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KR930005249B1 - Metal Oxide Thermistor Material - Google Patents

Metal Oxide Thermistor Material Download PDF

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KR930005249B1
KR930005249B1 KR1019900012585A KR900012585A KR930005249B1 KR 930005249 B1 KR930005249 B1 KR 930005249B1 KR 1019900012585 A KR1019900012585 A KR 1019900012585A KR 900012585 A KR900012585 A KR 900012585A KR 930005249 B1 KR930005249 B1 KR 930005249B1
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oxide
metal oxide
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temperature
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KR920004300A (en
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정형진
윤상옥
홍기룡
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한국과학기술연구원
박원희
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01C—RESISTORS
    • H01C7/00—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material
    • H01C7/04—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material having negative temperature coefficient
    • H01C7/042—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material having negative temperature coefficient mainly consisting of inorganic non-metallic substances
    • H01C7/043—Oxides or oxidic compounds
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01C—RESISTORS
    • H01C7/00—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material
    • H01C7/04—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material having negative temperature coefficient
    • H01C7/042—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material having negative temperature coefficient mainly consisting of inorganic non-metallic substances
    • H01C7/043—Oxides or oxidic compounds
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    • 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
    • C04B35/016—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 manganites
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    • 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
    • C04B35/26—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 ferrites
    • C04B35/265—Compositions containing one or more ferrites of the group comprising manganese or zinc and one or more ferrites of the group comprising nickel, copper or cobalt
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3262—Manganese oxides, manganates, rhenium oxides or oxide-forming salts thereof, e.g. MnO

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  • Thermistors And Varistors (AREA)
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Abstract

내용 없음.No content.

Description

금속산화물계 써미스터 재료Metal Oxide Thermistor Material

제1도는 본 발명 금속산화물계 써미스터 재료의 조성비를 나타낸 3원계도.1 is a ternary diagram showing the composition ratio of the metal oxide thermistor material of the present invention.

제2도는 본 발명의 일실시예에 대한 저항-온도 특성관계를 보인 그래프.Figure 2 is a graph showing the resistance-temperature characteristic relationship for one embodiment of the present invention.

본 발명은 MnCO3-NiO-ZnO-Co3O4-Fe2O3-TiO2계를 기본조성으로 하는 금속산화물계 NTC써미스터 재료에 관한 것이다.The present invention relates to a metal oxide based NTC thermistor material based on a MnCO 3 -NiO-ZnO-Co 3 O 4 -Fe 2 O 3 -TiO 2 system.

일반적으로 써미스터는 온도변화에 따라 대단히 크고 비직선적인 저항변화를 나타내는 반도체소자의 일종으로서 주로 철(Fe), 니켈(Ni), 망간(Mn), 몰리브덴(Mo) 및 코발트(Co)등의 산화물을 혼합하여 소결함으로써 제조되어 진다.In general, thermistor is a kind of semiconductor device that shows a very large and nonlinear resistance change with temperature change, and mainly oxides such as iron (Fe), nickel (Ni), manganese (Mn), molybdenum (Mo), and cobalt (Co) It is prepared by mixing and sintering.

특히, 전이금속산화물을 조합하여 제조된 금속산화물계 써미스터는 온도에 따라 전기저항이 지수함수적으로 감소하는 반도체소자로서 그 원료성분의 조성이나 소결온도에 따라 결정구조 및 소결성에 큰 차이가 나타나기 때문에 상온저항 및 온도에 따른 저항변화에 큰 차이를 나타낸다.Particularly, metal oxide thermistors manufactured by combining transition metal oxides are semiconductor devices whose electrical resistance decreases exponentially with temperature, and thus the crystal structure and sinterability of the metal oxides vary greatly depending on the composition of the raw material and the sintering temperature. It shows big difference in resistance change according to room temperature resistance and temperature.

이와같은 금속산화물계 써미스터는 상기 온도에 따른 저항치의 지수함수적 감소특성을 이용하여 온도감지소자, 온도보상 및 조절소자, 전압조절용소자를 비롯한 각종 정밀측정 및 분석기기의 핵심소자로 널리 사용되고 있다.Such metal oxide thermistors are widely used as core elements of various precision measurement and analyzer devices, including temperature sensing devices, temperature compensation and control devices, voltage control devices, and the like by using an exponentially decreasing characteristic of the resistance value according to the temperature.

종래의 금속산화물계 써미스터 재료로는 스핀넬계인 망간-니켈-코발트-구리계와 헤마타이트계인 철-티타늄계가 사용되고 있으며, 전자의 스핀넬계 써미스터의 경우 조성에 따라 넓은 저항범위와 큰 B정수를 나타냄으로써 광범위하게 응용될 수 있는 것으로 알려져 있다[참조 : 1. Thermistors(ed. by E.D. Macklen), Electrochemical Pub., Ayr, Scotland(1979). 2. Semiconducting temperature sensors and their applications(ed. by H.B. Sachse), John and Wiley, New York(1975). 3. Ceramic Materials for electronic(ed. by R.C. Buchanan), Marcel Dekker, New York(1986)].Conventional metal oxide thermistor materials include spinel manganese-nickel-cobalt-copper and hematite iron-titanium. The former spinel thermistors have a wide resistance range and a large B constant depending on their composition. It is known that the present invention can be widely applied to the present invention. 1. Thermistors (ed. By ED Macklen), Electrochemical Pub., Ayr, Scotland (1979). Semiconducting temperature sensors and their applications (ed. By H.B. Sachse), John and Wiley, New York (1975). 3. Ceramic Materials for electronic (ed. By R. C. Buchanan), Marcel Dekker, New York (1986)].

그러나, 이같은 스핀넬계의 망간-니켈-코발트-구리계 써미스터의 경우 산화 코발트의 가격이 매우 높기 때문에 제조비용면에서 불리한 점이 있으며, 또한 산화동은 인체에 흡수되는 경우 건강을 해치는 유해물질로 작용하기 때문에 써미스터의 제조시 공해발생의 문제점을 지니고 있다[참조 : Hawley′s condensed chemical dictionary, 11th edition(ed. by N.L. Sax and R.J. Lewis, Sr.), Van Nostrand Reinhold Co., New York(1987)].However, such spinel manganese-nickel-cobalt-copper thermistors have disadvantages in terms of manufacturing cost due to the high price of cobalt oxide, and copper oxide acts as a harmful substance to health when absorbed by the human body. Pollution problems occur in the manufacture of thermistors (Hawley's condensed chemical dictionary, 11th edition (ed. By NL Sax and RJ Lewis, Sr.), Van Nostrand Reinhold Co., New York (1987)).

따라서, 본 발명은 금속산화물계 써미스터 재료로서 고가의 산화코발트를 값싼 산화철과 산화티타늄으로 대체하여 써미스터 재료의 제조원가를 낮추는 한편 유해물질인 산화동을 무해한 산화아연으로 치환함으로써 써미스터 재료의 제조시에 뒤따르는 공해문제를 제거함과 아울러 다성분계 산화물계에서 존재하는 공융반응(eutecticreaction)에 의해 액상소결을 유도하여 소결온도를 낮춤으로써 적은 제조비용으로 양호한 특성을 갖는 써미스터를 제조할 수 있는 금속산화물계 써미스터 재료를 제공하는데 그 목적이 있다.Therefore, the present invention is to replace the expensive cobalt oxide as a metal oxide thermistor material with cheap iron oxide and titanium oxide to reduce the production cost of thermistor material and to replace the harmful copper oxide with harmless zinc oxide, which is followed in the manufacture of thermistor material In addition to eliminating the pollution problem and inducing liquid phase sintering by eutecticreaction present in the multi-component oxide system, the sintering temperature is lowered. The purpose is to provide.

이같은 본 발명의 금속산화물계 써미스터 재료의 조성은, a탄산망간(MnCO3)+b산화니켈(NiO)+c산화아연(ZnO)+d산화코발트(Co3O4)+e산화철(Fe2O3)+f산화티탄(TiO2)계를 기본조성으로 하고, 그 조성 비율은 중량비로,The composition of the metal oxide thermistor material of the present invention is a manganese carbonate (MnCO 3 ) + b nickel oxide (NiO) + c zinc oxide (ZnO) + d cobalt oxide (Co 3 O 4 ) + e iron oxide (Fe 2 O 3 ) + f titanium oxide (TiO 2 ) based composition, the composition ratio is by weight,

29≤a+b≤6629≤a + b≤66

0≤c≤480≤c≤48

4≤d+e+f≤634≤d + e + f≤63

(단, a+b+c+d+e+f=100)(Where a + b + c + d + e + f = 100)

이같은 본 발명의 금속산화물계 써미스터 재료의 조성을 3성분계로 나타내면 제1도와 같다.The composition of the metal oxide thermistor material of the present invention is shown in FIG.

본 발명의 금속산화물계 써미스터 재료를 이용하여 NTC써미스터를 제조하는 과정은 일반적으로 널리 사용되는 산화물 혼합방법을 통해 이루어진다.The process of manufacturing NTC thermistor using the metal oxide thermistor material of the present invention is generally accomplished through a widely used oxide mixing method.

이하, 본 발명의 실시예를 통하여 써미스터의 제조과정을 설명한다.Hereinafter, the manufacturing process of the thermistor will be described through an embodiment of the present invention.

먼저, 아래의 표 1과 같은 망간-니켈-아연-코발트-철-티타늄계 금속산화물로서 aMnCO3+bNiO+cZnO+dCo3O4+eFe2O3+fTiO2, 27.86≤a≤41.85, 6.17≤b≤10.97, 0≤c≤47.02, 0≤d≤8.97, 4.13≤e≤51.14, 0.23≤f≤3.09(단, a+b+c+d+e+f=100)조성으로 탄산망간, 산화니켈, 산화동, 산화아연, 산화코발트, 산화철 및 산화티탄올 10-4g까지 정확히 칭량하여 지르코니아 볼밀중에서 증류수와 함께 충분히 혼합 및 분쇄를 행한다.First, aMnCO 3 + bNiO + cZnO + dCo 3 O 4 + eFe 2 O 3 + fTiO 2 , 27.86 ≦ a ≦ 41.85, 6.17 as manganese-nickel-zinc-cobalt-iron-titanium metal oxides as shown in Table 1 below. ≤ b ≤ 10.97, 0 ≤ c ≤ 47.02, 0 ≤ d ≤ 8.97, 4.13 ≤ e ≤ 51.14, 0.23 ≤ f ≤ 3.09 (where a + b + c + d + e + f = 100) Accurately weigh up to 10 -4 g of nickel oxide, copper oxide, zinc oxide, cobalt oxide, iron oxide and titanium oxide, and thoroughly mix and grind with distilled water in a zirconia ball mill.

이때 사용되는 원료로는 하소(calcination) 공정을 통하여 산화물로의 전환이 용이한 화합물 즉, 수산화물 및 탄산염등이 포함된 원료화합물도 가능하다.In this case, as a raw material used, a compound which can be easily converted into an oxide through a calcination process, that is, a raw material compound including hydroxide and carbonate can be used.

혼합 및 분쇄가 완료된 시료는 750℃~850℃에서 하소를 한 다음 PVA수용액과 같은 일반적인 결합제를 미량 첨가하여 1ton/cm2의 압력으로 가압성형한 후 알루미나판 위에 올려놓고 전기로중에서 1000℃~1200℃의 온도로 2시간동안 소결을 행한다. 소결시에 결합제를 비롯한 유기물의 휘발을 위하여 600℃에서 1시간 유지하며 승온 및 냉각속도는 300℃/hr로 한다.After mixing and grinding, the sample is calcined at 750 ℃ ~ 850 ℃, and then, after adding a small amount of a general binder such as PVA solution, it is press-molded at a pressure of 1ton / cm 2 and placed on an alumina plate, and 1000 ℃ ~ 1200 ℃ in an electric furnace. Sintering is carried out at a temperature of 2 hours. During sintering, the mixture is kept at 600 ° C. for 1 hour for volatilization of organic matter including binder, and the temperature rising and cooling rate is 300 ° C./hr.

이후, 소결체의 양면에 은페이스트를 스크린인쇄하여 전극을 형성하며 550℃에서 10분간 열처리하고 24시간 방치한 후 전기적 특성을 측정한다. 시편의 전기적 특성 측정은 25℃로 유지된 실리콘 오일 항온조에서 2단자법을 통해 행해지며 B정수는 다음과 같은 식에 의해 계산된다.Thereafter, silver paste is screen printed on both surfaces of the sintered body to form an electrode, and heat-treated at 550 ° C. for 10 minutes and left for 24 hours to measure electrical characteristics. The electrical properties of the specimens are measured by a two-terminal method in a silicon oil thermostat maintained at 25 ° C. The B constant is calculated by the following equation.

Figure kpo00001
Figure kpo00001

[표1]Table 1

망간-니켈-아연-코발트-철-티타늄계 금속산화물 써미스터의 조성 및 특성Composition and Properties of Manganese-Nickel-Zinc-Cobalt-Iron-Titanium Metal Oxide Thermistors

Figure kpo00002
Figure kpo00002

제2도는 위의 표 1에 나타나 있는 본 발명의 실시예 조성으로 이루어진 금속산화물계 써미스터의 저항과 온도와의 관계를 보인 그래프이다.2 is a graph showing the relationship between the temperature and the resistance of the metal oxide thermistor made of the composition of the present invention shown in Table 1 above.

이같은 제조과정을 통하여 얻어진 본 발명의 금속산화물계 써미스터는 스핀넬계 구조를 띠며, 위의 표 1에서와 같이 산화철이 산화티탄과 함께 상당량 첨가된다 하더라도 충분히 고용되어 넓은 저항범위의 우수한 써미스터 제조가 가능함을 알 수 있다.The metal oxide thermistor of the present invention obtained through such a manufacturing process has a spinel structure, and even if iron oxide is added with titanium oxide in a considerable amount as shown in Table 1 above, it can be sufficiently employed to produce a superior thermistor having a wide resistance range. Able to know.

따라서, 본 발명의 금속산화물계 써미스터 재료는 고가의 산화코발트 전부 또는 대부분을 값싼 산화철 및 산화티타늄으로 대체시킴에 의해 써미스터의 제조비용을 절감할 수 있음은 물론 써미스터의 제조시 유해물질로 작용하는 산화구리의 사용을 배제함으로써 제조작업의 안전성을 도모할 수 있는 장점이 있다.Therefore, the metal oxide thermistor material of the present invention can reduce the manufacturing cost of the thermistor by replacing all or most of the expensive cobalt oxide with inexpensive iron oxide and titanium oxide, as well as oxidation acting as a harmful substance in the manufacture of the thermistor. By eliminating the use of copper, there is an advantage that the safety of manufacturing operations can be achieved.

한편, 본 발명의 금속산화물계 써미스터 재료는 다성분계 조성으로써 상호 공융반응(eutectic reaction)에 의해 1000℃~1200℃에서 소결이 행해짐에 따라 종래의 망간-니켈-코발트-동계써미스터의 소결 온도에 비해 100℃~250℃정도 소결온도를 낮출 수 있어 써미스터의 제조비용을 낮출 수 있는 이점이 있다.On the other hand, the metal oxide thermistor material of the present invention is a multi-component composition is sintered at 1000 ℃ ~ 1200 ℃ by the eutectic reaction (eutectic reaction) compared to the sintering temperature of the conventional manganese-nickel-cobalt-winter thermistor Since the sintering temperature can be lowered by about 100 ° C. to 250 ° C., the manufacturing cost of the thermistor can be lowered.

Claims (1)

aMnCO3+bNiO+cZnO+dCo3O4+eFe2O3+fTiO2계를 기본조성으로 하고 중량비로,aMnCO 3 + bNiO + cZnO + dCo 3 O 4 + eFe 2 O 3 + fTiO 2 system as a basic composition and by weight ratio, 27.86≤a≤41.8527.86≤a≤41.85 6.17≤b≤10.976.17≤b≤10.97 0≤c≤47.020≤c≤47.02 0≤d≤8.970≤d≤8.97 4.13≤e≤51.144.13≤e≤51.14 0.23≤f≤3.090.23≤f≤3.09 (단, a+b+c+d+e+f=100)(Where a + b + c + d + e + f = 100) 의 조성범위를 갖는 금속산화물계 써미스터 재료.Metal oxide thermistor material having a composition range of.
KR1019900012585A 1990-08-16 1990-08-16 Metal Oxide Thermistor Material Expired - Fee Related KR930005249B1 (en)

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GB9116910A GB2247015A (en) 1990-08-16 1991-08-06 Metal oxide group thermistor material
US08/006,697 US5246628A (en) 1990-08-16 1993-01-21 Metal oxide group thermistor material
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