EP0062314A2 - Nichtlinearer Widerstand und Verfahren zu dessen Herstellung - Google Patents

Nichtlinearer Widerstand und Verfahren zu dessen Herstellung Download PDF

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Publication number
EP0062314A2
EP0062314A2 EP82102784A EP82102784A EP0062314A2 EP 0062314 A2 EP0062314 A2 EP 0062314A2 EP 82102784 A EP82102784 A EP 82102784A EP 82102784 A EP82102784 A EP 82102784A EP 0062314 A2 EP0062314 A2 EP 0062314A2
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EP
European Patent Office
Prior art keywords
sintered body
oxide
film
linear resistor
indium
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP82102784A
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English (en)
French (fr)
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EP0062314A3 (de
Inventor
Takeo Yamazaki
Ken Takahashi
Tadahiko Miyoshi
Kunihiro Maeda
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Hitachi Ltd
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Hitachi Ltd
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Filing date
Publication date
Application filed by Hitachi Ltd filed Critical Hitachi Ltd
Publication of EP0062314A2 publication Critical patent/EP0062314A2/de
Publication of EP0062314A3 publication Critical patent/EP0062314A3/de
Withdrawn legal-status Critical Current

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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
    • 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
    • H01C7/10—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 voltage responsive, i.e. varistors
    • H01C7/102—Varistor boundary, e.g. surface layers

Definitions

  • This invention relates to a non-linear resistor used for voltage stabilizers, surge absorbers, arresters, etc., and a process for producing the same.
  • a conventional non-linear resistor has a structure as shown in Fig. 1, wherein electrodes 2 are formed individually on upper and lower major surfaces of a sintered body 1 having as a major component zinc oxide and non-linear resistance characteristics.
  • a non-linear resistor is produced by a well-known ceramic sintering technique.
  • a suitable binder such as water, poly(vinyl alcohol), or the like to form granules, which are pressed into a body of a desired shape and size.
  • the body is then sintered in an electric furnace at a temperatxre of 900 - 1400°C.
  • the side surface of the body may be coated with a Bi 2 O 3 -Sb 2 O 3 -SiO 2 paste in order to prevent corona discharge and the like along the side surface before the sintering.
  • two major surfaces at which electrodes are to be formed are abraded to a desired thickness, followed by the formation of electrodes by a conventional process such as flame spraying, baking of a paste, or the like.
  • a glass film is sometimes formed around the side surface in order to improve prevention of discharge along the side surface.
  • non-linear resistor is excellent in non-lineality of voltage-current characteristics, but rather poor in stability and there is a problem in that its properties are subjected to deterioration by the load test which is carried out by applying a rated voltage for a long period of time, causing a gradual increase of leakage current and finally inducing thermal runaway.
  • the life of non-linear resistor elements used for lightning arresters for transmitting 1200 kV under the conditions of use temperature 40°C, and an applied voltage ratio (AVR) of 80% (100% AVR is the 1 mA voltage at the initial condition) should be longer than 100 years, but non-linear resistor elements having such a long life have not been obtained by using conventional non-linear resistors.
  • AVR applied voltage ratio
  • This invention provides a non-linear resistor comprising a sintered body having non-linear resistance characteristics and one or more electrodes formed on the upper and/or lower major surfaces of said sintered body, characterized in that one or more continuous films having no gas permeability and lower electrical resistivity than the resistivity of said sintered body are individually formed between the sintered body and one or more electrodes.
  • This invention also provides a process for producing a non-linear resistor which comprises
  • Fig. 1 is a cross-sectional view of a conventional non-linear resistor
  • Fig. 2 is a cross-sectional view of a non-linear resistor of this invention
  • Fig. 3 is a graph showing a relationship between resistivity and In 2 0 3 content in a mixture of indium oxide and tin oxide which mixture forms the continuous film between the sintered body and an electrode
  • Fig. 4 is a graph showing a relationship between a non-linearity coefficient and a heat treatment temperature of a sintered body containing zinc oxide as a major component.
  • the continuous film is formed between the sintered body and the electrodes, said film being constructed so dense that it has no gas permeability and having lower electrical resistivity than the resistivity of the sintered body and no y-bismuth oxide phase, various advantages are obtained, particularly by preventing the release of constituting atoms of the sintered body, e.g. oxygen ions or a gas adsorbed in the sintered body, e.g., oxygen gas, from the sintered body at the time of voltage application, which results in giving stability to the properties for a long period of time, e.g. more than 100 years under ordinary conditions.
  • constituting atoms of the sintered body e.g. oxygen ions or a gas adsorbed in the sintered body, e.g., oxygen gas
  • the continuous film 3 is interposed between the sintered body 1 having non-linear characteristics and the electrode 2.
  • the sintered body used in this invention may be any one having non-linear resistance characteristics and showing deterioration in non-linear characteristics by the release of atoms constituting the sintered body or adsorbed gas in the sintered body.
  • a sintered body are sintered bodies of oxides such as zinc oxide, titanium oxide, and the like and those of chalcogen such as selenium and the like.
  • non-linear resistors containing zinc oxide as a major component are excellent in non-linear resistance characteristics but show the property deterioration at the time of voltage application due to the release of oxygen from crystal grains or crystal boundary layers, so that the effects of this invention are greatly exhibited when this invention is applied to such zinc oxide based non-linear resistors.
  • the continuous film 3 formed between the sintered body 1 and the electrode 3 is preferably required to have the following properties:
  • the continuous film is good in denseness and adhesion to the sintered body.
  • the words "good in denseness” mean that a gas such as oxygen is not permeable through the continuous film.
  • the sintered body that having zinc oxide as a major component and as the continuous film that made of indium oxide type compound, tin oxide type compound or a mixture of indium oxide and tin oxide type compounds it is important that the continuous and electroconductive film can be baked on the sintered body at a temperature of 520°C or lower.
  • the continuous film is different from y-bismuth oxide phase layer formed on the surface portions of the sintered body.
  • the continuous film is low in hygroscopicity so as to produce non-linear resistors which can be used in high humidity.
  • the continuous film interposed between the sintered body and the electrode that made of indium oxide or the like compound, tin oxide or the like compound or a mixture of indium oxide and tin oxide or the like compounds.
  • the continuous film may contain other components which have thermal expansion coefficients near that of the sintered body so long as not lowering the properties of the film of indium oxide, tin oxide or indium oxide-tin oxide mixture.
  • other components are antimony oxide, tantalum oxide, manganese oxide, and the like.
  • Thickness of the continuous film changes depending on the kinds of sintered body and materials used for the film.
  • a preferable thickness of the continuous film is 1 to 30 ⁇ m in the case of indium oxide, tin oxide or the like compound being used singly and 1 to 50 ⁇ m in the case of a mixture of indium oxide and tin oxide type compounds. It is also preferable to use the continuous film having the same area and shape as the electrode to be formed thereon, considering the prevention of deterioration of the film during the production.
  • Zinc oxide sintered body has a thermal expansion coefficient of about 80 x 10 -7 °C -1
  • an indium oxide-tin oxide type film has a thermal expansion coefficient of about 160 x 10 -7 °C -1 . Therefore, if the film thickness of the indium oxide-tin oxide type film becomes too large, the film may easily be cracked due to differences of thermal expansion coefficients of the two. Since cracks are easily formed in the film when the film thickness is larger than 50 ⁇ m as shown in Table 10 below, it is preferable to make the film thickness 50 ⁇ m or less.
  • the film thickness 1 ⁇ m or more As mentioned above, the film thickness of 1 to 50 ⁇ m is preferable in the case of the film of a mixture of indium oxide and tin oxide type compounds when the sintered body contains zinc oxide as a major component. The same reasons may be applied to the case of the film of indium oxide or tin oxide or the like compound being used singly.
  • the sintered body there may be used any sintered body containing zinc oxide as a major component, more concretely 70% by mole or more.
  • the sintered body may further contain bismuth oxide and manganese oxide in amounts of 0.01 to 10% by mole, respectively and the resulting sintered body is more preferable.
  • Particularly preferable sintered bodies are those containing bismuth oxide, manganese oxide, cobalt oxide, antimony oxide, chromium oxide, boron oxide, silicon oxide and nickel oxide in amounts of 0.01 to 10% by mole, respectively, but not more than 30% by mole as a total in addition to zinc oxide.
  • These sintered body can usually be obtained by sintering raw material particles containing zinc oxide at a temperature of 900 to 1400°C. It is preferable that the sintered body contain no or substantially no y-bismuth oxide phase therein even after the heat treatment for baking the continuous film formed on the sintered body.
  • the non-linear resistor of this invention can be produced, for example, by the following processes.
  • the indium compound and/or tin compound not only indium oxide and tin oxide but also any indium compounds which can yield indium oxide by pyrolysis at a temperature preferably 520°C or lower such as indium nitrate, etc., and any tin compounds which can yield tin oxide by pyrolysis at a temperature preferably 520°C or lower such as tin nitrate, etc.
  • a film forming layer may be formed on the sintered body by a conventional process such as a chemical vapor deposition method (CVD), sputtering, a solution coating method such as dipping, brushing, or the like.
  • CVD chemical vapor deposition method
  • sputtering a solution coating method such as dipping, brushing, or the like.
  • the solution coating method when a solution containing above-mentioned raw materials, for example, a solution containing an indium compound and a tin compound, is coated on a major surface electrode forming area of the sintered body, a part of the solution penetrates into the inner portion of the sintered body, while the remaining part of the solution forms a film on the surface.
  • the raw materials penetrated into the inner portion of the sintered body fill pores and crystal grain boundaries present near the major surface portions of the sintered body on baking the raw material layer, which results in making greater the preventing effect of the release of atoms constituting the sintered body or the gas adsorbed in the sintered body.
  • the raw material layer formed on the electrode forming surface of the sintered body is baked at a temperature of 520°C or lower considering the decrease in non-linearity coefficient and the formation of y-bismuth oxide phase. In order to prevent the lowering in resistance to humidity of the baked film, it is preferable to bake the raw material layer at a temperature of 350°C or higher.
  • Electrodes are formed on individual continuous and electroconductive film thus formed by a conventional process such as flame spraying, baking of a paint, etc., to give a non-linear resistor.
  • the nonlinear resistor of this invention has excellent stability to the load lifetime test for a long period of time and can be used for voltage stabilizers, surge absorbers, arresters and the like with usual modifications.
  • an arrester can be formed by putting a plurality of non-linear resistors piled in a housing means such as a metal tank or an insulator.
  • Such an arrester has a long service lifetime and high reliability because of the long lifetime (under continuous AC operating stress) of the non- linear resister used therein.
  • a problem in that, due to the floating capacity between the non-linear resistor element and the ground, a strong electric field is applied to the elements in the upper portion to shorten the lifetime of such elements.
  • it is usually practiced to provide one or more capacitors or a metallic shield to thereby correct the electric field exerted.
  • the non-linear resistor element adopted therein has a long lifetime even if used in a high electric field, it is possible to omit the field corrector element from the mechanism in the housing means.
  • the housing means can be reduced in size, it is possible to attain a reduction of size and weight of the arrester and to improve its earth quake resistance.
  • the body After coating a Bi 2 O 3 -Sb 2 O 3 -SiO 2 -containing paste on the side surface of the body, the body was sintered in air at 1250°C for 2 hours. During the sintering, the above-mentioned paste was reacted with the zinc oxide to give a highly resistant layer containing Zn 2 SiO 4 and Zn 7 Sb 2 0 12 mainly. Two major surfaces of the sintered body were abraded so as to give a thickness of 3 mm.
  • the thus coated sintered body was heat trated (baked) in air at 450°C for 2 hours while raising the temperature to 450°C at a rate of 200°C/hr. After baking, Al electrodes were formed on the indium oxide-tin oxide films by a conventional flame spraying.
  • the above-mentioned paste was reacted with the ZnO to give a highly resistant layer containing Zn 2 SiO 4 and Zn 7 Sb 2 O 12 mainly.
  • Two major surfaces of the sintered body were abraded so as to give a thickness of 4 mm.
  • a solution was prepared by mixing metallic tin (Sn), CH 3 COCH 2 COCH 3 and HNO 3 in a weight ratio of 1 : 10 : 4.
  • the solution was applied to the abraded surfaces of the sintered body by the dip method so as to give a film having a thickness in the range of 2 - 10 ⁇ m after baked.
  • the thus coated sintered body was heat treated (baked) in air at 450°C for 2 hours while raising the temperature to 450°C at a rate of 200°C/hr. After baking, aluminum electrodes were formed on the tin oxide films by a conventional flame spraying.
  • Example 2 The same tests as conducted in Example 1 were conducted with the results as shown in Table 2.
  • a sintered body was prepared in the same manner as described in Example 2. Two major surfaces of the sintered body were abraded so as to give a thickness of 3 mm.
  • Example 3 The same tests as conducted in Example 1 were conducted with the results as shown in Table 3.
  • a solution containing tin obtained in the same manner as described in Example 2 together with antimony (3% by weight) was applied to the abraded surfaces of the sintered body by the dip method so as to give a film having a thickness in the range of 15 - 20 ⁇ m after baked.
  • the thus coated sintered body was heat treated (baked) in air at a temperature of 250°C, 300°C, 350°C, 450°C, 520°C or 600°C for 30 minutes, . while raising the temperature to the prescribed one at a rate of 100°C/hr.
  • the resulting tin oxide films were subjected to a humidity resistance test and resistivities of the films were also measured.
  • the humidity resistance test was conducted by dipping a tin oxide film coated sintered body in boiling water for 30 minutes and judging the surface appearance as to discoloration or peeling .of the tin oxide film.
  • Solutions having a' Sn/In ratio of 5/95, 10/90, 20/80, 50/50, or 80/20 were prepared by using the indium solution and the tin solution used in Example 1. Each solution was applied to the abraded surfaces of the sintered body by the dip method so as to give a film having a thickness in the range of 15 - 20 ⁇ m after baked. The thus coated sintered body was heat treated (baked) in air at 400°C for 30 minutes, while raising the temperature to 400°C at a rate of 150°C/hr. Single film of indium oxide and that of tin oxide were formed in the same manner as mentioned above. Aluminum electrodes were formed on each film of indium oxide-tin oxide, indium oxide or tin oxide by a conventional flame spraying.
  • the films made of indium oxide-tin oxide mixtures are particularly superior to the film made of indium oxide or tin oxide singly in the accelerated life test.
  • Example 3 The same indium solution as used in Example 3 was applied to the abraded surfaces of the sintered body by the dip method so as to give a film having a thickness in the range of 15 - 20 ⁇ m after baked.
  • the thus coated sintered body was heat treated (baked) in air at a temeprature of 250°C, 300°C, 350°C, 450°C, 520°C or 600°C for 30 minutes, while raising the temperature to the prescribed one at a rate of 100°C/hr.
  • a solution prepared by mixing the indium solution and the tin solution as used in Example 1 so as to give a Sn/In patio of 20/80 was applied to the abraded surfaces of the sintered body by the dip method so as to give an indium oxide-tin oxide film having a thickness in the range of 20 - 25 ⁇ m after baked.
  • the thus coated sintered body was heat treated (baked) in air at a temperature of 250°C, 300°C, 350°C, 450°C, 520°C or 600°C for 30 minutes, while raising the temperature to the prescribed one at a rate of 100°C/hr.
  • Example 2 Two major surfaces of the sintered body were abraded so as to give a thickness of 4 mm.
  • the tin solution used in Example 1 was applied to the abraded surfaces of the sintered body by brushing so as to give a tin oxide film having a thickness of 0.5 ⁇ m, 1 ⁇ m, 10 ⁇ m, 20 ⁇ m, 30 ⁇ m or 40 ⁇ m after baked.
  • Each thus coated sintered body was heat treated (baked) in air at 500°C for 30 minutes, while raising the temperature to 500°C at a rate of 100°C/hr.
  • aluminum electrodes were formed on the tin oxide films having no cracks thereon by a conventional flame spraying.
  • the resulting resistors were subjected to the same accelerated life test as Example 1 with the results as shown in Table 8.
  • a preferable thickness of the electroconductive tin oxide film is in the range of 1 to 30 ⁇ m.
  • a mixture of powders having the same composition as described in Exmaple 8 was granulated and pressed into a body of 20 mm in diameter and 6 mm in thickness. After coating a SiO 2 -Bi 2 O 3 -Sb 2 O 3 -containing paste on the side surface of the body, the body was sintered in air at 1270°C for 2 hours. Two major surfaces of the sintered body were abraded so as to give a thickness of 4 mm.
  • the indium solution used in Example 2 was 'applied to the abraded surfaces of the sintered body by brushing so as to give an indium oxide film having a thickness of 0.5 ⁇ m, 1 ⁇ m, 10 ⁇ m, 20 ⁇ m, 30 ⁇ m. or 45 ⁇ m after baked.
  • the thus coated sintered body was heat treated (baked) in air at 500°C for 30 minutes, while raising the temperature to 500°C at a rate of 100 °C/hr.
  • aluminum electrodes were formed on the indium oxide films having no cracks thereon by a conventional flame spraying.
  • the resulting resistors were subjected to the same accelerated life test as in Example 1 with the results as shown in Table 9.
  • tin oxide films were formed by a conventional sputtering method, followed by the formation of aluminum electrodes thereon by a conventional flame spraying.
  • the lifetime of resulting resistors under the accelerated life test was improved when the thickness of the tin oxide films was 1 ⁇ m or more.
  • indium oxide films were formed by a conventional sputtering method, followed by the formation of aluminum electrodes thereon by a conventional flame spraying.
  • the lifetime of resulting resistors under the accelerated life test was also improved when the thickness of the indium oxide films was 1 ⁇ m or more.
  • a solution was prepared by mixing the indium solution and the tin solution used in Example 1 so as to give a Sn/In ratio of 40/60.
  • the solution was applied to the abraded surfaces of the sintered body by brushing so as to give an indium oxide-tin oxide film having a thickness of 0.5 ⁇ m, 1 ⁇ m, 10 um, 20 ⁇ m, 30 ⁇ m, 50 ⁇ m or 65 ⁇ m after baked.
  • Each sintered body thus coated was heat treated (baked) in air at 500°C for 30 minutes, while raising the temperature to 500°C at a rate of 100°C/hr.
  • aluminum electrodes were formed on the tin oxide films having no cracks thereon by a conventional flame spraying.
  • the resulting non-linear resistors were subjected to the same accelerated life test as in Example 1 with the results as shown in Table 10.
  • a preferable thickness of the indium oxide-tin oxide film is in the range of 1 to 50 ⁇ m.
  • indium oxide-tin oxide films were formed by a conventional sputtering method, followed by the formation of aluminum electrodes thereon by a conventional flame spraying.
  • the lifetime of resulting resistors under the accelerated life test was improved when the thickness of the indium oxide-tin oxide film was 1 ⁇ m or more.
  • the non-linear resistor of this invention is excellent in stability when a rated voltage is applied for a long period of time compared with conventional ones having no such films.

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  • Engineering & Computer Science (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Thermistors And Varistors (AREA)
  • Apparatuses And Processes For Manufacturing Resistors (AREA)
  • Non-Adjustable Resistors (AREA)
EP82102784A 1981-04-03 1982-04-01 Nichtlinearer Widerstand und Verfahren zu dessen Herstellung Withdrawn EP0062314A3 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP56049455A JPS57164502A (en) 1981-04-03 1981-04-03 Voltage nonlinear resistor and method of producing same
JP49455/81 1981-04-03

Publications (2)

Publication Number Publication Date
EP0062314A2 true EP0062314A2 (de) 1982-10-13
EP0062314A3 EP0062314A3 (de) 1983-09-07

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EP82102784A Withdrawn EP0062314A3 (de) 1981-04-03 1982-04-01 Nichtlinearer Widerstand und Verfahren zu dessen Herstellung

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EP (1) EP0062314A3 (de)
JP (1) JPS57164502A (de)
KR (1) KR840001759A (de)
IN (1) IN157791B (de)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AT380971B (de) * 1983-02-22 1986-08-11 Sprecher & Schuh Ag Widerstandsanordnung fuer hochspannungsleistungsschalter
DE3826282A1 (de) * 1988-07-29 1990-02-08 Siemens Ag Elektrische maschine oder apparat mit einer wicklung, die metalloxid-widerstaende zur ueberspannungsbegrenzung aufweist, und verfahren zu ihrer herstellung
EP0351004A3 (en) * 1988-07-13 1990-03-21 Philips Patentverwaltung Gmbh Non-linear voltage-dependent resistor
DE4036997A1 (de) * 1989-11-21 1991-05-23 Murata Manufacturing Co Monolithischer varistor

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6265304A (ja) * 1985-09-17 1987-03-24 株式会社村田製作所 電圧非直線抵抗体
JP2021131379A (ja) * 2020-02-19 2021-09-09 三菱マテリアル株式会社 温度センサ及びその製造方法

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1556638A (en) * 1977-02-09 1979-11-28 Matsushita Electric Industrial Co Ltd Method for manufacturing a ceramic electronic component
JPS6055969A (ja) * 1983-09-05 1985-04-01 永田　暢良 初期消火布

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AT380971B (de) * 1983-02-22 1986-08-11 Sprecher & Schuh Ag Widerstandsanordnung fuer hochspannungsleistungsschalter
EP0351004A3 (en) * 1988-07-13 1990-03-21 Philips Patentverwaltung Gmbh Non-linear voltage-dependent resistor
DE3826282A1 (de) * 1988-07-29 1990-02-08 Siemens Ag Elektrische maschine oder apparat mit einer wicklung, die metalloxid-widerstaende zur ueberspannungsbegrenzung aufweist, und verfahren zu ihrer herstellung
DE4036997A1 (de) * 1989-11-21 1991-05-23 Murata Manufacturing Co Monolithischer varistor

Also Published As

Publication number Publication date
IN157791B (de) 1986-06-21
KR840001759A (ko) 1984-05-16
EP0062314A3 (de) 1983-09-07
JPS6243324B2 (de) 1987-09-12
JPS57164502A (en) 1982-10-09

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