CN103073302A - Low-temperature sintering method of high potential gradient voltage-sensitive ceramic material - Google Patents

Low-temperature sintering method of high potential gradient voltage-sensitive ceramic material Download PDF

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CN103073302A
CN103073302A CN2013100211671A CN201310021167A CN103073302A CN 103073302 A CN103073302 A CN 103073302A CN 2013100211671 A CN2013100211671 A CN 2013100211671A CN 201310021167 A CN201310021167 A CN 201310021167A CN 103073302 A CN103073302 A CN 103073302A
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徐志军
初瑞清
马帅
汪宁
李艳
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Liaocheng University
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Abstract

The invention discloses a ZnO-Bi2O3-based piezoresistor material with adjustable potential gradient of 600 V/mm to 1,450V/mm and a low-temperature sintering method thereof. The material consists of 92 to 98.5mol% of zinc oxide, 0.3 to 2mol% of bismuth trioxide Bi2O3 and the balance of additives such as Sb, Co,Mn, Cr, B elements and the like. According to a formula, the corresponding raw materials are weighed; and after heat is preserved for 2 to 5 hours at a temperature of 830 to 870 DEG C by utilizing a solid-phase sintering method, a corresponding voltage-sensitive ceramic material is obtained. The ZnO-Bi2O3-based piezoresistor material obtained by the invention has voltage-sensitive field intensity of 600V/mm to 1,450V/mm, nonlinear coefficient alpha of over 40 and leakage current IL of more than or equal to 0.1muA and has low sintering temperature and excellent comprehensive performance; and moreover, the preparation method disclosed by the invention has the advantages of simple process, low energy consumption, green, environmental-friendliness and the like and has wide application prospect.

Description

A kind of low-temperature sintering method of high potential gradient pressure-sensitive ceramic material
Technical field
The invention belongs to high-potential gradient zinc oxide bismuth series pressure-sensitive ceramic material and low-temperature sintering field thereof, specifically relate to a kind of high-potential gradient ZnO-Bi 2O 3Series pressure-sensitive ceramic material and low-temperature sintering method thereof.
Background technology
Along with the development of high-voltage power system etc., also more and more higher to the requirement for the protection of the pressure sensitive voltage of the piezoresistor of the systems such as electric power.And zinc oxide (ZnO) piezoresistor be a kind of be take ZnO as material of main part, add multiple other trace element, the poly semiconductor device made from ceramic process.It is large with nonlinear factor; fast response time; through-current capability waits by force excellent electric property to become rapidly leading material for the protection of systems such as electric power (1. M. Matsuoka. Nonohmic Properties of Zinc OxideCeramics. Japanese Journal of Applied Physics; 1971; (10): 736-746. 2. Leach; C.; Grain boundary structures in zinc oxide varisrors. J. Acta. Materialia; 2005; S ℃ of iety. 1990 of 53 (2): 237 ~ 141. 3. T.K. Gupta.Application of ZnO Oxide Varistors. Journal of the American Ceramic, 73:1817-1840.).
The grain size of zinc oxide pressure-sensitive ceramic and the crystal boundary number of plies determine its pressure sensitive voltage.Crystal grain is less, and the crystal boundary number of plies is just more, and the pressure sensitive voltage of zinc oxide pressure-sensitive ceramic is also higher.In order to obtain the zinc oxide pressure-sensitive ceramic of pressure-sensitive voltage, a lot of scholars utilize the synthetic ZnO powder research of wet chemistry method, in the hope of obtaining the less Zinc oxide pressure-sensitive ceramic material of crystal grain.For example, Yuan Fangli etc. adopt chemical precipitation method making ZnO voltage-sensitive ceramic powder, the more conventional solid sintering technology of its sintering temperature (1100-1200 ℃) has reduced about 100 ℃, and pressure sensitive voltage has improved 50V/mm (Yuan Fangli, Ling Yuanbing with the pressure sensitive voltage of component conventional solid-state method preparation, Li Jinlin, Ji Youzhang, " ZnO Varistors Prepared by Chemical Coprecipitation Powders ", Journal of Inorganic Materials, 1998,13[2]: 171-175.); Chu etc. have studied employing sol-gel method making ZnO-Bi 20 3Be pressure-sensitive powder, preparation technology compares with conventional powder, and its sintering temperature has reduced by 200 ℃, and its density reaches 5.4g/cm when 1000 ℃ of sintering 3, pressure sensitive voltage also increase (Chu S. Y., Yan T. M., Chen S. L., " Analysis of ZnO varistors prepared by sol-gel method ", Ceram. Inter., 2000,26[7]: 733-737.).
But common wet chemical method adopts soluble salt as raw material, and the soluble salt of rare earth element is expensive, and is difficult for relatively large preparation ceramic powder material, has limited in industrial application.
Summary of the invention
The present invention aims to provide a kind of high-potential gradient ZnO-Bi 2O 3Series pressure-sensitive ceramic material and low-temperature sintering method thereof.Adding an amount of B 2O 3After, not only make ZnO-Bi 2O 3The sintering temperature that is pressure sensitive reduces, and its pressure-sensitive field intensity can be adjustable in 600V/mm ~ 1450V/mm scope, and ZnO-Bi 2O 3Be the nonlinear factor of pressure sensitive greater than 40, leakage current is less than or equal to 0.10 μ A.The present invention not only provides effective means for the low-temperature sintering piezoresistive material, also for using fine silver to create condition as inner electrode in the preparation of multilayer chip varistor spare.The present invention obtains the subsidy of national " 863 " plan (2013AA030501), Shandong Province's Natural Science Fund In The Light (ZR2012EMM004), Shandong Province doctor fund (No. BS2010CL010).
One class high-potential gradient ZnO-Bi 2O 3The low-temperature sintering method of series pressure-sensitive ceramic material, its step is as follows:
(1) takes by weighing respectively ZnO, Bi for (100-y-z-m-n-p) %:y%: z%: m%: n%: p% in molar ratio 2O 3, Sb 2O 3, Co 2O 3, MnO 2And Cr 2O 3Starting material, y=0 ~ 2 wherein, z=0 ~ 1, m=0 ~ 1, n=0 ~ 1, p=0 ~ 1;
(2) total mass ratio that takes by weighing according to (1) adds B 2O 3, i.e. (ZnO+Bi 2O 3+ Sb 2O 3+ Co 2O 3+ MnO 2+ Cr 2O 3) total mass * x%=B 2O 3Quality, x=0.5 ~ 2.0;
(3) starting material that (1), (2) taken by weighing are put into respectively different ball grinders, ball milling;
(4) behind the ball milling, slurry is put into baking oven dry;
(5) raw material with oven dry directly adds polyvinyl alcohol (PVA) binding agent, and granulation is pressed into high-potential gradient ZnO-Bi 2O 3The series pressure-sensitive ceramic material.
Described low-temperature sintering method, preferential scheme are step (2) x=0.5,1.0,1.5 or 2.0.
Described low-temperature sintering method, preferential scheme are step (3) ball milling 4-8 hour.
Described low-temperature sintering method, preferential scheme are that step (4) bake out temperature is 80-120 ℃.
Described low-temperature sintering method, preferential scheme are that the add-on of step (5) polyvinyl alcohol is the 3-8% of raw material total mass.
Described low-temperature sintering method, preferential scheme are to be pressed into high-potential gradient ZnO-Bi under 80-120MPa pressure 2O 3The series pressure-sensitive ceramic material.
Described low-temperature sintering method, preferential scheme are that sintering temperature was 830-870 ℃ of insulation 2-5 hour.
The present invention is to provide a kind of high-potential gradient ZnO-Bi 2O 3Series pressure-sensitive ceramic material and low-temperature sintering method thereof are comprised of following steps: (1) chooses zinc oxide (ZnO), bismuthous oxide bismuth trioxide (Bi 2O 3), antimonous oxide (Sb 2O 3), cobalt sesquioxide (Co 2O 3), Manganse Dioxide (MnO 2), chromium sesquioxide (Cr 2O 3), boron trioxide (B 2O 3) etc. be starting material; (2) take by weighing respectively ZnO, Bi for (100-y-z-m-n-p) %:y%: z%: m%: n%: p% in molar ratio 2O 3, Sb 2O 3, Co 2O 3, MnO 2, Cr 2O 3Starting material, y=0 ~ 2 wherein, z=0 ~ 1, m=0 ~ 1, n=0 ~ 1, p=0 ~ 1; (3) total mass ratio that takes by weighing according to (2) adds B 2O 3, i.e. [ZnO+Bi 2O 3+ Sb 2O 3+ Co 2O 3+ MnO 2+ Cr 2O 3] total mass * x%=B 2O 3Quality ( x=0.5,1.0,1.5,2.0); (4) starting material that (2), (3) taken by weighing are put into respectively different ball grinders, ball milling 4-8 hour; (5) behind the ball milling, slurry is put into baking oven 80-120 ℃ of oven dry; (6) raw material with oven dry directly adds polyvinyl alcohol (PVA) binding agent (add-on of PVA is the 3-8% of raw material total mass), granulation, and being pressed into diameter under 80-120MPa pressure is 12mm, thickness is the thin discs of 0.8-1.5mm; (7) thin discs that suppresses is incubated 1-3 hour, the PVA binding agent of draining at 550 ℃; (8) with the ZnO-Bi after process (7) 2O 3Be that sample is at 2-5 hour sintering of 830-870 ℃ of insulation; (9) with the ZnO-Bi behind (8) sintering 2O 3Series pressure-sensitive ceramic sample upper and lower surface is coated the silver slurry; (10) sample after processing through (9) is incubated 20 minutes at 500 ℃, is fired into silver electrode; (11) with the ZnO-Bi after process (10) 2O 3The series pressure-sensitive ceramic sample carries out Properties Testing.
Aforementioned ZnO-Bi 2O 3Series pressure-sensitive ceramic material preparation method, described Manganse Dioxide presoma also can be by manganous carbonate (MnCO 3) substitute, prepare corresponding ZnO-Bi 2O 3The series pressure-sensitive ceramic material.
Aforementioned ZnO-Bi 2O 3Series pressure-sensitive ceramic material preparation method, the ball mill that described " ball milling " uses can all can produce a desired effect as planetary ball mill, sand mill or industrial ceramic powder blending device, as the KEQ type frequency conversion omnidirectional planetary ball mill that uses Qidong City grand Hong Yiqishebeichang in Jiangsu Province's to produce, the RT001 type horizontal sand mill that scholar special mechanical ﹠ electronic equipment corporation, Ltd in Shanghai produces, the ZSH mixer that Shanghai Kairi Electromechanic Device Manufacturing Co., Ltd. produces etc. all can.
The invention discloses a kind of potential gradient adjustable ZnO-Bi between 600V/mm ~ 1450V/mm 2O 3Be piezoresistive material and low-temperature sintering method thereof.Material is comprised of zinc oxide, bismuthous oxide bismuth trioxide and other additive, and wherein the content of zinc oxide is 92 ~ 98.5mol%, and the content of bismuthous oxide bismuth trioxide is 0.3% ~ 2mol%Bi 2O 3, residual content is the additives such as Sb, Co, Mn, Cr, B element.According to prescription, take by weighing corresponding starting material after, utilize solid sintering technology to obtain corresponding pressure-sensitive ceramic material 830-870 ℃ of insulation after 2-5 hour.The ZnO-Bi that the present invention obtains 2O 3The pressure-sensitive field intensity that is piezoresistive material is 600V/mm ~ 1450V/mm, nonlinear factor α＞40, leakage current I L≤ 0.1 μ A, and sintering temperature is low, and over-all properties is good; In addition, it is simple that preparation method of the present invention has technique, and energy consumption is little, and the advantages such as environmental protection are with a wide range of applications.
The present invention is to provide a class high-potential gradient ZnO-Bi 2O 3The series pressure-sensitive ceramic material, material prescription is: mol ratio is (100-y-z-m-n-p) %:y%: z%: the ZnO of m) %: n%: p%, Bi 2O 3, Sb 2O 3, Co 2O 3, MnO 2, Cr 2O 3, y=0 ~ 2 wherein, z=0 ~ 1, m=0 ~ 1, n=0 ~ 1, p=0 ~ 1; B 2O 3Quality add i.e. [ZnO+ Bi according to the total mass ratio of other element 2O 3The total mass of+(Sb, Co, Mn, Cr)] * x%=B 2O 3Quality (x=0.5 ~ 2.0).The weight that adds the PVA binding agent during forming process of ceramics is the 3-8% that material forms gross weight.The present invention also provides by such ZnO-Bi 2O 3The voltage dependent resistor components and parts that the series pressure-sensitive ceramic material is made.
Pass through ZnO-Bi 2O 3Series pressure-sensitive ceramic material Study on preparation can find out that characteristics of the present invention are mainly reflected in employing B 2O 3As outer doping, B 2O 3Both play the effect of sintering aid, played again the effect that improves potential gradient.The present invention compares with the technology such as wet chemistry method that reduce grain-size raising potential gradient that extensively adopt at present, has the following advantages:
1. without powder pre-synthesis process, only can prepare the ZnO-Bi of better performances through relatively low calcining temperature (850 ℃) 2O 3The series pressure-sensitive ceramic material;
2. such ZnO-Bi 2O 3The series pressure-sensitive ceramic material has relatively high potential gradient, E 1mA=600V/mm ~ 1450V/mm;
3. such ZnO-Bi 2O 3The series pressure-sensitive ceramic material has relatively high nonlinear factor, α＞40;
4. such ZnO-Bi 2O 3The series pressure-sensitive ceramic material has relatively low leakage current, I L≤ 0.1 μ A;
5. making ZnO-Bi that present method can be relatively large 2O 3The series pressure-sensitive ceramic material, suitable industrial production.
In a word, the present invention explores a kind of preferably low-temperature sintering and prepares high-potential gradient ZnO-Bi 2O 3The technique of series pressure-sensitive ceramic material; For preparing low cost, high-performance, high-potential gradient ZnO-Bi 2O 3The series pressure-sensitive ceramic material has been created condition; Exist widely application prospect in the industrial production.
Description of drawings
Fig. 1 is technical solution of the present invention embodiment process flow diagram.
Fig. 2 utilizes the technical program embodiment 1 at the ZnO-Bi of 850 ℃ of insulation preparations after 5 hours 2O 3The XRD analysis collection of illustrative plates of series pressure-sensitive ceramic.
Fig. 3 utilizes the technical program embodiment 1 at the ZnO-Bi of 850 ℃ of insulation preparations after 5 hours 2O 3The pressure-sensitive field intensity of series pressure-sensitive ceramic material is with B 2O 3The content curve spectrum.
Embodiment
Further illustrate characteristics of the present invention below by embodiment and accompanying drawing, apparent, embodiment only for the explanation goal of the invention, limits absolutely not the present invention.
Embodiment 1:With ZnO, Bi 2O 3, Sb 2O 3, Co 2O 3, MnO 2, Cr 2O 3And B 2O 3Be raw material, according to mol ratio 97.5%ZnO, 0.5%Bi 2O 3, 0.5%Sb 2O 3, 0.5%Co 2O 3, 0.5%MnO 2, 0.5%Cr 2O 3Carry out weighing, add and (97.5%ZnO+0.5%Bi respectively again 2O 3+ 0.5%Sb 2O 3+ 0.5%Co 2O 3+ 0.5%MnO 2+ 0.5%Cr 2O 3) mass ratio is 0.5%, 1.0%, 1.5%, 2.0% B 2O 3Routinely solid-phase synthesis prepare burden, ball milling mixing 8h, drying, adding 3wt%PVA binding agent, moulding, plastic removal (550 ℃, 1h), 850 ℃ of insulation 5h sintering, can form voltage-sensitive ceramic, following table 1 is electric property of the lower acquisition of this prescription voltage-sensitive ceramic.
Fig. 2 utilizes the technical program embodiment 1 at the ZnO-Bi of 850 ℃ of insulation preparations after 5 hours 2O 3The XRD analysis collection of illustrative plates of series pressure-sensitive ceramic.Fig. 3 utilizes the technical program embodiment 1 at the ZnO-Bi of 850 ℃ of insulation preparations after 5 hours 2O 3The pressure-sensitive field intensity of series pressure-sensitive ceramic material is with B 2O 3The content curve spectrum.Can be found out by Fig. 2-3: under the technical program material, stupalith is by ZnO principal crystalline phase, Bi 2O 3Phase, Zn 7Sb 2O 12Phase and Bi 16CrO 27Phase composite; Voltage gradient is with B 2O 3Content increases and improves, and works as B 2O 3Content reaches the highest when being 1.5%, begins subsequently to reduce.
Embodiment 2:With ZnO, Bi 2O 3, Sb 2O 3, Co 2O 3, MnO 2, Cr 2O 3And B 2O 3Be raw material, according to mol ratio 97.5%ZnO, 1%Bi 2O 3, 0.5%Sb 2O 3, 0.5%Co 2O 3, 0.3%MnO 2, 0.2%Cr 2O 3Carry out weighing, add and (97.5%ZnO+1%Bi respectively again 2O 3+ 0.5%Sb 2O 3+ 0.5%Co 2O 3+ 0.3%MnO 2+ 0.2%Cr 2O 3) mass ratio is 0.5%, 1.0%, 1.5%, 2.0% B 2O 3Routinely solid-phase synthesis prepare burden, ball milling mixing 8h, drying, adding 8wt%PVA binding agent, moulding, plastic removal (550 ℃ 1h), 870 ℃ of insulation 2h sintering, can form voltage-sensitive ceramic.
Following table 2 is the lower electric property that obtains voltage-sensitive ceramic of this prescription.
Figure 2013100211671100002DEST_PATH_IMAGE001

Claims (7)

1. a class high-potential gradient ZnO-Bi 2O 3The low-temperature sintering method of series pressure-sensitive ceramic material is characterized in that, step is as follows:
(1) takes by weighing respectively ZnO, Bi for (100-y-z-m-n-p) %:y%: z%: m%: n%: p% in molar ratio 2O 3, Sb 2O 3, Co 2O 3, MnO 2And Cr 2O 3Starting material, y=0 ~ 2 wherein, z=0 ~ 1, m=0 ~ 1, n=0 ~ 1, p=0 ~ 1;
(2) total mass ratio that takes by weighing according to (1) adds B 2O 3, i.e. (ZnO+Bi 2O 3+ Sb 2O 3+ Co 2O 3+ MnO 2+ Cr 2O 3) total mass * x%=B 2O 3Quality, x=0.5 ~ 2.0;
(3) starting material that (1), (2) taken by weighing are put into respectively different ball grinders, ball milling;
(4) behind the ball milling, slurry is put into baking oven dry;
(5) raw material with oven dry directly adds polyvinyl alcohol (PVA) binding agent, and granulation is pressed into high-potential gradient ZnO-Bi 2O 3The series pressure-sensitive ceramic material.
2. low-temperature sintering method according to claim 1 is characterized in that, step (2) x=0.5,1.0,1.5 or 2.0.
3. low-temperature sintering method according to claim 1 is characterized in that, step (3) ball milling 4-8 hour.
4. low-temperature sintering method according to claim 1 is characterized in that, step (4) bake out temperature is 80-120 ℃.
5. low-temperature sintering method according to claim 1 is characterized in that, the add-on of step (5) polyvinyl alcohol is the 3-8% of raw material total mass.
6. low-temperature sintering method according to claim 5 is characterized in that, is pressed into high-potential gradient ZnO-Bi under 80-120MPa pressure 2O 3The series pressure-sensitive ceramic material.
7. low-temperature sintering method according to claim 6 is characterized in that, sintering temperature was 830-870 ℃ of insulation 2-5 hour.
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Cited By (8)

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CN103387389A (en) * 2013-07-22 2013-11-13 聊城大学 Five-membered ZnO voltage-sensitive ceramic material having low leak current and sintering method thereof
CN104150900A (en) * 2014-07-28 2014-11-19 聊城大学 Low-voltage additive for ZnO varistor and preparation method thereof
CN104671771A (en) * 2013-12-03 2015-06-03 辽宁法库陶瓷工程技术研究中心 High voltage gradient zinc oxide based varistor material and preparation method thereof
CN104860671A (en) * 2015-05-18 2015-08-26 聊城大学 Low-temperature sintered high-performance high-voltage ZnO varistor material
CN110922182A (en) * 2019-11-28 2020-03-27 新疆大学 Preparation method of high-gradient low-leakage-current ceramic
CN111499373A (en) * 2020-04-28 2020-08-07 如东宝联电子科技有限公司 Laminated zinc oxide composition suitable for low-temperature co-firing with silver inner electrode and manufacturing method thereof
CN111848152A (en) * 2020-08-12 2020-10-30 重庆大学 High potential gradient ZnO voltage-sensitive ceramic based on cold sintering and preparation method thereof
CN113979740A (en) * 2021-10-11 2022-01-28 平高集团有限公司 Pressure-sensitive ceramic additive, pressure-sensitive ceramic material, pressure-sensitive ceramic and preparation method thereof, pressure-sensitive resistor and preparation method thereof, and resistor element

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CN101630553A (en) * 2009-07-17 2010-01-20 立昌先进科技股份有限公司 Preparation method of zinc oxide varister
CN101759431A (en) * 2009-12-10 2010-06-30 华中科技大学 Zinc oxide piezoresistor material with low electric potential gradient and preparation method thereof

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103387389A (en) * 2013-07-22 2013-11-13 聊城大学 Five-membered ZnO voltage-sensitive ceramic material having low leak current and sintering method thereof
CN104671771A (en) * 2013-12-03 2015-06-03 辽宁法库陶瓷工程技术研究中心 High voltage gradient zinc oxide based varistor material and preparation method thereof
CN104150900A (en) * 2014-07-28 2014-11-19 聊城大学 Low-voltage additive for ZnO varistor and preparation method thereof
CN104150900B (en) * 2014-07-28 2015-10-21 聊城大学 A kind of ZnO varistor low pressure additive and preparation method thereof
CN104860671A (en) * 2015-05-18 2015-08-26 聊城大学 Low-temperature sintered high-performance high-voltage ZnO varistor material
CN110922182A (en) * 2019-11-28 2020-03-27 新疆大学 Preparation method of high-gradient low-leakage-current ceramic
CN111499373A (en) * 2020-04-28 2020-08-07 如东宝联电子科技有限公司 Laminated zinc oxide composition suitable for low-temperature co-firing with silver inner electrode and manufacturing method thereof
CN111499373B (en) * 2020-04-28 2022-07-22 如东宝联电子科技有限公司 Laminated zinc oxide composition suitable for low-temperature co-firing with silver inner electrode and manufacturing method thereof
CN111848152A (en) * 2020-08-12 2020-10-30 重庆大学 High potential gradient ZnO voltage-sensitive ceramic based on cold sintering and preparation method thereof
CN113979740A (en) * 2021-10-11 2022-01-28 平高集团有限公司 Pressure-sensitive ceramic additive, pressure-sensitive ceramic material, pressure-sensitive ceramic and preparation method thereof, pressure-sensitive resistor and preparation method thereof, and resistor element
CN113979740B (en) * 2021-10-11 2023-12-15 平高集团有限公司 Pressure-sensitive ceramic additive, pressure-sensitive ceramic material, pressure-sensitive ceramic and preparation method thereof, piezoresistor and preparation method thereof, and resistor element

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