KR950004481B1 - Glass solders - Google Patents

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KR950004481B1
KR950004481B1 KR1019900014143A KR900014143A KR950004481B1 KR 950004481 B1 KR950004481 B1 KR 950004481B1 KR 1019900014143 A KR1019900014143 A KR 1019900014143A KR 900014143 A KR900014143 A KR 900014143A KR 950004481 B1 KR950004481 B1 KR 950004481B1
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weight
glass powder
sio
oxide
low
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KR1019900014143A
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KR920006242A (en
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홍유식
김기웅
이기연
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삼성코닝주식회사
한형수
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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
    • C03C8/24—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
    • C03C8/245—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 containing more than 50% lead oxide, by weight
    • 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
    • C03C27/00—Joining pieces of glass to pieces of other inorganic material; Joining glass to glass other than by fusing

Abstract

The glass of a low melting point composition for adhesion consists of PbO-B2O3-ZnO-SiO2 based glass powder and a filler. This composition has 50-80 wt% low melting point glass powder including 75-87 wt% lead oxide, 6-15 wt% boron oxide, 2-7 wt% zinc oxide, 0.5-2 wt% silica, 0.5-2 wt% alumina and 20-50 wt% the refractory filler composed of a mixture which comprises one or more compounds of willemanite, beta eucryptite, zircon, lead titanate, antimony oxide and cordierite and 3-50 wt% low thermal expansion crystallized glass powder. The crystalline glass powder has a low thermal expansion coefficient of 40-50×10-7/deg.C and comprises 4 wt% lead oxide, 22.5 wt% boron oxide, 62 wt% zinc oxide, 9.5 wt% silica, 9.5 wt% alumina, 1.5 wt% antimony oxide, 0.5 wt% cerium oxide and is prepared by melting the mixture at 1,400 deg.C, heating 400 deg.C for 30 min. and pulverizing to the particle size of less than 150 mesh.

Description

접착용 유리조성물Adhesive Glass Composition

본 발명은 접착용 유리조성물에 관한 것으로서, 더욱 상세하게는 저온의 열처리에 의해 비실투 상태에서 접착을 할수 있는 저융점 유리분말과, 저팽창의 무기내화점 필러로 이루어져 있어서, 특허 IC용 알루미나 세라믹팩케이지의 접착에 적합한 유리조성물에 관한 것이다.The present invention relates to a glass composition for bonding, more specifically, a low melting point glass powder capable of bonding in a non-devitrification state by a low temperature heat treatment, and a low expansion inorganic refractory point filler, alumina ceramic for IC The present invention relates to a glass composition suitable for bonding a package.

종래에 IC의 알루미니 세라믹팩케이지의 기밀접착에는 PbO-B2O3-ZnO-SiO2계의 열실투성 유리분말이 사용되었고, 이것은 480~500℃에서 열처리를 함에 따라 유리한 후 실투화해서 접착부를 형성했다. 그러나 이러한 종래의 유리는 상기와 같이 고온도의 열처리가 요구되는 바, 점점 고도화되고 열에 민감한 IC칩의 접착용으로 사용하기에는 부적합하였다.Conventionally, heat-permeable glass powders of PbO-B 2 O 3 -ZnO-SiO 2 type have been used for hermetic adhesion of alumini ceramic package of IC, which is advantageous by heat treatment at 480 ~ 500 ℃ and then devitrified Formed. However, such a conventional glass is required to be heat-treated at a high temperature as described above, it is not suitable for use in the bonding of increasingly sophisticated and heat-sensitive IC chip.

따라서, 본 발명의 목적은 430℃ 정도의 저온 열처리에 의해 유동이 일어나서 알루미나 세라믹스에 대해 기밀하게 접착부를 형성하고, 알루미나 세라믹스 및 전극으로 사용된 합금리드선에 적합한 열팽창계수를 가지며 접착 후 리드선의 도금공정에서 산처리에 의한 접착유리의 부식이 되지 않을 뿐아니라 도금된 리드선 사이가 통전되는 도금브리징이 발생하지 않는 등 IC용 알루미늄 세라믹팩케이지의 접착에 요구되는 제특성을 충분히 만족시켜주는 접착용 유리조성물을 제공하는데 있다.Therefore, an object of the present invention is to flow by a low temperature heat treatment of about 430 ℃ to form an airtight adhesive portion for alumina ceramics, and has a thermal expansion coefficient suitable for the alloy lead wire used as alumina ceramics and electrodes, the plating process of the lead wire after adhesion Adhesion glass composition that satisfies the characteristics required for the adhesion of the aluminum ceramic package for IC, such as not to corrode the adhesive glass by acid treatment and to conduct plating bridging between the plated lead wires. To provide.

이하, 본 발명을 상세히 설명하면 다음과 같다.Hereinafter, the present invention will be described in detail.

본 발명은 PbO-B2O3-ZnO-SiO2계 저융점 유리분말과 필러로 이루어진 접착용 유리조성물에 있어서, (가) PbO 75~87중량%와 B2O36~15중량%, ZnO 2~7중량%, SiO20.5~2중량%, Al2O30.5~2중량%로 이루어진 저융점 유리분말 50~80중량%와, (나) 윌레마이트(2ZnO·SiO2), β-유크

Figure kpo00001
타이트(Li2O·Al2O3·2SiO2), 지르콘(ZrO2·SiO2), 티탄산연(PbO·TiO2), 산화주석(SnO2), 코디에라이트(2MgO·2Al2O3·5SiO2)중에서 선택된 어느 하나 또는 그 이상에, 열팽창계수가 40∼50×10-7/℃인 저팽창성 결정화 유리분말 3~50중량%가 포함되어 있는 내화물 필러 20 내지 50중량%로 이루어진 것을 특징으로 하는 접착용 유리조성물인 것이다.The present invention relates to a glass composition for adhesion composed of PbO-B 2 O 3 -ZnO-SiO 2 -based low melting point glass powder and filler, (A) 75 ~ 87% by weight of PbO and 6 ~ 15% by weight of B 2 O 3 , 50 to 80% by weight of low melting glass powder consisting of 2 to 7% by weight of ZnO, 0.5 to 2% by weight of SiO 2, and 0.5 to 2% by weight of Al 2 O 3 , (B) Willemite (2ZnO.SiO 2 ), β -Yuk
Figure kpo00001
Tight (Li 2 O · Al 2 O 3 · 2SiO 2 ), zircon (ZrO 2 · SiO 2 ), lead titanate (PbO · TiO 2 ), tin oxide (SnO 2 ), cordierite (2MgO · 2Al 2 O 3 5 to 20% by weight of a refractory filler containing 3 to 50% by weight of low-expansion crystallized glass powder having a coefficient of thermal expansion of 40 to 50 × 10 −7 / ° C. in any one or more selected from 5 SiO 2 ). It is an adhesive glass composition characterized by.

이하, 본 발명을 더욱 상세히 설명하면 다음과 같다.Hereinafter, the present invention will be described in more detail.

본 발명에 따른 접착용 유리조성물은 저융점 유리분말과 내화물 필러로 이루어진다. 저융점 유리분말의 조성물은 PbO 75~87중량%, B2O36~15중량, ZnO 2~7중량%, SiO20.5∼2중량%, Al2O30.5~2중량%로 이루어진다.Adhesive glass composition according to the present invention consists of a low melting point glass powder and a refractory filler. The composition of the low melting glass powder consists of 75 to 87% by weight of PbO, 6 to 15% by weight of B 2 O 3 , 2 to 7% by weight of ZnO, 0.5 to 2% by weight of SiO 2 , and 0.5 to 2% by weight of Al 2 O 3 .

이와 같이 저융점 유리분말의 조성비율의 한정이유는 PbO가 75중량% 이하이면 유리의 전이점이 높게 되어 저온에서 접착이 어렵게 되고 또한 실투가 발생할 염려가 있고, PbO가 87중량%이상이면 유리의 열팽창계수가 크게 된다. B2O3가 6중량% 이하이면 유리용융시 실투가 발생되기 쉽고, B2O3가 15중량% 이상이면 유리의 전이점이 높게 되어 저은에서 접착이 어렵게 된다.As such, the reason for limiting the composition ratio of the low melting glass powder is that when the PbO is 75% by weight or less, the transition point of the glass becomes high, so that it is difficult to bond at low temperatures, and devitrification may occur. The coefficient becomes large. When B 2 O 3 is 6% by weight or less, devitrification is likely to occur during glass melting, and when B 2 O 3 is 15% by weight or more, the transition point of the glass becomes high and adhesion becomes difficult at low silver.

또한 ZnO가 2중량% 이하이면 유리이 내후성이 저하되고 ZnO가 7중량% 이상이면 유리의 결정화 속도가 빠르게 될 뿐아니라 유리용융시 실투가 발생하기 쉽다. SiO2와 Al2O3는 유리의 강도를 증가시키기 위하여 2중량% 이내에서 사용하였으며, 2중량% 이상에서는 유리의 유동성이 저하된다.In addition, when the ZnO is 2% by weight or less, the glass has poor weather resistance, and when the ZnO is 7% by weight or more, the crystallization rate of the glass is not only high, but also devitrification occurs during the melting of the glass. SiO 2 and Al 2 O 3 were used within 2% by weight in order to increase the strength of the glass, the flowability of the glass is lowered at 2% by weight or more.

상기 저융점 유리분말의 연화점은 350℃ 부근으로, 저온도에서도 열처리함에 따라 충분히 유동하고 비정질 유리상태에서 기밀한 접착을 할 수 있지만 평균 열팽창계수가 110∼120×-7/℃의 열팽창계수를 가지는 알루미나 세라막스 재료에는 접착부에 응력이 발생해서 기밀한 접착을 할 수가 없기 때문에 본 발명에서는 상기 저융점 유리분말에 대해 저팽창의 무기 내화물 첨가제인 필러를 20∼50중량% 첨가하게 된다.The softening point of the low-melting-point glass powder is around 350 ° C., and can be sufficiently flowed by heat treatment even at low temperatures, and can be hermetically bonded in an amorphous glass state, but has an average thermal expansion coefficient of 110 to 120 × -7 / ° C. In the present invention, 20-50% by weight of a filler, which is a low-expansion inorganic refractory additive, is added to the low-melting-point glass powder because the alumina ceramax material is stressed at the bonding portion to prevent hermetic bonding.

본 발명에 사용된 내화물 필러로서는 β-유크

Figure kpo00002
타이트(Li2O·Al2O3·SiO3), 지르콘(ZrNO2·SiO2), 티탄산염(PbO·TiO2), 윌레마이트(2ZnO·SiO2), 산화주석(SnO2), 코디에라이트(2MgO·2Al2O3·5SiO2) 중에서 선택된 어느 하나 또는 이 이상에, 열팽창계수자 40~50×10-7/℃인 저팽창성 결정화 유리분말 3∼50중량%로 이루어진다. 상기 내화물 필러에서 저팽창성 유리분말의 혼합량을 한정한 이유는 3중량% 미만이면 접착강도 증대의 효과가 없고, 50중량% 이상이면 저온에서 유동성이 저하되어 접착이 어렵게 되기 때문이다.As the refractory filler used in the present invention, β-yuk
Figure kpo00002
Tight (Li 2 O · Al 2 O 3 · SiO 3 ), Zircon (ZrNO 2 · SiO 2 ), Titanate (PbO · TiO 2 ), Willemite (2ZnO · SiO 2 ), Tin oxide (SnO 2 ), Cody erayi agent (2MgO · 2Al 2 O 3 · 5SiO 2) in any one or more selected from a thermal expansion coefficient chair 40 ~ 50 × 10 -7 / ℃ is made of a low-expansion crystallized glass powder, 3-50% by weight. The reason for limiting the mixing amount of the low-expansible glass powder in the refractory filler is that less than 3% by weight has no effect of increasing the adhesive strength, and if it is 50% by weight or more, fluidity is lowered at low temperatures, making the adhesion difficult.

이때 저팽창성 결정화 유리분말의 제조방법은 먼저 ZnO 62중량%, B2O322.5중량%, SiO29.5중량%, SiO29.5중량%, SnO21.5중량%, PbO 4중량%, CeO20.5중량%를 평량 혼합하고, 이것을 백금도가니를 사용하여 1400℃에서 용융한 후, 일정크기의 몰드로 성형한 다음, 이것을 800℃에서 30분간 열처리하고, 열처리된 시편을 볼밀로 분쇄하여 150메쉬로 체가름하면 된다.At this time, the low-expansion crystallized glass powder manufacturing method is first ZnO 62% by weight, B 2 O 3 22.5% by weight, SiO 2 9.5% by weight, SiO 2 9.5% by weight, SnO 2 1.5% by weight, PbO 4% by weight, CeO 2 0.5 The weight percent is mixed in a basis weight, which is melted at 1400 ° C. using a platinum crucible, and then molded into a mold of a predetermined size. You can do that.

이하, 본 발명에 대한 실시예를 들어보면 다음과 같다.Hereinafter, examples of the present invention will be described.

실시예 1∼6Examples 1-6

PbO, B2O3, ZnO2, Al2O3, SiO2를 다음 표 1과 같은 비율로 혼합하여 백금도가니에서 950℃, 30분간 용융하고 이 용융 조성물을 판상으로 성형한 다음, 볼밀을 사용하여 분쇄하고 150메쉬로 체가름하므로서 A형 및 B형 저융점 유리분말을 제조한다.PbO, B 2 O 3 , ZnO 2 , Al 2 O 3 , SiO 2 were mixed in the ratio as shown in Table 1 below, melted at 950 ° C. for 30 minutes in a platinum crucible, and the molten composition was formed into a plate, and then a ball mill was used. By grinding and sieving to 150 mesh, A and B low melting glass powders are prepared.

[표 1]TABLE 1

Figure kpo00003
Figure kpo00003

이렇게 하여 얻어진 저융점 유리분말에다, 내화물 필러를 혼합하되 이때 저융점 유리분물과 내화물 필러의 조성비율과, 내화물 필러의 구성성분은 다음 표 2와 같이 한다.The refractory filler is mixed with the low melting glass powder thus obtained, and the composition ratio of the low melting glass powder and the refractory filler and the components of the refractory filler are shown in Table 2 below.

이어서, 제조된 접착용 저융점 유리분맡이 IC용 알루미나 세라믹팩케이지 접착에 적합한가를 판단하기 위하여 다음과 같은 항목을 측정하여 그 결과를 표 2에 나타내었다.Subsequently, the following items were measured in order to determine whether the low-melting-point glass bed IC for bonding the alumina ceramic package was prepared, and the results are shown in Table 2.

항목별 측정방법으로는 전이점은 실시예 1~6의 각각의 시료 1gr을 처해서 시차 열분석기(SHIMAZU DT40 기종)로 실온에서 10℃/분의 승온 속도로 온도를 상승시켜 열분석곡선을 구하고, 이 곡선에서 나타나는 최초의 흡열개시 온도를 전이점, 두번개 흡열개시 온도를 연화점으로 했다.In the item-specific measurement method, the transition point was obtained by taking 1gr of each sample of Examples 1 to 6, and using a differential thermal analyzer (SHIMAZU DT40), raising the temperature at a temperature increase rate of 10 ° C / min from room temperature to obtain a thermal analysis curve. The first endothermic start temperature shown in this curve was the transition point and the second endothermic start temperature was the softening point.

열팽창계수 측정은 접착용 저융점 유리분말을 봉상으로 압축 성형한 후, 430℃에서 10분 동안 가열하여 얻어진 봉상기료를 RIKART 8140기종을 사용하여 30℃에서부터 300℃까지의 값을 표준물질로 하여 석영을 사용하여 측정하였다.The coefficient of thermal expansion was measured by compressing and molding a low melting glass powder for bonding into rods and then heating it at 430 ° C for 10 minutes using the RIKART 8140 model as a standard material. Measured using quartz.

유동성 측정은 각각의 분말시료를 그의 비중에 해당하는 gr수를 취해 12.5mm의 몰을 사용하여 가압 성형한 후 430℃에서 10분간 열처리하여 그때의 직경을 측정하였다.In the fluidity measurement, each powder sample was gr molded corresponding to its specific gravity, press-molded using a mole of 12.5 mm, and then heat-treated at 430 ° C. for 10 minutes to measure the diameter at that time.

내산성 측정은 일반적으로 IC공정에서 사용하는 방법에 따라 20% H2SO4를 사용해서 70℃에서 10분 동안 침적시켜 침식량을 구했다. 곡강도는 각각의 유리분말 시료를 사각몰드(40×10×10mm)를 사용하여 가압 성형한 후 430℃에서 10분간 성형하고 이것을 SAND PAPER를 사용하여 연마하여 30×5×5mm의 크기로 만들어 곡강도 측정기인 UTM M/C을 사용하여 3점 강도 측정법을 이용 측정하였다.Acid resistance was generally determined by immersion at 70 ° C. for 10 minutes using 20% H 2 SO 4 , depending on the method used in the IC process. The bending strength of each glass powder sample was formed by pressure molding using a square mold (40 × 10 × 10mm), and then molded at 430 ° C for 10 minutes and polished using SAND PAPER to make a size of 30 × 5 × 5mm. It was measured using the three-point strength measurement method using the UTM M / C.

[표 2]TABLE 2

Figure kpo00004
Figure kpo00004

이와 같이 본 발명에 따른 접착용 유리조성물은 비교적 저온의 열처리에 의해서도 유동이 일어나서 알루미나 세라믹스에 대해 기밀하게 접착부를 형성하고, 알루미나 세라믹스 및 전극으로 사용된 합금리드선에 적합한 열팽창계수를 가지고 있으며, 접착후 리드선의 도금공정에서 산처리에 의한 접착유리의 부식이 일어나지 않을 뿐 아닐 도금된 리드선 사이가 통전되는 도금브리징이 발생하지 않아서 특히 IC용 알루미나 세라믹 팩케이지의 접착에 유용한 것이다.As described above, the glass composition for adhesion according to the present invention is formed even by a relatively low temperature heat treatment to form an airtight seal portion with respect to alumina ceramics, and has a coefficient of thermal expansion suitable for alumina ceramics and alloy lead wires used as electrodes. It is particularly useful for bonding alumina ceramic package for IC because the plating process of lead wire does not cause corrosion of adhesive glass by acid treatment and plating bridging between plated lead wires does not occur.

Claims (2)

PhO-B2O3-ZnO-SiO2계 저융점 유리분말과 필러로 이루어진 접착용 유리조성물에 있어서, (가) PhO 75~87중량%와 B2O36~15중량%, ZnO 2∼7중량%, SiO20.5~2중량%, Al2O30.5~2중량%로 이루어진 저융점 유리분말 50~80중량%와, (나) 윌레마이트(2ZnO·SiO2), β-유크릴타이트(Li2O·Al2O3·2SiO2), 지르콘(ZrO2·SiO2), 티탄산염 (PbO·TiO2), 산화주석(SNO2), 코디에라이트(2MgO·2Al2O3·5SiO2)중에서 선택된 어느 하나 또는 그 이상에 열팽창계수가 40-50×10-7/℃인 저팽창성 결정화 유리분말 3~50중량%가 포함되어 있는 내화물필러 20 내지 50중량%로 이루어진 것을 특징으로 하는 접착용 유리조성물.Adhesion glass composition consisting of PhO-B 2 O 3 -ZnO-SiO 2 based low melting glass powder and filler, comprising: (a) 75 to 87% by weight of PhO, 6 to 15% by weight of B 2 O 3 , and ZnO 2 to 50-80% by weight of low melting glass powder consisting of 7% by weight, 0.5-2% by weight of SiO 2, 0.5-2% by weight of Al 2 O 3 , (B) Willemite (2ZnO.SiO 2 ), β-eucrylic Tight (Li 2 O · Al 2 O 3 · 2SiO 2 ), Zircon (ZrO 2 · SiO 2 ), Titanate (PbO · TiO 2 ), Tin Oxide (SNO 2 ), Cordierite (2MgO · 2Al 2 O 3 5 to 20% by weight of a refractory filler containing 3 to 50% by weight of low-expansion crystallized glass powder having a coefficient of thermal expansion of 40-50 × 10 −7 / ° C. in any one or more selected from 5SiO 2 ). Adhesive glass composition made of. 제1항에 있어서, 상기 괼러에 함유되는 저펑창성 결정화 유리분말은 ZnO 62중량%, B2O322.5중량%, SiO29.5중량%, SnO21.5중량%, PbO 4중량% 및 CeO20.5중량%를 1.400℃에서 용융, 몰딩하고, 400℃에서 30분 열처리한 후, 150메쉬로 분쇄한 것임을 특징으로 하는 접착용 유리조성물.According to claim 1, wherein the low crystalline crystallized glass powder contained in the muller is ZnO 62% by weight, B 2 O 3 22.5% by weight, SiO 2 9.5% by weight, SnO 2 1.5% by weight, PbO 4% by weight and CeO 2 0.5 A glass composition for adhesion, characterized in that the molten, molded by weight at 1.400 ℃, heat-treated at 400 ℃ 30 minutes, and then pulverized into 150 mesh.
KR1019900014143A 1990-09-07 1990-09-07 Glass solders KR950004481B1 (en)

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