CN102424577A - Low voltage varistor ceramic material and preparation method thereof - Google Patents

Low voltage varistor ceramic material and preparation method thereof Download PDF

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CN102424577A
CN102424577A CN2011102788932A CN201110278893A CN102424577A CN 102424577 A CN102424577 A CN 102424577A CN 2011102788932 A CN2011102788932 A CN 2011102788932A CN 201110278893 A CN201110278893 A CN 201110278893A CN 102424577 A CN102424577 A CN 102424577A
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base
low voltage
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CN102424577B (en
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王�华
巨锦华
许积文
袁昌来
张小文
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Guilin University of Electronic Technology
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Abstract

The invention discloses a low voltage varistor ceramic material and a preparation method thereof. The low voltage varistor ceramic material is realized by adding V2O5 and TiO2 simultaneously into a ZnO-Bi2O3 base low voltage varistor ceramic and sintered by a traditional ceramics. A material proportion is as below: a molar ratio of V2O5 to TiO2 to ZnO-Bi2O3 base is 0.05-0.08:0.80-1.30:98.62-99.15, wherein the ZnO-Bi2O3 base comprises components of ZnO, Bi2O3, Co2O3 and MnCO3, and a molar ratio of ZnO to Bi2O3 to Co2O3 to MnCO3 is 97.40-98.20:0.60-0.80:0.80-1.20:0.40-0.60. The invention has advantages of : (1) Ti doping can increase a nonlinear coefficient of a varistor ceramic material and reduce a potential gradient; (2) V doping can reduce a sintering temperature of the ceramic material, save energy consumption and lower cost; (3) pre-burning can enhance powder activity; (4) a technology of segment heating and insulation can enhance quality and performance of the ceramic, reduce energy consumption and save cost.

Description

A kind of low voltage varistor stupalith and preparation method thereof
Technical field
The present invention relates to piezoceramic material, specifically is a kind of low voltage varistor stupalith and preparation method thereof.
Background technology
The ZnO voltage-sensitive ceramic is with advantages such as its nonlinear factor are high, response speed is fast, leakage current is little, residual voltage is low, cheap for manufacturing cost; Become one of piezoresistive material that application is the widest, performance is best, be widely used in fields such as electric power, communication, traffic, unicircuit, automotive electronics, medical equipment and household electrical appliance.ZnO varistor is mainly used in the above circuit of WV 110V before 1975; Low voltage varistor begins to be applied afterwards; And constantly to low pressureization, miniaturized development, its Application Areas is constantly expansion, and its market demand is at present just with average annual about 25% rate increase.
At present, low voltage varistor pottery ultralow potential gradient of forward and low-temperature sintering direction develop, to adapt to industry demand and energy-saving and cost-reducing needs.But low-temperature sintering and low electric potential gradient are a pair of contradiction of mutual restriction.Therefore, development of new high-performance low voltage varistor stupalith and low temperature preparation technology thereof just become inevitable.In the low voltage varistor stupalith, ZnO-Bi 2O 3System be research at present the most extensively, one of the most sophisticated low pressure system, better performances, but sintering temperature generally is higher than 1000 ℃.People have also carried out some trials to the low temperature preparation method of zinc oxide pressure-sensitive ceramic in recent years.As: application number is 200910273178.2 Chinese invention patent, discloses a kind of at ZnO-Bi 2O 3-TiO 2Be the method for adding 0.4～3wt% bismuth boron glass in the piezoresistive material, its sintering temperature is at 850-950 ℃, but its potential gradient is still up to 210V/mm; Name is called the Chinese invention patent of " a kind of method of preparing high-potential gradient zinc oxide piezoresistive material by low-temperature sintering " [invention number: 200510110414.0], through in ZnO, adding Bi 2O 3, Sb 2O 3, Cr 2O 3, Co 2O 3, MnO 2And Y 2O 3Deng rare earth oxide, be implemented in 800 ℃ of following sintering, but prepared zinc oxide pressure-sensitive ceramic belongs to the high potential gradient pressure-sensitive resistive material, be not suitable for the preparation of low voltage varistor ceramics.
Summary of the invention
The object of the invention is to the deficiency of prior art, and a kind of low voltage varistor stupalith and preparation method thereof is provided, and this based varistor material nonlinearity coefficient is higher and potential gradient is lower, and is the low temperature sintering.
Low voltage varistor stupalith provided by the invention is at ZnO-Bi 2O 3Add V simultaneously in the base low voltage varistor ceramics 2O 5And TiO 2Realize materials amount V 2O 5︰ TiO 2︰ ZnO-Bi 2O 3The mol ratio of base is 0.05-0.08 ︰ 0.80-1.30 ︰ 98.62-99.15, wherein ZnO-Bi 2O 3Base comprises ZnO, Bi 2O 3, Co 2O 3, MnCO 3Moity, and ZnO ︰ Bi 2O 3︰ Co 2O 3︰ MnCO 3Mol ratio be 97.40-98.20 ︰ 0.60-0.80 ︰ 0.80-1.20 ︰ 0.40-0.60.
A kind of preparation method of low voltage varistor stupalith comprises the steps:
(1) by following moity and molar content weighing configuration raw material: V 2O 5, TiO 2And ZnO-Bi 2O 3The mol ratio of base is 0.05-0.08: 0.80-1.30: 98.62-99.15, wherein ZnO-Bi 2O 3Base moity ZnO, Bi 2O 3, Co 2O 3And MnCO 3Mol ratio be 97.40-98.20: 0.60-0.80: 0.80-1.20: 0.40-0.60.
(2) with the absolute ethyl alcohol be solvent, will be by the load weighted ZnO of composition proportion, Bi 2O 3, Co 2O 3And MnCO 3After the raw materials mix in ball mill with the speed ball milling 12-14h of 260-300r/min;
(3) add by the load weighted V of composition proportion 2O 5And TiO 2Ball milling 10-12h again behind the nano powder takes out the back in 100-120 ℃ of baking 8-10h;
(3) the final powder behind the ball milling is at 650-700 ℃ of following pre-burning 2.0-2.5h;
(4) to add concentration be that 5% an amount of polyvinyl alcohol water solution carries out granulation as tackiness agent to the powder after the pre-burning, granulation after 150 mesh sieve;
(5) screen underflow presses down the disk green compact of processing diameter 15mm, the about 1.7mm of thickness at 80MPa;
(6) ceramic green is under air ambient; Speed with 5-8 ℃/min is warming up to 600-650 ℃, insulation 1.5-2.0h, and the speed with 20-25 ℃/min is warming up to 880-900 ℃ then; Naturally cooling behind the insulation 2.0-2.5h can obtain required low voltage varistor pottery.
The optimum molar proportioning of above-mentioned raw materials is: V 2O 5, TiO 2And ZnO-Bi 2O 3The mol ratio of base is 0.06: 1.10: 98.84, wherein ZnO-Bi 2O 3Base moity ZnO, Bi 2O 3, Co 2O 3And MnCO 3Mol ratio be 97.80: 0.7 0:1.00: 0.50.
The optimum parameter of above-mentioned processing condition is: ball milling speed: 280r/min, ZnO, Bi 2O 3, Co 2O 3And MnCO 3The ball milling time of mixed powder: 13h adds V 2O 5And TiO 2After the ball milling time: 9h, the calcined temperature of final powder behind the ball milling: 630 ℃, the pre-burning time: 2.2h; Ceramic green is warming up to 680 ℃ with the speed of 6 ℃/min under air ambient, insulation 1.8h, and the speed with 23 ℃/min is warming up to 890 ℃ then, naturally cooling behind the insulation 2.2h.
Advantage of the present invention is: (1) Ti mixes and can improve the nonlinear factor of pressure-sensitive ceramic material, reduces potential gradient; (2) V mixes and can reduce the sintering temperature of stupalith, and energy efficient, reduces cost; (3) pre-burning can strengthen powder active; The technology of (4) temperature-gradient method, insulation can improve the quality and the performance of pottery, cuts down the consumption of energy simultaneously, practices thrift cost.
Description of drawings
Fig. 1 V, Ti codope ZnO-Bi 2O 3Base low voltage varistor ceramic material process flow sheet;
X-ray diffraction (XRD) figure of Fig. 2 instance 1 low voltage varistor stupalith;
Fig. 3 instance 1 low voltage varistor stupalith J- EPerformance diagram.
Embodiment
Embodiment 1:
(1) adopt following raw material moity and content its preparing materials thereof:
V 2O 50.06 mole, 10.913 grams
TiO 21.10 mole, 87.888 grams
96.666 moles of ZnO, 7866.582 grams
Bi 2O 30.692 mole, 322.442 grams
Co 2O 30.988 mole, 163.873 grams
MnCO 30.494 mole, 56.783 grams
Wherein: V 2O 5: TiO 2: ZnO-Bi 2O 3The mol ratio of base is 0.06: 1.10: 98.84; ZnO-Bi 2O 3Base moity ZnO: Bi 2O 3: Co 2O 3: MnCO 3Mol ratio be 97.8 0: 0.70: 1.00: 0.50.
(2) with the absolute ethyl alcohol solvent, with load weighted ZnO, Bi 2O 3, Co 2O 3And MnCO 3After the raw materials mix in ball mill with the speed ball milling 13h of 280r/min, add V 2O 5And TiO 2After ball milling 11h again, take out the back in 100 ℃ of baking 10h;
(3) the final powder behind the ball milling is at 630 ℃ of following pre-burning 2.2h;
(4) to add concentration be that 5% an amount of polyvinyl alcohol water solution carries out granulation as tackiness agent to the powder after the pre-burning, granulation after 150 mesh sieve;
(5) screen underflow presses down the disk green compact of processing diameter 15mm, the about 1.7mm of thickness at 80MPa;
(6) ceramic green is under air ambient, is warming up to 680 ℃ with the speed of 6 ℃/min, insulation 1.8h, and the speed with 23 ℃/min is warming up to 890 ℃ then, and naturally cooling behind the insulation 2.2h can obtain required low voltage varistor pottery.
For prepared based varistor sample is carried out electric performance test, need roughly grind sample surfaces, fine grinding handles, then by silver and under 600 ℃, carry out silver ink firing and handle 60min, can obtain test electrode.
Embodiment 2:
(1) adopt following raw material moity and content its preparing materials thereof:
V 2O 50.07 mole, 12.731 grams
TiO 21.00 mole, 79.898 grams
96.951 moles of ZnO, 7889.775 grams
Bi 2O 30.594 mole, 276.778 grams
Co 2O 30.989 mole, 164.039 grams
MnCO 30.396 mole, 45.519 grams
Wherein: V 2O 5: TiO 2: ZnO-Bi 2O 3The mol ratio of base is 0.07: 1.00: 98.93; ZnO-Bi 2O 3Base moity ZnO: Bi 2O 3: Co 2O 3: MnCO 3Mol ratio be 98.00: 0.60: 1.00: 0.4.
(2) with the absolute ethyl alcohol solvent, with load weighted ZnO, Bi 2O 3, Co 2O 3And MnCO 3After the raw materials mix in ball mill with the speed ball milling 14h of 260r/min, add V 2O 5And TiO 2After ball milling 12h again, take out the back in 120 ℃ of baking 8h;
(3) the final powder behind the ball milling is at 650 ℃ of following pre-burning 2.5h;
(4) to add concentration be that 5% an amount of polyvinyl alcohol water solution carries out granulation as tackiness agent to the powder after the pre-burning, granulation after 150 mesh sieve;
(5) screen underflow presses down the disk green compact of processing diameter 15mm, the about 1.7mm of thickness at 80MPa;
(6) ceramic green is under air ambient, is warming up to 600 ℃ with the speed of 5 ℃/min, insulation 2.0h, and the speed with 20 ℃/min is warming up to 880 ℃ then, and naturally cooling behind the insulation 2.5h can obtain required low voltage varistor pottery.
All the other are with embodiment 1.
Embodiment 3:
(1) adopt following raw material moity and content its preparing materials thereof:
V 2O 50.08 mole, 14.550 grams
TiO 21.20 mole, 95.878 grams
96.449 moles of ZnO, 7848.923 grams
Bi 2O 30.691 mole, 321.976 grams
Co 2O 31.086 mole, 180.127 grams
MnCO 30.494 mole, 56.783 grams
Wherein: V 2O 5: TiO 2: ZnO-Bi 2O 3The mol ratio of base is 0.08: 1.20: 98.72; ZnO-Bi 2O 3Base moity ZnO: Bi 2O 3: Co 2O 3: MnCO 3Mol ratio be 97.70: 0.70: 1.10: 0.50.
(2) with the absolute ethyl alcohol solvent, with load weighted ZnO, Bi 2O 3, Co 2O 3And MnCO 3After the raw materials mix in ball mill with the speed ball milling 12h of 300r/min, add V 2O 5And TiO 2After ball milling 10h again, take out the back in 110 ℃ of baking 9h;
(3) the final powder behind the ball milling is at 700 ℃ of following pre-burning 2.0h;
(4) to add concentration be that 5% an amount of polyvinyl alcohol water solution carries out granulation as tackiness agent to the powder after the pre-burning, granulation after 150 mesh sieve;
(5) screen underflow presses down the disk green compact of processing diameter 15mm, the about 1.7mm of thickness at 80MPa;
(6) ceramic green is under air ambient, is warming up to 650 ℃ with the speed of 8 ℃/min, insulation 1.5h, and the speed with 25 ℃/min is warming up to 900 ℃ then, and naturally cooling behind the insulation 2.0h can obtain required low voltage varistor pottery.
All the other are with embodiment 1.
To V, Ti codope ZnO-Bi 2O 3The structure and the performance test of base low voltage varistor stupalith are following:
1.V, Ti codope ZnO-Bi 2O 3The phase structure of base low voltage varistor stupalith
Adopt X-ray diffraction (XRD) to test V, Ti codope ZnO-Bi at ambient temperature 2O 3The phase structure of base low voltage varistor stupalith, the result is as shown in Figure 1.The principal crystalline phase of this ceramic material sample is consistent with ZnO, but has micro-Bi 2O 3Reach Bi mutually 4Ti 3O 12Phase.Explain that V, Ti codoped do not change the phase structure of material, V, Ti get in the material lattice with the solid solution mode.
2. V, Ti codope ZnO-Bi 2O 3The salient features of base low voltage varistor stupalith
At ambient temperature, adopt the potential gradient of CJ1001 type voltage dependent resistor dc parameter appearance to prepared based varistor U 1mA, nonlinear factor a, leakage current I LTest respectively, the result is as shown in table 1.
3. the strength of electric field of instance 1 sample-current density relation curve is as shown in Figure 3.Curve is divided into two zones by flex point among the figure: one is the linearity region before puncturing, and another is the nonlinear area after puncturing.Knee voltage is pressure sensitive voltage, with the ratio of thickness of sample be exactly potential gradient U 1mANonlinear area is very smooth in the curve, and interpret sample has non-linear behaviour preferably.
 
Table 1 V, Ti codope ZnO-Bi 2O 3The potential gradient of base low voltage varistor pottery U 1mA, nonlinear factor aAnd leakage current I L
Sample Potential gradient U 1mA(V/mm) Nonlinear factor a Leakage current I L(μA)
Instance 1 22.2 31.6 0.15
Instance 2 28.4 29.8 0.32
Instance 3 23.6 33.2 0.20
Though the present invention is with preferred embodiment openly as above, and non-limiting the present invention, any those skilled in the art is not breaking away from the spirit and scope of the present invention, and the suitable improvement of being done is all in protection scope of the present invention.

Claims (5)

1. low voltage varistor stupalith, it is characterized in that: this based varistor material is at ZnO-Bi 2O 3Add V simultaneously in the base low voltage varistor ceramics 2O 5And TiO 2Realize materials amount V 2O 5︰ TiO 2︰ ZnO-Bi 2O 3The mol ratio of base is 0.05-0.08 ︰ 0.80-1.30 ︰ 98.62-99.15.
2. stupalith according to claim 1 is characterized in that: said ZnO-Bi 2O 3Base is by ZnO, Bi 2O 3, Co 2O 3, MnCO 3Form materials amount ZnO ︰ Bi 2O 3︰ Co 2O 3︰ MnCO 3Mol ratio be 97.40-98.20 ︰ 0.60-0.80 ︰ 0.80-1.20 ︰ 0.40-0.60.
3. stupalith according to claim 1 and 2 is characterized in that: the mole proportioning of said raw material is: V 2O 5: TiO 2: ZnO-Bi 2O 3The mol ratio of base is 0.06: 1.10: 98.84, wherein ZnO-Bi 2O 3Base moity ZnO: Bi 2O 3: Co 2O 3: MnCO 3Mol ratio be 97.80: 0.7 0: 1.00: 0.50.
4. the preparation method of a low voltage varistor stupalith is characterized in that: comprise the steps:
(1) by following moity and molar content weighing configuration raw material: V 2O 5: TiO 2: ZnO-Bi 2O 3The mol ratio of base is 0.05-0.08: 0.80-1.30: 98.62-99.15, wherein ZnO-Bi 2O 3Base moity ZnO: Bi 2O 3: Co 2O 3: MnCO 3Mol ratio be 97.40-98.20: 0.60-0.80: 0.80-1.20: 0.40-0.60;
(2) with the absolute ethyl alcohol be solvent, will be by the load weighted ZnO of composition proportion, Bi 2O 3, Co 2O 3And MnCO 3After the raw materials mix in ball mill with the speed ball milling 12-14h of 260-300r/min;
(3) add by the load weighted V of composition proportion 2O 5And TiO 2Ball milling 10-12h again behind the nano powder takes out the back in 100-120 ℃ of baking 8-10h;
(3) the final powder behind the ball milling is at 650-700 ℃ of following pre-burning 2.0-2.5h;
(4) to add concentration be that 5% an amount of polyvinyl alcohol water solution carries out granulation as tackiness agent to the powder after the pre-burning, granulation after 150 mesh sieve;
(5) screen underflow presses down the disk green compact of processing diameter 15mm, the about 1.7mm of thickness at 80MPa;
(6) ceramic green is under air ambient; Speed with 5-8 ℃/min is warming up to 600-650 ℃, insulation 1.5-2.0h, and the speed with 20-25 ℃/min is warming up to 880-900 ℃ then; Naturally cooling behind the insulation 2.0-2.5h obtains required low voltage varistor pottery.
5. preparation method according to claim 4 is characterized in that: the parameter of processing condition is: ball milling speed: 280r/min, ZnO, Bi 2O 3, Co 2O 3And MnCO 3The ball milling time of mixed powder: 13h adds V 2O 5And TiO 2After the ball milling time: 9h, the calcined temperature of final powder behind the ball milling: 630 ℃, the pre-burning time: 2.2h; Ceramic green is warming up to 680 ℃ with the speed of 6 ℃/min under air ambient, insulation 1.8h, and the speed with 23 ℃/min is warming up to 890 ℃ then, naturally cooling behind the insulation 2.2h.
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103964837A (en) * 2014-04-30 2014-08-06 内蒙古科技大学 Voltage-sensitive ceramic resistor
CN106747408A (en) * 2016-12-23 2017-05-31 西安理工大学 A kind of TiO2The preparation method of base low-pressure pressure-sensitive ceramic material
CN110483100A (en) * 2019-08-22 2019-11-22 广西优艾斯提传感技术有限公司 A kind of aging technique of ceramic chip
CN110563457A (en) * 2019-09-05 2019-12-13 华南理工大学 nitrogen ion doped zinc oxide-based piezoresistor and preparation method thereof
CN112694324A (en) * 2020-12-14 2021-04-23 襄阳市三三电气有限公司 Zinc oxide nonlinear resistance card and preparation method thereof

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CN101704668A (en) * 2009-12-03 2010-05-12 陕西科技大学 ZnO ceramic resistor and preparation method thereof
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CN101265083A (en) * 2008-04-21 2008-09-17 上海大学 Rare earth nitrate doping zinc oxide pressure-sensitive ceramic material and preparation method thereof
CN102087898A (en) * 2009-12-02 2011-06-08 常州星翰科技有限公司 Method for preparing zinc oxide varistor by using pure silver as inner electrode
CN101704668A (en) * 2009-12-03 2010-05-12 陕西科技大学 ZnO ceramic resistor and preparation method thereof

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103964837A (en) * 2014-04-30 2014-08-06 内蒙古科技大学 Voltage-sensitive ceramic resistor
CN106747408A (en) * 2016-12-23 2017-05-31 西安理工大学 A kind of TiO2The preparation method of base low-pressure pressure-sensitive ceramic material
CN106747408B (en) * 2016-12-23 2019-11-22 西安理工大学 A kind of TiO2The preparation method of base low-pressure pressure-sensitive ceramic material
CN110483100A (en) * 2019-08-22 2019-11-22 广西优艾斯提传感技术有限公司 A kind of aging technique of ceramic chip
CN110563457A (en) * 2019-09-05 2019-12-13 华南理工大学 nitrogen ion doped zinc oxide-based piezoresistor and preparation method thereof
CN112694324A (en) * 2020-12-14 2021-04-23 襄阳市三三电气有限公司 Zinc oxide nonlinear resistance card and preparation method thereof

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