KR100246720B1 - Method of preparing paste for resistor for lcr co-firing, method of manufacturing thick film using it - Google Patents

Method of preparing paste for resistor for lcr co-firing, method of manufacturing thick film using it Download PDF

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KR100246720B1
KR100246720B1 KR1019970049103A KR19970049103A KR100246720B1 KR 100246720 B1 KR100246720 B1 KR 100246720B1 KR 1019970049103 A KR1019970049103 A KR 1019970049103A KR 19970049103 A KR19970049103 A KR 19970049103A KR 100246720 B1 KR100246720 B1 KR 100246720B1
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weight
resistor
paste
thick film
powder
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KR19990026804A (en
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박지애
이동아
김구대
이홍림
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박호군
한국과학기술연구원
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01C—RESISTORS
    • H01C17/00—Apparatus or processes specially adapted for manufacturing resistors
    • H01C17/06—Apparatus or processes specially adapted for manufacturing resistors adapted for coating resistive material on a base
    • H01C17/065—Apparatus or processes specially adapted for manufacturing resistors adapted for coating resistive material on a base by thick film techniques, e.g. serigraphy
    • H01C17/06506—Precursor compositions therefor, e.g. pastes, inks, glass frits
    • H01C17/06513—Precursor compositions therefor, e.g. pastes, inks, glass frits characterised by the resistive component
    • H01C17/06526—Precursor compositions therefor, e.g. pastes, inks, glass frits characterised by the resistive component composed of metals
    • 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
    • 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
    • C04B35/14—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 silica
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01C—RESISTORS
    • H01C17/00—Apparatus or processes specially adapted for manufacturing resistors
    • H01C17/06—Apparatus or processes specially adapted for manufacturing resistors adapted for coating resistive material on a base
    • H01C17/065—Apparatus or processes specially adapted for manufacturing resistors adapted for coating resistive material on a base by thick film techniques, e.g. serigraphy
    • H01C17/06506—Precursor compositions therefor, e.g. pastes, inks, glass frits
    • H01C17/06513—Precursor compositions therefor, e.g. pastes, inks, glass frits characterised by the resistive component
    • H01C17/06553—Precursor compositions therefor, e.g. pastes, inks, glass frits characterised by the resistive component composed of a combination of metals and oxides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01C—RESISTORS
    • H01C17/00—Apparatus or processes specially adapted for manufacturing resistors
    • H01C17/06—Apparatus or processes specially adapted for manufacturing resistors adapted for coating resistive material on a base
    • H01C17/065—Apparatus or processes specially adapted for manufacturing resistors adapted for coating resistive material on a base by thick film techniques, e.g. serigraphy
    • H01C17/06506—Precursor compositions therefor, e.g. pastes, inks, glass frits
    • H01C17/06513—Precursor compositions therefor, e.g. pastes, inks, glass frits characterised by the resistive component
    • H01C17/0656—Precursor compositions therefor, e.g. pastes, inks, glass frits characterised by the resistive component composed of silicides

Abstract

파이로클로(pyrochlore) 구조인 Pb2Ru2O6.5계의 원료 분말 70중량%와, 결합제(binder) 20중량% 및 유기용매 10중량%를 혼합하거나, 또는 5중량%의 RuO2분말과 95중량%의 유리 프릿트(SiO2-Bi2O3-CaO-Na2O )가 단순 혼합된 원료분말에 위와 같은 결합제 및 유기용매를 혼합하는 방법으로 저항체용 페이스트를 제조하였다.70% by weight of the Pb 2 Ru 2 O 6.5 raw material powder having a pyrochlore structure, 20% by weight binder and 10% by weight organic solvent, or 5% by weight of RuO 2 powder A resistor paste was prepared by mixing a binder and an organic solvent as described above in a raw material powder in which a glass frit (SiO 2- Bi 2 O 3 -CaO-Na 2 O) by weight was simply mixed.

이러한 페이스트를 알루미나, 유전체·자성체기판에 후막의 형태로 처리하고, 그 저항제를 고온·장시간의 열처리로 동시소성하여, 계면이 안정하고 전기적 특성이 양호한 후막저항체를 제조하였다. 또한, 도전상과 절연상의 혼합비율을 조절함으로써, 넓은 저항범위를 가지는 후막 저항체의 조성을 개발하였다.The paste was treated with alumina, a dielectric and magnetic substrate in the form of a thick film, and the resistor was simultaneously fired by a high temperature and a long heat treatment to prepare a thick film resistor having a stable interface and good electrical characteristics. In addition, by adjusting the mixing ratio of the conductive phase and the insulating phase, a composition of a thick film resistor having a wide resistance range was developed.

Description

LCR 동시소성을 위한 저항체용 페이스트 제조방법 및 그를 이용한 후막 저항체 제조방법Resistor paste manufacturing method for LCR co-firing and thick film resistor manufacturing method using the same

본 발명은 LCR (Inductor-Capacitor-Resistor) 동시소성을 위한 고온·장시간 소성용 Ru계 저항체 페이스트의 조성 및 그 제조 방법에 관한 것이다.The present invention relates to a composition of a Ru-based resistor paste for high temperature and long time firing for inductor-capacitor-resistor (LCR) co-firing and a method of manufacturing the same.

최근 전자 산업에서 각종 기기의 소형화에 따라 관련 전자 부품들의 경박단소화(經薄短小化)는 필수적이다. 이러한 회로의 소형화를 위한 고기능 LCR 복합소자를 구성하기 위해서 Ru계 저항체 페이스트는 다음과 같은 특성이 요구된다.With the recent miniaturization of various devices in the electronic industry, it is essential to reduce the thickness and thinning of related electronic components. In order to construct a high-performance LCR composite device for miniaturizing such a circuit, the Ru-based resistor paste requires the following characteristics.

1) 기판을 구성하는 유전체, 자성체와의 계면이 안정할 것.1) The interface between the dielectric and magnetic material forming the substrate should be stable.

2) 고온·장시간의 소성이 가능하고, 전기적 특성이 양호할 것.2) High temperature and long time firing should be possible and electrical characteristics should be good.

칩 저항기, 혼성집적회로 등에 사용되는 후막 저항체는, 절연상을 이루는 유리 프릿트(frit) 분말과 도전상을 이루는 금속 산화물을 혼합하여, 그 비율에 따라 원하는 저항값을 얻을 수 있는 복잡한 비평형계이다. 도전상으로는 루틸(rutile, 고산화티탄) 구조의 RuO2또는 파이로클로(pyrochlore) 구조의 Bi2Ru2O7, Pb2Ru2O6+x등이 상용화 되어 있으며, 이들 Ru계 산화물의 특징은 다음과 같다.Thick film resistors used in chip resistors, hybrid integrated circuits, etc., are complex non-equilibrium systems in which a glass frit powder forming an insulating phase and a metal oxide forming a conductive phase are mixed to obtain a desired resistance value according to the ratio thereof. . As the conductive phase, RuO 2 having a rutile (titanium oxide) structure or Bi 2 Ru 2 O 7 having a pyrochlore structure, Pb 2 Ru 2 O 6 + x, and the like are commercially available. Is as follows.

1) 산화물임에도 저항값이 낮다.1) The resistance value is low even though it is an oxide.

2) 유리에 혼합했을때의 저항값 변화가 완만하다.2) The resistance value changes slowly when mixed with glass.

3) 넓은 온도 영역에서 화학적으로 안정하다.3) It is chemically stable in a wide temperature range.

4) 유리와의 젖음성(wettability)이 양호하다.4) Wetability with glass is good.

5) 소성 조건의 의존성이 적고 저항값의 제어가 용이하다.5) Less dependence of firing conditions and easy control of resistance value.

후막 저항체는 일반적으로 알루미나 기판위에 회로 형태대로 인쇄하고, 휘발성 용매를 제거하기 위해 건조시킨 다음, 유리의 연화점 이상에서 약 10분동안 열처리시켜 소결한다. 소성 과정의 초기에는 유기 결합제(vehicle)가 열분해되고, 보다 높은 온도에서 유리상이 연화되어 전도상과 반응하게 된다. 유리가 연화되면서, 유리 입자사이의 공극이 줄어들과, 입자간 거리가 줄어들면서 전도성 입자들은 가까워지게 된다. 가까워진 전도성 입자들은 유리표면에 달라붙게 되고, 소결온도에 도달하면 날카로운 모서리를 가진 유리 입자들이 연화·변형되어 스폰지와 같은 막을 형성하며, 유리 입자의 계면을 따라 전도성 입자들이 축적되어 전도성 경로를 형성하게 된다. 소결후 후막 저항체의 두께는 10∼20 ㎛ 이며, 도전상과 절연상의 혼합비율을 조절함으로써 101∼ 107Ω/□의 저항값을 얻을 수 있다. 넓은 범위의 저항값을 얻을 수 있고, 시편의 준비 및 제조가 용이하기 때문에, 후막 저항체가 널리 사용되고 있다.Thick film resistors are generally printed in circuit form on an alumina substrate, dried to remove volatile solvents, and then sintered by heat treatment for about 10 minutes above the softening point of the glass. At the beginning of the firing process, organic binders are pyrolyzed and at higher temperatures the glass phase softens and reacts with the conductive phase. As the glass softens, the pores between the glass particles decrease, and the distance between the particles decreases, so that the conductive particles become closer. As the conductive particles near each other adhere to the glass surface, when the sintering temperature is reached, the glass particles with sharp edges soften and deform to form a sponge-like film, and conductive particles accumulate along the interface of the glass particles to form a conductive path. do. The thickness of the thick film resistor after sintering is 10 to 20 µm, and a resistance value of 10 1 to 10 7 Ω / □ can be obtained by adjusting the mixing ratio of the conductive phase and the insulating phase. Since a wide range of resistance values can be obtained and the preparation and manufacture of specimens are easy, thick film resistors are widely used.

종래의 후막 저항체용 페이스트는 유리의 연화점 이상의 온도에서 약 10분동안 소결되었는데, 이러한 페이스트는 유전체·자성체의 소성온도인 900 내지 920℃에서 2시간 동안 열처리하는 경우에, 저항체용 페이스트의 전도성 입자가 기판의 내부로 확산되거나 유리상이 휘발되어, 전기적 특성을 가질 수 없는 단점이 있었다.The conventional thick film resistor paste was sintered for about 10 minutes at a temperature above the softening point of the glass. When the paste is heat-treated at 900 to 920 ° C., which is the firing temperature of the dielectric and magnetic material, the conductive particles of the resistor paste Diffusion into the interior of the substrate or volatilization of the glass phase has the disadvantage that it cannot have electrical properties.

본 발명의 목적은 기판을 구성하는 유전체·자성체와 후막의 형태로 처리되는 저항체를 고온·장시간의 열처리로 동시소성하여, 계면이 안정하고 전기적 특성이 양호한 조성의 저항체용 페이스트를 얻는 것이다.SUMMARY OF THE INVENTION An object of the present invention is to simultaneously fire a dielectric material, a magnetic material constituting a substrate, and a resistor processed in the form of a thick film by a high temperature and a long heat treatment to obtain a resistor paste having a stable interface and good electrical properties.

따라서, 본 발명에서는 저항체 페이스트용 초기 분말의 소결온도를 높이기 위하여, 페이스트를 구성하는 절연상 유리 프릿트 중 Al2O3와 SiO2의 양을 증가시켰다.Therefore, in the present invention, in order to increase the sintering temperature of the initial powder for resistor paste, the amounts of Al 2 O 3 and SiO 2 in the insulating glass frit constituting the paste were increased.

제1도는 알루미나 기판에 각 조성의 저항체 페이스트(paste)를 후막 처리하여, 850℃에서 10분간 소결한 시편의 단면을 보여주는 주사형 전자현미경(SEM) 사진 및 Ru(루테늄)를 매핑한 X선 마이크로에널라이즈(EPMA) 사진이다.FIG. 1 is a scanning electron microscope (SEM) photograph showing a cross section of a specimen sintered at 850 ° C. for 10 minutes by thick film-resisting a paste of each composition on an alumina substrate, and X-ray micrographs mapped with Ru (ruthenium). Here's a picture of Analize.

제2도는 알루미나 기판에 각 조성의 저항체를 후막 처리하여 900℃에서 10시간 동안 소결한 시편의 단면을 보여주는 주사형 전자현미경(SEM) 사진 및 Ru를 매핑한 X선 마이크로에널라이즈(EPMA) 사진이다.2 is a scanning electron microscope (SEM) photograph showing a cross section of a specimen sintered at 900 ° C. for 10 hours by thick-film-resisting resistors of each composition on an alumina substrate, and an X-ray microanalysis (EPMA) photograph mapped with Ru. .

제3도는 본 발명에 의한 저항체 페이스트 제조용 초기분말의 X레이 분말회절(XRD) 결과를 나타낸다.3 shows the results of X-ray powder diffraction (XRD) of the initial powder for resistor paste production according to the present invention.

제4도는 알루미나, 자성체 및 유전체 기판에 저항체를 후막 처리하여 동시소성 열처리에 따라 900℃에서 2시간 동안 소결한 시편의 표면을 화학 에칭한 후 X레이 회절기(XRD)로 관찰한 결과를 나타낸다. (각각 모든 조성에서 그림과 같은 경향의 결과를 나타내었고, 이 경우의 저항체 조성은 A1 이다. X레이 회절분석(XRD) 결과 자성체 기판에서는 기판의 성분인 스피넬(spinel) 상이 나타났다.).4 shows the results of observing an X-ray diffractometer (XRD) after chemically etching the surface of a specimen sintered at 900 ° C. for 2 hours according to co-fired heat treatment by a thick film of alumina, magnetic material and dielectric substrate. (Each of the compositions showed the result of the trend as shown in the figure, and the resist composition in this case was A1. X-ray diffraction analysis (XRD) showed that the magnetic substrate had a spinel phase as a component of the substrate.)

이러한 발명의 내용을 실시예를 통하여 상세히 설명하고자 한다.The content of this invention will be described in detail by way of examples.

[실시예]EXAMPLE

도전상이 파이로클로(pyrochlore) 구조인 Pb2Ru2O6.5계인 경우에는, 99.7∼99.9의 순도를 갖는 RuO2, PbO, SiO2, Al2O3, CaO를, 표 1에 나타낸 각 페이스트의 조성에 따라 정확히 평량한 후 분말을 혼합하여, 백금 도가니에 넣고 1000℃, 1050℃에서 3시간 동안 용융한 다음 급냉시켜, 지르코니아 용기(zirconia jar)에 지르코니아 볼 (zirconia ball) 및 증류수와 함께 넣고 48시간 동안 분쇄하여 건조한 후 200 메시(mesh)로 체거름함으로써, 파이로클로(pyrochlore) 구조인 Pb2Ru2O6.5계의 원료 분말을 제조하였다. 이렇게 얻어진 분말 70중량%와, 에틸셀룰로오스(ethyle cellulose)계 결합제(binder) 20중량% 및 α-타피놀(α-terpineol) 10중량%를 혼합한 혼합물을, 3롤 밀(Three Roll Mill)을 사용하여 균일한 페이스트로 제조하였다. 또한 도전상이 루틸구조인 RuO2계인 경우에는, 5중량%의 RuO2분말과 95중량%의 유리 프릿트(SiO2-Bi2O3-CaO-Na2O)를 혼합하여 12시간 동안 볼 밀링(ball milling)하고 200메시(mesh)로 체거름하여 원료분말을 제조한 후에, 위에서와 같은 방법으로 페이스트를 제조하였다. 본 발명에 의한 페이스트 제조용 초기분말의 X선 회절결과가 제 3도에 도시되어 있다. 제3도에서 (a), (b)는 표 1에 나타낸 바와 같은 조성(A1, A2)을 가지는 페이스트용 분말의 X선 회절결과이고, (c)는 RuO2와 유리 프리트 분말을 단순혼합한 페이스트용 초기분말의 X선 회절결과이며, ●, ▲는 각각 RuO2와 Pb2Ru2O6.5를 의미한다.When the conductive phase is a Pb 2 Ru 2 O 6.5 system having a pyrochlore structure, RuO 2 , PbO, SiO 2 , Al 2 O 3 , and CaO having a purity of 99.7 to 99.9 are obtained from each paste shown in Table 1 below. Accurately weigh according to the composition, mix the powder, place it in a platinum crucible, melt for 3 hours at 1000 ° C and 1050 ° C, and then quench it, place it in a zirconia jar with zirconia ball and distilled water. After pulverizing and drying for a period of time to sieve 200 mesh, a raw material powder of Pb 2 Ru 2 O 6.5- based pyrochlore structure was prepared. The mixture obtained by mixing 70% by weight of the powder thus obtained, 20% by weight of ethyl cellulose-based binder and 10% by weight of α-terpineol was mixed with a three roll mill. To make a uniform paste. In addition, in the case of the RuO 2 system having a rutile structure, ball milling was performed by mixing 5 wt% RuO 2 powder and 95 wt% glass frit (SiO 2 -Bi 2 O 3 -CaO-Na 2 O) for 12 hours. After the ball milling and sieving to 200 mesh to prepare a raw powder, a paste was prepared in the same manner as above. X-ray diffraction results of the initial powder for paste production according to the present invention are shown in FIG. In FIG. 3, (a) and (b) show the X-ray diffraction results of the powder for paste having the composition (A 1 , A 2 ) as shown in Table 1, and (c) shows the RuO 2 and glass frit powder as simple. X-ray diffraction results of the mixed initial powder for paste, and ●, ▲ means RuO 2 and Pb 2 Ru 2 O 6.5 respectively.

그 다음으로, 기판위에 전극을 형성하기 위해 은 페이스트(silver paste)를 스크린 프린터에서 인쇄한 후 스크린 자국을 제거하고 일정한 막의 모양을 형성시키기 위하여 상온에서 10분간 레벨링(leveling) 한 후 150℃에서 10분간 건조하였다. 양 전극사이에 저항 페이스트를 위와 동일한 방법으로 인쇄, 건조시켰다. 이렇게 준비된 저항체를 다음과 같이 열처리 하였다.Next, silver paste was printed on a screen printer to form an electrode on the substrate, and then leveled at room temperature for 10 minutes to remove screen marks and to form a uniform film. Dried over minutes. A resist paste was printed and dried between the two electrodes in the same manner as above. The resistor thus prepared was heat treated as follows.

1) 본 발명에 의한 페이스트를 일반적 조성의 페이스트 소결과정을 따라, 알루미나 기판상에 후막 처리하여 소결하는 방법 : 850℃에서 10분간 소결1) A method of sintering a paste according to the present invention by thick film treatment on an alumina substrate according to a paste sintering process having a general composition: Sintering at 850 ° C. for 10 minutes

2) 소결하지 않은(green sheet) 유전체 또는 자성체 기판과의 동시소성 : 300℃, 520℃에서 각각 6시간씩 탈지하여 900℃, 2시간 동안 소결(또는 920℃, 2시간 소결)2) Simultaneous firing with a green sheet dielectric or magnetic substrate: Sintered at 300 ° C and 520 ° C for 6 hours each for sintering at 900 ° C for 2 hours (or 920 ° C for 2 hours)

3) 이미 소결된 유전체 또는 자성체 기판상에 페이스트를 후막 처리한 경우의 소결방법 : 850℃, 10분간 소결3) Sintering method for thick film paste on already sintered dielectric or magnetic substrate: Sintering at 850 ℃ for 10 minutes

위의 방법으로 소결된 후막 저항체의 전기 저항을 측정하여 다음식으로 면저항을 계산하였다.The sheet resistance was calculated by the following formula by measuring the electrical resistance of the thick film resistor sintered by the above method.

Figure kpo00002
Figure kpo00002

W : 저항체의 세로길이W: length of resistor

L : 저항체의 가로길이L: width of resistor

A : 저항체의 가로와 세로의 비A: ratio between width and length of resistor

R : 실제 측정한 저항값R: Actual measured resistance

Rs: 면저항R s : Sheet resistance

각 페이스트의 조성 및 각 실시 예에 의하여 소결된 시편의 제반 특성(면저항)을 표 1에 나타내었다.Table 1 shows the composition of each paste and the overall characteristics (surface resistance) of the specimens sintered according to the examples.

Figure kpo00003
Figure kpo00003

다음의 표 2에는 도전상이 루틸 구조인 RuO2계의 저항체를 알루미나 기판에 후막처리하여 소결한 시편의 특성을 나타내었다.Table 2 below shows the characteristics of the specimen sintered by a thick film of a RuO 2 based resistor having a rutile structure of a conductive phase on an alumina substrate.

Figure kpo00004
Figure kpo00004

위의 실험에서 알 수 있는 바와 같이, 본 발명에 의한 페이스트의 전도상과 절연상의 비율을 조정함으로써, 다양한 저항값을 가지는 저항체를 얻을 수 있다.As can be seen from the above experiment, the resistor having various resistance values can be obtained by adjusting the ratio of the conductive and insulating phases of the paste according to the present invention.

제4도는, 본 발명에 의한 페이스트를 알루미나, 자성체 및 유전체 기판에 후막 처리하고, 그를 900℃에서 2시간동안 열처리한 후의 각 저항체의 X선 회절결과를 도시한다. (a), (b) 및 (c)는 각각 알루미나, 유전체 및 자성체 기판을 사용한 경우이며, ●, ▲는 각각 RuO2와 Pb2Ru2O6.5를 의미한다. 이 결과로부터 고온·장시간의 열처리 후에도 알루미나 기판상에 후막 처리된 저항체가 안정(전도성 입자의 기판확산이나, 유리상 휘발이 없음)하다는 것을 알 수 있으며, 이는 종래의 페이스트를 850℃에서 10분간 열처리 한 것과 동일한 결과이다. 자성체 기판상의 저항체는 열처리 후 Pb2Ru2O6.5의 피크가 없어졌음을 알 수 있는데, 이는 RuO2가 Pb2Ru2O6.5보다 고온에서 안정한 상이기 때문이며, 전도성 입자인 RuO2가 존재하므로 전기적 특성을 띠게 된다. 이에 반하여, 유전체 기판상에서는, 도면에서 RuO2와 Pb2Ru2O6.5가 존재하지 않는 것으로부터 알 수 있듯이, 전도성 입자가 기판내부로 확산되고, 기판내의 프리트(frit)성분과 반응하여 전도성 경로가 형성되지 못한다.4 shows the X-ray diffraction results of the resistors after the paste according to the present invention is subjected to a thick film treatment on an alumina, a magnetic body, and a dielectric substrate and heat-treated at 900 占 폚 for 2 hours. (a), (b) and (c) are cases where alumina, dielectric and magnetic substrates are used, respectively, and? and ▲ denote RuO 2 and Pb 2 Ru 2 O 6.5 , respectively. From this result, it can be seen that even after a high temperature and a long time heat treatment, the resistor coated with a thick film on the alumina substrate is stable (there is no substrate diffusion of conductive particles or glassy volatilization). Same result as that. It can be seen that the resistor on the magnetic substrate had no peak of Pb 2 Ru 2 O 6.5 after heat treatment because RuO 2 is a stable phase at a higher temperature than Pb 2 Ru 2 O 6.5 , and since the conductive particles RuO 2 are present, Will be characterized. In contrast, on the dielectric substrate, as can be seen from the absence of RuO 2 and Pb 2 Ru 2 O 6.5 in the drawing, the conductive particles diffuse into the substrate and react with the frit component in the substrate to form a conductive path. Not formed

본 발명에 의한 저항체용 페이스트를 알루미나, 유전체 또는 자성체 기판에 후막 처리하고, 이를 유전체나 자성체의 소성온도인 고온하에서 장시간동안 열처리하여 동시소성하여, 계면이 안정하고 전기적 특성이 양호하며, 전기적 저항의 범위가 넓은 저항체를 얻을 수 있다. 이는 XRD결과인 제4도로부터, 고온·장시간(900℃에서 2시간)의 열처리 후에도 전도상인 RuO2와 Pb2Ru2O6.5가 존재하므로, 전도성 입자의 기판확산 및 유리상의 휘발이 없다는 것을 알 수 있다.The resist paste according to the present invention is subjected to a thick film treatment on an alumina, a dielectric or a magnetic substrate and subjected to simultaneous firing by heat treatment for a long time at a high temperature, which is the firing temperature of the dielectric or magnetic material, so that the interface is stable and the electrical properties are good. A wide range of resistors can be obtained. It is understood from Fig. 4 of the XRD results that the conductive phases RuO 2 and Pb 2 Ru 2 O 6.5 exist even after the heat treatment at high temperature and long time (2 hours at 900 ° C.), so that there is no substrate diffusion and volatilization of the conductive particles. Can be.

Claims (6)

PbO 60-65 중량%, Al2O32.5-7.5중량%, SiO221.5-30.5 중량%, CaO 1 중량% 및 RuO25-10 중량%로 이루어진 저항체용 페이스트 분말.Paste powder for resistors consisting of 60-65 weight percent PbO, 2.5-7.5 weight percent Al 2 O 3 , 21.5-30.5 weight percent SiO 2 , 1 weight percent CaO and 5-10 weight percent RuO 2 . PbO 60-65 중량%, Al2O32.5-7.5중량%, SiO221.5-30.5 중량%, CaO 1 중량% 의 조성으로 된 유리 프릿트 분말과 5-10중량%의 RuO2분말을 혼합하여, 용융 및 급냉시키는 것을 특징으로 하는 저항체용 페이스트 분말 제조 방법.A glass frit powder composed of 60-65 wt% PbO, 2.5-7.5 wt% Al 2 O 3 , 21.5-30.5 wt% SiO 2 , and 1 wt% CaO mixed with 5-10 wt% RuO 2 powder Melting and quenching, The paste powder production method for resistors. PbO 60-65 중량%, Al2O32.5-7.5중량%, SiO221.5-30.5 중량%, CaO 1 중량% 및 RuO25-10중량%로 이루어지는 분말 70 중량%과, 유기 결합제(vehicle) 20중량% 및 유기 용매 10 중량%의 혼합물로 이루어지는 틱소트로피(thixotropy) 성질을 가지는 저항체 페이스트.70% by weight of powder consisting of 60-65% by weight of PbO, 2.5-7.5% by weight of Al 2 O 3 , 21.5-30.5% by weight of SiO 2 , 1% by weight of CaO and 5-10% by weight of RuO 2 , and an organic binder A resistor paste having thixotropy properties consisting of a mixture of 20% by weight and 10% by weight of an organic solvent. RuO2분말 5-10중량%와 유리 프릿트(SiO2-Bi2O3-CaO-Na2O) 90-95 중량% 으로 이루어지는 분말 70중량%, 유기 결합제(vehicle) 20중량% 및 유기 용매 10 중량%의 혼합물로 이루어지는 틱소트로피(thixotropy) 성질을 가지는 저항체 페이스트.70% by weight powder consisting of 5-10% by weight RuO 2 powder and 90-95% by weight glass frit (SiO 2 -Bi 2 O 3 -CaO-Na 2 O), 20% by weight organic binder and organic solvent Resistor paste having thixotropy properties consisting of a mixture of 10% by weight. 알루미나 기판 상에 제3항 또는 제4항에 의한 저항체용 페이스트를 후막처리하여, 그를 매시간당 300-1200℃인 승온율로 850-920℃ 까지 승온하여, 10-120분간 유지한 후, 매시간당 200-400℃로 냉각시켜 소성함으로써, 다양한 범위의 소결 면저항을 가지는 저항체를 만드는 것을 특징으로 하는 후막 저항체 제조방법.After the thick film treatment of the resistor paste according to claim 3 or 4 on the alumina substrate, the temperature was raised to 850-920 ° C. at an elevated temperature rate of 300-1200 ° C. per hour, and maintained for 10-120 minutes. A method for producing a thick film resistor, which is produced by cooling to 200-400 ° C. to produce a resistor having a sintered sheet resistance in a wide range. 제5항에 있어서, 상기 알루미나 기판 상에 스크린 프린터를 이용하여 전극(은 페이스트)을 형성하고, 저항체를 후막처리 하여, 상기 전극과 저항체를 동시에 상기와 같은 방법으로 소성하는 것을 특징으로 하는 후막 저항체 제조방법.6. The thick film resistor according to claim 5, wherein an electrode (silver paste) is formed on the alumina substrate using a screen printer, the resistor is thick-filmed, and the electrode and the resistor are baked at the same time as described above. Manufacturing method.
KR1019970049103A 1997-09-26 1997-09-26 Method of preparing paste for resistor for lcr co-firing, method of manufacturing thick film using it KR100246720B1 (en)

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KR101138238B1 (en) * 2010-12-24 2012-04-24 (주) 케이엠씨 테크놀러지 Manufacturing method of paste composition for resistor using coating metal oxide, thick film resistor and manufacturing method of the resistor
KR101166709B1 (en) 2010-10-27 2012-07-19 (주) 케이엠씨 테크놀러지 Manufacturing method of paste composite for resistor, thick film resistor and manufacturing method of the resistor

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KR101501488B1 (en) * 2013-08-29 2015-03-11 전자부품연구원 Paste for Thick-film Resistor and Method thereof
KR102623406B1 (en) * 2021-12-15 2024-01-11 주식회사와이테크 Composition for manufacturing NTC thermistor Thick films having low resistance and the manufacturing method of the same

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KR101166709B1 (en) 2010-10-27 2012-07-19 (주) 케이엠씨 테크놀러지 Manufacturing method of paste composite for resistor, thick film resistor and manufacturing method of the resistor
KR101138238B1 (en) * 2010-12-24 2012-04-24 (주) 케이엠씨 테크놀러지 Manufacturing method of paste composition for resistor using coating metal oxide, thick film resistor and manufacturing method of the resistor

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