KR101027484B1 - Photosensitive Paste and Glass Powder Composition - Google Patents

Photosensitive Paste and Glass Powder Composition Download PDF

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KR101027484B1
KR101027484B1 KR1020080035562A KR20080035562A KR101027484B1 KR 101027484 B1 KR101027484 B1 KR 101027484B1 KR 1020080035562 A KR1020080035562 A KR 1020080035562A KR 20080035562 A KR20080035562 A KR 20080035562A KR 101027484 B1 KR101027484 B1 KR 101027484B1
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glass
powder
composition
photosensitive paste
glass powder
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KR20090110006A (en
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진근엽
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대주전자재료 주식회사
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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
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/14—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
    • C03C8/16—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions with vehicle or suspending agents, e.g. slip
    • 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
    • C03C12/00—Powdered glass; Bead compositions
    • 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
    • C03C3/064—Glass compositions containing silica with less than 40% silica by weight containing boron
    • C03C3/066—Glass compositions containing silica with less than 40% silica by weight containing boron containing zinc
    • 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
    • C03C4/04—Compositions for glass with special properties for photosensitive glass
    • 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
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
    • C03C8/04—Frit compositions, i.e. in a powdered or comminuted form containing zinc
    • 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
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
    • C03C8/08—Frit compositions, i.e. in a powdered or comminuted form containing phosphorus
    • 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
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/24—Fusion seal compositions being frit compositions having non-frit additions, i.e. for use as seals between dissimilar materials, e.g. glass and metal; Glass solders
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
    • H01B3/02—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances
    • H01B3/10—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances metallic oxides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
    • H01B3/02—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances
    • H01B3/12—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances ceramics
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J17/00—Gas-filled discharge tubes with solid cathode
    • H01J17/38—Cold-cathode tubes
    • H01J17/48—Cold-cathode tubes with more than one cathode or anode, e.g. sequence-discharge tube, counting tube, dekatron
    • H01J17/49—Display panels, e.g. with crossed electrodes, e.g. making use of direct current
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2211/00—Plasma display panels with alternate current induction of the discharge, e.g. AC-PDPs
    • H01J2211/20—Constructional details
    • H01J2211/34—Vessels, containers or parts thereof, e.g. substrates
    • H01J2211/38—Dielectric or insulating layers

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

Abstract

본 발명은 플라즈마 디스플레이 패널에서 고정밀 패턴을 얻어내기 위해 납 성분을 포함하지 않고 고정밀 가공을 용이하게 할 수 있는 감광성 페이스트 및 그린시트용 유리분말 조성물에 관한 것으로, Li2O, Na2O, K2O 등의 알칼리 성분, P2O5, SiO2, B2O3 및 Al2O3로 이루어진 조성물, 혹은 여기에 BaO, ZnO, CaO 및 MgO가 추가된 것이다.The present invention relates to a glass powder composition for a photosensitive paste and a green sheet which does not include a lead component to facilitate a high precision pattern in a plasma display panel, and which can facilitate high precision processing. Li 2 O, Na 2 O, K 2 Alkali components such as O, P 2 O 5 , SiO 2 , B 2 O 3 and Al 2 O 3 , or BaO, ZnO, CaO and MgO are added thereto.

상기 본 발명의 감광성 페이스트 및 그린시트용 유리분말 조성물은 상기 조성을 통해 원하는 굴절율과 열팽창계수, 유리전이온도, 연화점 등을 얻을 수 있고 소성 후 색상이 갈색으로 변색되지 않는 것을 특징으로 하고 있는 것이다.The glass powder composition for the photosensitive paste and the green sheet of the present invention can obtain a desired refractive index, thermal expansion coefficient, glass transition temperature, softening point, etc. through the composition, and is characterized in that the color does not turn brown after firing.

알칼리, 감광성, 유리, 페이스트, 조성물 Alkali, photosensitive, glass, paste, composition

Description

감광성 페이스트 및 그린시트용 유리분말 조성물{Photosensitive Paste and Glass Powder Composition}Photosensitive Paste and Glass Powder Composition for Photosensitive Paste and Green Sheet

본 발명은 플라즈마 디스플레이 패널에서 고정밀 패턴을 얻어내기 위해 납 성분을 포함하지 않고 고정밀 가공을 용이하게 할 수 있는 감광성 페이스트 및 그린시트용 유리분말 조성물에 관한 것으로, 좀 더 상세하게는 Li2O, Na2O, K2O 등의 알칼리 성분, P2O5, SiO2, B2O3 및 Al2O3로 이루어진 조성물, 혹은 여기에 BaO, ZnO, CaO 및 MgO가 추가된 것이다.The present invention relates to a glass powder composition for a photosensitive paste and a green sheet which can facilitate high-precision processing without containing lead in order to obtain a high-precision pattern in a plasma display panel. More specifically, the present invention relates to Li 2 O, Na. An alkali component such as 2 O, K 2 O, a composition composed of P 2 O 5 , SiO 2 , B 2 O 3, and Al 2 O 3 , or BaO, ZnO, CaO, and MgO are added thereto.

상기 본 발명의 감광성 페이스트 및 그린시트용 유리분말 조성물은 상기 조성을 통해 원하는 굴절율과 열팽창계수, 유리전이온도, 연화점 등을 얻을 수 있고, 소성 후 색상이 갈색으로 변색되지 않는 것을 특징으로 한다.The glass powder composition for the photosensitive paste and the green sheet of the present invention can obtain a desired refractive index, a thermal expansion coefficient, a glass transition temperature, a softening point, etc., through the composition, and the color does not turn brown after firing.

플라즈마 디스플레이 패널(PDP)의 격벽의 경우, 기존 샌드블라스트법 형성에 사용되는 격벽 재료로는 산화납이 중량대비 50%이상 사용된 유리분말이 주로 사용 되고 있다.In the case of a partition of a plasma display panel (PDP), glass powder in which 50% or more of lead oxide is used is used as the partition material used for forming the existing sand blasting method.

그런데, 상기 산화납은 인체 및 환경에 유해한 물질로 알려져 있으며, 이 때문에 유리 분말 생산 및 사용에 있어 추가 환경설비를 필요로 하게 되어, 공정 효율이 떨어지며, 제조 원가가 증가하는 문제점이 있었다.By the way, the lead oxide is known to be harmful to the human body and the environment, and because of this, additional environmental equipment is required for the production and use of glass powder, resulting in poor process efficiency and increased manufacturing cost.

또한, 에칭법에 의한 격벽 형성방법은 샌드법에 비해 무연을 사용하는 이점을 가지고 있지만, 에칭액을 통한 식각을 통해 격벽을 형성하여 고정밀 패턴을 형성하는데 한계점을 가지고 있는 것이 단점이다.In addition, the method of forming the partition wall by the etching method has the advantage of using lead-free compared to the sand method, but has a disadvantage in forming a high precision pattern by forming the partition wall by etching through the etching solution.

이러한 기존의 문제점을 해결하기 위해 산화납이 포함되지 않으면서도, 고정밀 패턴을 얻기 위하여 감광성 조성물을 통한 감광성 격벽 형성방법이 사용되고 있다.In order to solve such a conventional problem, a method of forming a photosensitive partition wall through the photosensitive composition is used to obtain a high precision pattern without including lead oxide.

현재 감광성 격벽 형성 방법에서 소성 온도를 맞추고 유리화를 용이하게 하고 굴절율을 맞추기 위해 사용되어지는 성분으로 인해 소성 후 갈색으로 변색하는 경우가 생겨 휘도에 좋지 않은 영향을 끼칠 수가 있어 변색을 방지할 수 있는 대체 성분의 개발이 필요하다 하겠다.In the current method of forming photosensitive bulkheads, the components used to adjust the firing temperature, to facilitate vitrification, and to adjust the refractive index may cause discoloration to brown after firing, which may adversely affect the luminance, thereby preventing discoloration. Development of ingredients is necessary.

따라서, 본 발명에서는 이러한 점을 감안하여 이루어진 것으로, 상기의 성분을 통해 원하는 굴절율과 열팽창계수 등을 얻을 수 있고 소성 후 변색이 되지 않는 감광성 페이스트 및 그린시트용 유리분말 조성물을 제공하고자 하는 것을 목적으로 한다.Accordingly, the present invention has been made in view of the above-described problems, and an object of the present invention is to provide a glass powder composition for photosensitive paste and green sheet, which can obtain desired refractive index and thermal expansion coefficient through the above components and which does not become discolored after firing. do.

본 발명은 Li2O, Na2O, K2O 등의 알칼리 성분, P2O5, SiO2, B2O3 및 Al2O3로 이루어진 조성물, 혹은 여기에 BaO, ZnO, CaO 및 MgO가 추가된 것이 특징이다.The present invention is a composition consisting of alkali components such as Li 2 O, Na 2 O, K 2 O, P 2 O 5 , SiO 2 , B 2 O 3 and Al 2 O 3 , or BaO, ZnO, CaO and MgO Is added.

본 발명에 따르면, 기존의 샌드법 혹은 에칭법보다 고정밀 패턴을 형성하고 납 성분을 함유하지 않으면서, 소성 온도 및 굴절율을 조정하고 색상의 변색 방지를 위해 P2O5를 사용하면서 열팽창 계수가 65~100 X 10-7/℃ 이며 굴절율이 1.5~1.7 사이의 감광성 격벽 형성 방법에 원하는 물성을 얻을 수 있다.According to the present invention, the thermal expansion coefficient is 65 while forming a higher-precision pattern and containing no lead component than the conventional sand method or etching method, and adjusting the firing temperature and refractive index and using P 2 O 5 to prevent color fading. Desired physical properties can be obtained in a method of forming a photosensitive partition wall having a refractive index of -100 X 10 -7 / ° C and a refractive index of 1.5 to 1.7.

상기한 목적을 달성하기 위하여 본 발명에서는 Li2O, Na2O, K2O 등의 알칼리 성분, P2O5, SiO2, B2O3, Al2O3, BaO, ZnO, CaO 및 MgO로 이루어진 것이 특징이다.In order to achieve the above object, in the present invention, an alkali component such as Li 2 O, Na 2 O, K 2 O, P 2 O 5 , SiO 2 , B 2 O 3 , Al 2 O 3 , BaO, ZnO, CaO and It is characterized by consisting of MgO.

여기서, Li2O, Na2O, K2O 등의 알칼리 성분은 1~20중량%, P2O5 2~30중량%, SiO2 5~30중량%, B2O3 10~40중량%, Al2O3 5~40중량%, BaO 1~30중량%, ZnO 1~30중량%, CaO 2~10중량% 및 MgO 1~15중량%가 바람직하다.Here, the alkali component such as Li 2 O, Na 2 O, K 2 O is from 1 to 20 weight%, P 2 O 5 2 ~ 30 wt%, SiO 2 5 ~ 30 wt%, B 2 O 3 10 ~ 40 wt. the%, Al 2 O 3 5 ~ 40 wt%, BaO 1 ~ 30 wt%, ZnO 1 ~ 30 wt%, CaO 2 ~ 10% by weight MgO and 1 ~ 15% by weight is preferred.

또한, 본 발명에서는 Li2O, Na2O 또는 K2O 가운데 1 이상의 성분, P2O5, SiO2, B2O3 및 Al2O3를 포함하는 조성도 가능하다.In the present invention, it is also possible composition containing Li 2 O, Na 2 O or K 2 O of one or more components, P 2 O 5, SiO 2 , B 2 O 3 and Al 2 O 3.

즉, 본 발명에서는 기존의 감광성 페이스트에 사용되는 구성 성분 대신에 P2O5를 사용하는 것이 특징이다.That is, the present invention is characterized by using P 2 O 5 in place of the constituents used in the conventional photosensitive paste.

또한, 본 발명에서는 상기 분말은 입도 분포가 쌍봉 형태(Bimodal)로서 평균 입경이 1.5 내지 5.5㎛, Dtop이 6~40㎛인 것이 바람직하다.In the present invention, the powder has a particle size distribution having a bimodal shape (Bimodal), the average particle diameter of 1.5 to 5.5㎛, Dtop is preferably 6-40㎛.

여기서, 상기 알칼리 성분은 유리전이온도를 낮춰주는 역할을 하는 것으로 Li2O, Na2O, K2O 가운데 1 이상을 사용하되 그 함량은 1~20중량%가 적당하고, 함량이 너무 많으면 온도가 너무 낮아져 바람직하지 않다.Here, the alkali component serves to lower the glass transition temperature, using at least one of Li 2 O, Na 2 O, K 2 O but the content is 1 ~ 20% by weight, if the content is too high temperature Is too low to be desirable.

P2O5는 밝은색을 나타내는 유리형성제로서, 무연 유리 조성물의 유리전이온도(Tg)와 에칭율을 약간 높이는 효과가 있으며, 유전율을 낮추고, 열팽창계수(TEC)와 겔화 빈도를 약간 낮추는 기능을 하며 과량 첨가 시 결정화를 유발한다. 따라서, 상기 P2O5의 함량이 전체 무연 유리 조성물의 중량에 대하여 30 중량%를 초과하는 경우에는 분상이나 결정화가 이루어질 수 있으므로, 2 내지 30 중량%로 포함되는 것이 바람직하며, 5 내지 20 중량%로 포함되는 것이 더 바람직하다.P 2 O 5 is a light-forming glass forming agent that has a slightly higher glass transition temperature (Tg) and etching rate of the lead-free glass composition, lowers the dielectric constant, slightly reduces the coefficient of thermal expansion (TEC) and gelation frequency. In addition, excessive addition causes crystallization. Therefore, when the content of the P 2 O 5 exceeds 30% by weight relative to the total weight of the lead-free glass composition, powder phase or crystallization may occur, so it is preferable to include 2 to 30% by weight, and 5 to 20% by weight. More preferably included in%.

B2O3는 밝은색을 나타내는 유리형성제로서 무연 유리 조성물의 유리전이온도(Tg)를 높이고, 열팽창계수(TEC)를 낮추며 유리를 안정하게 해주는 반면, 저굴절율에도 상당히 유효한 성분이다. 따라서, 상기 B2O3의 함량이 전체 무연 유리 조성물의 중량에 대하여 10 중량% 미만인 경우에는 유리형성이 되지 않으며, 40 중량%를 초과하는 경우에는 Tg가 과도하게 상승되고, 분상이 일어나며 화학적 내구성이 나빠지는 우려가 있다. 10 내지 40 중량%로 포함되는 것이 바람직하며, 20 내지 40 중량%로 포함되는 것이 더 바람직하다.B 2 O 3 is a light-forming glass forming agent that increases the glass transition temperature (Tg) of the lead-free glass composition, lowers the coefficient of thermal expansion (TEC), stabilizes the glass, and is also a very effective component for low refractive index. Therefore, when the content of the B 2 O 3 is less than 10% by weight based on the total weight of the lead-free glass composition, glass is not formed. When the content of the B 2 O 3 exceeds 40% by weight, the Tg is excessively increased, powder phase occurs, and chemical durability. There is a fear of getting worse. It is preferably included in 10 to 40% by weight, more preferably included in 20 to 40% by weight.

ZnO는 유리수식제로서 무연 유리 조성물의 유리전이온도(Tg), 유전율, 열팽창계수(TEC)와 겔화 빈도를 낮추는 기능을 한다. 따라서, 상기 ZnO의 함량이 30%이상일 경우에는 굴절율이 너무 커지게 된다. 따라서 1 내지 30 중량%로 포함되는 것이 바람직하며, 5 내지 20 중량%로 포함되는 것이 더 바람직하다.ZnO acts as a glass formula to lower the glass transition temperature (Tg), dielectric constant, coefficient of thermal expansion (TEC) and gelation frequency of lead-free glass compositions. Therefore, when the content of ZnO is 30% or more, the refractive index becomes too large. Therefore, it is preferably included in 1 to 30% by weight, more preferably included in 5 to 20% by weight.

SiO2는 밝은색을 나타내는 유리형성제로서, 무연 유리 조성물의 유리전이온도(Tg)를 높이고, 열팽창계수(TEC) 및 겔화 빈도를 낮추는 역할을 한다. 따라서, 상기 SiO2의 함량이 전체 무연 유리 조성물의 중량에 대하여 30 중량%를 초과하는 경우에는 Tg가 과도하게 상승되며, 5 내지 30 중량%로 포함되는 것이 바람직하며 5 내지 25 중량%로 포함되는 것이 더 바람직하다.SiO 2 is a light-forming glass forming agent, and serves to increase the glass transition temperature (Tg) of the lead-free glass composition, and to lower the coefficient of thermal expansion (TEC) and the gelation frequency. Therefore, when the content of SiO 2 exceeds 30% by weight relative to the total weight of the lead-free glass composition, the Tg is excessively increased, and it is preferably included in 5 to 30% by weight and is included in 5 to 25% by weight. More preferred.

Al2O3는 흰색을 나타내는 유리안정화제로서, 무연 유리 조성물의 유리전이온도(Tg)을 높이고 유리의 결정화도를 감소시키며, 열팽창계수(TEC)와 에칭율, 겔화 빈도를 낮추는 기능을 한다. 따라서 Al2O3의 함량이 전체 무연 유리 조성물의 중량에 대하여 40중량%를 초과하는 경우에는 유리 전이점과 연화점이 상승하게 되어 소성온도가 높아진다. 따라서, 5 내지 40 중량%로 포함되는 것이 바람직하며 5 내지 30 중량%로 포함되는 것이 더 바람직하다.Al 2 O 3 is a white glass stabilizer, which increases the glass transition temperature (Tg) of the lead-free glass composition, decreases the crystallinity of the glass, and lowers the coefficient of thermal expansion (TEC), etching rate, and gelation frequency. Therefore, when the content of Al 2 O 3 exceeds 40% by weight with respect to the total weight of the lead-free glass composition, the glass transition point and the softening point are increased to increase the firing temperature. Therefore, it is preferably included in 5 to 40% by weight, more preferably included in 5 to 30% by weight.

BaO는 어두운 유색을 나타내는 유리수식제로서, 무연 유리 조성물의 유리전이온도(Tg)를 낮추고, 유전율, 열팽창계수(TEC)와 겔화 빈도를 높이는 기능을 한다. 따라서, 상기 BaO의 함량이 전체 무연 유리 조성물의 중량에 30 중량%를 초과하는 경우에는 열팽창계수가 증가하여 PDP 격벽의 형태안정성을 저해할 수 있고 굴절율이 커지게 되는 영향을 줄 수 있어, 1 내지 30 중량%로 포함되는 것이 바람직하며, 1 내지 10 중량%로 포함되는 것이 더 바람직하다.BaO is a dark colored glass formulating agent, which lowers the glass transition temperature (Tg) of the lead-free glass composition, and increases the dielectric constant, coefficient of thermal expansion (TEC) and gelation frequency. Therefore, when the content of BaO exceeds 30% by weight of the total lead-free glass composition, the coefficient of thermal expansion increases, which may inhibit the morphological stability of the PDP partition wall and increase the refractive index. It is preferably included in 30% by weight, more preferably contained in 1 to 10% by weight.

또한, MgO는 고융점에서 점성유지용으로 사용되는 것으로 온도를 낮출 수 있어 유리화를 용이하게 하는 성분이나 함량이 너무 많으면 유리화에 어려움이 있기 때문에 1~15중량%로 하는 것이 적당하다.In addition, MgO is used for maintaining the viscosity at a high melting point can be lowered temperature, so if the component or content that facilitates vitrification is too difficult to vitrify it is suitable to be 1 to 15% by weight.

한편, 본 발명에서는 상기에서 얻어진 유리분말을 이용하여 유기 비이클을 통해 유리분말 조성물을 제조한다.In the present invention, the glass powder composition is prepared through the organic vehicle using the glass powder obtained above.

여기서, 유기 성분으로는 감광성 모노머(Monomer), 감광성 폴리머(Polymer)등의 감광성 바인더를 사용하되, 우레탄계, 아크릴계, 아민계 등의 바인더를 모두 사용할 수 있으며, 광개시제로는 장파장 혹은 단파장 광개시제를 사용할 수 있고, 기타 광 보조개시제, 중합방지제, 분산제를 첨가하고 밀링기를 통해 유리분말 조성물(페이스트)을 제조 한다.Here, a photosensitive binder such as a photosensitive monomer (Monomer) and a photosensitive polymer (Polymer) may be used as the organic component, and all binders such as urethane, acryl, and amine may be used, and long or short wavelength photoinitiators may be used as photoinitiators. And other light auxiliary initiators, polymerization inhibitors, dispersants are added to the glass powder composition (paste) to prepare a mill.

이하, 실시예를 통하여 좀더 상세히 설명한다.Hereinafter, the present invention will be described in more detail.

실시예 1~3(유리분말)Examples 1-3 (glass powder)

먼저, 하기 표1과 같은 조성을 준비한 다음, 다음과 같은 순서로 제조 및 측정을 진행하였다.First, to prepare a composition as shown in Table 1, and then proceed to manufacture and measure in the following order.

1). 상기 무연, 인산계 조성을 포함하며 굴절율이 1.5~1.7사의의 조성물 원료를 정확히 계량 하였다. One). The composition of the composition of the lead-free, phosphate-based composition and the refractive index of 1.5 ~ 1.7 was accurately weighed.

2). 상기 PDP 격벽용 무연 유리 조성물은 무중력 혼합기를 통해 모든 조성물들이 완전히 혼합이 되도록 충분한 시간을 두고 혼합하였다.2). The lead-free glass composition for the PDP partition wall was mixed with sufficient time to allow all the compositions to mix completely through a gravity-free mixer.

3). 상기 혼합된 원료를 용융시키는 단계3). Melting the mixed raw materials

용융 단계의 용융온도는 1000 내지 1500℃인 것이 바람직하며, 1300 내지 1450℃인 것이 더욱 바람직하다. 또한, 용융시간은 10 내지 60 분(min)을 유지하여 유리 조성물이 용융상태에서 고르게 혼합될 수 있도록 하는 것이 바람직하며 용융온도가 1000℃ 미만인 경우에는 용융점도가 높아 각 성분이 고르게 혼합되지 못하게 되는 경우가 발생하여 좋지 않다. The melting temperature of the melting step is preferably 1000 to 1500 ° C, more preferably 1300 to 1450 ° C. In addition, the melting time is preferably 10 to 60 minutes (min) so that the glass composition can be evenly mixed in the molten state, and when the melting temperature is less than 1000 ℃ high melt viscosity prevents each component evenly mixed It is not good to have a case.

용융 단계에서 용융된 무연 유리 조성물은 건식 및 습식 퀀칭(Quenching)을 통해 급냉시켰다.The lead-free glass composition melted in the melting step was quenched through dry and wet quenching.

4). 급냉된 유리 용융물은 볼밀을 통해 1차 조분쇄 작업을 통해 가는 입자로 분쇄하였다.4). The quenched glass melt was ground into fine particles through a first milling operation via a ball mill.

5). 1차로 조분쇄 된 유리 용융물은, 2차 미분쇄 공정을 통해 미분으로 분쇄하는데 이때 분쇄는 건식으로 진행되며, 볼밀 및 제트밀을 통해 2차 미분쇄 공정으로 유리 분말을 얻었다.5). The first coarsely ground glass melt was ground to a fine powder through a second milling process, where the grinding was carried out dry, and glass powder was obtained by a second milling process through a ball mill and a jet mill.

6) 입 도 측 정 6) Particle size measurement

상기 분쇄된 무연 유리 분말을 여과를 통해 평균 입경이 1.5 내지 4.5㎛, Dtop이 6~30㎛인 분말상태로 제조하였다. 분쇄된 유리 분말의 입도 분포는 쌍봉 형태(Bimodal)가 바람직하였다.The pulverized lead-free glass powder was manufactured in a powder state having an average particle size of 1.5 to 4.5 μm and a Dtop of 6 to 30 μm through filtration. The particle size distribution of the pulverized glass powder is preferably bimodal.

필러의 입도도 분쇄된 유리 분말의 평균 입경이 1.5 내지 4.5㎛, Dtop이 6~30㎛인 쌍봉형태의 분말을 제조 하였다.The particle size of the filler The bimodal powder having an average particle diameter of 1.5 to 4.5 µm and a Dtop of 6 to 30 µm was prepared.

그 결과를 도 1 내지 도 3에 나타낸다.The results are shown in FIGS. 1 to 3.

도면에서 도 1은 제트밀, 도 2,3은 볼밀을 사용한 예를 나타낸 것으로, 도면에서와 같이 모든 예가 쌍봉 형태이며, 모든 분말의 Dtop이 12~13㎛ 정도임을 확인할 수 있다.In the drawings, FIG. 1 shows an example using a jet mill, and FIGS. 2 and 3 are ball mills. As shown in FIG.

7) 열 특성7) thermal properties

용융된 유리를 채취하여 시편을 가공한 후 열분석기(TMA, SHIMADZU, TMA-50, Japan)를 이용하여 측정하였다The molten glass was sampled and processed using a thermal analyzer (TMA, SHIMADZU, TMA-50, Japan).

Tg(유리전이온도)는 450~520℃가 바람직하고, 열팽창 계수가 65~100 x 10-7℃정도가 바람직하다.As for Tg (glass transition temperature), 450-520 degreeC is preferable, and thermal expansion coefficient is about 65-100x10 <-7> degreeC .

8) 굴절율8) refractive index

용융된 유리를 채취하여 10 x 5 x 18mm 로 시편을 가공 한 후 굴절율 측정기(Abe 굴절계, ATAGO 4T, Japan) 을 이용하여 측정하였다.After the molten glass was taken and the specimen was processed to 10 x 5 x 18mm, it was measured using a refractive index meter (Abe refractometer, ATAGO 4T, Japan).

유리 조성물의 굴절율은 1.5~1.7 정도인 것이 바람직하다. 또한 감광성 유리페이스트 조성물에서 굴절율이 비슷한 성분의 것들을 사용해야 하는데 여기에 필러 로 사용되고 있는 고융점 유리의 굴절율은 1.5~1.7 인 것이 바람직하나 1.52~1.60 사이의 것이 더욱 바람직하다.It is preferable that the refractive index of a glass composition is about 1.5-1.7. In addition, in the photosensitive glass paste composition, those having similar refractive indices should be used, and the refractive index of the high melting point glass used as the filler is preferably 1.5 to 1.7, but more preferably between 1.52 to 1.60.

Figure 112008027341166-pat00001
Figure 112008027341166-pat00001

상기 표에서 확인할 수 있는 바와 같이, 본 발명의 실시예에서는 원하는 Tg, Ts(연화점) 및 CTE(열팽창계수)값을 얻을 수 있었다.As can be seen from the above table, in the examples of the present invention, desired Tg, Ts (softening point) and CTE (thermal expansion coefficient) values were obtained.

실시예 4(유리분말 페이스트 조성물)Example 4 (glass powder paste composition)

상기 실시예 1~3에서 얻어진 유리 분말을 이용하여 유기 비이클을 통해 유리분말 조성물을 제조하였다.Using the glass powder obtained in Examples 1 to 3 to prepare a glass powder composition through an organic vehicle.

유리 분말과 아크릴계 바인더, 광개시제(IC-379,369,시바사),광 보조개시제(벤조트리아졸,야쿠리사), 중합방지제(HQME), 분산제(Nopcosperse-092, 한국산노프코(주))의 혼합물을 3-롤 밀링(3-roll milling)을 사용하여 혼합 분산시킨 다음 탈포 공정을 거쳐 진공 여과시켜 유리분말 조성물(페이스트)을 제조 하였다.A mixture of a glass powder, an acrylic binder, a photoinitiator (IC-379, 369, Shiba Corporation), a light co-initiator (benzotriazole, Yakuri company), a polymerization inhibitor (HQME), and a dispersant (Nopcosperse-092, manufactured by Novoco Co., Ltd.) The glass powder composition (paste) was prepared by mixing and dispersing using 3-roll milling and vacuum filtration through a defoaming process.

도 1 내지 도 3은 본 발명의 실시예 1~3의 입도측정 결과를 나타내는 그래프1 to 3 are graphs showing the particle size measurement results of Examples 1 to 3 of the present invention.

Claims (9)

삭제delete 삭제delete Al2O3 5~40중량%, B2O3 10~40중량%, BaO 1~30중량%, ZnO 1~30중량%, P2O5 2~30중량%, SiO2 5~30중량%, Li2O, Na2O 또는 K2O로 이루어진 알칼리 성분들 중 1종 이상의 성분 1~20중량%, MgO 1~15중량% 및 CaO 2~10중량%로 이루어지는 것을 특징으로 하는 감광성 페이스트 및 그린시트용 유리분말.5-40% Al 2 O 3 , 10-40% B 2 O 3 , BaO 1-30%, ZnO 1-30%, P 2 O 5 2-30%, SiO 2 5-30% A photosensitive paste comprising 1 to 20% by weight of one or more components, 1 to 15% by weight of MgO and 2 to 10% by weight of CaO, of an alkali component consisting of%, Li 2 O, Na 2 O or K 2 O And glass powder for green sheets. 제3항에 있어서,      The method of claim 3, 상기 분말의 소성 후 색상이 갈색으로 변색 되지 않는 것을 특징으로 하는 감광성 페이스트 및 그린시트용 유리분말.The glass powder for the photosensitive paste and green sheet, characterized in that the color does not turn brown after firing of the powder. 제3항에 있어서,The method of claim 3, 상기 분말의 소성 후 색상이 갈색으로 변색 되지 않고 L값이 60 이상인 것을 특징으로 하는 감광성 페이스트 및 그린시트용 유리분말.The glass powder for photosensitive paste and green sheet, characterized in that, after baking the powder, the color does not turn brown and the L value is 60 or more. 제3항에 있어서,The method of claim 3, 상기 분말을 페이스트(Paste)화 하여 소성하였을 경우 색상이 갈색으로 변색 되지 않는 것을 특징으로 하는 감광성 페이스트 및 그린시트용 유리분말.The powder for the photosensitive paste and the green sheet, characterized in that the color does not turn brown when the powder is baked (Paste). 제3항에 있어서,The method of claim 3, 상기 분말을 페이스트화 하여 소성하였을 경우 색상이 갈색으로 변색 되지 않고 L값이 60 이상인 것을 특징으로 하는 감광성 페이스트 및 그린시트용 유리분말.When the powder is baked by baking, the color of the photosensitive paste and the green sheet glass powder, characterized in that the L value is 60 or more without changing color to brown. 제3항에 있어서,The method of claim 3, 상기 분말은 입도 분포가 쌍봉 형태(Bimodal)로서 평균 입경이 1.5 내지 5.5㎛, Dtop이 6~40㎛인 것을 특징으로 하는 감광성 페이스트 및 그린시트용 유리분말.The powder has a particle size distribution of bimodal form (Bimodal), the average particle diameter of 1.5 to 5.5㎛, Dtop glass powder for photosensitive paste and green sheet, characterized in that 6 ~ 40㎛. 제3항의 감광성 페이스트 및 그린시트용 유리분말에 감광성 폴리머, 모노머 및 광개시제를 혼합하여 이루어진 것을 특징으로 하는 감광성 페이스트 및 그린시트용 유리분말 조성물.A glass powder composition for photosensitive paste and green sheet, comprising mixing a photosensitive polymer, a monomer, and a photoinitiator with the photosensitive paste and glass sheet for green sheet.
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KR20060093506A (en) * 2005-02-22 2006-08-25 주식회사 파티클로지 Lead-free low-melting glass frit
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KR20060093506A (en) * 2005-02-22 2006-08-25 주식회사 파티클로지 Lead-free low-melting glass frit
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