , Si 3 N 4 , ZrO 2 , AlN or AlON; the materials of the low refractive index layer include But it is not limited to SiO 2 , MgF 2 or Al 2 O 3 .
  • the material of the low refractive index layer is Al 2 O 3 ; the material of the high refractive index layer is AlN or AlON.
  • the hardness of Al 2 O 3 is relatively high, Mohs. The hardness is about 9, which can improve the scratch resistance of glass.
  • the first anti-reflection film layer 2 has Al 2 O 3 /AlN/Al 2 O 3 /AlN/Al 2 O 3 /AlN/ Al 2 O 3 /AlN/Al 2 O 3 or Al 2 O 3 /AlN/Al 2 O 3 /AlN/Al 2 O 3 /AlN/Al 2 O 3 /AlN/Al 2 O 3 /AlN/Al 2 O 3 /AlN/Al 2 O 3 /AlN/Al 2 O 3 stacked structure, which makes the obtained anti-reflection Glass has low reflectivity, high transmittance, good scratch resistance and high hardness.
  • the first anti-reflection film layer 2 has SiO 2 /Nb 2 O 5 /SiO 2 /Nb 2 O 5 /SiO 2 /Nb 2 O 5 /SiO 2 / Nb 2 O 5 /SiO 2 /Si 3 N 4 laminate structure, this structure makes the anti-reflection glass have lower reflectivity, higher hardness and good friction resistance.
  • the anti-reflective glass is single-sided coated glass, that is, the first surface of the glass substrate 1 is superimposed with the first anti-reflective film layer 2 .
  • the anti-reflective glass may be double-sided coated glass, that is, a first anti-reflective film layer is superimposed on the first surface of the glass substrate 1 and a second anti-reflective film layer is superimposed on the second surface corresponding to the first surface. Reflective coating layer, double-sided coated glass has lower reflectivity and higher transmittance.
  • the second anti-reflective film layer and the first anti-reflective film layer may be the same or different; when the second anti-reflective film layer is different from the first anti-reflective film layer, the second anti-reflective film layer
  • the arrangement of the layers refers to the arrangement of the first anti-reflection film layer above, which will not be described again in this application.
  • the anti-reflective glass is tested with a haze meter or gloss meter, and its glossiness is greater than 85. In some possible embodiments, the glossiness of the anti-reflective glass is greater than 88, which is more conducive to obtaining higher transmittance and lower reflectivity.
  • the anti-reflective glass is tested by Vickers indentation hardness, with an indentation depth less than or equal to about 100 nm measured on the surface and a hardness greater than or equal to about 1100 HV. In one embodiment, the anti-reflective glass has a Vickers hardness greater than 1150 HV.
  • the surface hardness of the anti-reflective glass is tested with a Mohs hardness pen. Under a force of 500g, a Mohs hardness pen with a Mohs hardness of 7 scratches the glass surface, and no scratches are visible to the naked eye under 800lux light.
  • the optical properties of the anti-reflection glass are tested with a spectrophotometer.
  • the reflectance of the single-sided coating in the light wavelength range of 380 to 780 nm is ⁇ 2%, and the transmittance of the single-sided coating is >93%; the light wavelength of 940nm is transparent. Rate>92%.
  • a colorimeter is used to test the anti-reflective glass, and its reflection color value a value is ⁇ 2 , b value ⁇ 2, transmitted color value a value ⁇ 1, b value ⁇ 1.
  • a 10Kg force is applied on a marble surface with a surface roughness of 5.6um and a 5*5cm anti-reflective glass with a stroke of 10cm and a back and forth cycle. After 40 cycles of friction, there are no visible scratches under 800lux light.
  • the glass deformation amount is less than 0.20 mm using a glass profile test (CAV scan) for anti-reflective glass. In some embodiments, the deformation of the anti-reflective glass is less than 0.1 mm.
  • the first anti-reflection film layer 2 can be sequentially coated on the glass substrate 1 by magnetron sputtering.
  • the coating parameters can be selected according to the film layer system. There are no special restrictions in this application.
  • the embodiments of the present application also provide a method for preparing the above-mentioned anti-reflective glass, the schematic flow diagram of which is shown in Figure 10, including the following steps:
  • Step S1 forming a micro-nano structure on at least one surface of the glass substrate
  • Step S2 Superimpose the first anti-reflection film layer on the surface of the glass substrate with micro-nano structure.
  • a micro-nano structure is formed on at least one surface of the glass substrate. Specifically, it can be obtained by surface processing methods well known to those skilled in the art such as metal mask, diamond flying knife, acid etching, etc., and micro grooves are formed on the surface of the glass substrate. Micro-nano structures such as groove structure arrays, prism matrices, microstructure linear layers, and protrusions distributed in arrays.
  • a metal mask can be used to obtain a micro-nano structure.
  • the flow diagram is shown in Figure 11, which includes the following steps:
  • Step S11 forming a metal film on at least one surface of the glass substrate
  • Step S12 Process the metal film to form metal nanoparticles
  • Step S13 Perform plasma etching on the glass obtained in step S12 to construct a nanoprotrusion array structure on the glass surface;
  • Step S14 Strip the metal on the glass surface obtained in step S13.
  • a metal indium film is first formed on at least one surface of the glass substrate by vacuum sputtering or other methods, and then is treated, such as heat treatment, to cause the metal indium film to heat shrink to form a similar shape.
  • the nanoparticles are arranged in an array, and then the glass substrate is plasma etched.
  • the surface of the glass substrate covered with indium nanoparticles will not be etched, and the surface of the glass substrate not covered with indium nanoparticles will be etched, thereby forming a convex surface.
  • Surface structure after deplating indium nanoparticles, a glass substrate with a micro-nano structure can be obtained, and the surface has protrusions arranged in a similar array.
  • the embodiments of the present application have no special restrictions on the parameters for forming the metal indium film by vacuum sputtering, and those skilled in the art can select them according to needs.
  • the thickness of the metal indium film is 3 to 8 nm.
  • the indium film After the indium film is formed, it is heat treated to form indium nanoparticles.
  • the embodiments of the present application have no special restrictions on the parameters of the heat treatment. Those skilled in the art can choose according to needs. For example, the heating rate of the heat treatment is 15-25°C/min, heating to 100-200°C, and keeping the temperature for 5-10 minutes. . In order not to affect the optical properties of the final product, the indium nanoparticles are evenly distributed and have a diameter of 50 to 70nm.
  • plasma etching is to etch the surface of the glass substrate that is not covered by the indium nanoparticles, so that the surface of the glass substrate covered by the indium nanoparticles forms protrusions.
  • the embodiments of the present application have no special restrictions on the parameters of the plasma etching. Those skilled in the art can set the parameters according to the expected size of the bumps, control the etching thickness, and obtain bumps that do not affect the optical performance of the final product.
  • the indium nanoparticles on the surface of the glass substrate are removed, for example, by deplating, and a glass substrate with a micro-nano structure on the surface can be obtained.
  • part of the metal indium film may not be thermally shrunk to form nanoparticles, but may exist in the form of a residual metal indium layer.
  • the surface of the glass substrate covered with the metallic indium layer and the surface of the glass substrate covered with indium nanoparticles will undergo the same changes, and finally a glass substrate with a micro-nano structure on the surface will be obtained.
  • an anti-reflective film is superimposed on the surface to obtain anti-reflective glass.
  • Embodiments of the present application can form an anti-reflective film on the surface of a glass substrate through deposition, such as vacuum deposition, including chemical vapor deposition, physical vapor deposition, thermal deposition, electron beam evaporation deposition or atomic layer deposition, etc., or through the use of liquid-based Methods such as spray coating, dip coating, spin coating or slit coating (for example, using sol-gel materials), etc.
  • the coating parameters of the AlN layer can be: sputtering power of the aluminum target: 7000 ⁇ 8000W, Ar flow: 100 ⁇ 150sccm, N2 flow: 100 ⁇ 120sccm, and RadicalSource power: 4000 ⁇ 5000W.
  • the coating parameters of the Al 2 O 3 layer can be: sputtering power of the aluminum target: 7500 ⁇ 8500W, Ar flow: 200 ⁇ 300sccm, O2 flow: 100 ⁇ 150sccm; RadicalSource power: 4000 ⁇ 5000W.
  • the anti-reflective glass provided by this application sets a micro-nano structure on the surface of the glass substrate and then superimposes the first anti-reflective film layer. On the one hand, it can ensure the dense accumulation of atoms in the short-range upper film layer and improve the scratch resistance of the coated glass surface. On the other hand, The long-range undulating structure allows the film lamination stress to be released locally and reduces the stress deformation of the glass substrate.
  • a thicker hard anti-reflection film layer such as a thickness of more than 500nm, can be superimposed on the glass substrate to reduce the reflectivity of the glass, increase the scratch resistance of the glass, and at the same time reduce the stress deformation of the glass substrate.
  • a thicker hard anti-reflection film layer such as a thickness of more than 500nm
  • It can be used in small-sized structures ⁇ 50mm such as camera lenses and watch covers, and can also be used in larger-sized structures such as electronic equipment covers.
  • the material of the low refractive index layer in the first anti-reflection film layer can be Al 2 O 3 with higher hardness, which further increases the hardness of the anti-reflection film layer, thereby improving the scratch resistance of the anti-reflection glass.
  • the anti-reflective glass provided by this application has low reflectivity, good scratch resistance and small stress deformation. It can not only be used in small-sized structures ⁇ 50mm such as camera lenses and watch covers, but can also be used in In larger structures such as electronic equipment covers.
  • the anti-reflective glass provided by this application can be used as a cover for electronic equipment. It will not cause glare under strong sunlight, making it easier for users to see the content displayed on the screen clearly, and improving the user experience of the product.
  • the electronic equipment cover has good scratch resistance and is not prone to visible scratches. It does not affect the appearance of the electronic equipment and does not reduce the impact resistance of the glass.
  • the electronic device mentioned in this application can be any device with communication and storage functions, such as smartphones, cellular phones, cordless phones, Session Initiation Protocol (Session Initiation Protocol, SIP) phones, tablet computers, personal digital assistants (Personal Digital Assistant) ,PAD), notebook computers, digital cameras, e-book readers, portable multimedia players, handheld devices with wireless communication capabilities, computing devices or other processing devices connected to wireless modems, vehicle-mounted devices, wearable devices, 5G terminal devices etc., the embodiments of the present application are not limited to this.
  • the anti-reflective glass provided by the present application its preparation method, the display screen of the electronic device and the electronic device will be described in detail below with reference to the examples.
  • the glass substrate is 0.55mm thick tempered glass; the glossiness is tested by a gloss meter; the Vickers hardness is tested by a Vickers indentation instrument; the Mohs hardness is tested by a Mohs hardness pen; and the optical properties are tested by spectroscopy. Photometer test; color value is tested by colorimeter.
  • Step 1 Vacuum sputter the metal indium film on the glass substrate.
  • the specific steps are as follows:
  • Radio frequency magnetron sputtering is used for pretreatment before coating.
  • Radical Source power 4500W
  • Ar flow 0sccm
  • O2 flow 120sccm
  • N2 flow 0sccm
  • Time 240s;
  • Indium film coating parameters Indium target sputtering power: 3000W; Ar flow rate: 120sccm.
  • Step 2 Heat the metal indium film layer to shrink it into a ball.
  • the specific steps are as follows:
  • Step 3 Perform plasma etching on the glass substrate template. The specific steps are as follows:
  • the background vacuum is 5.0 ⁇ 10 -3 Pa; the reactive ion etching power is 500W, the chamber pressure is 10Pa, the argon flow rate is 40sccm, the trifluoromethane flow rate is 5sccm, the etching time is 10min, and a nano-protrusion array structure is constructed on the glass surface;
  • Step 4 Clean and remove the residual metal indium on the surface of the glass substrate template. The specific steps are as follows:
  • the residual metal indium is deplated, and then the glass surface is cleaned with pure water to obtain a glass substrate with a micro-nano structure on the surface.
  • Figure 12 is a scanning electron microscope photo of the glass substrate prepared in Example 1 of the present invention.
  • the surface of the glass substrate has nano-sized protrusions in an array-like structure.
  • the nano-protrusions are similar to a truncated cone shape, and the bottom size is larger than the top size.
  • the nano-protrusions are 120 nm high and the bottom size is 200 nm.
  • the performance of the glass substrate was tested. Its transmittance to light with a wavelength of 550 nm was 90%, its reflectance was 3%, and its glossiness was 92.
  • Step 5 Perform hard AR coating on the glass substrate with micro-nano structure on the surface.
  • the specific steps are as follows:
  • the average single-sided transmittance from 380 to 780nm is required to be greater than 93%. Due to the high transmittance requirements in the visible light band, the film stack 2H is used, and L is selected with high hardness and relatively low refractive index. Al 2 O 3 , H is selected as AlN, and the initial film system HL is formed in the optical thin film software, thus forming a stacked film system of L and H, and then the band optimization conditions are entered in the continuous target to ensure that the transmittance meets the requirements; Then enter the LAB value requirements in the color target to ensure that the color is colorless.
  • Table 1 is the AR film system structure provided in Embodiment 1 of the present invention:
  • the coating parameters of the AlN layer are: sputtering power of the aluminum target: 7500W, Ar flow: 120sccm, N2 flow: 80sccm, RadicalSource power: 4500W;
  • Coating parameters of Al 2 O 3 layer Sputtering power of aluminum target: 8000W, Ar flow: 250sccm, O 2 flow: 120sccm; Power of RadicalSource: 4500W;
  • Coating is performed to obtain a structure of glass substrate (0.55mm)/Al 2 O 3 (133.19nm)/AlN (16.63nm)/Al 2 O 3 (40.05nm)/AlN (151.03nm)/Al 2 O 3 (45.25 nm)/AlN(33.62nm)/Al 2 O 3 (32.28nm)/AlN (70.6nm)/Al 2 O 3 (80.1nm) anti-reflective glass.
  • the obtained anti-reflective glass was tested for performance and the results are as follows:
  • Vickers hardness is 1170HV
  • a Mohs hardness pen with a Mohs hardness of 7 scratches the glass surface, and there is no scratch visible to the naked eye under 800lux light; on a marble surface with a surface roughness of 5.6 ⁇ m, a 10Kg force is applied to the 5*5cm glass, the stroke is 10cm, and the round trip is After one cycle and 40 cycles of rubbing, there are no visible scratches under 800lux light.
  • the reflectance of the single-sided coating is 0.46%
  • the transmittance of the single-sided coating is 94.34%
  • the transmittance of 940nm light is 92.6%
  • the reflected color value a value is ⁇ 2
  • the b value is ⁇ 2
  • the transmitted color value a value is ⁇ 1
  • the b value is ⁇ 1.
  • the stress deformation of the glass substrate is measured using a glass profile test (CAV scan).
  • the glass deformation amount is less than 0.20 mm, as shown in Figure 13.
  • Figure 13 is the CAV scan result of the anti-reflective glass in Example 1 of the present application.
  • Step 1 Vacuum sputter the metal indium film on the glass substrate.
  • the specific steps are as follows:
  • RadicalSource power 4500W Ar flow: 0sccm; O2 flow: 120sccm; N2 flow: 0sccm; Time: 240s;
  • Indium film coating parameters Indium target sputtering power: 3000W, Ar flow rate: 120sccm.
  • Step 2 Heat the metal indium film layer to shrink it.
  • the specific steps are as follows:
  • Step 3 Perform plasma etching on the glass substrate template. The specific steps are as follows:
  • the background vacuum is 5.0 ⁇ 10 -3 Pa; the reactive ion etching power is 500W, the chamber pressure is 10Pa, the argon flow rate is 40sccm, the trifluoromethane flow rate is 10sccm, the etching time is 8min, and a nano-protrusion array structure is constructed on the glass surface;
  • Step 4 Clean and remove the residual metal indium film on the surface of the glass substrate template. The specific steps are as follows:
  • the residual metal indium film layer is deplated, and then the glass surface is cleaned with pure water to obtain a glass substrate with a micro-nano structure on the surface.
  • Figure 14 is a scanning electron microscope photo of the glass substrate prepared in Example 2 of the present invention.
  • the surface of the glass substrate has nano-sized protrusions in an array-like structure.
  • the nano-protrusions are similar to a truncated cone shape, and the bottom size is larger than the top size.
  • the nano-protrusions are 100 nm high and the bottom size is 400 nm.
  • the performance of the glass substrate was tested. Its transmittance to light with a wavelength of 550 nm was 90%, its reflectance was 1%, and its glossiness was 85.
  • Step 5 Perform hard AR coating on the glass substrate with micro-nano structure on the surface.
  • the specific steps are as follows:
  • the average single-sided transmittance from 380 to 780nm is required to be greater than 93%. Due to the high transmittance requirements in the visible light band, the film stack 2H is used, and L is selected with high hardness and relatively low refractive index. Al 2 O 3 , H is selected as AlN, and the initial film system HL is formed in the optical thin film software, thus forming a stacked film system of L and H, and then the band optimization conditions are entered in the continuous target to ensure that the transmittance meets the requirements; Then enter the LAB value requirements in the color target to ensure that the color is colorless.
  • Table 2 is the AR film system structure provided in Embodiment 2 of the present invention:
  • Coating parameters of AlN layer Sputtering power of aluminum target: 7500W; Ar flow rate: 120sccm, N2 flow rate: 80sccm; RadicalSource power: 4500W;
  • Coating parameters of Al 2 O 3 layer sputtering power of aluminum target: 8000W; Ar flow rate: 250 sccm, O 2 flow rate: 120 sccm; RadicalSource power: 4500W.
  • Coating is carried out to obtain a structure of glass substrate (0.55mm)/Al 2 O 3 (78nm)/AlN (125nm)/Al 2 O 3 (151nm)/AlN (272nm)/Al 2 O 3 (150nm)/AlN ( 131nm)/Al 2 O 3 (180nm)/AlN (21nm)/Al 2 O 3 (188nm)/AlN (47nm)/Al 2 O 3 (83nm) anti-reflective glass.
  • the obtained anti-reflective glass was tested for performance and the results are as follows:
  • Vickers hardness is 1138HV; under 500g force, a Mohs hardness pen with a Mohs hardness of 7 scratches the glass surface, and no scratches are visible to the naked eye under 800lux light; on a marble surface with a surface roughness of 5.6um, a 10Kg force is applied to 5*5cm glass , the stroke is 10cm, and the back and forth is one cycle. After 40 cycles of friction, there are no visible scratches under 800lux light.
  • the reflectance of the single-sided coating is 0.2%
  • the transmittance of the single-sided coating is 91.8%
  • the transmittance of 940nm light is 91.5%
  • the reflected color value a value is ⁇ 2
  • the b value is ⁇ 2
  • the transmitted color value a value is ⁇ 1
  • the b value is ⁇ 1.
  • the stress deformation of the glass substrate is measured using a glass profile test (CAV scan).
  • the glass deformation amount is less than 0.10 mm, as shown in Figure 15.
  • Figure 15 is the CAV scan result of the anti-reflective glass of Example 2 of the present application.
  • FIG. 16 is a schematic structural diagram of a mobile phone.
  • the mobile phone 100 includes a screen 10.
  • the outer screen (i.e. cover) of the screen 10 is composed of the above-mentioned Made of anti-reflective glass.
  • the surface of the external screen is flat and basically non-deformed; when the user uses the phone, it will not cause glare under strong sunlight, and the user can clearly see the content displayed on the screen, and the product usage experience is good.
  • the outer screen of the phone has good scratch resistance, and it is not prone to visible scratches without a film. The phone looks better after long-term use.

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Abstract

L'invention concerne un verre antireflet, comprenant : un substrat en verre (1), une première surface du substrat en verre (1) ayant une micro-nanostructure (11) ; et une première couche de film antireflet (2) empilée sur la première surface du substrat en verre (1), la première couche de film antireflet (2) étant formée par superposition alternée de couches à indice de réfraction élevé (21) et de couches à faible indice de réfraction (22). Divulgué en outre est un écran d'affichage de dispositif électronique et un dispositif électronique. La micro-nanostructure (11) d'une structure de surface de taille micrométrique ou nanométrique est disposée sur la surface du substrat en verre (1) pour assurer l'accumulation dense d'atomes dans une couche de film à une courte portée et augmenter la dureté de la couche de film, de telle sorte que la résistance aux rayures de la surface d'un verre revêtu de film. Pendant ce temps, une structure ondulée à une longue portée permet à la contrainte de couche de film d'être libérée localement à une longue portée, réduit la déformation de contrainte du substrat en verre, de telle sorte que le substrat en verre (1) n'est pas soumis à une grande déformation de contrainte lorsqu'une couche de film antireflet épaisse est empilée, et peut être utilisé dans des structures de grande taille telles que des écrans d'affichage de dispositif électronique.
PCT/CN2023/070076 2022-03-31 2023-01-03 Dispositif électronique WO2023185179A1 (fr)

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