WO2018199431A1 - Verre incurvé et son procédé de fabrication - Google Patents

Verre incurvé et son procédé de fabrication Download PDF

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Publication number
WO2018199431A1
WO2018199431A1 PCT/KR2018/000789 KR2018000789W WO2018199431A1 WO 2018199431 A1 WO2018199431 A1 WO 2018199431A1 KR 2018000789 W KR2018000789 W KR 2018000789W WO 2018199431 A1 WO2018199431 A1 WO 2018199431A1
Authority
WO
WIPO (PCT)
Prior art keywords
glass
coating layer
low reflection
reflection coating
tempered glass
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/KR2018/000789
Other languages
English (en)
Korean (ko)
Inventor
문병천
최학년
안정식
이진수
장봉철
황민규
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
LG Electronics Inc
Original Assignee
LG Electronics Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from KR1020170121969A external-priority patent/KR102048993B1/ko
Application filed by LG Electronics Inc filed Critical LG Electronics Inc
Priority to US16/608,070 priority Critical patent/US20200189951A1/en
Priority to EP18791491.6A priority patent/EP3617166A4/fr
Publication of WO2018199431A1 publication Critical patent/WO2018199431A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B23/00—Re-forming shaped glass
    • C03B23/02—Re-forming glass sheets
    • 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
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • 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
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/28—Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material
    • C03C17/32—Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material with synthetic or natural resins
    • 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
    • C03C21/00—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface

Definitions

  • the present invention relates to a curved cover glass used in a curved display and a manufacturing method thereof.
  • a cover glass for protecting the display is disposed.
  • the cover glass should be high in light transmittance and not easily broken.
  • various reinforcement methods have been utilized to prevent the glass from breaking easily.
  • the glass strengthening method As an example of the glass strengthening method, a chemical strengthening method has been utilized.
  • Conventional cover glass was prepared by replacing sodium ions contained in the glass with potassium ions through an ion exchange method. When the glass is cooled in a state in which potassium ions are relatively bulkier than sodium ions, the volume of the glass can be increased while maintaining the same volume as before.
  • the chemical strengthening method is a very useful glass strengthening method because it does not increase the thickness of the glass, and does not lower the transparency of the glass.
  • the chemical strengthening method has some disadvantages.
  • a low reflection coating layer is used that does not interfere with the driver's view.
  • the low reflection coating layer absorbs light introduced from the outside, thereby preventing the cover glass from reflecting light and obstructing the driver's view.
  • the low reflection coating layer may be destroyed at high temperatures and may interfere with chemical strengthening, it should be formed after the surface processing and chemical strengthening.
  • the thickness of the coating layer may vary depending on the curvature of the curved region.
  • the uniformity of the coating layer may be inferior as compared with forming the coating layer in the planar region. As a result, color differences between the planar region and the curved region may occur. This can give a sense of heterogeneity to the user.
  • the present invention provides a curved glass and a method of manufacturing the same that can solve the problems caused when chemically strengthening the curved glass while forming a low reflection coating layer.
  • a tempered glass and a manufacturing method thereof comprising a curved surface where the low reflection coating layer is uniformly formed in the curved area.
  • an object of the present invention is to provide a tempered glass including a curved surface for minimizing color difference between regions having different curvatures, and a method of manufacturing the same.
  • the present invention aims to be able to form a coating layer irrespective of the glass area by converting the low reflection coating treatment to a coating method instead of dry deposition.
  • the present invention comprises a glass comprising a curved area, a low reflection coating layer coated on the glass surface, a low reflection coating layer consisting of a mixture of a binder and a hollow material, the glass to a predetermined depth
  • a tempered glass characterized in that the ions have penetrated.
  • the content of the hollow material included in the low reflection coating layer, the central portion of the low reflection coating layer may be higher than the edge of the low reflection coating layer.
  • the binder may be in a state in which Tetraethyl orthosilicate and Trimethoxy-methylsilane are polymerized together.
  • the glass may include a first region having a first curvature and a second region having a second curvature different from the first curvature.
  • the color difference ⁇ E * ab between the first area and the second area may be 2 or less based on the first area.
  • the thickness of the low reflection coating layer coated on the first region and the thickness of the low reflection coating layer coated on the second region is 10% It can be different.
  • the weight average molecular weight of the binder may be 1500 to 3500.
  • the average particle diameter of the hollow material may be 60 to 90nm.
  • the low reflection coating layer may be formed of a single layer.
  • the depth of penetration of the potassium ions may be 30 to 50 ⁇ m.
  • the thickness of the low reflection coating layer may be 100 to 150 nm.
  • the present invention is a step of polymerizing the first monomer and the second monomer to form a binder polymer, by mixing the binder polymer and the hollow material and then polymerizing, to prepare a low reflection coating liquid, the low reflection coating liquid flat glass Forming a low reflection coating layer by baking on the glass, and forming a low reflection coating layer on the flat glass on which the low reflection coating layer is formed. It provides a method for producing tempered glass comprising the step of penetrating potassium ions.
  • the low reflection coating layer is formed before the curved surface processing, the low reflection coating layer can be uniformly formed even in regions having different curvatures. Through this, the present invention can minimize the color difference generated in the curved glass due to the low reflection coating layer.
  • the low reflection coating layer since the low reflection coating layer does not interfere with chemical strengthening, the low reflection coating layer can be formed on the glass surface before chemical strengthening. Through this, the present invention can form a low reflection coating layer before the glass is curved, it is possible to increase the uniformity of the low reflection coating layer.
  • FIG. 1 is a conceptual diagram illustrating a conventional method of performing chemical strengthening and low reflection coating on curved glass.
  • FIG. 2 is a conceptual diagram illustrating a method of manufacturing tempered glass according to the present invention.
  • FIG. 3 is a conceptual diagram showing a cross section of the tempered glass according to the present invention.
  • Figure 4a is a cross-sectional picture of the tempered glass before chemical strengthening.
  • Figure 4b is a cross-sectional picture of the tempered glass after chemical strengthening.
  • 5 is a graph showing reflectances before and after chemical strengthening.
  • Figure 6a is a graph showing the element distribution of the tempered glass chemically strengthened in the absence of a coating layer.
  • 6b is a graph showing an element distribution of tempered glass according to the present invention.
  • FIG. 1 is a conceptual diagram illustrating a conventional method of performing chemical strengthening and low reflection coating on curved glass.
  • the step (S120) of processing the flat glass of the desired size (S110), and the flat surface of the flat glass 110 (S120) proceeds first.
  • Curve forming is carried out at a high temperature of 600 ° C or higher. For this reason, when the chemical strengthening and the low reflection coating is performed before the surface forming, the chemical strengthening effect may disappear or the low reflection coating layer may be broken during the surface forming.
  • step S130 of chemically strengthening the curved glass is performed.
  • Chemical strengthening is a method of increasing the hardness of the glass by penetrating potassium ions into the glass, when the coating layer is formed on the glass surface, it is difficult to penetrate potassium ions. Because of this, chemical strengthening must be performed prior to forming a coating layer on the glass surface.
  • the present invention provides a method for uniformly forming a low reflection coating layer in performing chemical strengthening and low reflection coating on curved glass.
  • a method of manufacturing tempered glass according to the present invention will be described with reference to the accompanying drawings.
  • FIG. 2 is a conceptual diagram illustrating a method of manufacturing tempered glass according to the present invention.
  • the step S220 of processing a flat glass of a desired size and forming a low reflection coating layer on the flat glass is performed.
  • the low reflection coating layer 120 may be formed through a firing process after applying a coating liquid consisting of a mixture of a binder and a hollow material to the flat glass 110 surface.
  • the hollow material serves to lower the reflectance of the coating layer. Specifically, the hollow material lowers the reflectance by making an air layer on the glass surface to lower the refractive index.
  • the hollow material may be made of silica. Since the hollow silica made of silica does not decompose even at a high temperature of 600 ° C. or higher, the coating layer may not be broken even if the low reflection coating layer is formed and then the curved surface is formed.
  • the average particle diameter of the hollow material may be 60 to 90nm.
  • Hollow silica having a particle diameter of less than 60 nm is difficult to manufacture in fact, and when the particle diameter of the hollow silica exceeds 90 nm, the coating layer is difficult to form uniformly because it becomes similar to the thickness of the coating layer to be described later.
  • the binder serves to allow the hollow material to be fixed to the glass. Since the binder is exposed to a high temperature of 600 ° C. or higher during curved forming, the binder should be made of a material that does not break down even at a temperature of 600 ° C. or higher.
  • the binder may be made of a silane-based binder, and specifically, the binder may be a binder of tetraethyl orthosilicate (TEOS), trimethoxy-methylsilane (MTMS), Fluoro-Silaner series, Acryl-Silane series, Silazane series have.
  • TEOS tetraethyl orthosilicate
  • MTMS trimethoxy-methylsilane
  • Fluoro-Silaner series Acryl-Silane series
  • Silazane series have.
  • the weight average molecular weight of the binder may be 1500 to 3500.
  • the weight average molecular weight of the binder is less than 1500, since the viscosity of the coating liquid is lowered, the influence on foreign matters during coating may be increased, and the intermolecular interaction may be weakened, thereby decreasing the coatability.
  • the weight average molecular weight of the binder exceeds 3500, the viscosity is high, the smoothness of the coating layer is lowered, the stability of the coating layer may be lowered.
  • two or more kinds of binders may be mixed and used.
  • a mixture of TEOS and MTMS can be utilized as the binder.
  • the monomers of each of TEOS and MTMS may be mixed and polymerized first, and then mixed with a hollow material to prepare a coating solution.
  • the binder molecules surround the hollow material surface.
  • a core-cell structure can be formed in which the hollow material is the core and the binder molecules are the cell. This core-cell structure allows the hollow material to spread evenly when applied to the glass surface.
  • the present invention can protect the hollow material having a function of substantially lowering the reflectance from external impact or the like.
  • a low reflection coating layer may be formed through a firing process.
  • the firing may be performed for 4 to 6 minutes at a temperature of 400 to 750 °C in the kiln.
  • the low reflection coating layer formed in the above-described manner may have a thickness of 100 to 150 nm. If the thickness of the coating layer is less than 100nm, the effect of reducing the reflectance is inferior, and if it exceeds 150nm, the coating layer is inferior in uniformity, and the chemical strengthening to be performed later may not be performed properly.
  • the low reflection coating layer may be composed of a single layer so that potassium ions can pass through the coating layer.
  • the porosity of the low reflection coating layer according to the present invention may be 30 to 70%.
  • the porosity of the low reflection coating layer is less than 30%, it is difficult to expect the reflection suppression effect, and potassium ions hardly penetrate to the glass surface during chemical strengthening, which will be described later.
  • the porosity of the coating layer exceeds 70%, the durability of the coating layer may be excessively degraded.
  • the low reflection coating layer formed in the above-described manner has a reflectance of 1% or less.
  • the step of forming the curved surface of the flat glass is performed.
  • Curved molding may be performed by press molding, and may be performed at a pressure of 0.005 to 0.006 MPa at a temperature of 700 to 780 ° C.
  • the present invention is not limited thereto.
  • the hollow material and the binder according to the present invention are not decomposed at a temperature of 700 to 780 ° C., the low reflection coating layer is not destroyed even after the curved surface forming, and the uniform coating layer formed on the flat glass can be maintained as it is.
  • the radius of curvature of the curved glass may be 5R or more.
  • the present invention is not limited thereto, and the radius of curvature may vary depending on the thickness of the glass and the area of the glass.
  • step S240 is performed to chemically strengthen the curved surface.
  • Chemical strengthening may be carried out by immersing the glass in KNO 3 solution heated to a temperature of 380 to 435 ° C. for 2 to 8 hours. At this time, due to the difference in potassium ion concentration between the glass and the solution, potassium ions penetrate into the glass. As a result, the glass strength is improved.
  • the glass is implemented with a CS of 750 MPa or more. Since the low reflection coating layer according to the present invention is formed to a thickness of less than 150nm and has a porosity of 30% or more, potassium ions can easily penetrate the glass surface. That is, the low reflection coating layer according to the present invention does not interfere with the movement of potassium ions. An experimental example thereof will be described later.
  • TEOS and MTMS utilize primarily polymerized binders, the binder can surround the hollow material surface and protect the hollow material from strongly basic solutions.
  • FIG. 3 is a conceptual diagram showing a cross section of the tempered glass according to the present invention.
  • the tempered glass 100 manufactured by the above-described manufacturing method includes a glass 110 including a curved area, a low reflection coating layer coated on the glass surface and made of a mixture of a binder 120 and a hollow material 130.
  • the glass is characterized in that potassium ions penetrate to a predetermined depth.
  • the content of the hollow material included in the low reflection coating layer is higher than the edge of the low reflection coating layer .
  • This structure protects the hollow material from strongly basic solutions and protects the hollow material from external impacts upon chemical strengthening.
  • the tempered glass may include curved surfaces having different curvatures according to its use.
  • the glass may include a first region having a first curvature and a second region having a second curvature different from the first curvature.
  • the curvature when the curvature is 0, the curvature may be referred to as a plane, and the glass according to the present invention may include a planar region.
  • the thickness of the low reflection coating layer coated on the first region is based on the thickness of the low reflection coating layer coated on the first region.
  • the thickness of the low reflection coating layer coated on the second region may vary within 10%.
  • the color difference ⁇ E * ab between the first region and the second region may be 2 or less based on the first region.
  • the color difference ⁇ E * ab between a region having a maximum curvature and a region having a minimum curvature is 2 or less. That is, in the tempered glass according to the present invention, the color difference between all arbitrary regions is 2 or less.
  • the radius of curvature of the curved glass may be 5R or more.
  • the present invention is not limited thereto, and the radius of curvature may vary depending on the thickness of the glass and the area of the glass. That is, the tempered glass according to the present invention may have a curvature of at most 1 / 5R. Accordingly, the maximum curvature difference in the tempered glass according to the present invention may be 1 / 5R. In the tempered glass according to the present invention, the color difference ⁇ E * ab between two regions where the difference in curvature is maximum is 2 or less.
  • the depth of penetration of potassium ions into the glass may be 30 to 50 ⁇ m. This is the same depth as the potassium ions penetrated when the chemical strengthening is performed in the absence of the coating layer. That is, according to the present invention, even if the chemical strengthening after the coating layer is formed, the same chemical strengthening effect as in the prior art can be obtained.
  • Tempered glass was manufactured according to the above-mentioned manufacturing method using hollow silica having an average particle diameter of 73.29 nm and a dispersion degree of 0.031 as a hollow material, and a material obtained by primarily polymerizing TEOS and MTMS as a binder.
  • Figure 4a is a cross-sectional picture of the tempered glass before chemical strengthening
  • Figure 4b is a cross-sectional picture of the tempered glass after chemical strengthening.
  • the binder forms a coating layer in a state surrounding the surface of the hollow material. Accordingly, a binder is mainly disposed at the edge of the coating layer, and a hollow material is mainly disposed at the center of the coating layer.
  • the low reflection coating layer is 100 to 130nm.
  • the reflectance was measured before and after chemical strengthening.
  • 5 is a graph showing reflectances before and after chemical strengthening.
  • the tempered glass according to the present invention can be confirmed that the reflectance is less than 1% at a wavelength of 500nm or more. That is, it can be confirmed that the tempered glass according to the present invention has a reflectance of less than 1% even at a thickness of 100 to 150 nm.
  • ⁇ E * ab was 0.8 as a result of measuring the color difference between the curved area and the planar area of the tempered glass according to the present invention. This is difficult for the human eye to distinguish. Through this, the tempered glass according to the present invention is almost no color difference caused by the low reflection coating does not give a user a foreign object.
  • Element (Na, Si, K) distribution according to the depth of the tempered glass prepared in Example was measured.
  • element distribution of the tempered glass which was chemically strengthened in the absence of the coating layer was measured.
  • FIG. 6A is a graph showing an element distribution of tempered glass subjected to chemical strengthening in the absence of a coating layer
  • FIG. 6B is a graph showing an element distribution of tempered glass according to the present invention.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Surface Treatment Of Glass (AREA)

Abstract

La présente invention concerne un verre de revêtement incurvé utilisé pour un dispositif d'affichage incurvé et son procédé de fabrication. La présente invention concerne du verre trempé comprenant : du verre présentant une zone incurvée ; et une couche de revêtement à faible réflexion, revêtue sur une surface du verre, composée d'un mélange d'un liant et d'un matériau creux, le verre comprenant des ions potassium qui pénètrent jusqu'à une profondeur prédéterminée à l'intérieur de celui-ci. Selon la présente invention, une couche de revêtement à faible réflexion est formée avant le traitement de surface incurvée, et ainsi, la couche de revêtement à faible réflexion peut être formée uniformément, même sur des zones ayant des courbures différentes. La présente invention peut ainsi réduire au minimum la différence de couleur produite dans le verre incurvé en raison de couches de revêtement à faible réflexion.
PCT/KR2018/000789 2017-04-24 2018-01-17 Verre incurvé et son procédé de fabrication Ceased WO2018199431A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
US16/608,070 US20200189951A1 (en) 2017-04-24 2018-01-17 Curved glass and manufacturing method thereof
EP18791491.6A EP3617166A4 (fr) 2017-04-24 2018-01-17 Verre incurvé et son procédé de fabrication

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
US201762488867P 2017-04-24 2017-04-24
US62/488,867 2017-04-24
KR1020170121969A KR102048993B1 (ko) 2017-04-24 2017-09-21 곡면 글라스 및 그 제조방법
KR10-2017-0121969 2017-09-21

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WO2018199431A1 true WO2018199431A1 (fr) 2018-11-01

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PCT/KR2018/000789 Ceased WO2018199431A1 (fr) 2017-04-24 2018-01-17 Verre incurvé et son procédé de fabrication

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111691573A (zh) * 2019-03-11 2020-09-22 重庆大学 一种外挡墙结构

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20120098668A (ko) * 2009-10-20 2012-09-05 후구비카가구코오교우가부시끼가이샤 반사 방지 강화 유리의 제조 방법
KR20130034693A (ko) * 2011-09-29 2013-04-08 (주)석경에이티 고순도 중공 실리카 나노분말의 제조방법 및 동 나노분말을 포함하는 저반사 코팅막
KR20140026535A (ko) * 2011-05-02 2014-03-05 코닝 인코포레이티드 반사방지층을 갖는 유리 제품 및 이의 제조방법
KR20140058962A (ko) * 2012-11-07 2014-05-15 (주)엘지하우시스 실록산 화합물을 포함하는 초친수성 반사방지 코팅 조성물, 이를 이용한 초친수성 반사방지 필름 및 이의 제조방법
WO2015186753A1 (fr) * 2014-06-06 2015-12-10 旭硝子株式会社 Plaque de verre trempée chimiquement dotée d'un film fonctionnel, son procédé de production et article

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20120098668A (ko) * 2009-10-20 2012-09-05 후구비카가구코오교우가부시끼가이샤 반사 방지 강화 유리의 제조 방법
KR20140026535A (ko) * 2011-05-02 2014-03-05 코닝 인코포레이티드 반사방지층을 갖는 유리 제품 및 이의 제조방법
KR20130034693A (ko) * 2011-09-29 2013-04-08 (주)석경에이티 고순도 중공 실리카 나노분말의 제조방법 및 동 나노분말을 포함하는 저반사 코팅막
KR20140058962A (ko) * 2012-11-07 2014-05-15 (주)엘지하우시스 실록산 화합물을 포함하는 초친수성 반사방지 코팅 조성물, 이를 이용한 초친수성 반사방지 필름 및 이의 제조방법
WO2015186753A1 (fr) * 2014-06-06 2015-12-10 旭硝子株式会社 Plaque de verre trempée chimiquement dotée d'un film fonctionnel, son procédé de production et article

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See also references of EP3617166A4 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111691573A (zh) * 2019-03-11 2020-09-22 重庆大学 一种外挡墙结构
CN111691573B (zh) * 2019-03-11 2021-05-07 重庆大学 一种外挡墙结构

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