WO2017188477A1 - 눈부심 방지 유리 및 이의 제조 방법 - Google Patents

눈부심 방지 유리 및 이의 제조 방법 Download PDF

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Publication number
WO2017188477A1
WO2017188477A1 PCT/KR2016/004460 KR2016004460W WO2017188477A1 WO 2017188477 A1 WO2017188477 A1 WO 2017188477A1 KR 2016004460 W KR2016004460 W KR 2016004460W WO 2017188477 A1 WO2017188477 A1 WO 2017188477A1
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WIPO (PCT)
Prior art keywords
glass
glare
polysilazane
solvent
coating composition
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PCT/KR2016/004460
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English (en)
French (fr)
Inventor
김명운
박만영
김현관
송기훈
오재원
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(주)디엔에프
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Priority to US16/096,950 priority Critical patent/US11230492B2/en
Priority to PCT/KR2016/004460 priority patent/WO2017188477A1/ko
Priority to CN201680086128.1A priority patent/CN109153601B/zh
Priority to JP2018556462A priority patent/JP6882337B2/ja
Publication of WO2017188477A1 publication Critical patent/WO2017188477A1/ko

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Classifications

    • 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
    • C03C17/30—Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material with silicon-containing compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
    • B05D5/02—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain a matt or rough surface
    • 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
    • C03C2217/00—Coatings on glass
    • C03C2217/70—Properties of coatings
    • C03C2217/73—Anti-reflective coatings with specific characteristics
    • C03C2217/732—Anti-reflective coatings with specific characteristics made of a single layer
    • 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
    • C03C2217/00—Coatings on glass
    • C03C2217/70—Properties of coatings
    • C03C2217/77—Coatings having a rough surface
    • 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
    • C03C2217/00—Coatings on glass
    • C03C2217/70—Properties of coatings
    • C03C2217/78—Coatings specially designed to be durable, e.g. scratch-resistant
    • 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
    • C03C2218/00—Methods for coating glass
    • C03C2218/10—Deposition methods
    • C03C2218/11—Deposition methods from solutions or suspensions
    • C03C2218/112—Deposition methods from solutions or suspensions by spraying
    • 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
    • C03C2218/00—Methods for coating glass
    • C03C2218/30—Aspects of methods for coating glass not covered above
    • C03C2218/32—After-treatment

Definitions

  • the present invention relates to anti-glare glass which has improved anti-glare and visibility.
  • Reflected light on the display surface reduces contrast, reduces image visibility due to image reflection, and makes the screen dazzling and difficult to recognize, making it easier to increase eye and tiredness or headaches.
  • Antiglare technology is a technology that prevents reflection of external light by coating a mixture of organic / inorganic fine particles, binder resin or curable resin and forming irregularities on the surface.
  • Haze is a measure of anti-glare, usually in%
  • the anti-glare means the degree of glare caused by the external reflection of light.
  • the transmittance of light refers to the ratio of the intensity of light transmitted through the material layer or boundary and the intensity of incident light, usually expressed in%.
  • Korean Patent No. 10-1137206 discloses that a material is processed into a desired shape, sanded to form irregularities on the surface, and finished for improvement in perspective rate.
  • Korean Patent Application Laid-Open No. 10-2011-0060233 discloses a ceramic coating layer having a uniform thickness on a glass substrate, and peeling the ceramic coating layer from the glass substrate with an etchant solution based on the surface of the glass substrate. After forming the first roughness, the surface of the glass substrate is etched with the second etching solution to form a total roughness on the surface of the glass substrate.
  • Another way to improve anti-glare is to attach an antiglare film that can be refracted on the glass surface.
  • the film must be alternately attached to the high and low refractive films.
  • the unit price can be higher.
  • the purpose of the present invention is to solve the problem of blurred white screen caused by reflection of external light, deterioration of visibility due to deterioration of sharpness caused by excessive increase of haze, low anti-glare and high manufacturing cost. It is to provide an anti-glare glass and a method of manufacturing the same that can give visibility and visibility.
  • the above method has the advantage of minimizing glare, but the problem is that the light transmittance is reduced to reduce the visibility. Therefore, the transmittance at the appropriate haze value Should be able to maximize.
  • the present invention is meaningful in that it provides both a high haze and a high transmittance antiglare glass.
  • glass refers to all glass, polymers, and substrates commonly used in displays, in addition to which light entering the back of the substrate can penetrate the substrate and allow light to be identified. It can mean anything.
  • the present invention has a weight average molecular weight of 30,000 or less that satisfies the following formula (1).
  • a coating composition containing 1 to 40% by weight of polysilazane is applied to an antiglare glass which is sprayed onto a glass surface and laminated.
  • the haze of the antiglare glass may be 1 to 5%, and the transmittance of the antiglare glass is 90%. Can be more than%
  • the polysilazane is represented by the following formula (1).
  • R :, R 2 and R 3 are any of hydrogen, alkyl group, alkenyl group, cycloalkyl group, aryl group, group directly connected to silicon is selected from carbon group, alkylsilyl group, alkylamino group and alkoxy group) Or two or more, n is an integer .
  • the polysilazane may be an inorganic polysilazane or an organic polysilazane having a repeating unit of Chemical Formula 1.
  • the inorganic polysilazane does not have a group including R, R 2, and R 3 all containing carbon. , preferably R ,, R 2 and 3 ⁇ 4 both can be illustrated a hydrogen, inorganic polysilazane.
  • the organic polysilazane is at least one selected from R l5 R 2 and R 3 is an alkyl group, an alkenyl group, a cycloalkyl group,
  • the aryl group, the group directly connected to silicon may have a group containing any one or two or more selected from carbon group, alkylsilyl group, alkylamino group and alkoxy group.
  • N is the weight of polysilazane having a repeating unit of formula (1). If the average molecular weight is 30,000 or less, it is not limited.
  • the inorganic polysilazane and the organic polysilazane may be soluble in a solvent and may be prepared by any method including a conventionally known method.
  • the manufacturing method of the inorganic polysilazane is Pyridine and dihalosilane, preferably silane substituted by C1 to form a silane adduct, there is a method of combining the silane adduct and ammonia and then removing the resulting ammonium salt to synthesize.
  • anti-glare glass is significantly improved in wear resistance and durability with anti-glare properties as a coating composition containing polysilazane and a solvent is applied after spray spraying on the glass surface.
  • the spray spraying method described above can be used while maintaining the range of haze properly when applied with various conditions such as polysilazane content, viscosity, spraying amount, sprayed layer density, spraying time, and post-injection firing time. This can increase significantly.
  • the appropriate haze value can be maintained.
  • the transmittance can be significantly improved.
  • the layer having the concave-convexity is formed on the glass surface by the polysilazane itself without the incorporation of heterogeneous elements, the transmittance is remarkably improved compared to the case of the concave-convex formation caused by the incorporation of heterogeneous elements.
  • the temperature and time when the solvent is removed may be in the range of 50 to 100 ° C. and in the range of 1 to 5 minutes. Contrast transmittance can be increased more.
  • a coating composition containing polysalazan is applied when a coating composition containing polysilazane and a solvent is sprayed onto a glass surface and the heat treatment proceeds after the solvent is removed within 60 seconds.
  • the heat treatment may preferably include heat treatment at 400 to 700 ° C., more preferably, primary heat treatment at 50 to 200 ° C. and 400 to 700 ° C., preferably 450 to 700 ° C. May include C secondary heat treatment. Heat-treated at temperatures above 400 ° C to make polysilazane layers into glass layers above glass hardness
  • the anti-glare glass can have very good properties of haze and permeability as described above, in particular primary and secondary heat treatments.
  • the coating composition may include 1 to 40% by weight of polysilazane and 60 to 99% by weight of solvent based on the total weight, preferably 2 to 25% by weight of polysilazane and 75 to 98% by weight of solvent. And, more preferably, 2 to 20% by weight of polysilazane and 80 to 98% by weight of solvent. If the polysilazane comprises inorganic polysilazane and organic polysilazane, inorganic polysilazane 1 to 40 parts by weight of organic polysilazane, based on 100 parts by weight,
  • polysilazane inorganic When both polysilazane and organic polysilazane are included, haze and visibility control is easier
  • the solvent may be any one which can be dissolved in polysilazane, and may include any one or two or more selected from aromatic hydrocarbons, aliphatic hydrocarbons, halogenated hydrocarbons, esters, ketones, ethers, and alcohols.
  • Examples of the aliphatic hydrocarbons include pentane, nucleic acid, octane, nonan, decane, decalin, undecane, dodecane, tridecane, tetradecane, isononane, isodedecane, isododecane, isododecane and iso Tridecane, isotetradecane, cyclononan, cyclodecane, cyclodecane,
  • Cyclododecane, cyclotridecane, and cyclotetedecane may be exemplified.
  • the halogenated hydrocarbons may be exemplified by chloroform and dichloromethane.
  • Esters include benzyl acetate, allyl nucleosanate, butyl butyrate,
  • Ketones may be exemplified by acetone, methyl ethyl ketone and methyl isobutyl ketone.
  • the ether is diethyl ether, dimethoxyethane, dimethoxymethane, dioxane, tetrahydrofuran. Examples include alcohols, isols, crown ethers and polyethylene glycols.
  • Exemplified are alcohols containing three or more carbons, such as echosanol, heptadecafloodecanol, nucleated decaflorononanol, and dodecaflotemtanol, and halogenated alcohols containing three or more carbons.
  • the coating composition may have a viscosity of 0.5 to 2.0 cp.
  • the weight balance of polysilazane can be adjusted according to its weight and content, preferably from 0.8 to 1.7 cp.
  • the antiglare glass of the present invention may have a haze in the range of 1 to 5%, preferably 1 to 3%, and a transmittance in the range of 90% or more and preferably 91% or more. If the above range is not satisfied, the antiglare effect may be insignificant, and the transmittance may be significantly reduced without significantly increasing the antiglare effect, and the visibility may be significantly reduced.
  • the antiglare glass of the present invention can be laminated on the glass surface with a coating layer formed by the coating composition of 5 to 15 g / m 2 , preferably 7 to 13 g / m 2 . If it exceeds 15 g / m 2 , the haze may be higher, but the transmittance may be drastically reduced. If it is less than 5 g / m 2 , the haze is too low to provide even more anti-glare property. May not be expressed.
  • the anti-glare glass of the present invention is made of polysilazane itself, as described above.
  • the surface roughness of the layer may be in the range of 1 to 20 nm.
  • Surface roughness means surface roughness and indicates the degree of minute unevenness formed on the surface. it means. If it is less than 1 nm, the anti-glare effect is hardly expressed. If it exceeds 20 nm, the transmittance of light may be lowered and the visibility may be drastically reduced.
  • the method of manufacturing glare atrial glass of the present invention comprises the steps of: S1) preparing a coating composition
  • the step S3) is the coating in the step S2)
  • the transmittance and haze can be significantly reduced due to hardening, and further improvement in wear resistance and durability can be achieved even after further heat treatment.
  • step S3) may include drying the solvent for 1 to 5 minutes in a temperature range of 50 to 100 ° C.
  • the drying method is known. It may be used, for example hot air drying.
  • the step S3) is the first heat treatment for 2 to 10 minutes at 50 to 200 ° C, the second heat treatment for 30 to 90 minutes at 400 to 700 ° C May include this.
  • the anti-glare glass of the present invention can be used on the surface of glass without the presence of heterogeneous elements.
  • the glass with the surface irregularities derived from polysilazane is formed, which has the effect of having excellent anti-glare property and visibility.
  • the anti-glare glass of the present invention has an effect of significantly improving wear resistance and durability by polysilazane being thermally modified on the glass surface by heat treatment.
  • the antiglare glass of the present invention has a transmittance of 90% or more and 1-5%.
  • 1 is a graph showing the surface roughness of the coating surface.
  • SK Chemicals 950 g of solvent was added to the reaction vessel and mixed and stirred for 10 minutes to prepare a coating composition.
  • the coating composition was sprayed onto a glass plate of 50 cm X 50 cm in size (spray pressure 20 psi, spray amount 10 g / m 2). Solvent was removed by drying for 2 minutes under hot air conditions of 80 C within 60 seconds after application.), And then the first heat treatment was performed for 5 minutes at 150 ° C by the heat curing method, and then at 450 ° C. Secondary heat treatment was performed for 60 minutes at to produce anti-glare glass.
  • Example 1 the inorganic polysilazane 50 g and the solvent 950 g instead of the weapon
  • Example 2 The procedure was the same as in Example 1, except that 70 g of polysilazane and 930 g of a solvent were used.
  • Example 1 the inorganic polysilazane 50 g and the solvent 950 g instead of the weapon
  • Example 2 The procedure was the same as in Example 1 except that 90 g of polysilazane and 910 g of a solvent were used.
  • Example 1 the inorganic polysilazane 50 g and the solvent 950 g instead of the weapon
  • Example 2 The procedure was the same as in Example 1, except that 120 g of polysilazane and 880 g of a solvent were used.
  • Example 1 50 g of the inorganic polysilazane and 950 g of the solvent instead of the inorganic
  • Example 2 The procedure was the same as in Example 1 except that 180 g of polysilazane and 820 g of a solvent were used.
  • Example 6 [71] The same procedure as in Example 1 except that 940 g of the solvent was used instead of 940 g of the solvent, and 10 g of an organic polysilazane having a weight average molecular weight of 2,000 was added to the reaction vessel. It was.
  • Example 1 the same procedure as in Example 1 was carried out except that the coating composition was dried within 60 seconds to remove the solvent after drying in 100 seconds instead of removing the solvent.
  • Example 1 the inorganic polysilazane 50 g and the solvent 950 g instead of the weapon
  • Example 2 The procedure was the same as in Example 1 except that 9 g of polysilazane and 991 g of a solvent were used.
  • Example 1 the coating composition is applied in the same manner as in Example 1 except that the coating composition is applied for 5 seconds at a rate of 2 g / sec using a flow coating instead of using a spray gun. Proceeded.
  • Example 1 instead of the inorganic polysilazane having a weight average molecular weight of 15,000
  • Example 2 The same procedure as in Example 1 was conducted except that an inorganic polysilazane having a weight average molecular weight of 40,000 was used.
  • a transmittance of 500 nm was measured using a UVVis spectrophotometer (SCINCO, S 3 100).
  • Haze uses a haze meter (HM150; Murakami Color Research Institute)
  • Viscosity was measured using a viscosity meter (VL700; Hydramotion).
  • the anti-glare glass coated with the coating composition according to Example 6 was further added to the organic polysilazane, and it was confirmed that the glass had an improved haze with an appropriate haze.
  • Comparative Example 1 was prepared by lowering the inorganic polysilazane content to 0.9%, and it was confirmed that the haze at this time was significantly reduced and the anti-glare property disappeared.
  • Comparative Example 2 is a coating composition manufactured by floor coating method, which is a general transparent glass without surface roughness with a haze of 0.21%, and does not exhibit antiglare characteristics.
  • Comparative Example 3 also contains inorganic polysilazanes having a weight average molecular weight of more than 30,000.
  • variable that can exist to maximize the anti-glare and transmittance was found to be affected by the content of the plysilazane (or the viscosity by the content of the polysilazane), that is, the composition ratio.

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  • Geochemistry & Mineralogy (AREA)
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Abstract

본 발명의 눈부심 방지 유리는 이종원소의 혼입 없이 유리 표면 상에 폴리실라잔 유래의 표면 요철이 부여된 유리가 형성됨으로써, 우수한 방현성 및 시인성을 갖는 효과가 있으며, 유리 표면 상에 폴리실라잔이 열처리에 의해 유리로 변성됨으로써, 내마모성 및 내구성이 현저히 향상되는 효과가 있다.

Description

명세서
발명의명칭:눈부심방지유리및이의제조방법 기술분야
[1] 본발명은방현성및시인성을향상시킨눈부심방지유리에관한것이다.
[2]
배경기술
[3] 디스플레이는자연광또는조명광등과같은외부빛에노출되는경우,
디스플레이표면으로입사한빛이반사되면서콘트라스트 (Contrast)가감소되고, 이미지반사에의해시인성이저하된다.뿐만아니라화면이눈부시게되고문자 인식이어려워쉽게눈와피로감을증가시키거나두통을유발하게된다.
[4] 이를방지하기위한기술로서，디스플레이를포함하는유리또는필름과같은 표시면에서외광의반사를방지하기위한안티글레어 (anti glare)기술이있다. 안티글레어기술은유 /무기미립자와바인더수지또는경화성수지의흔합물을 기재에도포하고,표면에요철을형성함으로써외광의반사를방지할수있는 기술이다.
[5] 헤이즈 (Haze)는방현성 (防弦性， Anti glare)의척도가되며,일반적으로 %로
표시하고，헤이즈가증가할수록빛의난반사가증가하여방현성이증가하게 된다.상기방현성은빛의외광반사에따른눈부심의정도를의미한다.
[6] 빛의투과율은물질층또는경계면을투과한빛의강도와입사한빛의강도에 대한비를의미하며 ,일반적으로 %로표시한다.
[7] 한편，한국등록특허제 10-1137206호에는소재를원하는형상으로가공하고， 샌딩하여표면에요철을형성하고,투시율향상을위해정삭하는
절삭가공단계를포함하는눈부심방지유리의제조방법이공지되어있다.
[8] 또한한국공개특허계 10-2011-0060233호에는유리기판상에균일한두께를 갖는세라믹코팅층을형성하고，계 1식각용액으로상기세라믹코팅층을상기 유리기판으로부터박리하여유리기판의표면에제 1거칠기를형성한후， 제 2식각용액으로상기유리기판의표면올식각하여상기유리기판의표면에 계 2거칠기를형성하는눈부심방지유리의제조방법이공지되어있다.
[9] 방현성을향상시키기위해요철형상의크기또는빈도를증가시킬경우,
역으로외광의반사에의해화면이하얗게흐려지거나,헤이즈의과도한상승에 따른선명도가저하되어시인성이악화되는문제가있다.또한요철형상의크기 또는빈도를증가시킬경우,빛의난반사가일어나눈부심을방지할수있으나， 요철의크기또는빈도의조절이어려운문제가있다.
[10] 반대로，표면의헤이즈를감소시키면외광의반사에의해하얗게흐려지는
정도는억제할수있지만，기재표면에면반사현상이강하게나타난다.이를 해소하기위해방현층내부의헤이즈를증가시키는방법이있지만,미립자와 수지의굴절률차에서기인한내부헤이즈에의해오히려투과율이저하되는 문제가있다.
[11] 방현성을향상시키기위한다른방법으로，유리표면상에무기미립자 A1203, Y 203, Zr02, A1C, TiN, A1N, TiC, MgO, CaO, Ce02, Ti02, Si02, SiC및 A1F3등을 사용하여코팅층을형성하기위해,기재표면을건식또는습식에칭에의해 발수제가부착될수있는표면적을증가시키는방법이있다.하지만이러한 방법은플라즈마처리와같은건식에칭의경우고가장비에대한부담이크고， 습식에칭의경우보통강알칼리세정제나묽은물산에기판을침적시키는 과정에서별도의세정공정과부산물의처리비용등에대한부담이큰문제가 있다.
[12] 방현성을향상시키기위한또다른방법으로,유리표면에빛이굴절될수있는 안티글래어필름을부착하는방법이있다.하지만상기필름은고굴절필름과 저굴절필름을교대로부착하여야하므로,단가가높아질수있다.
[13]
발명의상세한설명
기술적과제
[14] 본발명의목적은외광의반사에의한화면이하얗게흐려지는문제，헤이즈의 과도한상승에따른선명도저하에의해시인성이악화되는문제및낮은방현성 및높은제조단가를해결하기위한것으로，우수한방현성및시인성을부여할 수있는눈부심방지유리및이의제조방법을제공하는것이다.
[15] 또한본발명의목적은방현성및시인성의제어정확도가향상된눈부심방지 유리및이의제조방법을제공하는것아다.
[16] 또한본발명의목적은우수한내마모성및내구성을가지는눈부심방지유리 및이의제조방법을제공하는것이다.
[17]
과제해결수단
[18] 눈부심유발을최소화하기위한방법으로，빛의난반사를유도하는등의
헤이즈를증가시켜방현성을향상시키는방법이있다.상기방법의경우,눈부심 유발을최소화할수있는장점이있으나，빛의투과율이저하되어시인성이 감소하는문제가발생한다.따라서적절한헤이즈값을가지면서투과율을 극대화할수있어야한다.
[19] 하지만상술한바와같이，일반적으로헤이즈및투과율은서로반비례관계를 갖는경향을가지기때문에，난반사를방지할정도의적절한헤이즈를가지면서 투과율을최대화시키는것이무엇보다중요하다.
[20] 즉，헤이즈가증가하면눈부심방지효과가향상되며，투과율이감소하면
시인성이저하되므로,본발명은높은헤이즈및투과율을모두양립하여 투과율이높은눈부심방지유리를제공하는것에그의의가있다. [21]
[22] 본명세서에서언급하는 "유리 "는일반적으로디스플레이에사용되는모든 유리，고분자및기재를의미하며，이외에도기재후면으로입사되는빛이상기 기재를투과하여상기빛을식별하기위한빛이투과할수있는모든기재를 의미할수있다.
[23]
[24] 본발명은하기화학식 1을만족하는중량평균분자량이 30,000이하인
폴리실라잔 1내지 40증량 %를포함하는코팅조성물이유리표면상에분사 도포되어적층되는눈부심방지유리에관한것이며,상기눈부심방지유리의 헤이즈는 1내지 5%일수있고,상기눈부심방지유리의투과율은 90%이상일 수있다.
[25] 본발명의일예에있어서，상기폴리실라잔은하기화학식 1로표기된다.
[26] [화학식 1]
Figure imgf000004_0001
[28] (R:, R2및 R3는독립적으로수소，알킬기，알케닐기，시클로알킬기，아릴기, 규소에직결하는기가탄소인기，알킬실릴기,알킬아미노기및알콕시기중에서 선택되는어느하나또는둘이상을포함하며， n은정수이다.)
[29] 상기폴리실라잔은상기화학식 1의반복단위를가지는무기폴리실라잔또는 유기폴리실라잔일수있다.상기무기폴리실라잔은 R,, R2및 R3모두탄소를 포함하는기를가지지않으며 ,바람직하게는 R,, R2및 ¾모두수소인무기 폴리실라잔이예시될수있다.상기유기폴리실라잔은 Rl5 R2및 R3중에서 선택되는적어도하나는알킬기，알케닐기，시클로알킬기 ,아릴기,규소에 직결하는기가탄소인기，알킬실릴기,알킬아미노기및알콕시기등에서 선택되는어느하나또는둘이상을포함하는기를가질수있다.또한 n은 화학식 1의반복단위를가지는폴리실라잔의중량평균분자량이 30,000이하를 만족하도록하는정수라면크게제한되지않는다.
[3이 상기무기폴리실라잔및상기유기폴리실라잔은용매에가용성일수있으며 종래에공지된방법올포함한임의의방법에의해제조될수있다.구체적인일 예로，상기무기폴리실라잔의제조방법은，피리딘과디할로실란，바람직하게는 C1로치환된실란을배합하여실란부가물을형성시킨후，당해실란의부가물과 암모니아를배합한후생성되는암모늄염올제거하여합성하는방법등이있다. [31] 상기폴리실라잔의중량평균분자량이 30,000을초과하는경우，공기중 노출만으로도경화가촉진되어코팅층의표면거칠기가심해지고，해이즈증가 및투과율의급격한감소를일으킬수있다.뿐만아니라，조절및제어가어려워 요구되는방현성및투과율의재현성이저하될수있다.
[32] 본발명의일예에있어서，눈부심방지유리는폴리실라잔및용매를포함하는 코팅조성물이유리표면상에스프레이분사법으로도포된후열처리됨에따라 방현성과함께내마모성및내구성이현저히향상될수있다.상기의스프레이 분사법은폴리실라잔의함량,점도，분사량및분사되어적층된층밀도,분사 시간，분사후소결시간등의여러조건들과함께적용될경우，헤이즈의범위를 적절히유지할수있으면서，투과율이현저히증가할수있다.
[33] 본발명의바람직한일예로，폴리실라잔및용매를포함하는코팅조성물이 유리표면상에분사되어 90초，바람직하게는 60초이내에상기용매가제거될 경우,적절한헤이즈값을유지할수있으면서，투과율이현저히향상될수있다. 상세하게,이종원소의흔입없이폴리실라잔자체만으로유리표면상에요철이 부여된층이형성되므로，이종원소의흔입에의한요철형성의경우대비 투과율이현저히향상되는효과가있다.
[34] 본발명의일예에있어서，상기용매가제거될경우의온도및시간은 50내지 100oC범위및 1내지 5분범위일수있다.상기범위의건조온도및건조시간을 만족하는경우,헤이즈대비투과율을보다증가될수있다.
[35] 본발명의바람직한일예로，폴리실라잔및용매를포함하는코팅조성물이 유리표면상에분사되어 60초이내에상기용매가제거된후에열처리가 진행될경우，폴리살라잔을포함하는코팅조성물층이유리경도이상올갖는 요철이형성된유리로변성됨으로써，헤이즈및투과성이모두우수한것은 물론，내마모성및내구성이현저히향상될수있다.
[36] 이때상기열처리는바람직하게는 400내지 700°C에서의열처리를포함할수 있으며,보다바람직하게는 50내지 200°C에서의 1차열처리및 400내지 700°C, 바람직하게는 450내지 700°C의 2차열처리를포함할수있다. 400°C이상의 온도에서열처리되어폴리실라잔층이유리경도이상의유리층으로
변성됨으로써，눈부심방지유리는상술한헤이즈및투과성이매우우수한 특성을가질수있다.특히 1차열처리및 2차열처리가순차적으로
진행됨으로써,보다안정적으로내마모성및내구성이향상될수있다.
[37] 상기코팅조성물은전체중량에대하여폴리실라잔 1내지 40중량 %및용매 60내지 99중량 %를포함할수있으며，바람직하게는폴리실라잔 2내지 25 중량 %및용매 75내지 98중량%를포함할수있으며，보다바람직하게는 폴리실라잔 2내지 20중량 %및용매 80내지 98중량 %를포함할수있다.상기 폴리실라잔이무기폴리실라잔및유기폴리실라잔을포함할경우,무기 폴리실라잔 100중량부에대하여유기폴리실라잔 1내지 40중량부，
바람직하게는 5내지 30중량부를포함할수있다.상기폴리실라잔이무기 폴리실라잔및유기폴리실라잔을모두포함할경우，헤이즈및시인성의제어가 보다용이할수있다
[38] 상기용매는폴리실라잔이용해될수있는것이면무방하며，예컨대방향족 탄화수소,지방족탄화수소，할로겐화탄화수소，에스테르，케톤,에테르및 알코올등에서선택되는어느하나또는둘이상을포함할수있다.방향족 탄화수소는벤젠,를루엔,에틸벤젠，클로로벤젠, 0-자일렌, m-자일렌， P-자일렌， 스타이렌，이소프로필벤젠，노르말프로필벤젠，클로로톨루엔,부틸벤젠, 디클로로벤젠，디이소프로필벤젠및니트로톨루엔등이예시될수있다.지방족 탄화수소는펜탄,핵산，옥탄，노난,데칸,데칼린，운데칸,도데칸，트리데칸， 테트라데칸,이소노난,이소데칸,이소운데칸，이소도데칸,이소트리데칸, 이소테트라데칸，사이클로노난,사이클로데칸，사이클로운데칸,
사이클로도데칸，사이클로트리데칸및사이클로테트라데칸등이예시될수 있다.할로겐화탄화수소는클로로포름및디클로로메탄등이예시될수있다. 에스테르는벤질아세테이트,알릴핵사노에이트,부틸부티레이트,
에틸아세테이트，에틸부티레이트,에틸핵사노에이트，에틸시나노에이트, 에틸헵타노에이트，에틸노나노에이트，에틸펜타노에이트，
이소부틸아세테이트，이소부틸포르메이트，이소아밀아세테이트，
이소프로필아세테이트및메틸페닐아세테이트등이예시될수있다.케톤은 아세톤,메틸에틸케톤및메틸이소부틸케톤등이예시될수있다.에테르는 디에틸에테르,디메톡시에탄，디메톡시메탄，디옥산,테트라하이드로퓨란, 안이솔,크라운에테르및폴리에틸렌글리콜등이예시될수있다.알코올은 이소프로필알코을，노르말부탄올，이소부탄올，세크부탄올，노르템탄올， 노르말옥탄올，노르말노난올,노르말데칸올，노르말테트라데칸올，에이코산올, 헵타데카플로로데칸올，핵사데카플로로노난올및도데카플로로템탄올등의 3 개이상의탄소를포함하는알코올및 3개이상의탄소를포함하는할로겐화 알코올등이예시될수있다.
[39] 상기코팅조성물은점도가 0.5내지 2.0 cp일수있다.상기점도는
폴리실라잔의중량평군뷴자량및함량에따라조절될수있으며,바람직하게는 0.8내지 1.7 cp일수있다.
[40] 본발명의눈부심방지유리는 1내지 5%,바람직하게는 1내지 3%범위의 헤이즈와, 90%이상,바람직하게는 91%이상범위의투과율을가질수있다. 상기범위를만족하지않는경우，방현성효과가미미할수있으며，방현성의 효과는크게상승하지않으면서투과율이현저하게저하될수있어시인성이 현저하게감소될수있다.
[41] 본발명의눈부심방지유리는유리표면상에상기코팅조성물에의해형성된 코팅층은 5내지 15 g/m2,바람직하게는 7내지 13 g/m2으로적층될수있다 . 15 g/m2으를초과하는경우,헤이즈가보다상승될수있지만투과율이급격히 감소할수있으며， 5 g/m2미만일경우，헤이즈가너무낮아층분한방현성이 발현되지않을수있다.
[42] 본발명의눈부심방지유리는상술한바와같이，폴리실라잔자체만으로
요철이부여된층을가질수있으며，상기층의표면조도는 1내지 20 nm범위일 수있다.표면조도 (表面粗度; Suface roughness)란표면거칠기를의미하며，표면 상에형성된미세한요철의정도를의미한다. 1 nm미만일경우,눈부심방지 효과가실질적으로발현되기어려우며 , 20 nm을초과하는경우,빛의투과율이 저하되어시인성이급격히저하될수있다.
[43] 본발명의눈부심방자유리의제조방법은 S1)코팅조성물을제조하는단계,
52)유리표면상에상기코팅조성물올스프레이분사방법으로도포하는단계，
53)용매를제거하는단계및 S4)열처리하는단계를포함할수있다.
[44] 본발명의일예에있어서，상기 S3)단계는상기 S2)단계에서상기코팅
조성물이도포된후 90초.바람직하게는 60초이내에용매를제거하는과정을 포함할수있다.상기코팅조성물이도포된후 90초를초과한후에용매가 제거되거나,제거되지않을경우,상온에의한건조또는경화로인하여투과율 및헤이즈가현저히감소될수있으며,이후열처리과정이더진행되어도 내마모성및내구성의향상이미미할수있다.
[45] 본발명의일예에있어서，상기 S3)단계는 50내지 100oC의온도범위에서 1 내지 5분범위동안건조하여용매를제거하는과정을포함할수있다.상기 건조방법은공지된다양한방법이사용되어도무방하며,예컨대열풍건조등이 있다.
[46] 발명의일실시예에있어서,상기 S3)단계는 50내지 200°C에서 2내지 10분 동안 1차열처리를한후， 400내지 700°C에서 30내지 90분동안 2차열처리하는 과정올포함할수있다.
[47]
발명의효과
[48] 본발명의눈부심방지유리는이종원소의흔입없이유리표면상에
폴리실라잔유래의표면요철이부여된유리가형성됨으로써,우수한방현성및 시인성을갖는효과가있다.
[49] 또한본발명의눈부심방지유리는유리표면상에폴리실라잔이열처리에 의해유리로변성됨으로써，내마모성및내구성이현저히향상되는효과가있다.
[50] 또한본발명의눈부심방지유리는 90%이상의투과율및 1내지 5%의
헤이즈를가지므로，우수한시인성및우수한방현성효과가있다.
[51]
도면의간단한설명
[52] 도 1은코팅표면의표면조도를나타낸그래프이다.
[53] 도 2는전자현미경으로관찰한이미지이다.
[54] 발명의실시를위한최선의형태
[55] 이하첨부한도면들을참조하여본발명의눈부심방지유리및이의제조
방법을상세히설명한다.
[56] 이때,사용되는기술용어및과학용어에있어서다른정의가없다면,이
발명이속하는기술분야에서통상의지식을가진자가통상적으로이해하고 있는의미를가지며，하기의설명및첨부도면에서본발명의요지를
불필요하게흐릴수있는공지기능및구성에대한설명은생략한다.
[57]
[58] 이하본발명을실시예를통해상세히설명하나，이들은본발명을보다
상세하게설명하기위한것으로，본발명의권리범위가하기의실시예에의해 한정되는것은아니다.
[59]
[60] [실시예 1]
[61] 중량평균분자량이 15,000인무기폴리실라잔 50 g과오쏘-자일렌 (ortho-Xylene;
SK케미칼)용매 950 g을반웅기에넣어 10분동안흔합및교반하여코팅 조성물을제조하였다.상기코팅조성물을 50 cm X 50 cm크기의유리판에 스프레이건 (분사압력 20 psi,분사량 10 g/m2)을사용하여도포한후 60초 이내에 80 C의열풍조건에서 2분동안건조하여용매를제거하였다.그다음열 경화방식으로 150°C온도에서 5분동안 1차열처리를진행하고， 450°C온도에서 60분동안 2차열처리를진행하여눈부심방지유리를제조하였다.
[62] [실시예 2]
[63] 실시예 1에서，상기무기폴리실라잔 50 g및상기용매 950 g대신무기
폴리실라잔 70 g및용매 930 g을사용한것을제외하고，실시예 1과동일하게 진행하였다.
[64] [실시예 3]
[65] 실시예 1에서，상기무기폴리실라잔 50 g및상기용매 950 g대신무기
폴리실라잔 90 g및용매 910 g을사용한것을제외하고,실시예 1과동일하게 진행하였다.
[66] [실시예 4]
[67] 실시예 1에서,상기무기폴리실라잔 50 g및상기용매 950 g대신무기
폴리실라잔 120 g및용매 880 g을사용한것을제외하고，실시예 1과동일하게 진행하였다.
[68] [실시예 5]
[69] 실시예 1에서,상기무기폴리실라잔 50 g및상기용매 950 g대신무기
폴리실라잔 180 g및용매 820 g을사용한것을제외하고,실시예 1과동일하게 진행하였다.
[70] [실시예 6] [71] 실시예 1에서，상기용매 950 g대신용매 940 g을사용하고，중량평균분자량이 2,000인유기폴리실라잔 10 g을반웅기에더투입한것올제외하고，실시예 1과 동일하게진행하였다.
[72] [실시예 7]
[73] 실시예 1에서,상기코팅조성물을 60초이내에건조하여용매를제거한대신 100초이후에건조하여용매를제거한것을제외하고,실시예 1과동일하게 진행하였다.
[74] [비교예 1]
[75] 실시예 1에서，상기무기폴리실라잔 50 g및상기용매 950 g대신무기
폴리실라잔 9 g및용매 991 g을사용한것을제외하고,실시예 1과동일하게 진행하였다.
[76] [비교예 2]
[77] 실시예 1에서，상기코팅조성물을스프레이건을사용하여도포하는것대신 플로어코팅 (Flow coating)을이용하여 2 g/초의속도로 5초동안도포한것을 제외하고，실시예 1과동알하게진행하였다.
[78] [비교예 3]
[79] 실시예 1에서，중량평균분자량이 15,000인무기폴리실라잔대신
중량평균분자량이 40,000인무기폴리실라잔을사용한것을제외하고실시예 1과동일하게진행하였다.
[8이
[81] 시험및측정방법
[82]
[83] 1.투과율
[84] UVVis spectrophotometer (SCINCO, S3100)을이용하여 500nm영역의투과율을 측정하였다.
[85] 2.헤이즈 (방현성)
[86] 헤이즈는해이즈미터 (HM150;무라카미색채기술연구소)를사용하여
측정하였다.
[87] 3.점도
[88] 점도는점도계측기 (VL700; Hydramotion)를사용하여측정하였다.
[89] 4.경도
[90] 경도는 MITSU-BISHI PENCIL을사용하여연필경도를측정하였다.
[91]
[92] 측정결과 [94] [표 1]
Figure imgf000010_0001
[96] 실시예 1내지실시예 5를비교해보면,무기폴리실라잔함량이증가할수록 투과율은감소하고，헤이즈는증가하는경향을보였다ᅳ
[97] 또한실시예 1내지실시예 6에따른코팅조성물을도포한눈부심방지유리는
5%미만의헤이즈및 90%이상의투과율로서우수한안티글래어특성을보였다. 실시예 6에따른코팅조성물을도포한눈부심방지유리는유기폴리실라잔을 더첨가한것으로，적절한헤이즈를가지면서보다향상된투과율을가짐을 확인하였다.
[98] 반면비교예 1은무기폴리실라잔의함량을 0.9%로낮춰제조하였고，이때의 헤이즈는현저히감소되어방현성이사라지는것을확인하였다.
[99] 반면비교예 2는플로어코팅방법으로코팅조성물을제조한것으로，헤이즈가 0.21%인표면조도가없는일반적인투명한유리로서，안티글래어특성이 나타나지않았다.
[100] 또한비교예 3은 30,000이상의중량평균분자량을갖는무기폴리실라잔을
사용한것으로，공기중노출만으로도경화가촉진되어코팅층의표면거칠기가 심해지고헤이즈가증가하여투과율이현저히감소하는것을확인하였다.
따라서안티글래어특성이현저히감소함을알수있었다.
[101] 따라서상기폴리실라잔의함량에따라방현성및투과율의차이가상당히
존재하고，상기방현성및투과율을극대화할수있는변수는상기플리실라잔의 함량 (또는상기폴리실라잔의함량에의한점도)，즉조성비에의해상당이 영향을받는것을확인할수있었다.
[102] 특히실시예 1및실시예 7에서와같이，코팅조성물이분사된후의용매제거 시간에따라요철이형성되는정도가변화하는것을확인하였으며，실시예 7의 경우，헤이즈및투과도가실시예 1에비하여매우좋지않음을확인하였다.

Claims

청구범위
하기화학식 1을만족하는중량평균분자량이 30,000이하인폴리실라잔 1 내지 40중량 %를포함하는코팅조성물이유리표면상에분사도포되어 적층되며，헤이즈는 1내지 5%이고,투과율은 90%이상인것인눈부심 방지유리.
화학식 1]
Figure imgf000012_0001
(R,, R2및 R3는독립적으로수소，알킬기，알케닐기，시클로알킬기 , 아릴기,규소에직결하는기가탄소인기,알킬실릴기，알킬아미노기및 알콕시기중에서선택되는어느하나또는둘이상을포함하며，！은 정수이다.)
계 1항에있어서，
상기눈부심방지유리의표면조도는 1내지 20 nm인것인눈부심방지 유리.
제 2항에있어서，
상기코팅조성물이유리표면상에분사도포된후, 90초이내에용매가 제거되는것인눈부심방지유리.
제 3항에있어서,
상기용매가제거된후, 400내지 700°C에서열처리되는것인눈부심방지 유리.
저 항에있어서,
상기눈부심방지유리는유리표면상에코팅조성물이 5내지 15 g/m2 으로적층된것인눈부심방지유리.
51)폴리실라잔및용매를포함하는코팅조성물을제조하는단계;
52)유리표면상에상기코팅조성물을분사하여도포하는단계;
53)상기 S2)단계에서코팅조성물이도포된후， 90초이내에용매를 제거하는단계；및
54)열처리하는단계;
를포함하는눈부심방지유리제조방법 .
제 6항에있어서，
상기 S3)단계의열처리는 400내지 700oC에서열처리하는과정을 포함하는눈부심방지유리의제조방법ᅳ
[청구항 8] 제 7항에있어서，
상기 S3)단계의열처리는 50내지 200°C에서 1차열처리후, 400내지 700°C에서 2차열처리하는과정올포함하는눈부심방지유리의제조 방법.
PCT/KR2016/004460 2016-04-28 2016-04-28 눈부심 방지 유리 및 이의 제조 방법 WO2017188477A1 (ko)

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