EP0357113A2 - Procédé de production d'une résistance non linéaire dépendant de la tension - Google Patents

Procédé de production d'une résistance non linéaire dépendant de la tension Download PDF

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Publication number
EP0357113A2
EP0357113A2 EP89201988A EP89201988A EP0357113A2 EP 0357113 A2 EP0357113 A2 EP 0357113A2 EP 89201988 A EP89201988 A EP 89201988A EP 89201988 A EP89201988 A EP 89201988A EP 0357113 A2 EP0357113 A2 EP 0357113A2
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EP
European Patent Office
Prior art keywords
grains
grain size
range
varistors
resistance material
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.)
Granted
Application number
EP89201988A
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German (de)
English (en)
Other versions
EP0357113B1 (fr
EP0357113A3 (en
Inventor
Detlef Dr. Hennings
Rüdiger Hartung
Piet Prof. Dr. Reijnen
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Philips Intellectual Property and Standards GmbH
Koninklijke Philips NV
Original Assignee
Philips Patentverwaltung GmbH
Philips Gloeilampenfabrieken NV
Koninklijke Philips Electronics NV
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Publication of EP0357113A2 publication Critical patent/EP0357113A2/fr
Publication of EP0357113A3 publication Critical patent/EP0357113A3/de
Application granted granted Critical
Publication of EP0357113B1 publication Critical patent/EP0357113B1/fr
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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
    • H01C7/10—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
    • 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
    • H01C7/105—Varistor cores
    • H01C7/108—Metal oxide
    • H01C7/112—ZnO type
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01C—RESISTORS
    • H01C17/00—Apparatus or processes specially adapted for manufacturing resistors
    • H01C17/30—Apparatus or processes specially adapted for manufacturing resistors adapted for baking

Definitions

  • the invention relates to a method for producing a non-linear voltage-dependent resistor with a ceramic sintered body based on the oxides of titanium, bismuth and at least one transition metal containing zinc oxide as the resistance material, wherein the sintered body by deforming the powdery resistance material and then sintering in air at a temperature in Range from 1200 to 1350 o C and then provided with electrodes.
  • ⁇ current index, non-linearity coefficient or control factor; it depends on the material and is a measure of the steepness of the current-voltage characteristic; typical values are in the range from 20 to 80.
  • Varistors are used in many ways to protect electrical systems, devices and expensive components against voltages and voltage peaks.
  • the response voltage U A of varistors is in the order of 3 V to 3000 V; it is usually defined as the voltage at which a current density of 1 mA / cm2 is reached in the varistor.
  • low-voltage varistors are increasingly required, whose response voltage U A is below approximately 30 V and which have the highest possible values for the non-linearity coefficient ⁇ . The larger the value for the non-linearity coefficient ⁇ , the better the effect as a surge limiter and the lower the power consumption of the varistor.
  • Zinc oxide-based varistors have sintered bodies which are produced from materials in which components are provided which act as donor doping and thus make the zinc oxide grains semiconducting, and which also contain components such as titanium dioxide and bismuth oxide. Titanium dioxide additives promote grain growth and thus reduce the response voltage U A.
  • the interior of the polycrystalline ZnO grains becomes low-resistance and high-resistance barriers form at the grain boundaries due to the addition of bismuth oxide.
  • the contact resistance between two grains is relatively high at voltages ⁇ 3.2 V, but decreases at voltages> 3.2 V with increasing voltage by several orders of magnitude.
  • the response voltage U A of varistors is essentially determined by the number of grain boundaries that the current I must pass between the electrodes.
  • Low-voltage varistors must therefore either consist of very thin layers with only a few grain boundaries per layer or of materials with very coarse grains. While thin varistor layers made of ceramic based on zinc oxide have so far hardly been used for technical reasons due to a lack of mechanical stability, varistors with coarse-grained sintered bodies based on zinc oxide are the usual way of producing low-voltage varistors.
  • Sintered bodies made of doped zinc oxide with a relatively coarse grain structure with grain sizes> 100 ⁇ m are obtained, for example, when material of the ZnO-Bi2O3 system is mixed with about 0.3 to about 1 mol% TiO2.
  • the TiO2 addition promotes the reactivity between the liquid Bi2O3 and the solid ZnO phase and accelerates the grain growth of the ZnO.
  • the disadvantage is that relatively long, rod-shaped ZnO crystallites often form here, which make it very difficult to check the microstructure of the ceramic structure.
  • the grain density in the structure of the sintered body (number of large grains / volume) is directly proportional to the number of seed nuclei added to the unsintered ceramic mass.
  • the invention has for its object to provide varistors and in particular low-voltage varistors, which have a sintered body with an improved structural homogeneity and thus an improved mechanical and electrical stability.
  • the powdery resistance material comprises grains of resistance material prebaked at a temperature in the range from 1200 to 1400 ° C. (hereinafter also referred to as “prebaked grains”) with an average grain size in the range from 4 to 12 ⁇ m and in one Amount of 1 to 50% by weight can be added.
  • the invention is based on the following finding:
  • the causes of the electrical degradation and the mechanical destruction of varistors based on zinc oxide with pulse loading are not yet sufficiently known. However, it can be assumed that an inhomogeneity of the microstructure leads to an uneven distribution of the energy in the varistor under pulse load. With an uneven distribution of the grain sizes and the grain boundary phases, there is then a partial electrical overload and degradation of individual grains in the varistor.
  • grains are added to the resistance material in an amount of 3 to 15% by weight and preferably an average grain size of 6 and / or 4.3 ⁇ m. If grains of pre-fired resistance material with an average grain size of ⁇ 6 ⁇ m are added to the unfired resistance mass, a sintered body with a relatively fine-grained structure and a grain size distribution within relatively narrow limits is obtained. The grain size distribution is homogeneous over the entire sintered body and compensates for fluctuations in the density of the unfired green body.
  • zinc oxide with an addition of the oxides of titanium, antimony, bismuth, manganese, cobalt and nickel is used as the powdery resistance material.
  • Zinc oxide with an average grain size in the range from 0.7 to 1 ⁇ m is preferably used.
  • the selection of the grain size range from 0.7 to 1 ⁇ m is advantageous because the resistance material thereby becomes more reactive during sintering, which promotes natural nucleation and supports the growth-regulating influence exerted by the prebaked grains.
  • a conventional starting mass for varistors based on zinc oxide with an average grain size in the range of 0.7 to 1 ⁇ m with the addition of about 1 to 5 wt.% Bi2O3, about 0.5 wt.% Sb2O3, about 0.5 wt % Mn2O3, about 0.5% by weight of CoO and about 0.5% by weight of TiO2 according to the present process with different amounts of prebaked grains of the same composition with an average grain size in the range of 4 to 12 ⁇ m, so it can be with small amounts of 1 to 3% by weight of the additive, a drastic decrease in the "giant grains" otherwise present in such masses after sintering can be found in the microstructure.
  • the average grain size in sintered bodies from starting materials produced in this way by the present process does not differ significantly from that of sintered bodies which were sintered under the same conditions, but without the addition of prebaked grains from the resistance material with a defined grain size .
  • the structure of sintered bodies produced by the present method is much more homogeneous than that of sintered bodies produced by the known method. This means that the grain growth of the individual grains proceeds more evenly during the sintering process if the present method is used.
  • the average grain size With the addition of grains with an average grain size of 12 ⁇ m in an amount of up to 3% by weight, the average grain size remains constant, with additions of> 3 to 7% by weight, the average grain size within the structure of the sintered body increases by a factor ⁇ 2 observed. With additions in the range> 7 to ⁇ 20% by weight, the average grain size in the structure of the sintered body decreases again continuously.
  • the structure or the microstructure of such sintered bodies are relatively homogeneous.
  • the grain density (number of large grains / volume) in sintered bodies produced by the present method does not increase proportionally, but rather to the third power of the added number of grains of a defined narrow grain size range.
  • the added grains of a defined narrow grain size range influencing the microstructure of the sintered bodies produced according to the present method therefore do not represent seed germs for increasing the growth of individual grains, but rather represent additives with a growth-regulating influence.
  • the individual improvements were as follows: When adding 3 to 15% by weight of the additives mentioned from pre-fired grains with an average grain size of 12 ⁇ m, the values for the nonlinearity coefficient ⁇ increased by about 20%.
  • the result was adjustable values for the response voltage U A , irrespective of the sintering temperature and the sintering time, with the addition of grains of a defined average grain size range from 4.3 to 12 ⁇ m in an amount of 7 to 50% by weight in the range from 30 V to 200 V with a thickness of the sintered body of 1 mm.
  • the values for the response voltage U A were halved when prebaked grains with a grain size of 12 ⁇ m were added in an amount of 7% by weight.
  • a particular advantage in the case of varistors produced by the present method is a minimization of the standard deviations of the values for the nonlinearity coefficient ⁇ and the response voltage U A by a factor of 5 to 10 compared to the values in the case of varistors produced by known methods.
  • Another particular advantage of the varistors produced by the present method is the increase in their electrical and mechanical stability when subjected to electrical impulses.
  • the production of a starting mass for a ceramic sintered body for a varistor based on zinc oxide is described as an exemplary embodiment.
  • the starting mass was mixed by mixing 950 g ZnO, 15 g Bi2O3, 10 g Co3O4, 15 g NiCO3.2 Ni (OH) 2.4 H2O, 5 g TiO2, 8 g Mn3O4, 1 g Sb2O3 and 5 g H3BO3 in a ball mill produced.
  • the same oxide mixture as for the starting mass is granulated with an aqueous dilute solution of polyvinyl alcohol and then prebaked as granules in an open Al2O3 crucible over a period of 2 h at a temperature of 1350 o C.
  • the pre-fired mass is ground in a ball mill over a period of 12 h to an average grain size of ⁇ 100 ⁇ m.
  • Grain fractions from the prebaked, ground oxide mixture, which are to be used as an additive to green starting materials, are produced in a sedimentation column.
  • a 0.1% aqueous solution of Na4P2O7.10 H2O is used as the medium for sedimentation.
  • the following grain fractions were produced: I: 12 ⁇ m; (10%> 16.5 ⁇ m, 10% ⁇ 8.5 ⁇ m) II: 6 ⁇ m; (10%> 8.9 ⁇ m, 10% ⁇ 5.8 ⁇ m) III: 4.3 ⁇ m; (10%> 5.5 ⁇ m, 10% ⁇ 3.7 ⁇ m).
  • the grain fractions I, II and III were then wet-mixed with the starting mass prepared as described above in the ratios: Mix 1) 1: 100 Mix 2) 3: 100 Mix 3) 7: 100 Mix 4) 15: 100 Mix 5) 100: 100.
  • the powder mixtures were mechanically pressed at a pressure of 1700 bar to cylindrical bodies with a diameter of 15 mm and a thickness of 1.8 mm.
  • the green density was about 55% of the theoretical density.
  • the compacts were then sintered in air at sintering temperatures T S in the range from 1200 o C to 1350 o C and a duration of the maximum temperature t in the range from 30 to 480 min. Is advantageously a heating rate during sintering of 40 o C / min; it has been shown that the rate of heating during sintering is directly proportional to the number of nuclei formed here.
  • the density of the sintered bodies was 90 to 97% of the theoretical density. After sintering, the sintered bodies had a diameter in the range from 13 to 13.5 mm and a thickness of 1.2 mm.
  • Metal layer electrodes were applied as electrodes, preferably in the form of Cr-Ni / Au layers, which were reinforced by tin or conductive silver layers for some measurements.
  • the measurement of the electrical characteristic data nonlinearity coefficient ⁇ and response voltage U A took place in the range from 10 ⁇ 5 to 10 ⁇ 2 A.
  • the response voltage U A was defined as the voltage (V / mm) standardized to 1 mm sintered body thickness, at which a current density in the varistor of 1 mA / cm2 occurs.
  • Table 1 shows values for the non-linearity coefficient ⁇ and the response voltage U A for samples of the compositions I1 to I5, II2, II3 and III2, which were sintered at sintering temperatures T S of 1200, 1275 and 1350 o C, the maximum sintering temperature in each case was held over a duration t of 30, 60, 120, 240 and 480 min.
  • Table 2 shows the statistical scatter of the values for the nonlinearity coefficient ⁇ and the response voltage U A of varistors, the sintered bodies of the compositions I3 and II3 have compared to a varistor with a sintered body without the addition of pre-fired grains (sample "0").
  • Varistors with sintered bodies with the addition of prebaked grains with an average grain size of 12 ⁇ m in an amount of 6.5% by weight showed, under appropriate test conditions, an average reduction in the values for the response voltage U A measured in the pulse direction by only up to 20% and counter Pulse direction measured by only up to 40%.

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  • Engineering & Computer Science (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Manufacturing & Machinery (AREA)
  • Thermistors And Varistors (AREA)
  • Compositions Of Oxide Ceramics (AREA)
EP89201988A 1988-08-03 1989-07-28 Procédé de production d'une résistance non linéaire dépendant de la tension Expired - Lifetime EP0357113B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3826356A DE3826356A1 (de) 1988-08-03 1988-08-03 Verfahren zur herstellung eines nichtlinearen spannungsabhaengigen widerstandes
DE3826356 1988-08-03

Publications (3)

Publication Number Publication Date
EP0357113A2 true EP0357113A2 (fr) 1990-03-07
EP0357113A3 EP0357113A3 (en) 1990-03-21
EP0357113B1 EP0357113B1 (fr) 1994-01-12

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EP89201988A Expired - Lifetime EP0357113B1 (fr) 1988-08-03 1989-07-28 Procédé de production d'une résistance non linéaire dépendant de la tension

Country Status (4)

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EP (1) EP0357113B1 (fr)
JP (1) JPH0279402A (fr)
KR (1) KR0126468B1 (fr)
DE (2) DE3826356A1 (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0507517A2 (fr) * 1991-03-30 1992-10-07 Kabushiki Kaisha Toshiba Interrupteur et résistance de puissance
EP0594120A2 (fr) * 1992-10-20 1994-04-27 Matsushita Electric Industrial Co., Ltd. Une méthode de fabrication d'une varistance type ZnO
EP0762438A2 (fr) * 1995-09-07 1997-03-12 Mitsubishi Denki Kabushiki Kaisha Elément de résistance électrique à caractéristiques de tension nonlinéaire et méthode de fabrication

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19509075C2 (de) * 1995-03-14 1998-07-16 Daimler Benz Ag Schutzelement für einen elektrochemischen Speicher sowie Verfahren zu dessen Herstellung
BRPI0701878A2 (pt) * 2007-07-25 2009-03-10 Univ Fed De Santa Catarina Ufsc sistema de anÁlise de degradaÇço de varistores de àxido de zinco (zno) utilizando os parÂmetros do modelo langevin modificado

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3950274A (en) * 1973-09-27 1976-04-13 General Electric Company Process for making a low voltage varistor
JPS5457699A (en) * 1977-10-18 1979-05-09 Matsushita Electric Ind Co Ltd Manufacturing method of voltage non-linear resistor
JPS60169103A (ja) * 1984-02-10 1985-09-02 株式会社明電舎 電圧非直線抵抗体

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3950274A (en) * 1973-09-27 1976-04-13 General Electric Company Process for making a low voltage varistor
JPS5457699A (en) * 1977-10-18 1979-05-09 Matsushita Electric Ind Co Ltd Manufacturing method of voltage non-linear resistor
JPS60169103A (ja) * 1984-02-10 1985-09-02 株式会社明電舎 電圧非直線抵抗体

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
CHEMICAL ABSTRACTS, Band 104, Nr. 20, Mai 1986, Seite 672, Zusammenfassung Nr. 178543h, Columbus, Ohio, US; & JP-A-60 169 103 (MEIDENSHA ELECTRIC Mfg. CO., LTD) 02-09-1985 *
J. APPL. PHYS., Band 54, Nr. 2, Februar 1983, Seiten 1095-1099, American Institute of Physics, New York, NY, US; K. EDA et al.: "Grain growth control in ZnO varistors using seed grains" *
PATENT ABSTRACTS OF JAPAN, Band 3, Nr. 78 (E-121), 5. Juli 1979, Seite 148 E 121; & JP-A-54 57 699 (MATSUSHITA DENKI SANGYO K.K.) 09-05-1979 *

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0507517A2 (fr) * 1991-03-30 1992-10-07 Kabushiki Kaisha Toshiba Interrupteur et résistance de puissance
EP0507517A3 (en) * 1991-03-30 1993-05-05 Kabushiki Kaisha Toshiba Power circuit breaker and power resistor
US5254816A (en) * 1991-03-30 1993-10-19 Kabushiki Kaisha Toshiba Power circuit breaker and power resistor
EP0594120A2 (fr) * 1992-10-20 1994-04-27 Matsushita Electric Industrial Co., Ltd. Une méthode de fabrication d'une varistance type ZnO
EP0594120A3 (fr) * 1992-10-20 1995-07-26 Matsushita Electric Ind Co Ltd Une méthode de fabrication d'une varistance type ZnO.
EP0762438A2 (fr) * 1995-09-07 1997-03-12 Mitsubishi Denki Kabushiki Kaisha Elément de résistance électrique à caractéristiques de tension nonlinéaire et méthode de fabrication
EP0762438A3 (fr) * 1995-09-07 1997-12-10 Mitsubishi Denki Kabushiki Kaisha Elément de résistance électrique à caractéristiques de tension nonlinéaire et méthode de fabrication
US5807510A (en) * 1995-09-07 1998-09-15 Mitsubishi Denki Kabushiki Kaisha Electric resistance element exhibiting voltage nonlinearity characteristic and method of manufacturing the same

Also Published As

Publication number Publication date
DE58906686D1 (de) 1994-02-24
KR0126468B1 (ko) 1997-12-22
DE3826356A1 (de) 1990-02-08
EP0357113B1 (fr) 1994-01-12
JPH0279402A (ja) 1990-03-20
KR900003919A (ko) 1990-03-27
EP0357113A3 (en) 1990-03-21

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