CN107021751A - A kind of high-potential gracient arrester zinc oxide piezoresistor ceramic - Google Patents

A kind of high-potential gracient arrester zinc oxide piezoresistor ceramic Download PDF

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CN107021751A
CN107021751A CN201710229077.XA CN201710229077A CN107021751A CN 107021751 A CN107021751 A CN 107021751A CN 201710229077 A CN201710229077 A CN 201710229077A CN 107021751 A CN107021751 A CN 107021751A
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zinc oxide
temperature
grinding
oxide piezoresistor
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袁能
刘凌云
张政军
王建
王强
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Three or three Electric Applicance Co., Ltd of Xiangyang City
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Hubei University of Technology
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    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/453—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
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    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract

The present invention provides a kind of high-potential gracient arrester zinc oxide piezoresistor ceramic, including the component with following molar content：Nanoscale ZnO 95.05%~95.8%, Bi2O30.7%th, MnO20.5%th, Sb2O31%th, Co2O31%th, Cr2O30.5%th, Ni2O30.5%th, Tm2O30~0.5%, Lu2O30~0.25%；Its manufacture method comprises the following steps：First ball milling, secondary ball milling, pre-sintering, three ball millings, granulating and forming, double sintering and silver-colored, high-potential gracient arrester zinc oxide piezoresistor ceramic of the present invention has the advantages that voltage gradient is high, leakage current is small, nonlinear factor is big, crystallite dimension is small, can also obtain the high-performance arrester zinc oxide piezoresistor ceramic with different voltage gradients by adjusting food ingredient and its ratio, sintering temperature etc..

Description

A kind of high-potential gracient arrester zinc oxide piezoresistor ceramic
Technical field
The present invention relates to electrical material field, particularly a kind of high-potential gracient arrester is made pottery with Zinc-oxide piezoresistor Porcelain.
Background technology
Piezo-resistance is that a class has non-linear volt-ampere（U-I）The resistive element of characteristic, they are used as overvoltage protection device The fields such as electrical equipment, electronics, building, communication, military affairs are widely used to voltage limiter.
The mankind just have carborundum from 1908（SiC）The research of pressure-sensitive character, is led using the unidirectional of SiC material first Current rectifier electrically is made, SiC arresters are then prepared in nineteen thirty, it is in zinc oxide（ZnO）There is it in piezo-resistance Preceding is always the important materials for making piezo-resistance.
Japanese Matsushita Electric Industrial company successfully have developed ZnO varistor in nineteen sixty-eight, and be opened in 1976 and 1979 Unit of an arrester and high-energy current absorber are sent, ZnO varistor has then obtained rapid development and has been widely applied, into To manufacture the leading material of piezo-resistance.
The 1980s, titanium dioxide（TiO2）Piezo-resistance is developed, and lot of domestic and foreign scholar is to TiO2 Piezo-resistance has done extensive research.The palace woods of Japan enters etc. by by Sb2O3、Bi2O3With Si O2Etc. being incorporated into TiO2In, system Standby to go out to have capacity effect and the complex function electron ceramic material of voltage-sensitive effect simultaneously, pressure sensitive voltage scope is 7~30V, non-thread Property coefficient is about 3.Later Kutty et al. is with BaTiO3Nonlinear factor scope 30 is prepared using grain boundary decision technology for matrix ~50 piezo-resistance.Domestic Li Hong is weeded et al. by TiO2CeO is mixed in piezo-resistance2Improve its microstructure and non-thread Property, breakdown voltage gradient is about 15V/mm, and nonlinear factor is 6.
Nineteen ninety-five, Pianaro et al. reports tin ash（SnO2）Piezo-resistance has significant non-linear volt-ampere special Property, occur in that many on SnO after this2The relevant report of piezo-resistance.Domestic long roc of Shandong University Lee et al. is in SnO2Pressure Quick resistance has done substantial amounts of research, it was recently reported that SnO2-Co2O3-Sb2O3System and SnO2-LiCO3-Nb2O5It is piezo-resistance, it is prepared Sample nonlinear factor scope be 9.9~19.6.Lu Zhenya of South China Science ＆ Engineering University et al. prepared electric property in 2009 Close to practical SnO2Piezo-resistance sample, breakdown voltage gradient is about 350V/mm, and nonlinear factor reaches 50, electric leakage Piezo-resistance sample of the stream less than 5 μ A, a diameter of 14mm can be subjected to 2000A 8/20 μ s pulse current impact tests.
Up to the present, according to the difference of piezo-resistance material of main part, piezo-resistance mainly has SiC systems, TiO2System, SnO2This different materials system of system, ZnO systems：
(1) SiC piezo-resistances.SiC is found to have pressure-sensitive character earliest, but there is non-linear and energy absorption capability and have The shortcoming of limit, it is impossible to which the need for meeting growing electronic circuit and Hyper-Voltage of Power Systems protection, it leads in piezo-resistance Domain is substantially replaced by other materials system.
(2) TiO2Piezo-resistance.TiO2The simple production process of piezo-resistance, production cost are low, through-current capability and electric capacity Amount will be higher than ZnO varistor, low pressure is easily realized, wherein having become the one of better performances in low voltage varistor field Class overvoltage protection element, but TiO2Piezo-resistance is difficult to high-pressure trend and limits its answering in high voltage varistor field With.
(3) SnO2Piezo-resistance.In current report, SnO2Piezo-resistance is either in low current performance or big electricity Fluidity can have been moved closer in can be with practical level, but is compared with piezo-resistance mainstay material ZnO varistor, There is certain gap in especially resistance to pulse current impact capacity in performance.
(4) ZnO varistor.Compared with SiC piezo-resistances, ZnO varistor develops later, but several recently Its performance obtains very big improvement within 10 years, with cost is low, easily manufactured, nonlinear factor is big, the response time is short, residual voltage is low, Service life length and a series of good characteristics such as Leakage Current is small.ZnO varistor has taken in most of electric power application fields For SiC piezo-resistances, its correlative study, exploitation and production have become the main contents of piezo-resistance.
With the continuous improvement of transmission voltage grade, the system to conveying extra-high voltage is particularly to transmission system, equipment is exhausted Edge problem becomes increasingly conspicuous, and develops high gradient, the ZnO varistor of low residual voltage, and it is high performance lightning-arrest that name is assembled them into Device reduces the weight and volume of power transmission and transforming equipment to reduce the dielectric level of system, and the reliability for improving transmission system is then one The individual good method solved the problems, such as.
Chinese invention patent（Application number：201410673596.1, the application time：2014-11-21）It refer to a kind of high electricity Potential gradient ZnO varistor material, using Nano-class zinc oxide as material of main part, adds micron order additive, concrete component is included： Nanoscale ZnO 94.0~97.0%, micron order additive Bi2O30.35~0.8%, Sb2O31.0~2.0%, Cr2O30.4~ 0.7%、Co2O30.35~0.7%, MnO2 0.5~0.7%, rare earth oxide 0.02~1.1%, wherein, rare earth oxide is Pr6O11、La2O3、Y2O3、Sm2O3、Nd2O3、CeO2、Eu2O3、Dy2O3、Er2O3In 2~3 kinds.A kind of above-mentioned high-potential gracient The voltage gradient maximum of ZnO varistor material is 1100V/mm, and leakage current scope is 1.2~4.3 μ A.
In view of this, the present invention is obtained using new basic components, different rare earth oxides and different sintering process A kind of stronger high-potential gracient arrester zinc oxide piezoresistor ceramic of combination property is arrived, to solve the above problems.
The content of the invention
It is an object of the invention to provide a kind of high-potential gracient arrester zinc oxide piezoresistor ceramic, it has electricity Press the advantages of gradient is higher, leakage current is smaller, nonlinear factor is bigger.
Technical scheme：A kind of high-potential gracient arrester zinc oxide piezoresistor ceramic, it is characterised in that Including the component with following molar content：Nanoscale ZnO 95.05%~95.8%, Bi2O3 0.7%、MnO2 0.5%、 Sb2O3 1%、Co2O3 1%、Cr2O3 0.5%、Ni2O30.5%、Tm2O30~0.5%, Lu2O30~0.25%；
A kind of method of high-potential gracient arrester zinc oxide piezoresistor ceramic described in manufacturing claims 1, its feature It is, including following preparation process：
（1）First ball milling
By the Bi of above-mentioned mol ratio2O3、MnO2、Sb2O3、Co2O3、Cr2O3、Ni2O3、Tm2O3And Lu2O3With adjusting lubrication prescription, dispersant In being well mixed in agate pot, 5~10h of wet ball grinding in planetary ball mill is subsequently poured into；
（2）Secondary ball milling
Nanoscale ZnO is added to step by above-mentioned mol ratio（1）In slurry after grinding, secondary ball milling 10h is carried out, then The wet slurry of grinding is dried at 60~80 DEG C, mixed slurry is obtained；
（3）It is pre-sintered
Using the pre-sintered above-mentioned mixed slurry of high-temperature electric resistance furnace, then natural cooling, is down to room temperature；
（4）Three ball millings
First the powder after pre-sintering is placed in agate pot, adds and adjusts lubrication prescription, 5~10h of wet ball grinding in planetary ball mill, Drying；
（5）Granulating and forming
The polyvinyl alcohol of first configuration quality fraction 5%（PVA）Deionized water solution, then by step（4）In powder and the PVA The aqueous solution in mass ratio 10:1 is well mixed, and levigate rear 80 eye mesh screens of crossing are granulated, and dry particulate material finally is put into hydraulic pressure pressure Compression molding in piece machine；
（6）Double sintering
Double sintering is carried out using high-temperature electric resistance furnace, based varistor piece is obtained；
（7）It is silver-colored
Potsherd upper and lower surface after cleaning and drying coats middle temperature silver electrode paste, and in 600 DEG C of burning infiltrations 20 minutes with shape Into Ohmic contact.
It is preferred that, the temperature control in above-mentioned pre-sintering step is with time control：
From room temperature to 450 DEG C, the heating-up time is 45min；
The keeping temperature at 450 DEG C, soaking time is 120min.
It is preferred that, in above-mentioned granulating and forming step, using diameter 15mm cylindrical die, briquetting pressure is 10MPa, into Type time 3min.
It is preferred that, in above-mentioned double sintering step, temperature control is with time control：
From room temperature to 500 DEG C, the heating-up time is 160-180min；
Insulation dumping is carried out at 500 DEG C, soaking time is 60-90min；
From 500 DEG C to 800 DEG C, the heating-up time is 60-90min；
From 800 DEG C to 1200 DEG C, the heating-up time is 120-150min；
The keeping temperature at 1200 DEG C, soaking time is 120-160min；
Natural cooling, is down to room temperature.
Beneficial effects of the present invention：Add Ni2O3Contribute to the grain boundaries in ZnO varistor to generate the second phase, play suppression The effect of grain growth processed, so that reducing crystallite dimension improves voltage gradient；Rare earth oxide Tm2O3、Lu2O3With Bi2O3Solid solution A large amount of Lu-Tm phases for being rich in Bi are formed, it, which is distributed in grain boundary layer, plays " pinning " effect, will be further refined the crystal grain of ceramics Size improves voltage gradient；The ceiling voltage gradient of zinc oxide piezoresistor ceramic prepared by the present invention up to 1200V/mm, Have the advantages that voltage gradient is high, nonlinear factor is big, leakage current is small, crystallite dimension is small, combination property is good；In addition, may be used also The high-performance arrester zinc oxide with different voltage gradients is obtained by adjusting food ingredient and its ratio, sintering temperature etc. Based varistor.
Brief description of the drawings
Fig. 1 is the SEM spectrum of the zinc oxide pressure-sensitive material of embodiment 6 of the present invention；
Fig. 2 is the SEM spectrum of the zinc oxide pressure-sensitive material of embodiment 7 of the present invention；
Fig. 3 is the SEM spectrum of the zinc oxide pressure-sensitive material of embodiment 8 of the present invention；
Fig. 4 is the XRD spectrum of the zinc oxide pressure-sensitive material of embodiment 6 of the present invention；
Fig. 5 is the XRD spectrum of the zinc oxide pressure-sensitive material of embodiment 7 of the present invention；
Fig. 6 is the XRD spectrum of the zinc oxide pressure-sensitive material of embodiment 8 of the present invention.
Embodiment
Embodiment one
The formula of the present embodiment is as follows：Nanoscale ZnO 95.8%, Bi2O3 0.7%、MnO2 0.5%、Sb2O3 1%、Co2O3 1%、 Ni2O30.5%、Cr2O3 0.5%。
Preparation method：
（1）First ball milling
By the Bi of above-mentioned mol ratio2O3、MnO2、Sb2O3、Co2O3、Cr2O3、Ni2O3It is put in agate grinding pot, adds anhydrous Ethanol makees lubricant, and wet ball grinding 5h in planetary ball mill is poured into after being well mixed.
（2）Secondary ball milling
Nanoscale ZnO is added to step by above-mentioned mol ratio（1）In slurry after grinding, secondary ball milling 10h is carried out, then The wet slurry of grinding is dried at 60 DEG C, mixed slurry is obtained.
（3）It is pre-sintered
Using the pre-sintered above-mentioned mixed slurry of Muffle furnace, temperature control is with time control：
From room temperature to 450 DEG C, the heating-up time is 45min；
The keeping temperature at 450 DEG C, soaking time is 120min；
Then natural cooling, is down to room temperature.
（4）Three ball millings
First the powder after pre-sintering is placed in agate grinding pot, absolute ethyl alcohol is added as lubrication prescription is adjusted, in planetary ball mill Middle wet ball grinding 5h, is then dried.
（5）Granulating and forming
The polyvinyl alcohol of first configuration quality fraction 5%（PVA）Deionized water solution, then by step（4）In powder and the PVA The aqueous solution in mass ratio 10:1 is well mixed, and levigate rear 80 eye mesh screens of crossing are granulated, and dry particulate material finally is put into hydraulic pressure pressure Diameter 15mm cylindrical die is used in compression molding in piece machine, wherein hydraulic pressure tablet press machine, briquetting pressure is 10MPa, shaping Time 3min.
（6）Double sintering
The tabletting of shaping is positioned in Muffle furnace and carries out double sintering, based varistor piece, temperature control and time is obtained Control be：
From room temperature to 500 DEG C, the heating-up time is 180min；
Insulation dumping is carried out at 500 DEG C, soaking time is 60min；
From 500 DEG C to 800 DEG C, the heating-up time is 60 min；
From 800 DEG C to 1100 DEG C, the heating-up time is 120min；
The keeping temperature at 1100 DEG C, soaking time is 120min；
Natural cooling, is down to room temperature.
（7）It is silver-colored
Potsherd upper and lower surface after cleaning and drying coats middle temperature silver electrode paste, and in 600 DEG C of burning infiltration 20min to be formed Ohmic contact.
The zinc oxide piezoresistor ceramic of gained is subjected to performance test, voltage gradient is 596V/mm, and nonlinear factor is 26, leakage current is 3.6 μ A.
Embodiment two
The formula of the present embodiment is as follows：Nanoscale ZnO 95.55%, Bi2O3 0.7%、MnO2 0.5%、Sb2O3 1%、Co2O3 1%、 Cr2O3 0.5%、Ni2O30.5%、Lu2O3 0.25%。
Preparation method：
（1）First ball milling
By the Bi of above-mentioned mol ratio2O3、MnO2、Sb2O3、Co2O3、Cr2O3、Ni2O3And Lu2O3It is put in agate grinding pot, plus Enter absolute ethyl alcohol and make lubricant, wet ball grinding 5h in planetary ball mill is poured into after being well mixed.
（2）Secondary ball milling
Nanoscale ZnO is added to step by above-mentioned mol ratio（1）In slurry after grinding, secondary ball milling 10h is carried out, then The wet slurry of grinding is dried at 60 DEG C, mixed slurry is obtained.
（3）It is pre-sintered
Using the pre-sintered above-mentioned mixed slurry of Muffle furnace, temperature control is with time control：
From room temperature to 450 DEG C, the heating-up time is 45min；
The keeping temperature at 450 DEG C, soaking time is 120min；
Then natural cooling, is down to room temperature.
（4）Three ball millings
First the powder after pre-sintering is placed in agate grinding pot, absolute ethyl alcohol is added as lubrication prescription is adjusted, in planetary ball mill Middle wet ball grinding 5h, is then dried.
（5）Granulating and forming
The polyvinyl alcohol of first configuration quality fraction 5%（PVA）Deionized water solution, then by step（4）In powder and the PVA The aqueous solution in mass ratio 10:1 is well mixed, and levigate rear 80 eye mesh screens of crossing are granulated, and dry particulate material finally is put into hydraulic pressure pressure Diameter 15mm cylindrical die is used in compression molding in piece machine, wherein hydraulic pressure tablet press machine, briquetting pressure is 10MPa, shaping Time 3min.
（6）Double sintering
The tabletting of shaping is positioned in Muffle furnace and carries out double sintering, based varistor piece, temperature control and time is obtained Control be：
From room temperature to 500 DEG C, the heating-up time is 180min；
Insulation dumping is carried out at 500 DEG C, soaking time is 60min；
From 500 DEG C to 800 DEG C, the heating-up time is 60 min；
From 800 DEG C to 1100 DEG C, the heating-up time is 120min；
The keeping temperature at 1100 DEG C, soaking time is 120min；
Natural cooling, is down to room temperature.
（7）It is silver-colored
Potsherd upper and lower surface after cleaning and drying coats middle temperature silver electrode paste, and in 600 DEG C of burning infiltration 20min to be formed Ohmic contact.
The zinc oxide piezoresistor ceramic of gained is subjected to performance test, voltage gradient is 390V/mm, and nonlinear factor is 33, leakage current is 2.7 μ A.
Embodiment three
The formula of the present embodiment is as follows：Nanoscale ZnO 95.45%, Bi2O3 0.7%、MnO2 0.5%、Sb2O3 1%、Co2O3 1%、 Cr2O3 0.5%、Ni2O30.5%、Lu2O3 0.25%、Tm2O3 0.1%。
Preparation method：
（1）First ball milling
By the Bi of above-mentioned mol ratio2O3、MnO2、Sb2O3、Co2O3、Cr2O3、Ni2O3、Tm2O3And Lu2O3It is put in agate grinding pot In, add absolute ethyl alcohol and make lubricant, wet ball grinding 5h in planetary ball mill is poured into after being well mixed.
（2）Secondary ball milling
Nanoscale ZnO is added to step by above-mentioned mol ratio（1）In slurry after grinding, secondary ball milling 10h is carried out, then The wet slurry of grinding is dried at 60 DEG C, mixed slurry is obtained.
（3）It is pre-sintered
Using the pre-sintered above-mentioned mixed slurry of Muffle furnace, temperature control is with time control：
From room temperature to 450 DEG C, the heating-up time is 45min；
The keeping temperature at 450 DEG C, soaking time is 120min；
Then natural cooling, is down to room temperature.
（4）Three ball millings
First the powder after pre-sintering is placed in agate grinding pot, absolute ethyl alcohol is added as lubrication prescription is adjusted, in planetary ball mill Middle wet ball grinding 5h, is then dried.
（5）Granulating and forming
The polyvinyl alcohol of first configuration quality fraction 5%（PVA）Deionized water solution, then by step（4）In powder and the PVA The aqueous solution in mass ratio 10:1 is well mixed, and levigate rear 80 eye mesh screens of crossing are granulated, and dry particulate material finally is put into hydraulic pressure pressure Diameter 15mm cylindrical die is used in compression molding in piece machine, wherein hydraulic pressure tablet press machine, briquetting pressure is 10MPa, shaping Time 3min.
（6）Double sintering
The tabletting of shaping is positioned in Muffle furnace and carries out double sintering, based varistor piece, temperature control and time is obtained Control be：
From room temperature to 500 DEG C, the heating-up time is 180min；
Insulation dumping is carried out at 500 DEG C, soaking time is 60min；
From 500 DEG C to 800 DEG C, the heating-up time is 60 min；
From 800 DEG C to 1100 DEG C, the heating-up time is 120min；
The keeping temperature at 1100 DEG C, soaking time is 120min；
Natural cooling, is down to room temperature.
（7）It is silver-colored
Potsherd upper and lower surface after cleaning and drying coats middle temperature silver electrode paste, and in 600 DEG C of burning infiltration 20min to be formed Ohmic contact.
The zinc oxide piezoresistor ceramic of gained is subjected to performance test, voltage gradient is 426V/mm, and nonlinear factor is 35, leakage current is 2.1 μ A.
Example IV
The formula of the present embodiment is as follows：Nanoscale ZnO 95.3%, Bi2O3 0.7%、MnO2 0.5%、Sb2O3 1%、Co2O3 1%、 Cr2O3 0.5%、Ni2O30.5%、Lu2O3 0.25%、Tm2O3 0.4%。
Preparation method：
（1）First ball milling
By the Bi of above-mentioned mol ratio2O3、MnO2、Sb2O3、Co2O3、Cr2O3、Ni2O3、Tm2O3And Lu2O3It is put in agate grinding pot In, add absolute ethyl alcohol and make lubricant, wet ball grinding 5h in planetary ball mill is poured into after being well mixed.
（2）Secondary ball milling
Nanoscale ZnO is added to step by above-mentioned mol ratio（1）In slurry after grinding, secondary ball milling 10h is carried out, then The wet slurry of grinding is dried at 60 DEG C, mixed slurry is obtained.
（3）It is pre-sintered
Using the pre-sintered above-mentioned mixed slurry of Muffle furnace, temperature control is with time control：
From room temperature to 450 DEG C, the heating-up time is 45min；
The keeping temperature at 450 DEG C, soaking time is 120min；
Then natural cooling, is down to room temperature.
（4）Three ball millings
First the powder after pre-sintering is placed in agate grinding pot, absolute ethyl alcohol is added as lubrication prescription is adjusted, in planetary ball mill Middle wet ball grinding 5h, is then dried.
（5）Granulating and forming
The polyvinyl alcohol of first configuration quality fraction 5%（PVA）Deionized water solution, then by step（4）In powder and the PVA The aqueous solution in mass ratio 10:1 is well mixed, and levigate rear 80 eye mesh screens of crossing are granulated, and dry particulate material finally is put into hydraulic pressure pressure Diameter 15mm cylindrical die is used in compression molding in piece machine, wherein hydraulic pressure tablet press machine, briquetting pressure is 10MPa, shaping Time 3min.
（6）Double sintering
The tabletting of shaping is positioned in Muffle furnace and carries out double sintering, based varistor piece, temperature control and time is obtained Control be：
From room temperature to 500 DEG C, the heating-up time is 180min；
Insulation dumping is carried out at 500 DEG C, soaking time is 60min；
From 500 DEG C to 800 DEG C, the heating-up time is 60 min；
From 800 DEG C to 1100 DEG C, the heating-up time is 120min；
The keeping temperature at 1100 DEG C, soaking time is 120min；
Natural cooling, is down to room temperature.
（7）It is silver-colored
Potsherd upper and lower surface after cleaning and drying coats middle temperature silver electrode paste, and in 600 DEG C of burning infiltration 20min to be formed Ohmic contact.
The zinc oxide piezoresistor ceramic of gained is subjected to performance test, voltage gradient is 627V/mm, and nonlinear factor is 42, leakage current is 1.7 μ A.
Embodiment five
The formula of the present embodiment is as follows：Nanoscale ZnO 95.15%, Bi2O3 0.7%、MnO2 0.5%、Sb2O3 1%、Co2O3 1%、 Cr2O3 0.5%、Ni2O30.5%、Lu2O3 0.25%、Tm2O3 0.4%。
Preparation method：
（1）First ball milling
By the Bi of above-mentioned mol ratio2O3、MnO2、Sb2O3、Co2O3、Cr2O3、Ni2O3、Tm2O3And Lu2O3It is put in agate grinding pot In, add absolute ethyl alcohol and make lubricant, wet ball grinding 5h in planetary ball mill is poured into after being well mixed.
（2）Secondary ball milling
Nanoscale ZnO is added to step by above-mentioned mol ratio（1）In slurry after grinding, secondary ball milling 10h is carried out, then The wet slurry of grinding is dried at 60 DEG C, mixed slurry is obtained.
（3）It is pre-sintered
Using the pre-sintered above-mentioned mixed slurry of Muffle furnace, temperature control is with time control：
From room temperature to 450 DEG C, the heating-up time is 45min；
The keeping temperature at 450 DEG C, soaking time is 120min；
Then natural cooling, is down to room temperature.
（4）Three ball millings
First the powder after pre-sintering is placed in agate grinding pot, absolute ethyl alcohol is added as lubrication prescription is adjusted, in planetary ball mill Middle wet ball grinding 5h, is then dried.
（5）Granulating and forming
The polyvinyl alcohol of first configuration quality fraction 5%（PVA）Deionized water solution, then by step（4）In powder and the PVA The aqueous solution in mass ratio 10:1 is well mixed, and levigate rear 80 eye mesh screens of crossing are granulated, and dry particulate material finally is put into hydraulic pressure pressure Diameter 15mm cylindrical die is used in compression molding in piece machine, wherein hydraulic pressure tablet press machine, briquetting pressure is 10MPa, shaping Time 3min.
（6）Double sintering
The tabletting of shaping is positioned in Muffle furnace and carries out double sintering, based varistor piece, temperature control and time is obtained Control be：
From room temperature to 500 DEG C, the heating-up time is 180min；
Insulation dumping is carried out at 500 DEG C, soaking time is 60min；
From 500 DEG C to 800 DEG C, the heating-up time is 60 min；
From 800 DEG C to 1100 DEG C, the heating-up time is 120min；
The keeping temperature at 1100 DEG C, soaking time is 120min；
Natural cooling, is down to room temperature.
（7）It is silver-colored
Potsherd upper and lower surface after cleaning and drying coats middle temperature silver electrode paste, and in 600 DEG C of burning infiltration 20min to be formed Ohmic contact.
The zinc oxide piezoresistor ceramic of gained is subjected to performance test, voltage gradient is 909V/mm, and nonlinear factor is 45, leakage current is 1.2 μ A.
Embodiment six
The formula of the present embodiment is as follows：Nanoscale ZnO 95.05%, Bi2O3 0.7%、MnO2 0.5%、Sb2O3 1%、Co2O3 1%、 Cr2O3 0.5%、Ni2O30.5%、Lu2O3 0.25%、Tm2O3 0.5%。
Preparation method：
（1）First ball milling
By the Bi of above-mentioned mol ratio2O3、MnO2、Sb2O3、Co2O3、Cr2O3、Ni2O3、Tm2O3And Lu2O3It is put in agate grinding pot In, add absolute ethyl alcohol and make lubricant, wet ball grinding 5h in planetary ball mill is poured into after being well mixed.
（2）Secondary ball milling
Nanoscale ZnO is added to step by above-mentioned mol ratio（1）In slurry after grinding, secondary ball milling 10h is carried out, then The wet slurry of grinding is dried at 60 DEG C, mixed slurry is obtained.
（3）It is pre-sintered
Using the pre-sintered above-mentioned mixed slurry of Muffle furnace, temperature control is with time control：
From room temperature to 450 DEG C, the heating-up time is 45min；
The keeping temperature at 450 DEG C, soaking time is 120min；
Then natural cooling, is down to room temperature.
（4）Three ball millings
First the powder after pre-sintering is placed in agate grinding pot, absolute ethyl alcohol is added as lubrication prescription is adjusted, in planetary ball mill Middle wet ball grinding 5h, is then dried.
（5）Granulating and forming
The polyvinyl alcohol of first configuration quality fraction 5%（PVA）Deionized water solution, then by step（4）In powder and the PVA The aqueous solution in mass ratio 10:1 is well mixed, and levigate rear 80 eye mesh screens of crossing are granulated, and dry particulate material finally is put into hydraulic pressure pressure Diameter 15mm cylindrical die is used in compression molding in piece machine, wherein hydraulic pressure tablet press machine, briquetting pressure is 10MPa, shaping Time 3min.
（6）Double sintering
The tabletting of shaping is positioned in Muffle furnace and carries out double sintering, based varistor piece, temperature control and time is obtained Control be：
From room temperature to 500 DEG C, the heating-up time is 180min；
Insulation dumping is carried out at 500 DEG C, soaking time is 60min；
From 500 DEG C to 800 DEG C, the heating-up time is 60 min；
From 800 DEG C to 1100 DEG C, the heating-up time is 120min；
The keeping temperature at 1100 DEG C, soaking time is 120min；
Natural cooling, is down to room temperature.
（7）It is silver-colored
Potsherd upper and lower surface after cleaning and drying coats middle temperature silver electrode paste, and in 600 DEG C of burning infiltration 20min to be formed Ohmic contact.
The zinc oxide piezoresistor ceramic of gained is subjected to performance test, voltage gradient is 1200V/mm, nonlinear factor For 46, leakage current is 1.2 μ A.
Embodiment seven
The formula of the present embodiment is as follows：Nanoscale ZnO 95.05%, Bi2O3 0.7%、MnO2 0.5%、Sb2O3 1%、Co2O3 1%、 Cr2O3 0.5%、Ni2O30.5%、Lu2O3 0.25%、Tm2O3 0.5%。
Preparation method：
（1）First ball milling
By the Bi of above-mentioned mol ratio2O3、MnO2、Sb2O3、Co2O3、Cr2O3、Ni2O3、Tm2O3And Lu2O3It is put in agate grinding pot In, add absolute ethyl alcohol and make lubricant, wet ball grinding 5h in planetary ball mill is poured into after being well mixed.
（2）Secondary ball milling
Nanoscale ZnO is added to step by above-mentioned mol ratio（1）In slurry after grinding, secondary ball milling 10h is carried out, then The wet slurry of grinding is dried at 60 DEG C, mixed slurry is obtained.
（3）It is pre-sintered
Using the pre-sintered above-mentioned mixed slurry of Muffle furnace, temperature control is with time control：
From room temperature to 450 DEG C, the heating-up time is 45min；
The keeping temperature at 450 DEG C, soaking time is 120min；
Then natural cooling, is down to room temperature.
（4）Three ball millings
First the powder after pre-sintering is placed in agate grinding pot, absolute ethyl alcohol is added as lubrication prescription is adjusted, in planetary ball mill Middle wet ball grinding 5h, is then dried.
（5）Granulating and forming
The polyvinyl alcohol of first configuration quality fraction 5%（PVA）Deionized water solution, then by step（4）In powder and the PVA The aqueous solution in mass ratio 10:1 is well mixed, and levigate rear 80 eye mesh screens of crossing are granulated, and dry particulate material finally is put into hydraulic pressure pressure Diameter 15mm cylindrical die is used in compression molding in piece machine, wherein hydraulic pressure tablet press machine, briquetting pressure is 10MPa, shaping Time 3min.
（6）Double sintering
The tabletting of shaping is positioned in Muffle furnace and carries out double sintering, based varistor piece, temperature control and time is obtained Control be：
From room temperature to 500 DEG C, the heating-up time is 180min；
Insulation dumping is carried out at 500 DEG C, soaking time is 60min；
From 500 DEG C to 800 DEG C, the heating-up time is 60 min；
From 800 DEG C to 1080 DEG C, the heating-up time is 120min；
The keeping temperature at 1080 DEG C, soaking time is 120min；
Natural cooling, is down to room temperature.
（7）It is silver-colored
Potsherd upper and lower surface after cleaning and drying coats middle temperature silver electrode paste, and in 600 DEG C of burning infiltration 20min to be formed Ohmic contact.
The zinc oxide piezoresistor ceramic of gained is subjected to performance test, voltage gradient is 1056V/mm, nonlinear factor For 43, leakage current is 1.8 μ A.
Embodiment eight
The formula of the present embodiment is as follows：Nanoscale ZnO 95.05%, Bi2O3 0.7%、MnO2 0.5%、Sb2O3 1%、Co2O3 1%、 Cr2O3 0.5%、Ni2O30.5%、Lu2O3 0.25%、Tm2O3 0.5%。
Preparation method：
（1）First ball milling
By the Bi of above-mentioned mol ratio2O3、MnO2、Sb2O3、Co2O3、Cr2O3、Ni2O3、Tm2O3And Lu2O3It is put in agate grinding pot In, add absolute ethyl alcohol and make lubricant, wet ball grinding 5h in planetary ball mill is poured into after being well mixed.
（2）Secondary ball milling
Nanoscale ZnO is added to step by above-mentioned mol ratio（1）In slurry after grinding, secondary ball milling 10h is carried out, then The wet slurry of grinding is dried at 60 DEG C, mixed slurry is obtained.
（3）It is pre-sintered
Using the pre-sintered above-mentioned mixed slurry of Muffle furnace, temperature control is with time control：
From room temperature to 450 DEG C, the heating-up time is 45min；
The keeping temperature at 450 DEG C, soaking time is 120min；
Then natural cooling, is down to room temperature.
（4）Three ball millings
First the powder after pre-sintering is placed in agate grinding pot, absolute ethyl alcohol is added as lubrication prescription is adjusted, in planetary ball mill Middle wet ball grinding 5h, is then dried.
（5）Granulating and forming
The polyvinyl alcohol of first configuration quality fraction 5%（PVA）Deionized water solution, then by step（4）In powder and the PVA The aqueous solution in mass ratio 10:1 is well mixed, and levigate rear 80 eye mesh screens of crossing are granulated, and dry particulate material finally is put into hydraulic pressure pressure Diameter 15mm cylindrical die is used in compression molding in piece machine, wherein hydraulic pressure tablet press machine, briquetting pressure is 10MPa, shaping Time 3min.
（6）Double sintering
The tabletting of shaping is positioned in Muffle furnace and carries out double sintering, based varistor piece, temperature control and time is obtained Control be：
From room temperature to 500 DEG C, the heating-up time is 180min；
Insulation dumping is carried out at 500 DEG C, soaking time is 60min；
From 500 DEG C to 800 DEG C, the heating-up time is 60 min；
From 800 DEG C to 1120 DEG C, the heating-up time is 120min；
The keeping temperature at 1120 DEG C, soaking time is 120min；
Natural cooling, is down to room temperature.
（7）It is silver-colored
Potsherd upper and lower surface after cleaning and drying coats middle temperature silver electrode paste, and in 600 DEG C of burning infiltration 20min to be formed Ohmic contact.
The zinc oxide piezoresistor ceramic of gained is subjected to performance test, voltage gradient is 1100V/mm, nonlinear factor For 39, leakage current is 2.1 μ A.
Above-described embodiment is elaborated to the present invention.Certainly, described above not limitation of the present invention, the present invention It is also not limited to above-mentioned example, person skilled change made in the essential scope of the present invention, retrofits, adds and add deduct Less, replace, fall within protection scope of the present invention.

Claims (5)

1. a kind of high-potential gracient arrester zinc oxide piezoresistor ceramic, it is characterised in that including with following mole hundred Divide the component of content：Nanoscale ZnO 95.05%~95.8%, Bi2O30.7%th, MnO20.5%th, Sb2O31%th, Co2O3 1%th, Cr2O30.5%th, Ni2O30.5%th, Tm2O30~0.5%, Lu2O30~0.25%.
2. a kind of method of the high-potential gracient arrester zinc oxide piezoresistor ceramic described in manufacturing claims 1, it is special Levy and be, including following preparation process：
(1) first ball milling
By the Bi of above-mentioned mol ratio2O3、MnO2、Sb2O3、Co2O3、Cr2O3、Ni2O3、Tm2O3And Lu2O3With adjusting lubrication prescription, dispersant In being well mixed in agate pot, 5~10h of wet ball grinding in planetary ball mill is subsequently poured into；
(2) secondary ball milling
Nanoscale ZnO is added in the slurry after step (1) grinding by above-mentioned mol ratio, secondary ball milling 10h is carried out, then The wet slurry of grinding is dried at 60~80 DEG C, mixed slurry is obtained；
(3) it is pre-sintered
Using the pre-sintered above-mentioned mixed slurry of high-temperature electric resistance furnace, then natural cooling, is down to room temperature；
(4) three ball millings
First the powder after pre-sintering is placed in agate pot, adds and adjusts lubrication prescription, 5~10h of wet ball grinding in planetary ball mill, Then dried at 60~80 DEG C；
(5) granulating and forming
Polyvinyl alcohol (PVA) deionized water solution of first configuration quality fraction 5%, then by the powder in step (4) and the PVA The aqueous solution in mass ratio 10:1 is well mixed, and levigate rear 80 eye mesh screens of crossing are granulated, and dry particulate material finally is put into hydraulic pressure pressure Compression molding in piece machine；
(6) double sintering
Double sintering is completed using high-temperature electric resistance furnace, based varistor piece is obtained；
(7) it is silver-colored
Potsherd upper and lower surface after cleaning and drying coats middle temperature silver electrode paste, and in 600 DEG C of burning infiltrations 20 minutes with shape Into Ohmic contact.
3. the method for manufacture high-potential gracient arrester zinc oxide piezoresistor ceramic according to claim 2, it is special Levy and be, the temperature control in above-mentioned pre-sintering step is with time control：
From room temperature to 450 DEG C, the heating-up time is 45min；
The keeping temperature at 450 DEG C, soaking time is 120min.
4. the method for manufacture high-potential gracient arrester zinc oxide piezoresistor ceramic according to claim 2, it is special Levy and be, in above-mentioned granulating and forming step, using diameter 15mm cylindrical die, briquetting pressure is 10MPa, molding time 3min。
5. wanting the preparation method of the high-potential gracient arrester zinc oxide piezoresistor ceramic described in 2 according to right, it is special Levy and be, in above-mentioned double sintering step, temperature control is with time control：
From room temperature to 500 DEG C, the heating-up time is 160-180min；
Insulation dumping is carried out at 500 DEG C, soaking time is 60-90min；
From 500 DEG C to 800 DEG C, the heating-up time is 60-90min；
From 800 DEG C to 1200 DEG C, the heating-up time is 120-150min；
The keeping temperature at 1200 DEG C, soaking time is 120-160min；
Natural cooling, is down to room temperature.
CN201710229077.XA 2017-04-10 2017-04-10 A kind of high-potential gracient arrester zinc oxide piezoresistor ceramic Pending CN107021751A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108484158A (en) * 2018-05-23 2018-09-04 江苏时瑞电子科技有限公司 A kind of dielectric material of piezoresistor and preparation method thereof
CN114133236A (en) * 2021-12-03 2022-03-04 国网河南省电力公司电力科学研究院 Preparation method of zinc oxide piezoresistor based on chemical precipitation method
CN114933469A (en) * 2022-06-07 2022-08-23 汕头市瑞升电子有限公司 Piezoresistor dielectric material and preparation method thereof
CN115346743A (en) * 2022-08-08 2022-11-15 安徽锦华氧化锌有限公司 Preparation method of zinc oxide of metal oxide arrester resistance card
CN115385682A (en) * 2022-08-30 2022-11-25 重庆大学 Ultrahigh potential gradient ZnO voltage-sensitive ceramic and low-carbon sintering preparation process thereof

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CN101383208A (en) * 2008-10-27 2009-03-11 清华大学 Preparation of high voltage gradient zinc oxide varistor valve
CN102515743A (en) * 2011-12-30 2012-06-27 朱颉安 Method for preparing zinc oxide varistors while increasing potential gradient and nonlinear coefficient
CN104478428A (en) * 2014-11-21 2015-04-01 四川大学 Zinc oxide piezoresistor material with high electric potential gradient

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Publication number Priority date Publication date Assignee Title
CN101383208A (en) * 2008-10-27 2009-03-11 清华大学 Preparation of high voltage gradient zinc oxide varistor valve
CN102515743A (en) * 2011-12-30 2012-06-27 朱颉安 Method for preparing zinc oxide varistors while increasing potential gradient and nonlinear coefficient
CN104478428A (en) * 2014-11-21 2015-04-01 四川大学 Zinc oxide piezoresistor material with high electric potential gradient

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108484158A (en) * 2018-05-23 2018-09-04 江苏时瑞电子科技有限公司 A kind of dielectric material of piezoresistor and preparation method thereof
CN114133236A (en) * 2021-12-03 2022-03-04 国网河南省电力公司电力科学研究院 Preparation method of zinc oxide piezoresistor based on chemical precipitation method
CN114933469A (en) * 2022-06-07 2022-08-23 汕头市瑞升电子有限公司 Piezoresistor dielectric material and preparation method thereof
CN115346743A (en) * 2022-08-08 2022-11-15 安徽锦华氧化锌有限公司 Preparation method of zinc oxide of metal oxide arrester resistance card
CN115346743B (en) * 2022-08-08 2023-12-01 安徽锦华氧化锌有限公司 Preparation method of metal oxide arrester resistor disc
CN115385682A (en) * 2022-08-30 2022-11-25 重庆大学 Ultrahigh potential gradient ZnO voltage-sensitive ceramic and low-carbon sintering preparation process thereof

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