CN104944935A - ZnO varister ceramic and preparation method thereof - Google Patents
ZnO varister ceramic and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a ZnO varister ceramic with high energy absorption capacity and a preparation method thereof. The ZnO varister ceramic is prepared through ball-milling, mixing, dry-pressing molding and atmosphere sintering of zinc oxide varister basic raw materials and a metal powder additive, wherein the following raw materials at molar ratio are included: 91.494-94.894 mol% of ZnO, 1.0-1.5 mol% of Bi2O3, 0.8-1.2 mol% of Sb2O3, 0.3-0.5 mol% of Cr2O3, 0.2-0.4 mol% of Ni2O3, 0.5-1.0 mol% of MnCO3, 0.5-1.5 mol% of SiO2, 0.5-1.0 mol% of Co2O3, 0.5-1.0 mol% of MgO and 0-0.006 mol% of Al(NO3)3.9H2O; the metal powder additive is one of Zn and Al and has the molar ratio of 0.08-3.0 mol%. According to the preparation method, after the atmosphere sintering process is added to the traditional sintering process, the low-current and high-current properties of a ZnO varister are effectively improved, the residual pressure performance is reduced, the high-current impact resistance is improved and the electrical performance is excellent.
Description
Technical field
The invention belongs to a kind of research of new varistor ceramics materials, particularly the interpolation of metal powder and atmosphere sintering process, belong to materials science field.
Background technology
Metal oxide (being mainly zinc oxide) thunder arrester is the key equipment of the anti-lightning strike and flashover fault of high pressure, supergrid and high voltage electric power equip ment, is widely used in ultra-high-tension power transmission line, city underground direct current supply line and power network system.The core component of direct current arrester is direct current zinc oxide varistor, and Zinc-oxide piezoresistor take zinc oxide as material of main part, by adding other trace element multiple, the poly semiconductor device made by conditional electronic ceramic process.Because of its fast response time, nonlinear factor is large, through-current capability is strong etc., and excellent electric property becomes rapidly the main raw manufacturing piezoresistor, is mainly used in overcurrent-overvoltage protecting circuit.The U.S., Japan and other countries have grasped rapidly at 20 century 70s the technology preparing Zinc-oxide piezoresistor, its electric property is broken through, thus is widely used in high-voltage power system.
The major function of Zinc-oxide piezoresistor is surge impact of releasing, and is restricted to by voltage for the harmless degree of protected electric installation.But voltage dependent resistor itself also can be subject to various surge impact, pressure sensitive voltage not only should be thermally-stabilised under steady state working voltage in this case, and after standing repeat impact, thermal runaway must can not occur, and its I-V index (volt-ampere characteristic) keeps being stabilized in original state.Current existing zinc oxide resistance sheet potential gradient is all at 180-200V/cm; the sharpest edges improving potential gradient in use can obtain higher protection voltage on less volume; be equivalent to the production cost reducing enterprise under identical condition, improve rate of profit.But suppose that the energy absorption capability of element remains unchanged, component size be reduced to original 1/2nd, the Energy value of the surge impact that element must be caused to keep out reduces to original half, therefore while its potential gradient improves, only improve its energy absorption capability (the two should meet growth in proportion substantially), effectively could improve the potential gradient of element, reach the object reducing volume.
The approach improving ZnO varistor electrical property is mainly divided into the optimization of formula and improvement two aspects of technique.The optimization of wherein filling a prescription comprises the adding proportion of adjustment additive, adds the doping vario-property element etc. that some are new.The improvement of technique comprises the adjustment of sintering temperature, the adjustment of silver ink firing temperature, and the aspect such as thermal treatment.But at present during doping vario-property, everybody for be the power dissipation characteristics in leakage current region of voltage dependent resistor, as improved potential gradient, improve nonlinear factor etc., less concern reduces voltage dependent resistor residual voltage when pressure sensitive voltage velocity of variation, and residual voltage ratio and pressure sensitive voltage velocity of variation are performance perameters very important in practical application.
Summary of the invention
The object of the invention is to, Zinc-oxide piezoresistor of a kind of high energy absorption capability and preparation method thereof is provided, the residual voltage ratio of voltage dependent resistor and pressure sensitive voltage velocity of variation index are significantly improved, are more suitable for practical application.
A kind of zinc oxide piezoresistor ceramic that the present invention proposes, is prepared from through ball mill mixing, dry pressing and atmosphere sintering by raw material and metal powder additive, it is characterized in that:
Described raw material and mol ratio are ZnO (91.494-94.894mol%), Bi
2o
3(1.0-1.5mol%), Sb
2o
3(0.8-1.2mol%), Cr
2o
3(0.3-0.5mol%), Ni
2o
3(0.2-0.4mol%), MnCO
3(0.5-1.0mol%), SiO
2(0.5-1.5mol%), Co
2o
3(0.5-1.0mol%), MgO (0.5-1.0mol%), Al (NO
3)
39H
2o (0-0.006mol%); Described metal powder additive is the one in Zn, Al, and its mol ratio is 0.08-3.0mol%.
Correspondingly, the present invention proposes this zinc oxide piezoresistor ceramic preparation method, it is characterized in that comprising the steps:
(1) pre-burning powder step is prepared:
Will except ZnO, Al (NO
3)
39H
2raw material outside O according to described molar ratio, with deionized water ball milling 4-8 hour after mixing, dry at 80-120 DEG C 3-4 hour, pulverize, cross 40-60 mesh sieve, gained mixed powder loads corundum crucible, and heating obtains pre-burning powder;
(2) atmosphere sintering forming step:
In described pre-burning powder, add Al (NO according to described molar ratio
3)
39H
2o, ZnO and metal powder additive, with deionized water ball milling 4-8 hour, dry, cross 60-80 mesh sieve, obtain ceramic powder after pulverizing at 100 DEG C-120 DEG C; In described ceramic powder, add and account for the PVA solution that its mass percent is 5 ~ 8%, described PVA solution mass percent is 3-5%; After dry-pressing slabbing under granulation, 8-10MPa pressure, at 1150 ~ 1200 DEG C of temperature, sinter 2 ~ 3 hours, obtain zinc oxide piezoresistor ceramic.
Preferably, in described preparation pre-burning powder step, pre-sinter process condition is heated to 700 ~ 800 DEG C with the temperature rise rate of 5 DEG C/min, and be incubated 1 ~ 2 hour, obtain preburning powder, the material obtained like this has better stable physics-chem characteristic.
Preferably, in described atmosphere sintering forming step, after sintering temperature reaches 500-600 DEG C, O is passed into
2atmosphere, allows pottery at O
2sintering is completed in atmosphere.Allow pottery at O
2complete sintering in atmosphere, form more metal interstitial ion, thus reduce grain resistance rate, reduce residual voltage ratio.
Further, in described atmosphere sintering forming step, burn till rear oxidation zinc based varistor thickness 2mm (± 0.10mm), diameter 13.30mm (± 0.05mm).
Further, utilize described zinc oxide piezoresistor ceramic, through abrasive disc, section, ultrasonic cleaning 10min, resistor disc two sides coated electrode after cleaning, at 600 DEG C, be incubated 10min, grid for welding goes between, after then using alcohol washes solder joint, coated organic insullac, makes zinc oxide varistor.Describedly it is characterized in that, the coated electrode of described zinc oxide varistor is copper, aluminium or silver electrode.
Based varistor prepared by the present invention, because the metal powder radius of doping is less than Zn ionic radius, metal ion enters in ZnO crystal grain, improve conducting carriers concentration thus reduce grain resistance rate, reduce residual voltage ratio, improve resistance to high current impulse withstanding capability, be more suitable for industrial application.But the Zn powder adulterating too much can produce bad impact to the aging resistance of ZnO voltage-sensitive ceramic, so Zn powder ratio wants appropriate.
Embodiment
Below by specific embodiment, further illustrate feature of the present invention and effect:
Reference examples:
Formula is: ZnO (94.894mol%), Bi
2o
3(1.0mol%), Sb
2o
3(1.0mol%), Cr
2o
3(0.4mol%), Ni
2o
3(0.2mol%), MnCO
3(0.5mol%), SiO
2(0.5mol%), Co
2o
3(0.5mol%), MgO (1.0mol%), Al (NO
3)
39H
2o (0.006mol%)
(1) preparation process of pre-burning powder:
Will except ZnO, Al (NO
3)
39H
2according to described mixed in molar ratio in Zinc-oxide piezoresistor raw material outside O, with deionized water ball milling 4 hours, 4 hours, pulverizing, excessively 40 mesh sieves is dried at 80 DEG C, then mixed powder is loaded corundum crucible, 750 DEG C are heated to the temperature rise rate of 5 DEG C/min, be incubated 2 hours, obtain preburning powder;
(2) ZnO varistor ceramic preparation step:
In the powder that step (1) obtains, add Al (NO according to formula
3)
39H
2o and ZnO, with deionized water ball milling 4 hours, dries at 120 DEG C of temperature, cross 80 mesh sieves after pulverizing, add the PVA solution of concentration 5%, the mass percent that solution accounts for powder is 5%, again after dry-pressing formed under granulation, 8MPa, at 1150 DEG C of temperature, burn 3 hours in atmosphere.Burn till rear ceramic plate thickness 2mm (± 0.10mm), diameter 13.30mm (± 0.05mm);
ZnO varistor sheet after sintering carries out abrasive disc, ultrasonic cleaning 10min, and the disk two sides coating Ag electrode after cleaning, is incubated 10min at 600 DEG C, welding lead, after then using alcohol washes solder joint, coated organic insullac, make zinc oxide varistor, can use.
Embodiment 1:
The present embodiment is that different Zn powder dopings affects Zinc-oxide piezoresistor, wherein Zn powder doping is respectively 0mol% (formula 1), 1mol% (formula 2), 2mol% (formula 3), 3mol% (formula 4).
Formula 1:ZnO (94.794mol%), Bi
2o
3(1.5mol%), Sb
2o
3(0.8mol%), Cr
2o
3(0.5mol%), Ni
2o
3(0.4mol%), MnCO
3(0.5mol%), SiO
2(0.5mol%), Co
2o
3(0.5mol%), MgO (0.5mol%), Al (NO
3)
39H
2o (0.006mol%)
Formula 2:ZnO (94.294mol%), Bi
2o
3(1.0mol%), Sb
2o
3(1.2mol%), Cr
2o
3(0.3mol%), Ni
2o
3(0.2mol%), MnCO
3(0.5mol%), SiO
2(0.5mol%), Co
2o
3(0.5mol%), MgO (0.5mol%), Al (NO
3)
39H
2o (0.006mol%), Zn (1mol%)
Formula 3:ZnO (92.394mol%), Bi
2o
3(1.0mol%), Sb
2o
3(1.0mol%), Cr
2o
3(0.4mol%), Ni
2o
3(0.2mol%), MnCO
3(1.0mol%), SiO
2(0.5mol%), Co
2o
3(1.0mol%), MgO (0.5mol%), Al (NO
3)
39H
2o (0.006mol%), Zn (2mol%)
Formula 4:ZnO (91.494mol%), Bi
2o
3(0.8mol%), Sb
2o
3(1.0mol%), Cr
2o
3(0.5mol%), Ni
2o
3(0.2mol%), MnCO
3(0.5mol%), SiO
2(1.5mol%), Co
2o
3(0.5mol%), MgO (0.5mol%), Al (NO
3)
39H
2o (0.006mol%), Zn (3mol%) (1) will except ZnO, Al (NO
3)
39H
2outside O and Zn powder, Zinc-oxide piezoresistor raw material is according to described mixed in molar ratio, with deionized water ball milling 8 hours, 3 hours, pulverizing, excessively 40 mesh sieves is dried at 120 DEG C, then mixed powder is loaded corundum crucible, 750 DEG C are heated to the temperature rise rate of 5 DEG C/min, be incubated 1 hour, obtain preburning powder;
(2), in the powder obtained in step (1), Al (NO is added according to basic components ratio
3)
39H
2o, ZnO and Zn powder, with deionized water ball milling 4 hours, dry at 100 DEG C of temperature, cross 60 mesh sieves after pulverizing, add the PVA solution of concentration 8%, the mass percent that solution accounts for powder is 3%, then after dry-pressing formed under granulation, 10MPa, at 1150 DEG C of temperature, sinters 2 hours.O is passed into after sintering temperature reaches 600 DEG C
2atmosphere, allows pottery at O
2sinter in atmosphere, burnt till rear ceramic plate thickness 2mm (± 0.10mm), diameter 13.30mm (± 0.05mm);
(3) the ZnO varistor sheet after sintering carries out abrasive disc, ultrasonic cleaning 10min, and the disk two sides coating Ag electrode after cleaning, is incubated 10min at 600 DEG C, welding lead, after then using alcohol washes solder joint, coated organic insullac, make zinc oxide varistor, can use.
Embodiment 2:
Adopt Al powder as additive in the present embodiment, wherein the doping ratio of Al is 0.08mol%.Experimental formula is: ZnO (94.894mol%), Bi
2o
3(1mol%), Sb
2o
3(0.8mol%), Cr
2o
3(0.5mol%), Ni
2o
3(0.226mol%), MnCO
3(0.5mol%), SiO
2(0.5mol%), Co
2o
3(0.5mol%), MgO (1mol%), Al (0.08mol%)
(1) will except ZnO, Zinc-oxide piezoresistor basic material outside Al powder is according to described mixed in molar ratio, with deionized water ball milling 4 hours, 3 hours, pulverizing, excessively 60 mesh sieves is dried at 100 DEG C, then mixed powder is loaded corundum crucible, be heated to 700 DEG C with the temperature rise rate of 5 DEG C/min, be incubated 2 hours, obtain preburning powder;
(2) in the powder obtained in step (1), ZnO and Al powder is added according to basic components ratio, with deionized water ball milling 8 hours, dry at 120 DEG C of temperature, cross 60 mesh sieves after pulverizing, add the PVA solution of concentration 8%, the mass percent that solution accounts for powder is 3%, again after dry-pressing formed under granulation, 8MPa, at 1200 DEG C of temperature, sinter 2 hours.O is passed into after sintering temperature reaches 500 DEG C
2atmosphere, allows pottery at O
2sinter in atmosphere, burnt till rear ceramic plate thickness 2mm (± 0.10mm), diameter 13.30mm (± 0.05mm);
ZnO varistor sheet after sintering carries out abrasive disc, ultrasonic cleaning 10min, and the disk two sides coating Ag electrode after cleaning, is incubated 10min at 600 DEG C, welding lead, after then using alcohol washes solder joint, coated organic insullac, make zinc oxide varistor, can use.
Embodiment 3:
Sintering process in the present embodiment is at N
2sinter in atmosphere, the formula 4 of filling a prescription in same embodiment 1.
(1) will except ZnO, Al (NO
3)
39H
2zinc-oxide piezoresistor basic material outside O and additive is according to mixed in molar ratio described in claim 1, with deionized water ball milling 4 hours, 4 hours, pulverizing, excessively 40 mesh sieves is dried at 90 DEG C, then mixed powder is loaded corundum crucible, 800 DEG C are heated to the temperature rise rate of 5 DEG C/min, be incubated 1 hour, obtain preburning powder;
(2), in the powder obtained in step (1), Al (NO is added according to basic components ratio
3)
39H
2o, ZnO and 3mol%Zn powder, with deionized water ball milling 4 hours, dry at 120 DEG C of temperature, cross 80 mesh sieves after pulverizing, add the PVA solution of concentration 5%, the mass percent that solution accounts for powder is 5%, then after dry-pressing formed under granulation, 8MPa, at 1190 DEG C of temperature, sinters 3 hours.N is passed into after sintering temperature reaches 500 DEG C
2atmosphere, allows pottery at N
2sinter in atmosphere, burnt till rear ceramic plate thickness 2mm (± 0.10mm), diameter 13.30mm (± 0.05mm);
ZnO varistor sheet after sintering carries out abrasive disc, ultrasonic cleaning 10min, and the disk two sides coating Ag electrode after cleaning, is incubated 10min at 600 DEG C, welding lead, after then using alcohol washes solder joint, coated organic insullac, make zinc oxide varistor, can use.
Embodiment 4:
Sintering process in the present embodiment has sintered in air atmosphere, the formula 4 of filling a prescription in same embodiment 1.
(1) will except ZnO, Al (NO
3)
39H
2outside O and additive, Zinc-oxide piezoresistor basic material is by mixed in molar ratio according to claim 1, with deionized water ball milling 4 hours, 3 hours, pulverizing, excessively 40 mesh sieves is dried at 80 DEG C, then mixed powder is loaded corundum crucible, 750 DEG C are heated to the temperature rise rate of 5 DEG C/min, be incubated 1 hour, obtain preburning powder;
(2), in the powder obtained in step (1), Al (NO is added according to basic components ratio
3)
39H
2o, ZnO and 3mol%Zn powder, with deionized water ball milling 4 hours, dry at 120 DEG C of temperature, cross 60 mesh sieves after pulverizing, add the PVA solution of concentration 5%, the mass percent that solution accounts for powder is 5%, again after dry-pressing formed under granulation, 8MPa, (in air) sintering 2 hours at 1190 DEG C of temperature.Burn till rear ceramic plate thickness 2mm (± 0.10mm), diameter 13.30mm (± 0.05mm);
ZnO varistor sheet after sintering carries out abrasive disc, ultrasonic cleaning 10min, and the disk two sides coating Ag electrode after cleaning, is incubated 10min at 600 DEG C, welding lead, after then using alcohol washes solder joint, coated organic insullac, make zinc oxide varistor, can use.
Power dissipation characteristics in leakage current region test is carried out to sample and 8/20 μ s pulsed current impact experiment (it is 8 μ s that pulsed current ripple arrives time of crest, and the time dropping to half-wave (half of crest) from crest is 20 μ s), its result is as shown in table 1.
Can find out, in the present invention, additive metal oxide is replaced to join in the raw material of experiment with metal-powder, pre-treatment is carried out to portions additive, use the ZnO varistor sheet that traditional ceramics preparation technology and atmosphere sintering technique are prepared, there is higher potential gradient, while larger nonlinear factor and lower leakage current, its varistor voltage E
1mAfor about 300V/mm, nonlinear factor α >75, leakage current <0.2 μ A.The more important thing is, under 6KA, 8/20 μ s pulse shock performance improves, and residual voltage ratio reduces, and pressure sensitive voltage velocity of variation is stabilized within 10%.
Table 1 sample Specifeca tion speeification
Wherein:
K
6KA: at 6KA, the voltage at sample two ends and the ratio of 1mA voltage under 8/20 μ s impulse of current, i.e. R=U
6KA/ U
1mA.
△ U
1mA/ (%): 6KA, front and back U is impacted in 8/20 μ s impulse of current
1mAvelocity of variation, i.e. △ U
1mA/ (%)=(U
1mAbefore-U
1mAafter)/U
1mAbefore× 100%
From above-described embodiment, as long as ensure that preparation process Raw proportioning is in scope listed by claim, can obtain high-performance zinc oxide piezoresistive material.The present invention is not only confined to above-mentioned embodiment; persons skilled in the art are according to content disclosed by the invention; other multiple embodiment can be adopted to implement the present invention; therefore; every employing project organization of the present invention and thinking; do the design that some simply change or change, all fall into the scope of protection of the invention.
Claims (5)
1. a zinc oxide piezoresistor ceramic, is prepared from through ball mill mixing, dry pressing and atmosphere sintering by raw material and metal powder additive, it is characterized in that:
Described raw material and mol ratio are ZnO (91.494-94.894mol%), Bi
2o
3(1.0-1.5mol%), Sb
2o
3(0.8-1.2mol%), Cr
2o
3(0.3-0.5mol%), Ni
2o
3(0.2-0.4mol%), MnCO
3(0.5-1.0mol%), SiO
2(0.5-1.5mol%), Co
2o
3(0.5-1.0mol%), MgO (0.5-1.0mol%), Al (NO
3)
39H
2o (0-0.006mol%); Described metal powder additive is the one in Zn, Al, and its mol ratio is 0.08-3.0mol%.
2. the preparation method of zinc oxide piezoresistor ceramic according to claim 1, is characterized in that comprising the steps:
(1) pre-burning powder step is prepared:
Will except ZnO, Al (NO
3)
39H
2raw material outside O according to described molar ratio, with deionized water ball milling 4-8 hour after mixing, dry at 80-120 DEG C 3-4 hour, pulverize, cross 40-60 mesh sieve, gained mixed powder loads corundum crucible, and heating obtains pre-burning powder;
(2) atmosphere sintering forming step:
In described pre-burning powder, add Al (NO according to described molar ratio
3)
39H
2o, ZnO and metal powder additive, with deionized water ball milling 4-8 hour, dry, cross 60-80 mesh sieve, obtain ceramic powder after pulverizing at 100 DEG C-120 DEG C;
In described ceramic powder, add and account for the PVA solution that its mass percent is 5 ~ 8%, described PVA solution mass percent is 3-5%; After dry-pressing slabbing under granulation, 8-10MPa pressure, at 1150 ~ 1200 DEG C of temperature, sinter 2 ~ 3 hours, obtain zinc oxide piezoresistor ceramic.
3. preparation method according to claim 2, is characterized in that, in described preparation pre-burning powder step, pre-sinter process condition is heated to 700 ~ 800 DEG C with the temperature rise rate of 5 DEG C/min, is incubated 1 ~ 2 hour.
4. preparation method according to claim 2, is characterized in that, in described step 2, sintering process conditions is, after sintering temperature reaches 500-600 DEG C, pass into O
2atmosphere, allows pottery at O
2sintering is completed in atmosphere.
5. preparation method according to claim 2, is characterized in that, burns till rear oxidation zinc based varistor thickness 2mm (± 0.10mm) in step 2, diameter 13.30mm (± 0.05mm).
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