KR0166682B1 - Colored-alumina ceramic composition - Google Patents

Colored-alumina ceramic composition Download PDF

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KR0166682B1
KR0166682B1 KR1019910019093A KR910019093A KR0166682B1 KR 0166682 B1 KR0166682 B1 KR 0166682B1 KR 1019910019093 A KR1019910019093 A KR 1019910019093A KR 910019093 A KR910019093 A KR 910019093A KR 0166682 B1 KR0166682 B1 KR 0166682B1
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colored
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ceramic composition
alumina ceramic
alumina
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KR930007857A (en
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유영창
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한형수
삼성코닝주식회사
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide

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Abstract

본 발명은 Al2O3를 주성분으로 하는 전자부품용 착색 알루미나 세라믹 조정물에 관한 것으로, 좀 더 구체적으로는 알루미나를 기본으로 하는 산화물 95.5~98.7wt%와, 착색조제로 Cr2O31~3wt%, TiO20.2~0.8wt%, Nb2O20.1~0.7wt%를 첨가시킨 전자부품용 암색계 착색 알루미나 절연체 자기 조성물에 관한 것이다.BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to colored alumina ceramic modulators for electronic components having Al 2 O 3 as a main component. More specifically, 95.5 to 98.7 wt% of oxides based on alumina, and Cr 2 O 3 1 to The present invention relates to a dark colored colored alumina insulator ceramic composition for an electronic component containing 3 wt%, TiO 2 0.2 to 0.8 wt%, and Nb 2 O 2 0.1 to 0.7 wt%.

Cr2O3, TiO2, Nb2O5의 착색제를 동시에 사용함으로서 환원 분위기중 소성온도 1500~1650℃에서 소성 가능하며 흑색으로 착색될 뿐만 아니라 절연저항이 5Ω·cm이상이고, 유전상수 9.10이며, 유전손실 1×10-3이하인 착색알루미나 세라믹 조성물을 얻을 수 있었다.By using Cr 2 O 3 , TiO 2 , Nb 2 O 5 colorant at the same time, it can be fired at the firing temperature of 1500 ~ 1650 ℃ in reducing atmosphere, it can be colored black, insulation resistance is over 5Ω · cm, dielectric constant is 9.10. A colored alumina ceramic composition having a dielectric loss of 1 × 10 −3 or less could be obtained.

Description

착색 알루미나 세라믹 조성물Colored alumina ceramic composition

본 발명은 Al2O3를 주성분으로 하는 전자부품용 착색 알루미나 세라믹 조정물에 관한 것으로, 좀 더 구체적으로는 알루미나를 기본으로 하는 산화물 95.5~98.7wt%와, 착색조제로 Cr2O31~3wt%, TiO20.2~0.8wt%, Nb2O20.1~0.7wt%를 첨가시킨 전자부품용 암색계 착색 알루미나 절연체 자기조성물에 관한 것이다.BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to colored alumina ceramic modulators for electronic components having Al 2 O 3 as a main component. More specifically, 95.5 to 98.7 wt% of oxides based on alumina, and Cr 2 O 3 1 to The present invention relates to a dark colored colored alumina insulator magnetic composition for an electronic component containing 3 wt%, TiO 2 0.2 to 0.8 wt%, and Nb 2 O 2 0.1 to 0.7 wt%.

반도체 IC용 팩키지등의 전자부품용 세라믹스는 전기적 절연 특성이 우수하고 기계적 강도가 크며 연전도성이 우수해야 한다.Ceramics for electronic components such as packages for semiconductor ICs should have excellent electrical insulation properties, high mechanical strength, and excellent electrical conductivity.

또한, 열 방산성이 우수하며 반도체로부터 발산되는 열을 외부로 쉽게 방출하게 광토과가 되지 않으며 빛을 잘 흡수할 수 있도록 암색계로 착색하는 것이 필요하다.In addition, it is excellent in heat dissipation, it is not light transmissive to easily emit heat emitted from the semiconductor to the outside, it is necessary to color in a dark system to absorb light well.

IC기판, 집적회로용 기판 및 팩키지등의 전자부품용 착색 알루미나 세라믹스의 제조방법으로서 종래에는 일반적으로 천이금속, 특히 TiO2를 이용하여 환원성 분위기에서 1500~1650℃의 온도를 소결하여 TiO2의 환원을 유발시킴으로서 TiO2-X형태로 변화됨으로써 착색하는 방법을 사용하였다.As a method for manufacturing colored alumina ceramics for electronic parts such as IC substrates, integrated circuit boards, and packages, conventionally, a transition metal, in particular, TiO 2 is used to sinter a temperature of 1500 to 1650 ° C. in a reducing atmosphere to reduce TiO 2 . The method of coloring by changing the TiO 2-X form by causing it was used.

그러나, 이러한 방법은 흑색으로의 착색은 용이하나 TiO2격자 결함에 의한 물질의 절열 저항 및 유전 특성이 크게 저하되는 결점이 있었다. 또한 이러한 결점을 감소시키기 위해 Cr2O3를 동시에 첨가하나 이 경우에도 크게 개선되지 못했으며, TiO2의 사용량을 감소시키는 경우 제품으로서 통상적으로 요구되는 착색이 제대로 이루어지지 않는 문제점이 있었으므로 상술한 물성 저하를 발생시키지 않고 보다 물성이 안정되고 착색 가능한 알루미나계 세라믹 조성물이 요구되고 있다.However, this method has a drawback that the coloration to black is easy, but the thermal resistance and dielectric properties of the material due to TiO 2 lattice defects are greatly reduced. In addition, Cr 2 O 3 is added at the same time to reduce such defects, but in this case, it was not greatly improved, and when the amount of TiO 2 is reduced, there is a problem in that the coloring required as a product is not properly performed. There is a demand for an alumina-based ceramic composition which is more stable in physical properties without causing a decrease in physical properties.

따라서 본 발명의 목적은 환원 분위기에서 소성이 세라믹스의 절연 저항 및 유전 특성을 저하시키지 않고 흑색으로 착색가능한 전자부품용 착색 세라믹의 조성물을 제공하는 데 그 목적이 있다.Accordingly, it is an object of the present invention to provide a composition of colored ceramics for electronic parts that can be colored in black without sintering reducing the insulation resistance and dielectric properties of ceramics in a reducing atmosphere.

본 발명의 목적을 달성하기 위하여 본 발명에서는 Al2O3를 주성분으로 하고 착색제로서 Cr2O31~3wt%, TiO20.2~0.8wt%, Nb2O50.1~07wt%를 첨가함으로서 통상적인 알루미나 소성온도인 1500~1650℃에서 환원 분위기중 소성 가능하고 치밀하며 우수한 전기적 물성을 나타냄과 동시에 흑화도가 우수하여 집적회로용 기판 및 팩키지등의 전자부품용 절연체로서 사용가능한 알루미나 세라믹 조성물을 얻었다.In order to achieve the object of the present invention, in the present invention, Al 2 O 3 is the main component and Cr 2 O 3 1 to 3 wt%, TiO 2 0.2 to 0.8 wt%, Nb 2 O 5 0.1 to 07 wt% The alumina ceramic composition, which is calcinable in a reducing atmosphere at 1500 to 1650 ° C., which is a phosphorus alumina, exhibits excellent electrical properties and excellent blackening properties, can be used as an insulator for electronic parts such as an integrated circuit board and a package.

즉, 본 발명자는 알루미나계 세라믹스에 착색하는 소결조제를 검토한 결과, 일반적인 착색제인 Cr2O3, TiO2이외에 Nb2O5를 동시에 소결조제로서 사용하는 것이 절연저항과 유전 특성 향상에 유효하다는 것을 인식하여 본 발명을 완성하였다.In other words, the present inventors have studied sintering aids for coloring alumina-based ceramics, and as a result, it is effective to use Nb 2 O 5 simultaneously as sintering aids in addition to the usual colorants Cr 2 O 3 and TiO 2 to improve insulation resistance and dielectric properties. It was recognized that the present invention was completed.

본 발명을 좀 더 구체적으로 설명하면 다음과 같다.The present invention is described in more detail as follows.

본 발명의 착색 알루미나 세라믹 조성물은 착색제로서 Cr2O31~3wt%, TiO20.2~0.8wt%, Nb2O50.1~0.7wt% 및 소량의 SiO2, CaO, MgO등의 소결 조제 성분이 포함된 Al2O3로 구성된다.The colored alumina ceramic composition of the present invention is a sintering aid component such as Cr 2 O 3 1-3 wt%, TiO 2 0.2-0.8 wt%, Nb 2 O 5 0.1-0.7 wt% and a small amount of SiO 2 , CaO, MgO, etc. It consists of Al 2 O 3 contained.

Al2O3에 Cr2O3 ,TiO2, Nb2O5의 첨가량을 각각 1~3wt%, 0.2~0.8wt%, 0.1~0.7wt%로 한정하는 것은 Cr2O31wt%이하에서는 착색효과가 저하되고 3wt%이상에서는 전기적 특성을 저하시킨다. 또한, TiO20.2wt%이하에서는 전기적 특성은 증진되나 착색효과가 저하되며 0.8wt%이상에서는 전기적 물성이 크게 저하된다.Limiting the amount of Cr 2 O 3, TiO 2 , and Nb 2 O 5 added to Al 2 O 3 to 1 to 3 wt%, 0.2 to 0.8 wt%, and 0.1 to 0.7 wt%, respectively, is less than 1 wt% of Cr 2 O 3. The effect is lowered and the electrical properties are lowered above 3wt%. In addition, the electrical properties of TiO 2 below 0.2wt% are enhanced, but the coloring effect is lowered. At 0.8wt% or above, the electrical properties are greatly reduced.

Nb2O50.1wt% 이하에서는 전기적 물성과 착색효과가 저하되며 0.7wt%이상에서는 전기적 물성이 저하된다. TiO2는 환원 분위기에서 Ti2O3, TiO, TiO2-X등의 여러 형태를 가지며 이것이 Al2O3와 고온에서 고용되어 흑색을 나타내는 것으로 알려져 있다. 그러나 TiO2만 사용할 경우 TiO2-X의 간한 휘발성으로 인해 소결체의 치밀화가 억제되고 절연성이 크게 떨어지므로 Al2O3와 같은 결정구조를 갖는 Cr2O3를 첨가하여 고용을 촉진시킴으로써 소결성 및 물성을 증진시킨다.At 0.1 wt% or less of Nb 2 O 5 , electrical properties and coloring effects are reduced, and at 0.7 wt% or more, electrical properties are degraded. TiO 2 has various forms such as Ti 2 O 3 , TiO, TiO 2 -X in a reducing atmosphere, and it is known that TiO 2 is solid-solution at high temperature with Al 2 O 3 . However, TiO 2 man sintering property and physical properties by the densification of the sintered body due to the inhibition ganhan volatility of TiO 2 -X and promote employment and insulating a significant drop since the addition of Cr 2 O 3 having a crystal structure such as Al 2 O 3 when used Promote

상기 목적을 위하여 Cr2O3를 TiO2와 더불어 동시에 첨가시키지만 Cr2O3는 소결시 입성장에 기여하여 기계적 강도가 저하된다. 또한, 착색제로서 이 2가지 성분만을 사용할 경우 전기적 특성, 특히 절연저항 및 유전손실이 크게 저하되며 이러한 특성저하를 개선하기 위해 본 발명에서는 제3의 착색제 성분으로 Nb2O5를 첨가하여 특성이 향상되도록 하였다. 착색용 첨가제인 Cr2O3, TiO2, Nb2O5를 동시에 사용한 본 발명의 Al2O3소결체는 환원 분위기중 소성온도 1500~1650℃에서 소성 가능하며 흑색으로 착색되는 한편, 절연저항 1014~1015Ω·cm이상, 유전상수 9.10, 유전손실 1×10-3이하의 착색알루미나가 제조될 수 있다.Cr 2 O 3 is added simultaneously with TiO 2 for this purpose, but Cr 2 O 3 contributes to grain growth during sintering, thereby lowering the mechanical strength. In addition, when only these two components are used as the colorant, the electrical properties, in particular the insulation resistance and dielectric loss, are greatly reduced, and in order to improve such property degradation, the present invention improves the properties by adding Nb 2 O 5 as the third colorant component. It was made. The Al 2 O 3 sintered body of the present invention using the coloring additives Cr 2 O 3 , TiO 2 , and Nb 2 O 5 simultaneously can be fired at a firing temperature of 1500 to 1650 ° C. in a reducing atmosphere and colored in black, and has insulation resistance 10 Colored alumina of 14 ~ 10 15 Ω · cm or more, dielectric constant 9.10, dielectric loss 1 × 10 -3 or less can be prepared.

다음의 실시예는 본 발명의 착색 알루미나 세라믹 조성물을 좀 더 구체적으로 설명하는 것이지만 본 발명의 범주를 한정하는 것은 아니다.The following examples illustrate the colored alumina ceramic compositions of the present invention in more detail, but do not limit the scope of the invention.

[실시예 1~4]EXAMPLES 1-4

하기 표1에 기재된 바와 같이 산화물(Al2O3, SiO2, CaO, MgO) 및 착색 첨가제 혼합분말(Cr2O3, TiO2, Nb2O5) 100wt%에 대하여 용제로서 에탄올 50wt%와 결합제로서 폴리비닐부티랄(PVB) 5wt%, 가소제로서 폴리에틸렌 글리콜(PEG) 2wt%, 분산제로서 글리세릴트리올레이트 1wt%를 첨가하고 볼 밀로 혼합하여 슬러리(Slurry)를 제조한 후 닥터 브레이드(Doctor Blade)방법에 의해 두께 0.6mm의 그린 쉬이트(Green Sheet)로 캐스팅(Casting)한 뒤 가습수소 및 질소 혼합 분위기 중에서 160℃의 온도에서 소성한다.As shown in Table 1, with respect to 100 wt% of oxides (Al 2 O 3 , SiO 2 , CaO, MgO) and coloring additive mixed powders (Cr 2 O 3 , TiO 2 , Nb 2 O 5 ), 50 wt% of ethanol and 5 wt% of polyvinyl butyral (PVB) as a binder, 2 wt% of polyethylene glycol (PEG) as a plasticizer, and 1 wt% of glyceryl trioleate as a dispersant were added and mixed in a ball mill to prepare a slurry, followed by a doctor blade. It is cast into a green sheet having a thickness of 0.6 mm by a blade method and then fired at a temperature of 160 ° C. in a mixed atmosphere of humidified hydrogen and nitrogen.

상술한 방법으로 제조된 착색 알루미나 세라믹 조성물에 대한 유전상수와 유전손실계수는 LCR meter를 이용하여 상온(25℃), 1MHz에서 측정하고, 절연저항은 DC 500V, 25℃, 부하시간 1분하에서 측정하였으며 색조는 육안으로 관찰하여 그 물성치를 하기 표1에 기재하였다.The dielectric constant and dielectric loss coefficient of the colored alumina ceramic composition prepared by the above-described method were measured at room temperature (25 ° C) and 1MHz using an LCR meter, and the insulation resistance was measured at DC 500V, 25 ° C and load time of 1 minute. The color tone was visually observed and its physical properties are shown in Table 1 below.

[비교예 1~3][Comparative Examples 1-3]

하기 표1에 기재된 바와 같이 본 발명의 범위를 벗어난 산화물 및 착색 첨가제 혼합분말(Al2O3, Cr2O3, TiO2, Nb2O5, SiO2, CaO, MgO)을 사용하고 실시예 1~4와 동일한 방법으로 착색 알루미나 세라믹 조성물을 제조하였다.Example using an oxide and coloring additive mixed powder (Al 2 O 3 , Cr 2 O 3 , TiO 2 , Nb 2 O 5 , SiO 2 , CaO, MgO) outside the scope of the present invention as shown in Table 1 below Colored alumina ceramic compositions were prepared in the same manner as in 1 to 4.

제조된 착색 알루미나 세라믹 조성물에 대한 유전상수, 유전손실계수, 절연저항 및 색조를 실시예 1~4의 방법과 동일한 방법으로 측정하고 그 결과를 하기 표1에 기재하였다.Dielectric constant, dielectric loss factor, insulation resistance and color tone of the prepared colored alumina ceramic composition were measured in the same manner as in Examples 1 to 4, and the results are shown in Table 1 below.

상술한 바와 같이 CrO, TiO, NbO의 착색제를 동시에 사용함으로서 환원분위기중, 소성온도 1500~1600℃에서 소성 제조하며 흑색으로 착색될 뿐만 아니라 절연저항이 10 Ω·cm이상이고, 유전 상수가 9~10이며, 유전손실이 1×10 이하인 착색 알루미나 세라믹 조성물을 얻을 수 있었다.As described above, by using the coloring agent of CrO, TiO, NbO at the same time in the reducing atmosphere, firing at 1500 ~ 1600 ℃ firing temperature is not only colored black but also insulation resistance 10 Ω · cm or more, dielectric constant is 9 ~ 10, dielectric loss is 1 × 10 The colored alumina ceramic composition which is the following was obtained.

Claims (1)

Al2O3를 주성분으로 하는 착색 알루미나 세라믹 조정물에 있어서, 전체 조성중에 착색제로서 Cr2O31~3wt%, TiO20.2~0.8wt%, Nb2O50.1~0.7wt%를 포함함을 특징으로 하는 착색 알루미나 세라믹 조성물.In the colored alumina ceramic modifier mainly composed of Al 2 O 3 , 1 to 3 wt% of Cr 2 O 3 , 0.2 to 0.8 wt% of TiO 2 , and 0.1 to 0.7 wt% of Nb 2 O 5 as a colorant in the total composition. Colored alumina ceramic composition, characterized in that.
KR1019910019093A 1991-10-29 1991-10-29 Colored-alumina ceramic composition KR0166682B1 (en)

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