KR20090067831A - Environment-friendly transparent dielectric material containing titanium oxide and method of manufacturing the same - Google Patents
Environment-friendly transparent dielectric material containing titanium oxide and method of manufacturing the same Download PDFInfo
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 15
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 239000003989 dielectric material Substances 0.000 title description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 title description 4
- 238000000034 method Methods 0.000 claims abstract description 20
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims abstract description 16
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000002844 melting Methods 0.000 claims abstract description 15
- 230000008018 melting Effects 0.000 claims abstract description 15
- 239000000843 powder Substances 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- 238000000227 grinding Methods 0.000 claims abstract description 4
- 239000011812 mixed powder Substances 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 239000000155 melt Substances 0.000 claims abstract description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 19
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 15
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 15
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- 239000011734 sodium Substances 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 3
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims 1
- 229910001930 tungsten oxide Inorganic materials 0.000 claims 1
- 239000000203 mixture Substances 0.000 abstract description 37
- 239000011521 glass Substances 0.000 abstract description 25
- 238000004017 vitrification Methods 0.000 description 8
- 229910052797 bismuth Inorganic materials 0.000 description 6
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 6
- 238000010304 firing Methods 0.000 description 5
- 229910001948 sodium oxide Inorganic materials 0.000 description 4
- 238000002076 thermal analysis method Methods 0.000 description 4
- 239000011787 zinc oxide Substances 0.000 description 4
- 229910001385 heavy metal Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 229910052810 boron oxide Inorganic materials 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000005357 flat glass Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 description 1
- 229910018068 Li 2 O Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 1
- 239000012768 molten material Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
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- 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
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Abstract
본 발명은 저융점 무연 투명 유전체 유리 조성물 및 그의 제조방법에 관한 것으로 보다 상세하게는 산화티타늄(TiO2)을 주성분으로 하여 인체 및 환경에 유해한 납을 함유하지 않는 저융점 무연 투명 유전체 유리 조성물 및 그의 제조방법에 관한 것이다. 본원 발명의 친환경 투명 유전체 유리 조성물은 산화티타늄(TiO2)을 8~40 중량%를 포함하고, 나머지는 산화붕소(B2O3), 산화나트륨(Na2O)인 것을 특징으로 한다. 상기 친환경 투명 유전체 유리 조성물의 제조방법은 산화티타늄(TiO2), 산화붕소(B2O3), 산화나트륨(Na2O)를 분말형태로 혼합하는 단계; 상기 혼합된 분말을 열처리하여 용윰 및 화학반응을 시키는 단계; 상기 용융물을 냉각시킨후 분쇄과정을 거쳐 분말을 제조하는 단계를 포함하는 것을 특징한다. The present invention relates to a low melting lead-free transparent dielectric glass composition and a method for manufacturing the same, and more particularly, to a low melting lead-free transparent dielectric glass composition containing titanium oxide (TiO 2 ) as a main component and containing no lead harmful to a human body and the environment. It relates to a manufacturing method. Eco-friendly transparent dielectric glass composition of the present invention comprises 8 to 40% by weight of titanium oxide (TiO 2 ), the rest is characterized in that the boron oxide (B 2 O 3 ), sodium oxide (Na 2 O). The method for preparing an environmentally friendly transparent dielectric glass composition may include mixing titanium oxide (TiO 2 ), boron oxide (B 2 O 3 ), and sodium oxide (Na 2 O) in powder form; Heat-treating the mixed powder to perform melting and chemical reaction; After cooling the melt is characterized in that it comprises a step of producing a powder through a grinding process.
Description
본 발명은 저융점 무연 투명 유전체 유리 조성물 및 그의 제조방법에 관한 것으로 보다 상세하게는 산화티타늄(TiO2)을 주성분으로 하여 인체 및 환경에 유해한 납을 함유하지 않는 저융점 무연 투명 유전체 및 그의 제조방법에 관한 것이다.The present invention relates to a low melting lead-free transparent dielectric glass composition and a method for manufacturing the same. More specifically, a low melting lead-free transparent dielectric and a method for manufacturing the same, based on titanium oxide (TiO 2 ), containing no lead harmful to humans and the environment It is about.
PDP 등에 적용되는 저융점 투명 유전체 유리의 경우 종래에는 540~580℃의 비교적 낮은 소성온도에서 소성이 가능하여야 하므로, 저온에서 녹는 유리 특성을 위하여 융점이 낮은 산화납(PbO)을 주성분으로 하는 PbO-B2O3계 유리 조성물이 주로 사용되고 있다.In the case of low melting transparent dielectric glass applied to PDP, it should be possible to fire at relatively low firing temperature of 540 ~ 580 ° C. Therefore, PbO- containing PbO- which has low melting point (PbO) as the main component for glass melting at low temperature B 2 O 3 based glass compositions are mainly used.
그런데 최근에는 환경 문제의 관점에서 유리 재료로부터 납 성분을 제거하는 것이 요구되고 있고, 이러한 요구에 부응하여 납 함유 재료를 대체할 수 있는 조성물에 대한 연구가 활발히 이루어지고 있다. 그 대표적인 것으로는 비스무스(Bi)계 유전체 조성물 및 아연(Zn)계 유전체 조성물이 널리 알려져 있다.However, in recent years, it is required to remove lead components from glass materials from the viewpoint of environmental problems, and research has been actively conducted on compositions capable of replacing lead-containing materials in response to these requirements. Representative examples thereof include bismuth (Bi) based dielectric compositions and zinc (Zn) based dielectric compositions.
한국공개특허 제10-1999-0046605호에는 PbO 50~85 중량%, SiO2 7~25 중량% 및 B2O3 7~25 중량%가 주성분인 유전체 조성을 소개하고 있고, 한국공개특허 제2003-10416 호에서 Bi2O3 는 60~75 중량%, B2O3 4~15 중량%, SiO2 5~8 wt%, P2O5 1~18 중량%, Al2O3 1~3 중량%를 주성분으로 하는 저융점 무연 조성물의 유리에 관한 기술을 소개하고 있다. Korean Patent Publication No. 10-1999-0046605 discloses a dielectric composition composed of 50 to 85 wt% of PbO, 7 to 25 wt% of SiO 2, and 7 to 25 wt% of B 2 O 3. In No. 10416, Bi 2 O 3 is 60-75 wt%, B 2 O 3 4-15 wt%, SiO 2 5-8 wt%, P 2 O 5 1-18 wt%, Al 2 O 3 1-3 wt The technique regarding glass of the low melting lead-free composition which has% as a main component is introduced.
또한 일본 공개특허 제2000-226231호에 의하면 ZnO가 20 내지 45중량%이고, B2O3가 20 내지 34중량%이고, SiO2가 20 내지 45중량%, R2O(K2O, Na2O 및 Li2O)가 4 내지 12중량%이고, RO(BaO 및 CaO의 합)가 0 내지 3중량%이고, NaF가 0.5 내지 8중량%인 것을 특징으로 하는 무연 유리조성물을 소개하고 있다. 또한 미합중국 등록특허 제6,417,123호는 ZnO가 20 내지 45중량%이고, BaO가 15 내지 45중량%이고, B2O3가 15 내지 35중량%이고, SiO2가 3 내지 15중량%이고, PbO가 0 내지 24.5중량%인 유리조성물을 소개하고 있다. 상기 유리조성물들은 모두 PDP 투명유전체 및 격벽형성제등에 쓰일 유리조성물을 제공하고 있다. In addition, according to Japanese Patent Laid-Open No. 2000-226231, ZnO is 20 to 45% by weight, B 2 O 3 is 20 to 34% by weight, SiO 2 is 20 to 45% by weight, and R 2 O (K 2 O, Na Lead-free glass compositions are characterized in that 2 O and Li 2 O) are 4-12 wt%, RO (sum of BaO and CaO) is 0-3 wt%, and NaF is 0.5-8 wt%. . In addition, U.S. Patent No. 6,417,123 has 20 to 45 wt% ZnO, 15 to 45 wt% BaO, 15 to 35 wt% B 2 O 3 , 3 to 15 wt% SiO 2 , and PbO Introducing a glass composition of 0 to 24.5% by weight. All of the glass compositions provide glass compositions for use in PDP transparent dielectrics and partitioning agents.
이 중에서 비스무스(Bi)계 유전체 조성물은 그 정도의 차이는 있으나 그 역시도 환경오염을 유발하고, 더욱 문제가 되는 것은 단가가 높다는 것이다. 이에 비해 아연(Zn)계 유전체 조성물은 환경오염으로 부터 자유로울 뿐만 아니라 비스무스(Bi)계 유전체 조성물에 비하여 50% 정도의 가격 이점이 있기 때문에 장점이 있으나, 다만 유리화 온도가 높기 때문에 전체 소성 조건에 맞지 않는다는 문제점이 있다. 또한 소성 온도를 낮추는 데 한계가 있어, 조성 상에 알칼리 성분을 사용할 수 밖에 없는데, 알칼리 성분을 사용하면 소성 후 색상이 노랑게 변화는 황변 현상이 발생하는 문제점이 있다.Of these, bismuth (Bi) -based dielectric composition has a degree of difference, but it also causes environmental pollution, and more problematic is that the unit price is high. On the other hand, zinc (Zn) -based dielectric compositions are advantageous because they are free from environmental pollution and have a 50% price advantage over bismuth (Bi) -based dielectric compositions. There is a problem. In addition, there is a limit in lowering the firing temperature, but there is no choice but to use an alkali component in the composition. When the alkali component is used, a yellowing phenomenon occurs when the color changes to yellow after firing.
본 발명은 상기와 같은 문제점을 해결하기 위해 안출된 것으로, 인체에 유해한 중금속 인 납(Pb) 또는 비스무스(Bi)를함유하지 않으면서도 가시광선의 투과율이 높고, 유리화 온도가 낮으며 유전상수가 적절한 저융점 유전체와 그의 제조방법을 제공하는 것을 목적으로 한다.The present invention has been made to solve the above problems, it does not contain a heavy metal lead (Pb) or bismuth (Bi) harmful to the human body, high visible light transmittance, low vitrification temperature and low dielectric constant is appropriate It is an object to provide a melting point dielectric and a method of manufacturing the same.
상기 목적을 달성하기 위한 본 발명의 친환경 투명 유전체는 산화티타늄(TiO2)을 8~40 중량%를 포함하고, 나머지는 산화붕소(B2O3), 산화나트륨(Na2O)를 포함하는 것을 특징으로 한다. 상기 유전체 조성에는 산화아연(ZnO)를 더 포함될 수 있으며, 또한 산화규소(SiO2)가 더 포함될 수 있다. 상기 산화아연(ZnO)은 5~30 중량%, 산화붕소(B2O3)는 15~50 중량%, 산화규소(SiO2) 10~15 중량%, 산화나트륨(Na2O)은 8~40%, 산화규소(SiO2) 10~15 중량%인 것을 특징으로 한다. 상기 산화나트륨은 탄산나트륨(Na2CO3)으로 대체될 수 있다. 본 발명에 따른 친환경 투명 유전체는 플라즈마 디스플레이 패널 투명 유전막에 이용되는 것을 특징으로 한다.Environment-friendly transparent dielectric of the present invention for achieving the above object comprises 8 to 40% by weight of titanium oxide (TiO 2 ), the remainder containing boron oxide (B 2 O 3 ), sodium oxide (Na 2 O) It is characterized by. The dielectric composition may further include zinc oxide (ZnO), and may further include silicon oxide (SiO 2 ). The zinc oxide (ZnO) is 5 to 30% by weight, boron oxide (B 2 O 3 ) is 15 to 50% by weight, silicon oxide (SiO 2 ) 10 to 15% by weight, sodium oxide (Na 2 O) is 8 ~ 40%, silicon oxide (SiO 2 ) It is characterized in that 10 to 15% by weight. The sodium oxide may be replaced with sodium carbonate (Na 2 CO 3 ). Eco-friendly transparent dielectric material according to the invention is characterized in that it is used in a plasma display panel transparent dielectric film.
본 발명에 따른 친환경 투명 유전체의 제조방법은 산화티타늄(TiO2) 8~40 중량%, 나머지는 산화붕소(B2O3), 산화나트륨(Na2O)을 분말형태로 혼합하는 단계; 상기 혼합된 분말을 열처리하여 용융 및 화학반응을 시키는 단계; 상기 용융물을 냉 각시킨 후 분쇄과정을 거쳐 분말을 제조하는 단계를 포함하는 것을 특징으로 한다. Method for producing an environmentally friendly transparent dielectric according to the present invention comprises the steps of mixing titanium oxide (TiO 2 ) 8 to 40% by weight, the rest of boron oxide (B 2 O 3 ), sodium oxide (Na 2 O) in the form of a powder; Heat treating the mixed powder to perform melting and chemical reaction; After cooling the melt is characterized in that it comprises a step of producing a powder through a grinding process.
상기 유전체 조성에는 산화아연(ZnO)를 더 포함될 수 있으며, 또한 산화규소(SiO2)가 더 포함될 수 있다. 상기 혼합단계에서의 원료는 산화아연(ZnO)은 5~30 중량%, 산화붕소(B2O3)는 15~50 중량%, 산화규소(SiO2) 10~15 중량%, 산화나트륨(Na2O)은 8~40%, 산화규소(SiO2) 10~15 중량%인 것을 특징으로 한다. 또한, 상기 용융 및 화학반응을 시키는 단계는 800~1500℃의 온도범위에서 1~10시간 동안 수행하는 것을 특징으로 한다.The dielectric composition may further include zinc oxide (ZnO), and may further include silicon oxide (SiO 2 ). The raw material in the mixing step is 5-30% by weight of zinc oxide (ZnO), 15-50% by weight of boron oxide (B 2 O 3 ), 10-15% by weight of silicon oxide (SiO 2 ), sodium oxide (Na 2 O) is characterized in that 8 to 40%, silicon oxide (SiO 2 ) 10 to 15% by weight. In addition, the melting and the step of the chemical reaction is characterized in that carried out for 1 to 10 hours in the temperature range of 800 ~ 1500 ℃.
본 발명에 의한 유전체 유리는 중금속인 납(Pb) 또는 비스무스(Bi)를 함유하지 않고, 가시광선 투과율이 높고, 유리화 온도가 낮으며, 유전상수가 적절하여 환경친화적인 유전체 유리로 사용될 수 있다. 특히 PDP용 상판 유전체의 재료로서 적합하며, TiO2가 다량 함유되어 있어 광촉매 특성을 갖는 건축의 외장유리로도 사용될 수 있다.The dielectric glass according to the present invention does not contain lead metal (Pb) or bismuth (Bi), which is a heavy metal, has a high visible light transmittance, a low vitrification temperature, and an appropriate dielectric constant, and can be used as an environmentally friendly dielectric glass. In particular, it is suitable as a material for the top plate dielectric for PDP, and it can be used as an exterior glass of construction having a photocatalyst property because a large amount of TiO 2 is contained.
본 발명의 친환경 투명 유전체의 성분은 산화티타늄, 산화붕소, 산화나트륨을 포함하는 것을 특징으로 한다. 또한, 산화아연 및 산화규소가 더 포함될 수 있다. 상기 조성물은 중금속인 납이나 비스무스 성분을 함유하지 않기 때문에 환경친화적이다. 또한 종래 유연 유전체가 갖는 특성에 비해 향상된 특성을 가지며, 저온 소성이 가능한 특징이 있다. 상기 조성물의 유전상수는 8~13 이며 유리화 전이온도는 400~500℃이다.Components of the environmentally friendly transparent dielectric of the present invention is characterized in that it comprises titanium oxide, boron oxide, sodium oxide. In addition, zinc oxide and silicon oxide may be further included. The composition is environmentally friendly because it does not contain lead or bismuth components, which are heavy metals. In addition, it has an improved characteristic compared to the characteristics of the conventional flexible dielectric, it has a feature capable of low-temperature firing. The dielectric constant of the composition is 8 ~ 13 and the vitrification transition temperature is 400 ~ 500 ℃.
본 발명에 의한 친환경 투명 유전체 조성물의 제조 방법은 다음과 같다. 유리를 구성하고 있는 성분 분말들을 혼합하여 혼합물을 제조하는 단계와, 혼합물을 800~1400℃에서 열처리 하여 용융 및 냉각 시켜 유리를 합성하는 단계로 구분된다.Method for producing an environmentally friendly transparent dielectric composition according to the present invention is as follows. It is divided into a step of preparing a mixture by mixing the component powders constituting the glass, and a step of synthesizing the glass by heat-treating the mixture at 800 ~ 1400 ℃ to melt and cool.
상기 제조방법은 비용이 저렴하고 공정이 간단하여 대량생산이 가능한 장점이 있다. 본 발명에서 사용된 구성성분은 고체 산화물로서 산화티타늄, 산화아연, 산화붕소, 산화규소, 산화나트륨을 주원료로서 이루어짐을 특징으로 한다. 상기 산화나트륨은 탄산나트륨으로 대체될 수 있다. 상기 원료의 구성비율은 산화티타늄(TiO2)을 8~40 중량%을 포함하는 것이 바람직하다. 또한, 상기 산화아연(ZnO)은 5~30 중량%, 산화붕소(B2O3)는 15~50 중량%, 산화규소(SiO2) 10~15 중량%, 산화나트륨(Na2O) 또는 탄산나트륨(Na2CO3)은 8~40%을 포함하는 것이 바람직하다. 산화티타늄을 8~40%으로 한정하는 이유는 8 중량% 미만의 경우 융점이 높아 투명 유전체로서의 역할을 하지 못하고 40%를 초과하는 경우 투명성을 갖지 못하는 문제점이 있기 때문이다.The manufacturing method is advantageous in that the mass production is possible due to the low cost and simple process. The component used in the present invention is characterized in that the solid oxide comprises titanium oxide, zinc oxide, boron oxide, silicon oxide, and sodium oxide as the main raw materials. The sodium oxide may be replaced with sodium carbonate. Composition ratio of the raw material is preferably titanium oxide (TiO 2) contains 8 to 40% by weight. In addition, the zinc oxide (ZnO) is 5 to 30% by weight, boron oxide (B 2 O 3 ) is 15 to 50% by weight, silicon oxide (SiO 2 ) 10 to 15% by weight, sodium oxide (Na 2 O) or Sodium carbonate (Na 2 CO 3 ) preferably contains 8 to 40%. The reason for limiting the titanium oxide to 8 to 40% is that a melting point of less than 8% by weight does not play a role as a transparent dielectric, and if it exceeds 40%, there is a problem in that it does not have transparency.
상기 비율로 천칭하여 원료 분말들을 혼합한다. 혼합 분말은 지르코니아 볼을 이용한 볼 밀링(ball milling) 방법으로 기계적으로 분쇄, 혼합과정을 거친다. 상기 분쇄된 혼합물은 800~1500℃의 고온 열처리 노에서 1~10시간 동안 열처리 하여 완전히 용융 및 화학반응을 시킨 용융물을 두께 5mm의 스테인리스 철판위에 부 어서 냉각을 시킨다. 상기 냉각된 용융물은 판상 유리형태로써 상기 볼밀링과 동일한 방법으로 분쇄과정으로 거쳐 1~5㎛ 크기로 미세분말로 제조된다.Balance in the above proportion to mix the raw powders. The mixed powder is mechanically pulverized and mixed by a ball milling method using zirconia balls. The pulverized mixture is heat-treated in a high temperature heat treatment furnace at 800 to 1500 ° C. for 1 to 10 hours to cool the molten material that has been completely melted and chemically reacted on a stainless steel plate having a thickness of 5 mm. The cooled melt is produced in the form of fine powder with a size of 1 to 5 μm through a grinding process in the same manner as the ball mill in the form of a plate glass.
이하에서 본 발명이 속하는 기술분야에서 통상의 지식을 가진 자가 본 발명의 기술적 사상을 용이하게 실시할 수 있도록 본 발명의 실시예를 첨부된 도면을 참조하여 설명하기로 한다. 그러나, 본 발명은 여기서 설명되는 실시예들에 한정되지 않고 다른 형태로 구체화될 수 있다. 오히려, 여기소 소개되는 실시예는 개시된 내용이 철처하고 완전해 질 수 있도록 그리고 당업자에게 본 발명의 기술적 사상이 충분히 전달될 수 있도록 제공되는 것이다. DETAILED DESCRIPTION Hereinafter, exemplary embodiments of the present invention will be described with reference to the accompanying drawings so that those skilled in the art may easily implement the technical idea of the present invention. However, the invention is not limited to the embodiments described herein and may be embodied in other forms. Rather, the embodiments introduced herein are provided so that the disclosed contents may be thorough and complete, and the technical spirit of the present invention may be sufficiently delivered to those skilled in the art.
<실시예> TiO2-계 투명 유전체 조성물 및 그의 제조방법EXAMPLES TiO 2 -based Transparent Dielectric Compositions and Methods for Manufacturing the Same
산화티타늄(TiO2), 산화아연(ZnO), 산화 붕소(B2O3), 산화규소(SiO2), 산화나트륨(Na2O)를 표1과 같은 중량비로 천칭하여 혼합한다음, 혼합물을 백금 도가니에 넣고 대기중에서 1200℃까지 승온시키고 1시간을 유지한 후 급랭하였다. 제조된 조성물의 유전상수 및 유리화 온도를 표1에 나타내었다.Titanium oxide (TiO 2 ), zinc oxide (ZnO), boron oxide (B 2 O 3 ), silicon oxide (SiO 2 ) and sodium oxide (Na 2 O) are mixed in a weight ratio as shown in Table 1, followed by mixing The mixture was placed in a platinum crucible and heated to 1200 ° C. in the air, and maintained at an hour before quenching. The dielectric constant and vitrification temperature of the prepared composition are shown in Table 1.
[표1]Table 1
<시험예 1> 투명성 확인<Test Example 1> Check the transparency
실시예1, 8의 조성으로 제조된 유전체 유리의 사진의 사진을 도1에 도시하였다. 무색 투명한 것을 확인할 수 있었다.The photograph of the photograph of the dielectric glass manufactured by the composition of Example 1, 8 is shown in FIG. It was confirmed that it was colorless and transparent.
<시험예2> 결정구조Test Example 2 Crystal Structure
실시예1의 조성으로 제조된 유전체 유리에 대해 X-선 회절 분석기와 전자현미경을 이용하여 분석한 결과 모두 비정질 구조임을 확인하였고, 실시예5에 대한 X-선 회절 분석 결과를 도2에 도시하였다. 도2에 나타낸 바와 같이 비정질 상태임을 확인할 수 있었다. 상기 도2에서 20°이하에서의 완만한 피크는 테트라헤드랄 또는 옥타헤드락 기본 단위(unit cell)를 형성함으로써 비정질 구조가 잘 형성되었 음을 나타낸다. 즉 본 발명에 따른 투명 유전체 유리는 X-선 회전 분석결과 테트라 헤드랄 기본 단위들이 불규칙하게 배열된 전형적인 비정질 유리의 패턴을 가진다.The dielectric glass prepared in the composition of Example 1 was analyzed using an X-ray diffractometer and an electron microscope, and it was confirmed that both were amorphous structures. The results of X-ray diffraction analysis for Example 5 are shown in FIG. 2. . As shown in Figure 2 it could be confirmed that the amorphous state. In FIG. 2, a gentle peak at 20 ° or less indicates that an amorphous structure is well formed by forming a tetrahedral or octahead lock unit unit. In other words, the transparent dielectric glass according to the present invention has a pattern of typical amorphous glass in which tetrahedral basic units are irregularly arranged as a result of X-ray rotation analysis.
<시험예3> 유리화 온도 측정Test Example 3 Vitrification Temperature Measurement
본 발명에 의해 제조된 유전체 유리에 대해 독일 Netzch 사의 열분석 장비를 이용하여 유리화 온도를 측정하였다. 열분석 조건은 승온속도를 5℃/min, 온도범위를 200~800℃로 하여 측정하였다. 측정결과 유리화 온도는 400~500℃로 측정되었다. 실시예8에 대한 열분석 그래프를 도3에 도시하였다.The vitrification temperature of the dielectric glass prepared according to the present invention was measured using a thermal analysis equipment manufactured by Netzch, Germany. Thermal analysis conditions were measured with a temperature increase rate of 5 ℃ / min, a temperature range of 200 ~ 800 ℃. As a result of the measurement, the vitrification temperature was measured at 400 to 500 ° C. A thermal analysis graph for Example 8 is shown in FIG.
<시험예4> 유전상수 측정Test Example 4 Dielectric Constant Measurement
유전상수를 측정하기 위해 본 발명에 의제 제조된 유전체 유리 조성물을 판유리 형태로 제조한 다음 표면을 매끄럽게 연마하고 10×10×5 mm 크기로 절단하여, 양면에 실버페이스트를 도포한 후 250℃에서 30 분간 소성하여 전극을 구성하였다. 측정된 유전상수값을 표1에 나타내었다. 측정된 유전상수 값들이 8~13의 범위로 PDP 상판 유전체에 적합함을 알 수 있었다.In order to measure the dielectric constant, the dielectric glass composition prepared by the present invention was prepared in the form of plate glass, and then the surface was smoothly polished and cut into a size of 10 × 10 × 5 mm. Firing for a minute constituted the electrode. Table 1 shows the measured dielectric constant values. It was found that the measured dielectric constants are suitable for PDP top dielectrics in the range of 8 ~ 13.
도1은 본 발명에 따른 실시예1 및 실시예8의 조성으로 이루어진 투명 유전체의 사진이다.1 is a photograph of a transparent dielectric composed of the compositions of Examples 1 and 8 according to the present invention.
도2는 본 발명에 따른 실시예5의 조성으로 이루어진 투명 유전체의 X-선 회절도이다.2 is an X-ray diffraction diagram of a transparent dielectric composed of the composition of Example 5 according to the present invention.
도3은 본 발명에 따른 실시예8의 조성으로 이루어진 투명유전체의 유리화 전이온도를 나타내는 열분석 그래프이다.3 is a thermal analysis graph showing the vitrification transition temperature of the transparent dielectric composed of the composition of Example 8 according to the present invention.
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| KR1020070135622A Active KR101431000B1 (en) | 2007-12-21 | 2007-12-21 | Environment friendly dielectric glass composition with titanium dioxide and its synthetic method |
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Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6309595B1 (en) * | 1997-04-30 | 2001-10-30 | The Altalgroup, Inc | Titanium crystal and titanium |
| JPH1125865A (en) * | 1997-06-27 | 1999-01-29 | Matsushita Electric Ind Co Ltd | Plasma display panel |
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