CN116655368B - Preparation method of resistor disc capable of improving high-current impact resistance - Google Patents

Preparation method of resistor disc capable of improving high-current impact resistance Download PDF

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CN116655368B
CN116655368B CN202310602540.6A CN202310602540A CN116655368B CN 116655368 B CN116655368 B CN 116655368B CN 202310602540 A CN202310602540 A CN 202310602540A CN 116655368 B CN116655368 B CN 116655368B
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powder
resistor disc
zno
mixing
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CN116655368A (en
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董建洪
陈伟
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Jiaxing Ruijia Electric Co ltd
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Jiaxing Ruijia Electric Co ltd
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Abstract

The invention discloses a preparation method of a resistor disc capable of improving high-current impact resistance, and belongs to the technical field of resistor disc preparation. Firstly, respectively preparing a raw material A and a raw material B of a resistor disc, and sequentially pouring blank making powder A, blank making powder B and blank making powder A into a die cavity of a press to obtain blank making powder; pressing and molding the obtained blank-making powder to obtain a blank; calcining the green body at high temperature after the gel discharging treatment to obtain a resistor disc green body; and carrying out heat treatment on the resistor disc blank to obtain the finished ZnO varistor. The resistance sheet prepared by the method obviously improves the high-current impact resistance.

Description

Preparation method of resistor disc capable of improving high-current impact resistance
Technical Field
The invention relates to the technical field of resistor disc preparation, in particular to a resistor disc preparation method for improving the high-current impact resistance.
Background
The ZnO varistor is a resistor device with nonlinear volt-ampere characteristics, and is mainly used for voltage clamping when a circuit is subjected to overvoltage, and absorbing redundant current to protect devices connected in parallel. When the ZnO resistor disc is impacted by large current, a voltage critical value exists in the resistor disc, when the applied voltage is lower than the critical voltage, the passing current is small, the resistor disc resistance value is large, when the applied voltage is higher than the critical voltage, the resistor is rapidly reduced, the current passing through the resistor disc is exponentially increased, and excellent nonlinear characteristics are presented.
When a short-time large current passes through the resistor disc, the energy passing through the resistor disc also increases exponentially, and huge internal stress is generated inside the resistor disc. In the existing green pressing process, because the granular powder has certain friction force, the pressure is gradually lost towards the middle part during pressing, the density of the middle part or the middle lower part of the powder blank is minimum, the diameter of the middle part of the sintered blank is slightly smaller than that of the upper end and the lower end, and therefore, the resistance of the middle part is slightly larger, and the situation is more serious in a resistor sheet with large thickness. When the resistor is impacted by large current, the current density flowing through the middle part of the resistor is maximum, and the bearing energy is maximum, so that the probability of bursting of the resistor is increased.
Disclosure of Invention
The invention aims to provide a preparation method of a resistor disc capable of improving the high-current impact resistance, and the resistor disc prepared by the method obviously improves the high-current impact resistance.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a resistor disc for improving the high-current impact resistance comprises the following steps:
(1) Preparing raw materials for preparing the resistor disc:
the preparation raw materials of the resistor disc comprise raw materials A and raw materials B, wherein the raw materials A comprise the following components in percentage by weight: znO 82-92%, bi 2 O 3 2～4％，Sb 2 O 3 2～4％，NiO 0～5％，Cr 2 O 3 0～2％，Mn 3 O 4 0.5～4％，Co 3 O 4 0.5～5％，SiO 2 0-2%, glass powder 0-2%;
the raw material B comprises the following components in percentage by weight: 80-90% of ZnO and Bi 2 O 3 3～5％，Sb 2 O 3 1～3％，NiO 0～5％，Cr 2 O 3 0～2％，Mn 3 O 4 0.5～4％，Co 3 O 4 0.5～5％，SiO 2 0-2%, glass powder 0-2%;
(2) Preparing blank powder A:
mixing the components except ZnO in the raw material A with deionized water, stirring, grinding and mixing for 2-6h, and drying and crushing the obtained mixed slurry into powder to obtain a mixed powder material; mixing the powder material with ZnO, al (NO) 3 ) 3 ·9H 2 Mixing O with deionized water, adding a dispersing agent and a binder, stirring and grinding for 1-3 hours to obtain mixed slurry, wherein the particle size of the mixed slurry reaches 0.5-2 mu m; spraying, granulating and aging the obtained mixed slurry to obtain blank powder A;
(3) Preparing blank powder B:
mixing other components except ZnO in the raw material B with deionized water, stirring, grinding and mixing for 2-6h, and drying and crushing the obtained mixed slurry into powder to obtain a mixed powder material; mixing the powder material with ZnO, al (NO) 3 ) 3 ·9H 2 Mixing O with deionized water, adding a dispersing agent and a binder, stirring and grinding for 1-3 hours to obtain mixed slurry, wherein the particle size of the mixed slurry reaches 0.5-2 mu m; spraying, granulating and aging the obtained mixed slurry to obtain blank powder B;
(4) Pressing a blank: pouring the blank making powder A, the blank making powder B and the blank making powder A into a die cavity of a press in sequence to obtain blank making powder; pressing and molding the obtained blank-making powder to obtain a blank;
(5) Sintering a green body: the green body is subjected to glue discharging treatment (pre-calcination treatment) and then is subjected to high-temperature calcination to obtain a resistor disc green body; and carrying out heat treatment on the resistor disc blank to obtain the finished ZnO varistor.
In the steps (2) - (3), the spray granulation is carried out by adopting a spray dryer to carry out spray granulation on the mixed slurry to obtain granules; the aging treatment is to supplement proper amount of water to the granular materials collected by a 30-120 mesh screen, so that the mass percentage water content of the powder reaches 1.0-1.5%, and then the powder is sealed and kept stand for 24-48 hours to obtain blank making powder A or blank making powder B.
In the step (4), the blank making powder A poured into the die cavity of the press for the first time accounts for 30% -45% of the total amount of powder required by the blank; the poured blank-making powder B accounts for 10% -40% of the total powder required by the blank; the second poured blank-making powder A accounts for 30% -45% of the total powder required by the blank.
In the step (4), the pressure of the press is controlled so that the density of the formed blank is 3.1-3.4g/cm < 3 >.
In the step (5), the glue discharging treatment is to perform the glue discharging treatment on the green body at 420-520 ℃ so as to discharge the organic matters in the green body.
In the step (5), the high-temperature combustion temperature is 1000-1200 ℃ and the calcination time is at least 1.5h.
In the step (5), the resistor blank after high-temperature calcination is sequentially subjected to grinding, cleaning and drying, a sample is subjected to heat treatment at 500-520 ℃ for 0.5-2 hours after being dried and glass glaze or organic insulating paint is applied, and then metal electrodes are prepared on the upper surface and the lower surface of the sample, so that the finished ZnO varistor is obtained.
In the above steps (2) - (3), al (NO) is added 3 ) 3 ·9H 2 O is 0.02-0.05% of the weight of the prepared blank powder A or blank powder B; the amount of the dispersant added is 0.3-1.3% of the weight of the prepared blank powder A or blank powder B; the amount of the binder added is 0.2-1.5% of the weight of the prepared green compact powder A or green compact powder B.
The average grain size of the middle part of the ZnO varistor ceramic body prepared by the method is 6-12 mu m and slightly larger than the average grain size of the upper end and the lower end by 5-11 mu m.
The design principle and the beneficial effects of the invention are as follows:
1. in the green compact pressing stage, the distribution of Bi and Sb in the green compact is adjusted by a sectional feeding mode, so that the grain size of the middle part of the fired resistor disc porcelain body is slightly larger than that of the upper end and the lower end, and the bearing energy of the middle part of the resistor disc is minimum when large current is impacted, the tensile stress of the resistor disc is reduced, the cracking probability of the resistor disc is reduced, and the resistor disc can bear larger impact current;
2. according to the method, the preparation process of the existing resistor disc is optimized and adjusted on the basis of the original piezoresistor disc formula, the high-current impact resistance of the prepared resistor disc is obviously improved, and other electrical performance parameters of the resistor disc are basically unchanged.
Drawings
FIG. 1 is an SEM photograph of the upper end porcelain of a ZnO varistor.
FIG. 2 is an SEM photograph of the porcelain body of the middle part of the ZnO varistor.
FIG. 3 is an SEM photograph of the lower porcelain of the ZnO varistor.
Detailed Description
For a further understanding of the present invention, the present invention is described below with reference to the examples, which are only illustrative of the features and advantages of the present invention and are not intended to limit the scope of the claims of the present invention.
Example 1:
the preparation process of the resistor disc of the embodiment is as follows:
a. preparing raw materials for preparing the resistor disc:
the raw materials A and B are prepared according to the mass percentage of the components by adopting the following raw material formula:
the formula of the raw material A comprises the following components: 90.1wt.% ZnO, bi 2 O 3 2.3wt.％，Sb 2 O 3 2.0wt.％，Mn 3 O 4 1.5wt.％，Co 3 O 4 1.2wt.％，NiO 1.0wt.％，Cr 2 O 3 0.5wt.％，SiO 2 0.5wt.% glass frit 0.9wt.%.
The formula of the raw material B comprises the following components: 90.1wt.% ZnO, bi 2 O 3 2.5wt.％，Sb 2 O 3 1.8wt.％，Mn 3 O 4 1.5wt.％，Co 3 O 4 1.2wt.％，NiO 1.0wt.％，Cr 2 O 3 0.5wt.％，SiO 2 0.5wt.% glass frit 0.9wt.%.
b. Preparation of the slurry:
b1. mixing the raw materials A prepared in the step a except ZnO with deionized water, performing vertical stirring and ball milling for mixing for 4 hours, and drying and crushing the obtained mixed slurry into powder to obtain a mixed powder material;
b2. mixing the mixed powder material obtained in the step b1 with ZnO and Al (NO 3 ) 3 ·9H 2 Mixing O with deionized water, adding a dispersing agent and a binder, stirring and grinding for 2 hours to enable the particle size of the mixed slurry to reach 1.2 mu m; added Al (NO) 3 ) 3 ·9H 2 O is 0.028wt% of the weight of the green compact powder A in the step b 3; the amount of the dispersant added is 1.0% of the weight of the prepared blank powder A; the amount of the binder added was 0.8% by weight based on the weight of the prepared green powder A.
b3. Spraying and granulating the mixed slurry prepared in the step b2 by adopting a spray dryer to obtain granules, ageing the sieved and collected granules for 24 hours to ensure that the mass percent water content of the powder is 1.3 percent, and obtaining blank-making powder A; the aging treatment is to supplement proper amount of water to the granular materials collected by a 30-120 mesh screen, so that the mass percentage water content of the powder reaches 1.3%, and then seal and stand for 24 hours to obtain blank-making powder A.
b4. Mixing the raw materials except ZnO of the raw material B prepared in the step a with deionized water, stirring, grinding and mixing for 4 hours, and drying and crushing the obtained mixed slurry into powder to obtain a mixed powder material;
b5. mixing the mixed powder material obtained in the step b4 with ZnO and Al (NO 3 ) 3 ·9H 2 Mixing O with deionized water, adding a dispersing agent and a binder, stirring and grinding for 2 hours to enable the particle size of the mixed slurry to reach 1.2 mu m; added Al (NO) 3 ) 3 ·9H 2 O is 0.028wt% of the total amount of powder in step b 6; the amount of the dispersant added is 1.0% of the weight of the prepared blank powder B; the amount of the binder added was 0.8% by weight of the prepared green compact powder B.
b6. And c, performing spray granulation on the mixed slurry prepared in the step B2 by adopting a spray dryer to obtain granules, and aging the sieved and collected granules for 24 hours to ensure that the mass percent water content of the powder is 1.3% to obtain blank-making powder B. The aging treatment is to supplement proper amount of water to the granular materials collected by a 30-120 mesh screen, so that the mass percentage water content of the powder reaches 1.3%, and then seal and stand for 24 hours to obtain blank-making powder B.
c. Pressing a blank:
c1. pouring the powder A prepared in the step b3 into a die cavity of a press, wherein the amount of the poured powder is 40% of the total weight of the powder required by the blank;
c2. pouring the powder B prepared in the step B6 into a die cavity of a same press, wherein the amount of the poured powder is 20% of the total amount of the powder required by the blank;
c3. pouring the powder A prepared in the step b3 into a die cavity of a same press, wherein the amount of the poured powder is 40% of the total amount of the powder required by the blank;
c4. compacting the blank-making powder obtained in the steps c1-c3, and controlling the pressure so as to obtain the formed blank-making powderThe density of the obtained green body is 3.3g/cm 3 ；
d. The sintering process comprises the following steps:
d1. c, performing glue discharging treatment on the green body prepared in the step c at 480 ℃ to discharge organic matters in the green body;
d2. calcining the green body obtained through the pre-calcining treatment of the step d1 at a high temperature of 1080 ℃ for 2 hours to obtain a sintered resistor disc green body;
d3. and d2, grinding, cleaning and drying the resistor disc blank obtained in the step, spraying glass glaze on the dried sample, drying again, performing heat treatment at 510 ℃ for 1h, and spraying aluminum on the upper surface and the lower surface of the sample to obtain the finished ZnO varistor.
Test analysis:
the ZnO varistor prepared in this example was used as a test sample for experimental examination.
The diameter of the finished ZnO varistor prepared by the method of the embodiment is 40.5mm, and the thickness is 22.5mm.
The distribution of Bi and Sb in the green body was adjusted so that the average grain size of the intermediate portion of the fired resistor tile porcelain was about 8.5 μm, and the average grain sizes of the upper and lower ends were about 7.8 μm and 7.9 μm, respectively, as shown in FIGS. 1-3.
The voltage-sensitive potential gradient of the piezoresistor is 235V/mm, the nonlinear coefficient is 43, the lightning wave residual voltage ratio of 10kA 8/20 mu s is 1.71, and the highest value of the high-current surge current resisting for 2 times 4/10 mu s is 110kA.
Comparative example 1:
the preparation process of the resistor disc in this example comprises the following steps:
a. the formula of the raw materials comprises: 90.1wt.% ZnO, bi 2 O 3 2.34wt.％，Sb 2 O 3 1.96wt.％，Mn 3 O 4 1.5wt.％，Co 3 O 4 1.2wt.％，NiO 1.0wt.％，Cr 2 O 3 0.5wt.％，SiO 2 0.5wt.% glass frit 0.9wt.%.
b. Preparation of the slurry:
b1. mixing the raw materials prepared in the step a except ZnO with deionized water, performing vertical stirring ball milling and mixing for 4 hours, and drying and crushing the mixed slurry into powder to obtain a mixed powder material;
b2. mixing the mixed powder material obtained in the step b1 with ZnO and Al (NO 3 ) 3 ·9H 2 Mixing O with deionized water, adding a dispersing agent and a binder, stirring and grinding for 2 hours to enable the particle size of the mixed slurry to reach 1.2 mu m; added Al (NO) 3 ) 3 ·9H 2 O is 0.028wt% of the total amount of powder in step b 3;
b3. spraying and granulating the mixed slurry prepared in the step b2 by adopting a spray dryer to obtain granules, ageing the sieved and collected granules for 24 hours to ensure that the mass percent water content of the powder is 1.3 percent, and obtaining blank-making powder;
c. pressing a blank:
pouring the powder prepared in the step b3 into a die cavity of a press, performing compression molding, and controlling the pressure so that the density of a molded blank is 3.3g/cm < 3 >;
d. the sintering process comprises the following steps:
d1. c, performing glue discharging treatment on the green body prepared in the step c at 480 ℃ to discharge organic matters in the green body;
d2. calcining the green body obtained through the pre-calcining treatment of the step d1 at a high temperature of 1080 ℃ for 2 hours to obtain a sintered resistor disc green body;
d3. and d2, grinding, cleaning and drying the resistor disc blank obtained in the step, spraying glass glaze on the dried sample, drying again, performing heat treatment at 510 ℃ for 1h, and spraying aluminum on the upper surface and the lower surface of the sample to obtain the finished ZnO varistor.
Test analysis:
the ZnO varistor prepared in this example was used as a test sample for experimental examination.
The diameter of the finished ZnO varistor prepared by the method of the embodiment is 40.5mm, and the thickness is 22.5mm. The voltage-sensitive potential gradient of the piezoresistor is 236V/mm, the nonlinear coefficient is 46, the lightning wave residual voltage ratio of 10kA 8/20 mu s is 1.71, and the highest value of the current surge resistance of 2 times of 4/10 mu s is 80kA.
In summary, according to the method for preparing the resistor disc capable of improving the high-current impact resistance, the distribution of additives in the resistor disc blank body is improved by separately preparing the A, B material of the resistor disc and filling the material in batches before the blank body is pressed on the basis of not changing the original piezoresistor formula, so that the size distribution of crystal grains in the resistor disc porcelain body is improved, the bearing energy of the middle part of the resistor disc during high-current impact is reduced, the tensile stress in the resistor disc is reduced, and the resistor disc can bear larger impact current.

Claims (7)

1. A preparation method of a resistor disc for improving the high-current impact resistance is characterized by comprising the following steps: the method comprises the following steps:
(1) Preparing raw materials for preparing the resistor disc:
the preparation raw materials of the resistor disc comprise raw materials A and raw materials B, wherein the raw materials A comprise the following components in percentage by weight: 90.1wt.% ZnO, bi 2 O 3 2.3wt.％，Sb 2 O 3 2.0wt.％，Mn 3 O 4 1.5wt.％，Co 3 O 4 1.2wt.％，NiO 1.0wt.％，Cr 2 O 3 0.5wt.％，SiO 2 0.5wt.% glass frit 0.9wt.%;
the raw material B comprises the following components in percentage by weight: 90.1wt.% ZnO, bi 2 O 3 2.5wt.％，Sb 2 O 3 1.8wt.％，Mn 3 O 4 1.5wt.％，Co 3 O 4 1.2wt.％，NiO 1.0wt.％，Cr 2 O 3 0.5wt.％，SiO 2 0.5wt.% glass frit 0.9wt.%;
(2) Preparing blank powder A:
mixing the components except ZnO in the raw material A with deionized water, stirring, grinding and mixing for 2-6h, and drying and crushing the obtained mixed slurry into powder to obtain a mixed powder material; mixing the powder material with ZnO, al (NO) 3 ) 3 ·9H 2 Mixing O with deionized water, adding a dispersing agent and a binder, stirring and grinding for 1-3 hours to obtain mixed slurry, wherein the particle size of the mixed slurry reaches 0.5-2 mu m; spraying and granulating the obtained mixed slurry,Ageing to obtain blank powder A;
(3) Preparing blank powder B:
mixing other components except ZnO in the raw material B with deionized water, stirring, grinding and mixing for 2-6h, and drying and crushing the obtained mixed slurry into powder to obtain a mixed powder material; mixing the powder material with ZnO, al (NO) 3 ) 3 ·9H 2 Mixing O with deionized water, adding a dispersing agent and a binder, stirring and grinding for 1-3 hours to obtain mixed slurry, wherein the particle size of the mixed slurry reaches 0.5-2 mu m; spraying, granulating and aging the obtained mixed slurry to obtain blank powder B;
(4) Pressing a blank: pouring blank making powder A, blank making powder B and blank making powder A into a die cavity of a press in sequence, wherein the die cavity comprises the following concrete steps: the blank making powder A poured into the die cavity of the press for the first time accounts for 30% -45% of the total amount of powder required by the blank; the poured blank-making powder B accounts for 10% -40% of the total powder required by the blank; the second poured blank-making powder A accounts for 30% -45% of the total powder required by the blank; obtaining blank making powder; pressing and molding the obtained blank-making powder to obtain a blank;
(5) Sintering a green body: the green body is subjected to high-temperature calcination after being subjected to glue discharging treatment, wherein the high-temperature combustion temperature is 1000-1200 ℃, and the calcination time is at least 1.5h, so that a resistor disc green body is obtained; and carrying out heat treatment on the resistor disc blank to obtain the finished ZnO varistor.
2. The method for manufacturing a resistor sheet for improving high current surge resistance according to claim 1, wherein: in the steps (2) - (3), the spray granulation is carried out by adopting a spray dryer to carry out spray granulation on the mixed slurry so as to obtain granules; the aging treatment is to supplement proper amount of water to the granular materials collected by a 30-120 mesh screen, so that the mass percentage water content of the powder reaches 1.0-1.5%, and then the powder is sealed and kept stand for 24-48 hours to obtain blank making powder A or blank making powder B.
3. The method for manufacturing a resistor sheet for improving high current surge resistance according to claim 1, wherein: in the step (4), the pressure of the press is controlled so that the density of the formed blank is 3.1-3.4g/cm < 3 >.
4. The method for manufacturing a resistor sheet for improving high current surge resistance according to claim 1, wherein: in the step (5), the glue discharging treatment is to discharge organic matters in the green body by carrying out the glue discharging treatment on the green body at 420-520 ℃.
5. The method for manufacturing a resistor sheet for improving high current surge resistance according to claim 1, wherein: in the step (5), the resistor blank body calcined at high temperature is sequentially subjected to grinding, cleaning and drying, a sample is subjected to heat treatment at 500-520 ℃ for 0.5-2 hours after being dried and glass glaze or organic insulating paint is applied, and then metal electrodes are prepared on the upper surface and the lower surface of the sample, so that the finished ZnO varistor is obtained.
6. The method for manufacturing a resistor sheet for improving high current surge resistance according to claim 1, wherein: in the steps (2) - (3), al (NO) is added 3 ) 3 ·9H 2 The amount of O is 0.02-0.05% of the weight of the prepared blank powder A or blank powder B; the amount of the dispersant added is 0.3-1.3% of the weight of the prepared blank powder A or blank powder B; the amount of the binder added is 0.2-1.5% of the weight of the prepared green compact powder A or green compact powder B.
7. The method for manufacturing a resistor sheet for improving high current surge resistance according to claim 1, wherein: the average grain size of the middle part of the prepared ZnO varistor ceramic body is 6-12 mu m and slightly larger than the average grain sizes of the upper end and the lower end by 5-11 mu m.
CN202310602540.6A 2023-05-26 2023-05-26 Preparation method of resistor disc capable of improving high-current impact resistance Active CN116655368B (en)

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