KR950004477B1 - Glass solders - Google Patents
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- KR950004477B1 KR950004477B1 KR1019900003237A KR900003237A KR950004477B1 KR 950004477 B1 KR950004477 B1 KR 950004477B1 KR 1019900003237 A KR1019900003237 A KR 1019900003237A KR 900003237 A KR900003237 A KR 900003237A KR 950004477 B1 KR950004477 B1 KR 950004477B1
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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
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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
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- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
Description
본 발명은 알루미나에 대해 기밀한 접착성을 갖는 저융점 유리조성물에 관한 것으로서, 더욱 상세하게는 비교적 저온에서 열처리를 하더라도 비실투상태에서 접착가능하고, 특히 알루미나와 부합되는 열팽창계수를 가지고 있으며, 접착성, 내열성, 내수성, 내산성, 절연성, 유전율 등 제특성이 우수한 신규 조성의 저융점 유리조성물에 관한 것이다.The present invention relates to a low melting glass composition having an airtight adhesion to alumina, and more particularly, even if heat treatment at a relatively low temperature can be bonded in an devitrification state, in particular has a coefficient of thermal expansion consistent with alumina, The present invention relates to a low melting glass composition having a novel composition having excellent properties such as resistance, heat resistance, water resistance, acid resistance, insulation, and dielectric constant.
종래의 IC용 알루미나질 패키지를 접착시키는데에는 PbO-B2O3-ZnO계의 결정성 저융점 유리가 사용되었는 바, 이러한 유리조성물은 약 450℃의 온도로 열처리를 하면 유리화되고 결정되어 알루미나의 열팽창계수와 부합되어 접착부를 형성시킬 수가 있었다.PbO-B 2 O 3 -ZnO-based crystalline low melting glass was used to bond the alumina package for the conventional IC. Such glass compositions are vitrified and crystallized when heat treated at a temperature of about 450 ° C. The adhesive part could be formed in accordance with the coefficient of thermal expansion.
그러나, 이와 같은 종래의 유리조성물은 비교적 고온에서 열처리를 함으로 말미암아 IC칩에 열충격을 주게되기 때문에 이를 개선시켜야 할 필요가 있었다.However, such a conventional glass composition has to be improved because it gives thermal shock to the IC chip by heat treatment at a relatively high temperature.
따라서, 본 발명은 상기와 같은 종래의 문제점을 해소하고자 유리분말의 조성을 달리하므로써 비교적 낮은 온도에서 열처리를 하더라도 유동하게 되어 알루미나에 대해 기밀한 접착성을 가지며 제특성도 우수하게 개선된 접착용 저융점 유리조성물을 제공하는데 그 목적이 있다.Therefore, the present invention is to solve the conventional problems as described above by varying the composition of the glass powder, even if the heat treatment at a relatively low temperature flows to the airtight adhesiveness to the alumina has excellent properties and excellent low melting point for adhesion The purpose is to provide a glass composition.
이하, 본 발명을 상세히 설명하면 다음과 같다.Hereinafter, the present invention will be described in detail.
본 발명은 PbO-B2O3-ZnO계의 접착용 유리조성물에 있어서, 그 유리분말의 조성이 PbO 70~87중량%, B2O36~15중량%, ZnO 2~12중량%, SiO20.5~3중량% 및 Al2O30.5∼3중량%로 이루어진 유리분말이 70~87중량% 함유되어 있고, SnO2를 고용시킨 윌레마이트(2ZnO·SiO2)가 5~50중량%로 함유되어 있는 것을 특징으로 한다.In the present invention, PbO-B 2 O 3 -ZnO-based glass composition for adhesion, the composition of the glass powder is 70 to 87% by weight of PbO, 6 to 15% by weight of B 2 O 3 , ZnO 2 to 12% by weight, 70 to 87% by weight of glass powder composed of 0.5 to 3% by weight of SiO 2 and 0.5 to 3% by weight of Al 2 O 3 , and 5 to 50% by weight of Willemite (2ZnO.SiO 2 ) containing SnO 2 It is characterized by containing.
이와 같은 본 발명을 더욱 상세히 설명하면 다음과 같다.Referring to the present invention in more detail as follows.
본 발명에서는 종래의 PbO-B2O3-ZnO의 접착용 유리조성물의 조성중에 SnO2를 고용시킨 윌레마이트를 휠러(filler)로서 첨가하므로서 저온에서 유동성이 향상되고 IC패키지에 대해 우수한 접착력을 가지는 특징이 있다.In the present invention, the flowability at low temperature is improved and excellent adhesion to the IC package is achieved by adding Willemite in which SnO 2 is dissolved as a filler in the composition of the conventional glass composition for bonding PbO-B 2 O 3 -ZnO. There is a characteristic.
이러한 본 발명의 조성에서 PbO 성분이 유리분말 조성에 있어서 70중량% 보다 적으면 유리의 전이점이 높아지게 되어 저온에서의 접착성이 나아지게 되고 87중량% 보다 많으면 유리의 열팽창계수가 높아져서 좋지 않게 된다.In the composition of the present invention, when the PbO component is less than 70% by weight in the glass powder composition, the transition point of the glass is increased to improve the adhesion at low temperature, and when it is more than 87% by weight, the thermal expansion coefficient of the glass is not good.
또한, B2O3가 6중량% 보다 적은량은 경우에는 유리용융시에 실투가 발생하게 되고, 15중량% 보다 많으면 유리의 전이점이 높아져서 저온접착성이 저하된다.In the case where the amount of B 2 O 3 is less than 6% by weight, devitrification occurs at the time of melting the glass. When the amount of B 2 O 3 is more than 15% by weight, the transition point of the glass is increased to lower the low temperature adhesiveness.
또한 ZnO의 경우 그 함량이 2중량% 보다 적으면 유리의 내후성이 저하될 뿐아니라 유리의 전이점 및 연화점이 높아져서 좋지 않게 되고, 12중량% 보다 많으면 유리의 결정화속도가 너무 빨라 좋지 않고 유리용융시 실투가 발생하기 쉬우므로 바람직하지 못하다.In addition, in the case of ZnO, when the content is less than 2% by weight, not only the weather resistance of the glass is lowered, but also the transition point and softening point of the glass are not good, and when it is more than 12% by weight, the crystallization rate of the glass is not so fast and the glass melting time is not good. It is not preferable because devitrification is likely to occur.
그리고, SiO2와 Al2O3는 각각 0.5 내지 3중량%로 함유되어 있는 것이 좋은데, 만일 3중량% 이상으로 함유되는 경우에는 유리의 유동성이 저하될 뿐만아니라 유리의 용융 온도가 높아져서 본 발명의 목적을 달성할 수가 없게 된다.SiO 2 and Al 2 O 3 are preferably contained in an amount of 0.5 to 3% by weight, but if contained in an amount of 3% by weight or more, the flowability of the glass is lowered and the melting temperature of the glass is increased so that You will not be able to achieve your purpose.
한편, 본 발명에서 사용하는 윌레마이트는 SnO2가 고용되어 있어야 하는데, 이러한 SnO2가 고용된 윌레마이트는 휠러인 내화물 첨가제로서 사용되며, 이 성분이 전체 조성물에 대해 5중량% 보다 적게 함유되어 있으면 알루미나에 알맞는 열팽창계수를 얻을 수 없고 접착성 향상을 기대할 수 없게 되며, 50중량% 보다 과량으로 함유되어 있으면 유리의 유동성이 저하될 뿐아니라 접착시 접착온도가 높게 되어 IC에 영향을 주고 또한 접착성이 저하되므로 바람직하지 못하다.On the other hand, the Willemite used in the present invention should be dissolved in SnO 2 , such WillOmite in which SnO 2 is dissolved is used as a refractory additive that is a wheeler, if the component is contained less than 5% by weight based on the total composition The thermal expansion coefficient suitable for alumina cannot be obtained, and the improvement of adhesion cannot be expected. If it is contained in excess of 50% by weight, the fluidity of the glass is not only decreased, but the adhesion temperature at the time of adhesion increases and affects the IC. It is unpreferable since property falls.
또한, 이때 윌레마이트에 고용되는 SnO2의 량은 최소한 전체 윌레마이트 성분에 대하여 1∼60중량%로 함유되어 있어야 한다.At this time, the amount of SnO 2 dissolved in the willemite should be contained at least 1 to 60% by weight based on the total willemite component.
이렇게하여 만들어진 SnO2고용 윌레마이트의 열팽창계수는 10∼20×10-7/℃로서, 이것을 상기 유리분말에 대해 5∼50중량% 사용하면 알루미나의 열팽창계수 68∼72×10-7/℃와 유사한 열팽창계수가 얻어지기 때문에 이것을 사용하게 되면 IC패키지에 대한 접착성이 우수하게 된다.The thermal expansion coefficient of the SnO 2 solid solution willemite produced in this way is 10-20 × 10 -7 / ° C, and when 5-50% by weight of the glass powder is used, the thermal expansion coefficient of alumina is 68-72 × 10 -7 / ° C and Since similar thermal expansion coefficients are obtained, the use of this leads to excellent adhesion to the IC package.
이와같은 휠러를 혼합 사용하는 경우에는 65∼75×10-7/℃ 정도의 열팽창계수를 가지는 저융점 유리분말이 얻어지게 되는데, 이것은 알루미나의 열팽창계수와 일치하는 것이다.When such wheelers are mixed, a low melting glass powder having a coefficient of thermal expansion of about 65 to 75 × 10 −7 / ° C. is obtained, which is consistent with the coefficient of thermal expansion of alumina.
이와 같이 본 발명에 따라 얻어지는 유리조성물은 400∼430℃의 온도에서 약 10여분 동안만 열처리하게 되면 적절하게 유동되어 알루미나에 대해 기밀하게 접착되는 접착특성을 가지게 되며, 또 우수한 내열성 및 내산성을 가지므로 특히, IC용 알루미나 패키지 접착에 사용시 제특성을 만족시킬 수 있는 저융점 유리조성물인 것이다.As described above, the glass composition obtained according to the present invention has an adhesive property to be properly flowed and hermetically adhered to alumina when heat treated only for about 10 minutes at a temperature of 400 to 430 ° C., and also has excellent heat and acid resistance. In particular, it is a low melting glass composition that can satisfy various properties when used for bonding alumina package for IC.
이러한 본 발명을 실시예에 의거 더욱 상세히 설명하겠는 바, 다음의 실시예에 의해 본 발명이 한정되는 것은 아니다.Although this invention is demonstrated in detail based on an Example, this invention is not limited by the following Example.
실시예 1~5Examples 1-5
PbO, B2O3, ZnO, Al2O3, SiO2를 다음 표에서와 같은 각각의 조성으로 혼합하여 백금도가니에서 900℃ 정도의 온도에서 30분간 용융시키고, 이 용융 유리조성물을 몰드를 사용하여 판상으로 성형한 후 볼밀을 사용해서 87분간 분쇄하고 150메쉬체로 체갈음한 것을 조성유리분말로 하였다.PbO, B 2 O 3 , ZnO, Al 2 O 3 , and SiO 2 were mixed in the respective compositions as shown in the following table and melted at a temperature of about 900 ° C. in a platinum crucible for 30 minutes, and the molten glass composition was used as a mold. After molding into a plate shape by using a ball mill, it was pulverized for 87 minutes and sieved to 150 mesh sieve as a composition glass powder.
다른 한편으로는 휠러로서 윌레마이트(2ZnO·SiO2)에 SnO2를 무게비로 윌레마이트 : SnO2=24 : 20으로 혼합한 후 1450℃에서 2시간 동안 소성한 다음, 일정크기가 되도록 손으로 알루미나 유발을 사용하여 분쇄하고 볼밀을 사용하여 80분간 분쇄한 후, 이것을 150메쉬체로 체갈음한 것을 저팽창성 첨가제로 하였다 이렇게 하여 만들어진 저융점 유리분말과 저팽창성 내화물 휠러를 표의 혼합비율로 평량·혼합해서 저융점 유리분말을 얻었다.On the other hand wilre mite (2ZnO · SiO 2) in wilre boehmite the SnO 2 in the weight ratio as Wheeler alumina hand to a fired for two hours at 1450 ℃ then a solution of 20, the following, a certain size: SnO 2 = 24 After grinding using a mortar and pulverizing for 80 minutes using a ball mill, the sifted into 150 mesh sieves is used as a low-expansion additive. A low melting glass powder was obtained.
얻어진 저융점 유리분말을 IC용 알루미나 패키지 기밀접착에 적합한가를 판단하기 위해 다음과 같은 측정방법을 사용하여 물성을 특정해서 그 결과를 다음 표에 나타내었다.In order to determine whether the obtained low melting glass powder is suitable for hermetic adhesion of the alumina package for IC, the physical properties were specified using the following measuring method, and the results are shown in the following table.
항목별 측정방법으로는 전이점은 실시예 1~5의 각각의 시료 1g을 취해서 시차열 분석기(SHIMAZU DT40기종)로 실온에서 10℃/min의 송온속도로 온도를 상승시켜 열분석곡선을 구하고 곡선에서 나타나는 최초의 흡열개시온도를 전이점으로 했다.As the measurement method for each item, the transition point was obtained by taking 1 g of each sample of Examples 1 to 5 and increasing the temperature at a temperature of 10 ° C./min at room temperature with a differential thermal analyzer (SHIMAZU DT40 model) to obtain a thermal analysis curve. The first endothermic start temperature shown at was taken as the transition point.
열팽창계수는 저융점 유리분말 시료를 봉상으로 압축성형하고 430℃에서 10분동안 머플로를 사용하여 가열한 후, 얻어진 봉상시료를 RIKAKU 8140기종을 사용하여 30℃에서부터 250℃까지의 값을 표준물질로 석영유리를 사용하여 측정하였다.The coefficient of thermal expansion was obtained by compression molding a low melting glass powder sample into a rod and heating it with muffle for 10 minutes at 430 ° C, and then using the RIKAKU 8140 model to obtain the rod-shaped sample from 30 ° C to 250 ° C. It was measured using quartz glass.
유동성 측정은 각각의 분말시료를 그의 비중에 해당하는 g수를 취해 ψ12.5mm의 몰드를 사용하여 원주상으로 가압성형한 후, 430℃에서 10분간 열처리하여 유동성을 측정하였다. 유전율은 20℃ 1MHz에서 HEWLETT PACKARD FREQUENCY LCRMETER를 사용하여 측정하였다.In the fluidity measurement, each powder sample was g-number corresponding to its specific gravity, press-molded in a circumferential shape using a mold of 12.5 mm, and then heat-treated at 430 ° C for 10 minutes to measure fluidity. Dielectric constant was measured using HEWLETT PACKARD FREQUENCY LCRMETER at 20 ℃ 1MHz.
내산성은 일반적으로 IC패키지 제조공정에서 사용하는 방법에 따라 20% H3SO4를 사용해서 70℃에서 10분동안 침식량을 구했다.Acid resistance was generally determined by erosion for 10 minutes at 70 ° C. using 20% H 3 SO 4 , depending on the method used in the IC package manufacturing process.
곡강도는 각각의 유리분말을 사각몰드(50×15×15mm)를 사용하여 가압성형한 후 430℃에서 10분간 성형하고, 이것을 사포(SAND PAPER)를 사용하여 40×10×5mm 크기로 만들어 곡강도 측정기기인 UTM M/C를 사용하여 3점 강도 측정법을 이용 측정하였다.The bending strength of each glass powder is press-molded by using a square mold (50 × 15 × 15mm), and then molded at 430 ° C for 10 minutes, and this is made into 40 × 10 × 5mm size by using sand paper and the bending strength measuring instrument. It was measured using a three-point intensity measurement method using a UTM M / C attributable.
[표 1]TABLE 1
Claims (2)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1019900003237A KR950004477B1 (en) | 1990-03-12 | 1990-03-12 | Glass solders |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1019900003237A KR950004477B1 (en) | 1990-03-12 | 1990-03-12 | Glass solders |
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| Publication Number | Publication Date |
|---|---|
| KR910016635A KR910016635A (en) | 1991-11-05 |
| KR950004477B1 true KR950004477B1 (en) | 1995-05-01 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| KR1019900003237A KR950004477B1 (en) | 1990-03-12 | 1990-03-12 | Glass solders |
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| Country | Link |
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| KR (1) | KR950004477B1 (en) |
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1990
- 1990-03-12 KR KR1019900003237A patent/KR950004477B1/en not_active IP Right Cessation
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| Publication number | Publication date |
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| KR910016635A (en) | 1991-11-05 |
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