JP3822798B2 - Voltage nonlinear resistor and porcelain composition - Google Patents

Voltage nonlinear resistor and porcelain composition Download PDF

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Publication number
JP3822798B2
JP3822798B2 JP2001040847A JP2001040847A JP3822798B2 JP 3822798 B2 JP3822798 B2 JP 3822798B2 JP 2001040847 A JP2001040847 A JP 2001040847A JP 2001040847 A JP2001040847 A JP 2001040847A JP 3822798 B2 JP3822798 B2 JP 3822798B2
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atomic
compound
ca
sr
converted
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Japanese (ja)
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JP2002246207A (en
Inventor
明久 松田
典之 神津
将典 長野
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太陽誘電株式会社
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Description

[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a voltage nonlinear resistor and a resistor ceramic composition mainly composed of zinc oxide (Zn0) suitable as a resistor for an overvoltage protection element.
[0002]
[Prior art]
A voltage non-linear resistor mainly composed of Zn0 generally has a low limiting voltage, a large voltage ratio linear coefficient, and the like, and an electronic device configured with a low overcurrent withstand capability such as a semiconductor element It is widely used as a varistor for the purpose of overvoltage protection.
[0003]
Various subcomponents are added to the voltage nonlinear resistor mainly composed of Zn0 in order to improve the characteristics. In Japanese Patent Publication No. 1-25205, Zn0 is a main component, and at least one rare earth element as a subcomponent is added in a total amount of 0.08 to 5.0 atomic%,
0.1 to 10.0 atomic percent of Co,
0.01-5.0 atomic% of at least one of Mg and Ca,
0.01-1.0 atomic% in total of at least one kind of K, Cs, Rb,
0.01 to 1.0 atomic% of Cr,
B is 0.0005 to 0.1 atomic%,
0.0001 to 0.05 atomic% in total amount of at least one of Al, GA, and In,
It is disclosed that it is added to improve the long-wave tail surge resistance.
[0004]
Japanese Patent Application Laid-Open No. 9-326305 discloses that Zn0 is a main component and at least one rare earth element as a subcomponent is added in a total amount of 0.08 to 5.0 atomic%,
0.1 to 10.0 atomic percent of Co,
0.1 to 0.5 atomic% of Ca,
0.01 to 1.0 atomic% of at least one of K, Cs, and Rb,
0.1 to 0.6 atomic percent of Cr,
Add at least one of Al, Ga and In in a total amount of 0.0004 to 0.03 atomic%, and add 0.0005 to 0.1 atomic% of B (boron) to the above components, and allow It is disclosed to increase power.
[0005]
[Problems to be solved by the invention]
By the way, subcomponents disclosed in the above two publications include K (potassium) and B (boron). K and B are supplied with these oxides or compounds that can become oxides during the firing process during the manufacture of the voltage nonlinear resistor. However, since the oxides of K and B have a low melting point and are easily scattered during the firing process, the variation in characteristics inevitably increases.
[0006]
Accordingly, an object of the present invention is to provide a voltage non-linear resistor that can be manufactured while suppressing variations in electrical characteristics, has a small change in leakage current, and has little asymmetric deterioration in the electric charging life characteristics, and a porcelain composition therefor Is to provide.
[0007]
[Means for Solving the Problems]
The present invention for solving the above problems and achieving the above object comprises a main component composed of ZnO (zinc oxide) and a subcomponent added to the main component,
The accessory component is
Pr (praseodymium) 0.05 to 3.00 atomic%,
Co (cobalt) 0.1-5.0 atomic%,
0.01 to 0.50 atomic% of Cr (chromium),
0.001 to 0.020 atomic% of at least one of Al (aluminum), Ga (gallium), and In (indium),
0.001 to 0.500 atomic% for Si (silicon) and 0.01 to 0.50 atomic% for Ca + Sr (where Ca / Sr is 0 to 50)
And does not contain K (potassium) and B (boron), and is related to a voltage nonlinear resistor.
[0008]
The composition for obtaining the resistor comprises a main component composed of ZnO (zinc oxide) and a subcomponent added to the main component,
The accessory component is
0.05 to 3.00 atomic% in terms of Pr compound converted to Pr (praseodymium),
0.1 to 5.0 atomic% when the Co compound is converted to Co (cobalt),
0.01 to 0.50 atomic% in terms of Cr compound converted to Cr (chromium),
0.001 to 0.020 atomic% by converting at least one of the Al compound, Ga compound and In compound into Al (aluminum), Ga (gallium) and In (indium),
The Si compound is converted into Si (silicon), 0.001 to 0.500 atomic%, and the Ca compound + Sr compound is converted into Ca + Sr (where Ca / Sr is 0 to 50), 0.01 to 0.00. 50 atomic%
And does not contain K (potassium) and B (boron) .
[0009]
【The invention's effect】
The invention of each claim has the following effects.
(1) Since it does not contain K (potassium) and B (boron) that are likely to scatter, variation in the characteristics of the voltage nonlinear resistor during mass production can be suppressed.
(2) K and B are not included, but Si and M (Ca, Sr) are included in a predetermined range, so that deterioration of various electrical characteristics is prevented, and leakage current variation and asymmetric degradation are suppressed in the charging life characteristics. Can be achieved. The reason why the charging life characteristics are improved by the subcomponent according to the present invention is not clear, but it is recognized that the subcomponent according to the present invention is segregated at the triple point of the sintered body, and is an element that hardly enters the crystal grains. It is thought that this is due to something. Thus, it is considered that the migration of interstitial Zn ions is suppressed when the sub-component element exists in the vicinity of the grain boundary. Since the above migration is considered to be involved in characteristic deterioration, the present invention reduces characteristic deterioration.
[0010]
Embodiment and Examples
Next, embodiments, examples, and comparative examples of the present invention will be described with reference to Tables 1 to 5 and FIG. In each table, the composition ratio of subcomponents expressed in atomic%, the ratio of Ca and Sr, and various characteristics are shown. Incidentally, △ V 1 mu column of A + is characteristic during forward, - denotes the characteristic in the negative direction.
[0011]
In order to obtain a voltage nonlinear resistor according to the present invention and the comparative example, zinc oxide ZnO powder as a main component and Pr (praseodymium), Co (cobalt), Cr (chromium), Al (aluminum) as subcomponents or Each compound of Ga (gallium) or In (indium), Si (silicon), Ca (calcium), and Sr (strontium) was prepared. Each of the subcomponent compounds is composed of praseodymium oxide Pr 6 O 11 , cobalt oxide Co 3 O 4 , chromium oxide Cr 2 O 3 , aluminum oxide Al 2 O 3 or gallium oxide Ga 2 O 3, or indium oxide In 2 O. 3 , silicon oxide SiO 2 , calcium carbonate CaCO 3, and strontium carbonate SrCO 3 . That is, the Zn0 as the main component to obtain a non-linear resistor according to the present invention, the Pr 6 O 11 as a secondary component in terms of Pr from .05 to 3.00 atomic%,
Co 3 O 4 is converted to Co, 0.1 to 5.0 atomic%,
0.01 to 0.50 atomic% in terms of Cr 2 O 3 converted to Cr,
Al 2 O 3 or a Ga 2 O 3 or In 2 O 3 in terms of Al or Ga, or an In 0.001 to 0.020 atomic%,
0.001 to 0.500 atomic% in terms of SiO 2 converted to Si,
CaCO 3 + SrCO 3 in terms of Ca + Sr is 0.01 to 0.50 atomic%
Many added porcelain compositions, ie porcelain materials, were prepared as shown in Tables 1 to 4. Moreover, the porcelain material of the comparative example shown in Table 1-Table 5 was prepared similarly.
In addition, the atomic% of the subcomponent in Table 1 to Table 5 (converted as a percentage of the metal element or Si) is defined such that the number of Zn atoms is 100, and Pr, Co, Cr, Al or Ga or the number of Zn atoms is It is shown by the ratio of the number of atoms of In, Ca, Sr. For example, the composition of the metal element and Si of sample number 2 can be expressed by the following chemical formula, that is, the composition formula.
Zn 100 Pr 0.02 Co 2.0 Cr 0.2 Al 0.005 Si 0.2 Ca 0.2 Sr 0.2
Zn0 is not shown in the samples of Tables 1 to 5, but Zn is 100 atomic%.
Sample numbers marked with * in Tables 1 to 5 indicate comparative examples.
[0012]
[Table 1]
[0013]
[Table 2]
[0014]
[Table 3]
[0015]
[Table 4]
[0016]
[Table 5]
[0017]
Next, an organic binder, an organic solvent, and an organic plasticizer were added to the porcelain material of each sample and mixed for 24 hours by a ball mill to prepare a slurry.
Next, using each slurry, a ceramic green sheet having a thickness of 30 μm was prepared by a doctor blade method, and a conductive paste made of palladium paste was screen-printed on this sheet to form a conductor layer for internal electrodes. Next, two green sheets are stacked so that a pair of internal electrodes can be obtained, and a dummy green sheet is stacked on top and bottom to form a laminate, and these are heated and pressed to form a predetermined chip shape. Into green chips. The green chip was debindered at 300 ° C. for 3 hours and then fired at 1200 ° C. for 2 hours to obtain a sintered body.
FIG. 1 shows a sintered body represented by first, second and third layers 1, 2, 3, first and second internal electrodes 4, 5 and first and second external terminal electrodes 6. , 7 is a varistor (voltage non-linear resistance element). The first layer 1 made of a voltage nonlinear resistor disposed between the first and second internal electrodes 4 and 5 is non-linear when a voltage is applied to the first and second internal electrodes 4 and 5. Shows sexual resistance. In this example, the second and third layers 2 and 3 are also voltage non-linear resistors, but some or all of them are made of porcelain having no voltage non-linearity, or the second and third layers. The layers 2 and 3 can also be omitted.
The first and second external terminal electrodes 6 and 7 are formed by applying an electrode paste mainly composed of Ag to the end face of each sintered body and baking at 800 ° C. The first and second external terminal electrodes 6 and 7 are electrically connected to the first and second internal electrodes 4 and 5.
[0018]
The sintered body according to the present invention is a porcelain resistor containing Pr, Co, Cr, Al or Ga or In, Si, Ca + Sr or Sr at a ratio specified in the claims with respect to Zn0. In addition, each element of a subcomponent is contained in the sintered compact after baking in the form of each oxide.
[0019]
The characteristics of each sample are as follows: varistor voltage V 1mA (V / mm) per 1 mm thickness when 1 mA is passed between the external electrodes 6 and 7 of the varistor of each sample configured as shown in FIG. Was measured, and the varistor voltage V 10 mA (V / mm) per 1 mm thickness was measured, and the non-linear coefficient α was obtained by the following equation.
α = log (10/1) / log ( V10mA / V1mA )
[0020]
In order to measure the service life characteristics, a dc constant voltage corresponding to 90% of V lmA was applied to the varistor of each sample for 500 hours in dry air at 85 ° C., and a current of 1 μA was applied before and after the application . the rate of change of the inter-electrode voltage V l μ a △ sought V l μ a. Incidentally, in the case where a current flows in the positive direction (+ direction), backward - was determined both in passing (direction) of △ V l μ A.
[0021]
As is apparent from Tables 1 to 5, the varistor having the composition according to the present invention has a nonlinear coefficient α of 20 or more, a varistor voltage V 1mA of 400 (V / mm) or more, a charging life characteristic, that is, a leakage current change rate ΔV. 1 mu a has the target properties of + 10%-10%. Further, according to the present invention, the difference due to the polarity of the leakage current change rate [Delta] V 1 mu A is reduced. That is, asymmetric deterioration is reduced. In addition, variation in characteristics between varistors during mass production is reduced.
[0022]
As is clear from Sample Nos. 2 to 4, the above target characteristics can be obtained when Pr is in the range of 0.05 to 3.0 atomic%, but as shown in Sample Nos. 1 and 5, Pr is 0.02 It becomes atomic% and 4.0 atomic%, alpha and [Delta] V 1 mu a deviates from the target characteristics. Therefore, the preferred amount of Pr is 0.05 to 3.0 atomic%.
[0023]
As is clear from Sample Nos. 7 and 8, the target characteristics can be obtained when Co is 0.1 and 5.0 atomic%, but as shown in Sample Nos. 6 and 9, Co is 0.05 and 6 When the 2.0 atomic%, alpha and [Delta] V 1 mu a deviates from the target characteristics. Accordingly, the preferred amount of Co is 0.1 to 5.0 atomic percent.
[0024]
As is clear from sample numbers 11 and 12, the target characteristics are obtained when Cr is 0.01 and 0.5 atomic%, but as is clear from sample numbers 10 and 13, Cr is 0.005 and 0. In the case of .6, not all items can fit in the target characteristics. Therefore, the preferable amount of Cr is 0.01 to 0.5 atomic%.
[0025]
As is clear from sample numbers 15, 16, 32, 33, 34, 37, 38, and 39, when Al, Ga, or In is 0.001 to 0.02 atomic%, target characteristics are obtained. As apparent from the numbers 14, 17, 31, 35, 36, and 40, when these are 0.0005 and 0.003 atomic%, not all items can be set as the target characteristics. Therefore, the preferred amount of Al, Ga or In is 0.001 to 0.02 atomic%.
[0026]
As is clear from sample numbers 19 and 20, the target characteristics can be obtained when Si is 0.001 and 0.5 atomic%, but as shown in sample numbers 18 and 21, Si is 0.0005 and 0. At 6 atomic%, all items cannot be included in the target characteristics. Accordingly, the preferred amount of Si is 0.001 to 0.5 atomic percent.
[0027]
As is clear from sample numbers 23, 24, 25, 26, 27, and 28, when Ca + Sr is 0.01 to 0.5 atomic% and the ratio Ca / Sr of Ca to Sr is 50 or less, Although the target characteristics can be obtained, as shown in sample numbers 22, 29, and 30, all items cannot be included in the target characteristics if the above conditions are not met. Therefore, the preferable amount of Ca + Sr is 0.001 to 0.5 atomic%.
[0028]
Although not shown in the above table, instead of Al 0.02 atomic% of sample number 16, Al 0.005 atomic% + Ga 0.005 atomic% + In 0.005%, and other varistors identical to sample number 16 were used. As a result of making and measuring the characteristics, almost the same characteristics as the material number 16 were obtained. Moreover, when the varistor which made the total of Al, Ga, and In or two total arbitrarily selected from these fall in the range of 0.001-0.02 atomic%, and measured these characteristics, The target characteristics were obtained.
Further, when many varistors having the same composition were prepared and the variation in characteristics was determined, the variation according to the present invention was smaller than that outside the scope of the present invention.
[0029]
[Modification]
The present invention is not limited to the above-described embodiment, and for example, the following modifications are possible.
(1) The subcomponent can be supplied as a compound or elemental element different from the oxide or carbonate of each element.
(2) The varistor structure can be different from that shown in FIG. For example, an electrode may be provided on one main surface and the other main surface of a plate-shaped voltage nonlinear resistor to form a varistor.
[Brief description of the drawings]
FIG. 1 is a cross-sectional view showing a varistor according to an embodiment of the present invention.
[Explanation of symbols]
1 Voltage Nonlinear Resistance Layers 4, 5 Internal Electrodes 6, 7 External Terminal Electrodes

Claims (2)

  1. It consists of a main component made of ZnO (zinc oxide) and a subcomponent added to this main component,
    The accessory component is
    Pr (praseodymium) 0.05 to 3.00 atomic%,
    Co (cobalt) 0.1-5.0 atomic%,
    0.01 to 0.50 atomic% of Cr (chromium),
    0.001 to 0.020 atomic% of at least one of Al (aluminum), Ga (gallium), and In (indium),
    0.001 to 0.500 atomic% for Si (silicon) and 0.01 to 0.50 atomic% for Ca + Sr (where Ca / Sr is 0 to 50)
    And a non-linear resistor having no K (potassium) and B (boron) .
  2. It consists of a main component made of ZnO (zinc oxide) and a subcomponent added to this main component,
    The accessory component is
    0.05 to 3.00 atomic% in terms of Pr compound converted to Pr (praseodymium),
    0.1 to 5.0 atomic% when the Co compound is converted to Co (cobalt),
    0.01 to 0.50 atomic% in terms of Cr compound converted to Cr (chromium),
    0.001 to 0.020 atomic% by converting at least one of the Al compound, Ga compound and In compound into Al (aluminum), Ga (gallium) and In (indium),
    The Si compound is converted into Si (silicon), 0.001 to 0.500 atomic%, and the Ca compound + Sr compound is converted into Ca + Sr (where Ca / Sr is 0 to 50), 0.01 to 0.00. 50 atomic%
    And a non-linear resistor-resistor ceramic composition characterized by not containing K (potassium) and B (boron) .
JP2001040847A 2001-02-16 2001-02-16 Voltage nonlinear resistor and porcelain composition Expired - Fee Related JP3822798B2 (en)

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