KR900003138B1 - Fusion seal compositions - Google Patents

Fusion seal compositions Download PDF

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KR900003138B1
KR900003138B1 KR1019880000185A KR880000185A KR900003138B1 KR 900003138 B1 KR900003138 B1 KR 900003138B1 KR 1019880000185 A KR1019880000185 A KR 1019880000185A KR 880000185 A KR880000185 A KR 880000185A KR 900003138 B1 KR900003138 B1 KR 900003138B1
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glass
weight
composition
fusion
powder
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KR1019880000185A
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KR890011797A (en
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채수철
김기동
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한국유리공업 주식회사
최영중
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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
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/062—Glass compositions containing silica with less than 40% silica by weight
    • C03C3/07—Glass compositions containing silica with less than 40% silica by weight containing lead
    • C03C3/072—Glass compositions containing silica with less than 40% silica by weight containing lead containing boron
    • 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
    • C03C4/00—Compositions for glass with special properties
    • C03C4/02—Compositions for glass with special properties for coloured glass

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

Abstract

The ceramic color frit is composed of 5-30 wt.% refractory pigment powder e.g. CuCr2O4, MnO2, Fe2O3, CoO, CdS, Cr2O3 and 70-95 wt.% glass powder binder of a low fusion point. The glass powderbinder of a low fusion point has a composition of 25-40 wt.% SiO2, 40-65 wt.% PbO, 0-10 wt.% B2O3, 0.5-3 wt.% TiO2, 0.1-3 wt.% ZrO2, 1-10 wt.% R2o CNa2O, K2O or Li2O, 0-3 wt.% CdO and 0-5 wt.% F. It is useful for a spandrel glass of building and a tempered glass of automoble.

Description

판 유리 착색용 융착유리 조성물Fusion Glass Composition for Plate Glass Coloring

본 발명은 판유리 착색용 융착유리 조성물(ceramic color Frit)에 관한 것으로 특히 자동차용 접합, 강화 유리의 착색과 건축용 스팬드럴(spandrel)유리의 착색에 적합한 신규한 조성비율로 되는 착색용 융착유리 조성물에 관한 것이다.BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a fused glass composition (ceramic color frit) for coloring a glass, particularly to a fusion fused glass composition having a novel composition ratio suitable for coloring automotive laminates, tempered glass, and coloring spandrel glass for construction. It is about.

종래의 착색용 용착유리는 일반적으로 10~30%의 내열성 안료와 70~90%의 저융점 결합제 유리(Binder glass)로 구성되어 있으며 코팅을 용이하게 하기 위해서 전색제(Vehicle)에 혼련하여 페이스트를 제조한 후 판유리 위에 코팅한 다음 건조 및 베이킹하여 사용했다. 피융착재가 자동차용 안전유리의 경우에는 강화 및 곡면 성형 공정에서, 그리고 건축용 스팬드럴 유리의 경우에는 반강화 공정에서 열처리 함으로써 착색용 융착유리가 유리의 표면에 융착된다. 그러나 자동차 안전유리에 착색 융착유리를 융착할 경우 판유리의 곡면성형 과정에서 몰드(Mold)틀에 부착되어 있는 세라믹 페퍼, 세라믹 포, 유리 울 등이 착색용 융착유리와 부착되는 현상이 발생하며, 이로 인해 세라믹 페퍼등의 소모가 심하고 유리의 비틀림에 의한 불량률이 커지는 큰 단점이 있다.Conventional colored welded glass is generally composed of 10-30% heat-resistant pigment and 70-90% low melting binder glass, and kneaded in a vehicle to facilitate coating to produce a paste. It was then coated on a plate glass and then dried and baked. The fusion-bonded glass is fused to the surface of the glass by heat treatment in the case of the safety glass for automobiles in the reinforcing and curved forming process, and in the case of building spanned glass in the semi-hardening process. However, in case of fusion of colored fusion glass on automobile safety glass, ceramic pepper, ceramic cloth, glass wool, etc., attached to mold frame are attached to colored fusion glass during curved molding of plate glass. Due to the high consumption of ceramic pepper, there is a big disadvantage that the defect rate due to the twist of the glass is increased.

이러한 현상을 제거하기 위한 방편으로 일부의 선행되는 발명, 예를들면 일본국 특허공보 제61-43296호에서는 융착 유리에 내화물 충전제(cordierite, Alumina)를 첨가하고 있으나, 이로 인해 융착유리의 접착강도가 저하되는 새로운 문제점이 제기되고, 또한 내화물 충전제가 고가인 관계로 생산 원가가 높은 단점이 있다. 또한 건축용 스팬드럴 유리의 경우에는 조작상의 문제는 없으나 착색용 융착유리가 화학적 내구성이 약하여 건물에 시공한 후 장기간 경과되면 대기에 함유된 산 또는 알카리 성분의 침식에 의해 얼룩 또는 변색이 발생되는 결점이 있었다.As a way to eliminate this phenomenon, some of the preceding inventions, for example, Japanese Patent Laid-Open No. 61-43296 add refractory fillers (cordierite, alumina) to the fusion glass, but the adhesive strength of the fusion glass A new problem is lowered, and since the refractory filler is expensive, the production cost is high. In addition, there is no operational problem in the case of building spandral glass, but the stained or discolored color is caused by the erosion of acid or alkaline components contained in the atmosphere when the colored fused glass is weak in chemical durability and prolonged after construction in buildings. there was.

또한 어느 경우에서나 착색부위의 투과율을 1%이하로 하기 위해서는 과량의 착색용 융착유리의 소비가 불가피한 단점도 있었다.In any case, in order to reduce the transmittance of the colored portion to 1% or less, there was also a disadvantage that consumption of excess colored fusion glass is inevitable.

본 발명은 상술한 선행기술의 문제점을 해결하기 위한 것으로, 세라믹 페퍼 등에 전혀 부착하지 않고 또한 화학적 내구성이 강한 특정 조성의 특정비율로 되는 판유리 착색용 융착유리 조성물을 발명함에 있다.The present invention is to solve the above-mentioned problems of the prior art, and to invent a fusion glass composition for coloring plate glass that is not attached to ceramic pepper or the like at all and has a specific ratio of a specific composition with strong chemical durability.

본 발명의 착색용 융착유리 조성물은 착색내열성 안료분말과 저융점 결합제 유리 분말로 구성되며, 그 구성비율은 내열성 안료 분말이 5 내지 30중량 %, 바람직하기는 7 내지 25중량 %이고, 저융점 결합제 유리분말이 70 내지 95중량 %이고, 바람직하기는 75 내지 93중량 %이다.The fusion glass composition for coloring of the present invention is composed of colored heat-resistant pigment powder and low melting point binder glass powder, the composition ratio of which is 5 to 30% by weight of heat-resistant pigment powder, preferably 7 to 25% by weight, low melting point binder The glass powder is 70 to 95% by weight, preferably 75 to 93% by weight.

본 발명의 착색용 융착유리 조성물의 중요 조성으로 사용되는 저융점 결합제 유리 분말은 그 조성으로 SiO225 내지 40중량 %, PbO 40 내지 65중량 %, B2O30 내지 10중량 %, Al2O30.5 내지 3중량 %, ZrO20.1 내지 3중량 %, TiO21 내지 7중량 %, R2O(Na2O, K2O 또는 Li2O) 1 내지 10중량 %, CdO 0 내지 3중량 %, 그리고 F 0 내지 5중량 %로 된다.The low melting binder glass powder used as an important composition of the colored fusion glass composition of the present invention is 25 to 40% by weight SiO 2 , 40 to 65% by weight PbO, 0 to 10% by weight B 2 O 3 , Al 2 0.5 to 3% O 3 , 0.1 to 3% ZrO 2 , 1 to 7% TiO 2, 1 to 10% R 2 O (Na 2 O, K 2 O or Li 2 O), CdO 0 to 3 Weight% and F 0-5 weight%.

본 발명에서 사용되는 착색 내열성 안료 분말로는 MnO2, Fe2O3, CoO, CdS, Cr2O3, CuCr2O4등이 사용될 수 있으나, 본 발명에서는 CuCr2O4를 사용한다.As the colored heat resistant pigment powder used in the present invention, MnO 2 , Fe 2 O 3 , CoO, CdS, Cr 2 O 3 , CuCr 2 O 4, etc. may be used, but in the present invention, CuCr 2 O 4 is used.

본 발명의 착색용 융착유리 조성물의 제조방법은 첫째로 본 발명의 상기한 조성비에 맞게 SiO2등 원료를 평량 및 혼합한 후에 이들의 융점 이상의 온도로 가열하여 용융하고 용융된 용융물을 수조에 넣어 냉각한후 중간 분쇄기와 볼밀과 같은 미분쇄기를 사용하여 계속적으로 분쇄하여 균일한 조성을 가지는 저융점 결합제 유리 분말을 만든다. 필요한 경우에는 생성된 분말을 재용융 및 분쇄를 되풀이하여 균일한 성분의 저융점 결합제 유리 분말을 얻을 수가 있다.First, the method for producing a colored fusion glass composition for coloring according to the above composition ratio of the present invention, after the basis weight and mixing of raw materials such as SiO 2 and heated to a temperature above their melting point to melt and put the molten melt in a water bath to cool Afterwards, continuous grinding is performed using a fine grinding machine such as an intermediate grinder and a ball mill to produce a low melting binder glass powder having a uniform composition. If necessary, the resultant powder may be remelted and pulverized repeatedly to obtain a low melting binder glass powder having a uniform component.

둘째로 상기 방법으로 얻어진 저융점 결합제 유리 분말과 상술한 착색 내열성 안료 분말과 요망되는 조성비로 혼합한 후에 건식 또는 습식분쇄를 하여 평균입경이 5μm이하의 착색용 융착유리 조성물을 얻는다.Secondly, the low melting binder glass powder obtained by the above method and the above-mentioned colored heat resistant pigment powder are mixed with a desired composition ratio, followed by dry or wet grinding to obtain a colored fusion glass composition having an average particle diameter of 5 μm or less.

본 발명의 착색용 융착유리 조성물을 사용하여 자동차 안전유리 또는 건축용스팬드럴 유리를 착색하는 착색방법은 상기 방법으로 얻어진 착색용 융착유리 조성물과 유기제 전색제(Vehicle), 예를들면, 질산셀룰로오스, 에틸셀룰로오스, 아세트산셀룰로오스 등을 에스테르계, 알코올계, 천연터핀 등의 용제에 용해시킨 전색제와 3 : 1 내지 5 : 1의 중량비율로 균일하게 혼합 및 혼련하여 스크린 인쇄용 또는 롤러코팅용 페이스트를 만든다. 자동차용 안전유리 등에 페이스트를 20 내지 40μm가 되게 인쇄하고 80 내지 220℃에서 건조하고 600 내지 800℃에서 실시되는 유리 강화공정에 베이킹하면 자동차 안전유리 표면에 융착하게 된다.The coloring method for coloring automobile safety glass or architectural spandex glass using the colored fusion glass composition of the present invention is a fusion glass composition for coloring and an organic vehicle vehicle (eg, cellulose nitrate, ethyl) The paste for screen printing or roller coating is prepared by uniformly mixing and kneading cellulose, cellulose acetate and the like in a solvent such as ester, alcohol, and natural terpene at a weight ratio of 3: 1 to 5: 1. When the paste is printed to an automobile safety glass to 20 to 40 μm, dried at 80 to 220 ° C. and baked in a glass tempering process performed at 600 to 800 ° C., the paste is fused to the surface of the automobile safety glass.

본 발명에서 저융점 결합제 유리 분말의 성분으로 사용된 SiO2, PbO, B2O3, Al2O3, ZrO2, TiO2, R2O(K2O, Na2O, Li2O), CdO 및 F는 새로운 조성비로서 구성되며, 특히 본 발명의 조성의 특징은 종래 선행기술에서 사용되는 ZnO나 SnO2성분을 전혀 사용하지 않고 또한 주기율표 IIa금속의 산화물(CaO, MgO, BaO, BeO)을 일체 사용하지 않으며, 또한 처음으로 ZrO2와 그리고 선택적으로 F를 특정범위로 사용하여 화학적 내구성의 향상과 세라믹 페퍼등에 부착하지 않는 저융점 결합제 조성물을 발명한 것이다.SiO 2 , PbO, B 2 O 3 , Al 2 O 3 , ZrO 2 , TiO 2 , R 2 O (K 2 O, Na 2 O, Li 2 O) used as components of the low melting binder glass powder in the present invention , CdO and F are configured as a new composition ratio, and in particular, the composition of the present invention is characterized by the fact that it does not use ZnO or SnO 2 components used in the prior art at all and the oxides of the periodic table IIa metals (CaO, MgO, BaO, BeO) Is not used at all, and for the first time ZrO 2 and optionally using F in a specific range to invent a low melting binder composition that improves chemical durability and does not adhere to ceramic pepper and the like.

본 발명에 있어서, SiO2가 25% 이하이면 화학적 내구성이 감소되고, 40%이상이면 유리의 연화점이 너무 높아지게 되어 융착되기 힘들다. 또한 PbO가 40% 이하이면 연화점이 높아져서 융착되기 힘들다. 65% 이상이면 열팽창 계수가 너무 크게되며 화학적 내구성이 좋지 않다. 그리고 B2O3가 융제로 사용되는데, 10% 이상이어도 좋으나 화학적 내구성을 유지하기 위해 10%를 상한선으로 함이 타당하며, Al2O3가 결정화 억제 및 화학적 내구성 개선의 역할을 하나 본 발명에서는 0.5%이하이면 효과가 없고 3%이상이면 연화점이 상승한다. 바람직하기는 0.5 내지 3%이다.In the present invention, if the SiO 2 is 25% or less, the chemical durability is reduced, and if it is 40% or more, the softening point of the glass becomes too high and it is difficult to be fused. In addition, when PbO is 40% or less, the softening point is high, and thus it is difficult to be fused. Above 65%, the coefficient of thermal expansion is too large and the chemical durability is poor. In addition, B 2 O 3 is used as a flux, but may be 10% or more, but it is reasonable to set the upper limit to 10% in order to maintain chemical durability, Al 2 O 3 plays a role in suppressing crystallization and improving chemical durability but in the present invention If it is less than 0.5%, it is ineffective and if it is more than 3%, the softening point will rise. Preferably it is 0.5 to 3%.

ZrO2는 본 발명에서는 규산지르코늄을 형성하여서 화학적 내구성(특히 내알카리성)을 크게 개선한다. 3% 이상이면 연화점이 상승하므로 3%를 상한선으로 함이 타당하며, Ti2O는 화학적 내구성(내산성 및 내수성)의 개선을 위해 사용하고 7% 이상이면 연화점이 급상승하고, 실투성이 높아지므로 7%가 상한선이다. R2O는 융제로 사용되며, 본 성분을 1종 또는 2종 이상을 혼합하여 사용함으로써 유리의 연화점을 저하시키고 화학적 내구성을 개선시킬 수 있다. 1%이하이면 연화점 저하의 효과가 적으며 10% 이상이면 열팽창 계수가 너무 크게 되어 좋지 않다. CdO는 반드시 필요한 성분은 아니지만 CdO계통의 안료를 사용할때 조색제 역할을 하며, 끝으로, F는 용융온도와 융착온도를 낮추는 목적으로 사용된다. 다만 5%이상이면 실투가 일어나거나 열팽창 계수가 높아지므로 5%를 상한선으로 한다.ZrO 2 forms zirconium silicate in the present invention and greatly improves chemical durability (particularly alkali resistance). If 3% or more, the softening point is increased, so it is reasonable to set 3% as the upper limit.Ti 2 O is used for improvement of chemical durability (acid resistance and water resistance), and if it is 7% or more, the softening point is rapidly increased and the devitrification becomes 7%. Is the upper limit. R 2 O is used as a flux, and by using one or two or more of these components, the softening point of the glass can be lowered and the chemical durability can be improved. If it is less than 1%, the softening point is less effective, and if it is more than 10%, the coefficient of thermal expansion is too large, which is not good. CdO is not necessary but serves as a colorant when using CdO pigments. Finally, F is used to lower the melting and melting temperatures. However, if more than 5%, devitrification occurs or the coefficient of thermal expansion increases, so 5% is the upper limit.

본 발명의 착색용 융착유리 조성물은 자동차 안전 유리에 착색시 세라믹 페퍼 등과의 부착관계를 해결하고, 스펜드럴 유리의 화학적 내구성을 향상시킬 수 있으며, 또한 착색용 융착유리의 사용량을 소량으로 하여도 투과율을 일정한 범위내로 (1% 이하) 유지시킬 수 있는 효과가 있다.The fusion glass composition for coloring of the present invention can solve the adhesion relationship with ceramic pepper, etc. when coloring the automobile safety glass, and improve the chemical durability of the pendant glass, and the transmittance even when the amount of the fusion glass for coloring is used in a small amount Can be maintained within a certain range (1% or less).

본 발명을 더욱 상세하게 설명하기 위해 다음의 실시예에서 상세히 기술한다.The present invention is described in detail in the following Examples to further illustrate the present invention.

[실시예 1-3]Example 1-3

다음 표 1에 표시한 조성이 되도록 각각 성분원료를 평량 및 혼합하고, 통상의 도가니에 넣어서 1100 내지 1400℃로 가열용융시킨다. 용융물을 수조에 부어 넣고 수세시킨 후에 볼밀에서 물을 가한뒤 입경 5μm이하로 분쇄, 건조시켜 저융점 결합제 유리 분말을 제조하였다.Next, the ingredients are basis weight and mixed so as to have the composition shown in the following Table 1, and are heated and melted at 1100 to 1400 ° C. in a conventional crucible. After the melt was poured into a water bath and washed with water, water was added in a ball mill, and then pulverized and dried to a particle diameter of 5 μm or less to prepare a low melting binder glass powder.

수득한 저융점 결합제 유리 분말에 착색안료 CuCr2O4를 20중량 % 첨가하여 다시 볼밀로 건식 분쇄 혼합하여 착색용 융착유리 조성물을 만들었다.To the obtained low melting binder glass powder, 20% by weight of colored pigment CuCr 2 O 4 was added, followed by dry milling mixing with a ball mill to prepare a colored fusion glass composition.

이어서, 수득된 착색용 융착유리 조성물과 에틸셀룰로스-터핀을 4 : 1의 중량비율로 혼련하여 페이스트를 만들었다.Subsequently, the obtained fusion glass composition for coloring and ethylcellulose-terpin were kneaded at a weight ratio of 4: 1 to form a paste.

[표 1]TABLE 1

Figure kpo00001
Figure kpo00001

유리 강화처리 : 현재 생산되고 있는 자동차용 안전유리의 원판과 크기와 모양이 같은 판유리를 준비하여 230메쉬 스크린으로 인쇄하고 약 150℃의 온도에서 5분간 건조함으로써 전색제 성분을 증발시켜, 도포막의 두께는 20 내지 40μm가 되게 한다. 이러한 방법으로 얻어진 유리를 700℃로 가열후 급냉 강화처리하면 착색용 융착 유리는 판유리 표면에 견고하게 융착된다.Glass reinforcement treatment: Prepare plate glass of the same size and shape as the original plate of automobile safety glass currently produced, print it on 230 mesh screen and dry it for 5 minutes at a temperature of about 150 ℃ to evaporate the colorant component, and the thickness of the coating film is Allow 20 to 40 μm. When the glass obtained by this method is heated to 700 ° C. and then quenched and tempered, the colored fusion glass is firmly fused to the plate glass surface.

세라믹 페퍼 등과의 부착관계 : 세라믹 페퍼와 착색용 융착유리의 부착관계를 육안관찰로 실시하였으며 표 1에 그 결과를 나타내었다.Bonding relationship with ceramic pepper: The bonding relationship between ceramic pepper and colored fusion glass was visually observed and the results are shown in Table 1.

[실시예 4-7]Example 4-7

실시예 4-7은 실시예 1의 방법으로 표 2의 조성으로 실시하였다.Example 4-7 was carried out in the composition of Table 2 by the method of Example 1.

[표 2]TABLE 2

Figure kpo00002
Figure kpo00002

실시예 4-7은 ZrO2의 함량이 내산 및 내알카리성에 미치는 영향을 나타낸 것으로 내산성의 경우 50-60메쉬 사이의 결합제 유리 입자를 상온에서 10% 구연산에 2시간 침적시킨 후의 무게감량을 조사하였으며 내알카리성 측정의 경우는 동일한 크기의 결합제 유리 입자를 90℃에서 10% NaOH용액에 2시간 동안 침적시킨 후의 무게 감량을 조사한 것이다.Example 4-7 shows the effect of ZrO 2 content on acid and alkali resistance. In acid resistance, the weight loss after immersion of binder glass particles between 50 and 60 mesh in 10% citric acid at room temperature for 2 hours was investigated. In the case of alkali resistance measurement, the weight loss after immersion of binder glass particles of the same size in 10% NaOH solution at 90 ° C. for 2 hours was investigated.

Claims (1)

착색 내열성 안료분말 5 내지 30중량 %와 저융점 결합제 유리 분말 70 내지 95중량 %로 되고, 저융점 결합제 유리 분말의 조성이 SiO225 내지 40중량 %, PbO 40 내지 65중량 %, B2O30내지 10중량 %, Al2O30.5 내지 3중량 %, TiO21 내지 7중량 %, ZrO20.1 내지 3중량 %, R2O(Na2O, K2O 또는 Li2O) 1 내지 10중량 %, CdO 0 내지 3중량 % 및 F 0 내지 5중량 %인 건축용 스팬드럴 유리 및 자동차 안전 유리 착색용 융착유리 조성물.5 to 30% by weight of the colored heat resistant pigment powder and 70 to 95% by weight of the low melting point binder glass powder, and the composition of the low melting point binder glass powder is 25 to 40% by weight SiO 2 , 40 to 65% by weight PbO, B 2 O 3 0 to 10% by weight, 0.5 to 3% by weight of Al 2 O 3 , 1 to 7% by weight of TiO 2 , 0.1 to 3% by weight of ZrO 2 , R 2 O (Na 2 O, K 2 O or Li 2 O) 1 to 10% by weight, 0-3% by weight of CdO and 0-5% by weight of fused glass composition for coloring architectural spanner glass and automobile safety glass.
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