CN104478428A - Zinc oxide piezoresistor material with high electric potential gradient - Google Patents
Zinc oxide piezoresistor material with high electric potential gradient Download PDFInfo
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- CN104478428A CN104478428A CN201410673596.1A CN201410673596A CN104478428A CN 104478428 A CN104478428 A CN 104478428A CN 201410673596 A CN201410673596 A CN 201410673596A CN 104478428 A CN104478428 A CN 104478428A
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Abstract
The invention discloses a zinc oxide piezoresistor material with a high electric potential gradient and belongs to the field of semiconductor electronic materials. The zinc oxide piezoresistor material is characterized in that nanoscale zinc oxide is taken as a main body, is added with micron-sized additives including bismuth oxide, antimony oxide, chromic oxide and cobalt oxide, is also added with a trace amount of manganese dioxide and 2-3 types of rare-earth oxides; all the components are fully mixed, dried, pre-roasted, granulated, compression-molded and then subjected to low-temperature glue discharging and high-temperature sintering to prepare a zinc oxide resistor valve plate, wherein the zinc oxide resistor valve plate is small in average grain size (less than 4 microns), has an electric potential gradient between 750V/mm and 1150V/mm, has a nonlinear coefficient being greater than 25, has leak current being smaller than 5 microamps and also has excellent electrical properties.
Description
Technical field
The invention belongs to semiconductor electronic Material Field, relate to a kind of high-potential gradient zinc oxide piezoresistive material.
Background technology
Zinc-oxide piezoresistor presents excellent nonlinear wind vibration and is subject to extensive concern.Zinc-oxide piezoresistor as overvoltage protection device, pressure limiter and thunder arrester, be widely used in electronics, electrically, the field such as communication and building.At present, in the Application Areas such as high-tension circuit and lightning-arrest device, voltage dependent resistor, to high-pressure trend, miniaturization, large through-current capacity future development, is had higher requirement to the over-all properties of zinc oxide piezoresistive material.Traditional zinc oxide piezoresistive material, voltage gradient, at 200 ~ 400 V/mm, is difficult to the application requiring meeting high pressure and ultra-high voltage resistance device.
Chinese scholars is had to carry out large quantity research for high potential gradient pressure-sensitive resistive material.The potential gradient of the high-voltage ZnO resistors valve block that patent CN 101383208B announces reaches 400 V/mm, but its coarse grains (>7.0 μm), and its binder removal, sintering process are complicated.The high potential gradient material that patent CN 100382205C announces, potential gradient reaches 820 ~ 900 V/mm, but it adopts the method for high-energy ball milling, too high to equipment requirements, and energy consumption is large, is unfavorable for energy efficiency promotion.Patent CN 1181502C discloses the preparation technology that part nano zine oxide substitutes micron zinc oxide, obtains potential gradient and reaches 580 V/mm, and method is simply effective, but its potential gradient still has much room for improvement.Therefore, in order to overcome prior art defect, research and development grain-size is tiny, the ZnO resistors valve block of high potential gradient, good over-all properties is most important, and has broad application prospects.
Summary of the invention
The object of the present invention is to provide a kind of high potential gradient pressure-sensitive resistive material; the resistor valve sheet that this material makes has the performances such as high-voltage gradient, higher nonlinear factor, less leakage current; can be applicable to the protector of power system, and be conducive to the miniaturization of varistor device.
Technical scheme of the present invention: a kind of high-potential gradient zinc oxide piezoresistive valve block, calculate according to molar ratio, it is made up of following raw material powder: nano-ZnO 94.0 ~ 97.0%, Bi
2o
30.35 ~ 0.8%, Sb
2o
31.0 ~ 2.0%, Cr
2o
30.4 ~ 0.7%, Co
2o
30.35 ~ 0.7%, MnO
20.5 ~ 0.7%, rare earth oxide 0.02 ~ 1.1%.
The preparation method of described high voltage varistor valve block, comprises the following steps:
(1) ball mill mixing
The micron powder of multielement additive is proportionally weighed, be placed in agate tank, add dehydrated alcohol or acetone makes lubricant, wet ball grinding 2 ~ 4 h in planetary ball mill, add nano-zinc oxide powder in proportion again, wet ball grinding 24 h, adds dehydrated alcohol or acetone is limited with mixed powder sufficient lubrication;
(2) oven dry, pre-burning
Mixed powder after ball milling through 60 ~ 80 DEG C of oven dry, and at 400 ~ 450 DEG C of pre-burning 1 ~ 2 h;
(3) granulation, shaping
Add 3 ~ 6 wt% polyvinyl alcohol (PVA) granulations afterwards, pressing machine is shaping, disk is of a size of Φ 15 mm, thickness 1.5 mm;
(4) sinter
Adopt continuous tunnel furnace or box-type furnace, temperature, at 400 DEG C of insulation 1 h binder removals, is then incubated 2 h in 1100 ~ 1200 DEG C;
(5) by silver electrode
Adopt continuous tunnel furnace or box-type furnace, 850 ~ 870 DEG C of temperature 0.5 ~ 1 h.
Compared with prior art, the zinc oxide varistor valve average grain size tiny (< 4 μm) that the present invention obtains, has Width funtion gradient scope (750 ~ 1150 V/mm), nonlinear factor α >25, leakage current I
l<5 μ A, over-all properties is good.Product obtains the voltage gradient of demand by adjustment sintering temperature and food ingredient, and it is interval that voltage gradient has larger adjustment.
Accompanying drawing explanation
Fig. 1 is preparation technology's schema of high-potential gradient zinc oxide pressure sensitive;
Fig. 2 is the SEM collection of illustrative plates of the zinc oxide pressure-sensitive material of embodiment 1;
Fig. 3 is the SEM collection of illustrative plates of the zinc oxide pressure-sensitive material of embodiment 2;
Fig. 4 is the XRD figure spectrum of the zinc oxide pressure-sensitive material of embodiment 1;
Fig. 5 is the XRD figure spectrum of the zinc oxide pressure-sensitive material of embodiment 2.
Embodiment:
Embodiment 1
The formula of the present embodiment is as follows:
Nano-ZnO 96.6%, micron Bi
2o
30.7%, Sb
2o
31.0%, Cr
2o
30.5%, Co
2o
30.5%, MnO
20.5%, La
2o
30.1%, Sm
2o
30.1%;
Add in agate grinding pot after the micron powder of multielement additive is proportionally weighed mixing, add dehydrated alcohol or acetone makes lubricant, wet ball grinding 2 h in planetary ball mill, the amount adding dehydrated alcohol or acetone is limited with mixed powder sufficient lubrication.Nano-zinc oxide powder is added by proportioning, wet ball grinding 24 h in additive powder upon mixing.Powder is dried at temperature 60 DEG C, and at 400 DEG C of pre-burning 2 h.Add 4%(massfraction after powder pre-burning) polyvinyl alcohol (PVA) as caking agent, dry-pressing becomes the green compact of Φ 15 mm, thickness 1.5 mm.Green compact are positioned in stove and are slowly warming up to 400 DEG C of insulation 1 h and carry out binder removal, then are warming up to 1100 DEG C, cool to room temperature with the furnace after heat preservation sintering 2 h, and in 850 DEG C of insulation 1 h by silver electrode.The zinc oxide varistor valve of gained is through performance test, and voltage gradient is 780 V/mm, and nonlinear factor is 46, and leakage current is 1.7 μ A.
Embodiment 2
The formula of the present embodiment is as follows:
Nano-ZnO 96.2%, micron Bi
2o
30.7%, Sb
2o
31.0%, Cr
2o
30.5%, Co
2o
30.5%, MnO
20.5%, La
2o
30.1%, Sm
2o
30.5%;
Add in agate grinding pot after the micron powder of multielement additive is proportionally weighed mixing, add dehydrated alcohol or acetone makes lubricant, wet ball grinding 3 h in planetary ball mill, the amount adding dehydrated alcohol or acetone is limited with mixed powder sufficient lubrication.Nano-zinc oxide powder is added by proportioning, wet ball grinding 24 h in additive powder upon mixing.Powder is dried at temperature 80 DEG C, and at 450 DEG C of pre-burning 1 h.Add 3%(massfraction after powder pre-burning) polyvinyl alcohol (PVA) as caking agent, dry-pressing becomes the green compact of Φ 15 mm, thickness 1.5 mm.Green compact are positioned in stove and are slowly warming up to 400 DEG C of insulation 1 h and carry out binder removal, then are warming up to 1100 DEG C, cool to room temperature with the furnace after heat preservation sintering 2 h, and in 870 DEG C of insulation 0.5 h by silver electrode.The zinc oxide varistor valve of gained is through performance test, and voltage gradient is 1100 V/mm, and nonlinear factor is 70, and leakage current is 4.3 μ A.
Embodiment 3
The formula of the present embodiment is as follows:
Nano-ZnO 97.0%, micron Bi
2o
30.35%, Sb
2o
31.3%, Cr
2o
30.45%, Co
2o
30.35%, MnO
20.53%, Nd
2o
30.01%, Y
2o
30.01%;
Add in agate grinding pot after the micron powder of multielement additive is proportionally weighed mixing, add dehydrated alcohol or acetone makes lubricant, wet ball grinding 4 h in planetary ball mill, the amount adding dehydrated alcohol or acetone is limited with mixed powder sufficient lubrication.Nano-zinc oxide powder is added by proportioning, wet ball grinding 24 h in additive powder upon mixing.Powder is dried at temperature 60 DEG C, and at 400 DEG C of pre-burning 2 h.Add 5%(massfraction after powder pre-burning) polyvinyl alcohol (PVA) as caking agent, dry-pressing becomes the green compact of Φ 15 mm, thickness 1.5 mm.Green compact are positioned in stove and are slowly warming up to 400 DEG C of insulation 1 h and carry out binder removal, then are warming up to 1100 DEG C, cool to room temperature with the furnace after heat preservation sintering 2h, and in 870 DEG C of insulation 0.5 h by silver electrode.The zinc oxide varistor valve of gained is through performance test, and voltage gradient is 950 V/mm, and nonlinear factor is 27, and leakage current is 2.6 μ A.
Embodiment 4
The formula of the present embodiment is as follows:
Nano-ZnO 95.5%, micron Bi
2o
30.55%, Sb
2o
31.7%, Cr
2o
30.6%, Co
2o
30.5%, MnO
20.6%, Eu
2o
30.25%, Y
2o
30.3%;
Add in agate grinding pot after the micron powder of multielement additive is proportionally weighed mixing, add dehydrated alcohol or acetone makes lubricant, wet ball grinding 3 h in planetary ball mill, the amount adding dehydrated alcohol or acetone is limited with mixed powder sufficient lubrication.Nano-zinc oxide powder is added by proportioning, wet ball grinding 24 h in additive powder upon mixing.Powder is dried at temperature 60 DEG C, and at 450 DEG C of pre-burning 1 h.Add 5%(massfraction after powder pre-burning) polyvinyl alcohol (PVA) as caking agent, dry-pressing becomes the green compact of Φ 15 mm, thickness 1.5 mm.Green compact are positioned in stove and are slowly warming up to 400 DEG C of insulation 1 h and carry out binder removal, then are warming up to 1100 DEG C, cool to room temperature with the furnace after heat preservation sintering 2 h, and in 850 DEG C of insulation 1 h by silver electrode.The zinc oxide varistor valve of gained is through performance test, and voltage gradient is 1000 V/mm, and nonlinear factor is 30, and leakage current is 2.1 μ A.
Embodiment 5
The formula of the present embodiment is as follows:
Nano-ZnO 94.5%, micron Bi
2o
30.75%, Sb
2o
31.8%, Cr
2o
30.65%, Co
2o
30.6%, MnO
20.65%, Dy
2o
30.45%, Y
2o
30.35%, Er
2o
30.25%;
Add in agate grinding pot after the micron powder of multielement additive is proportionally weighed mixing, add dehydrated alcohol or acetone makes lubricant, wet ball grinding 2 h in planetary ball mill, the amount adding dehydrated alcohol or acetone is limited with mixed powder sufficient lubrication.Nano-zinc oxide powder is added by proportioning, wet ball grinding 24 h in additive powder upon mixing.Powder is dried at temperature 70 DEG C, and at 400 DEG C of pre-burning 2 h.Add 6%(massfraction after powder pre-burning) polyvinyl alcohol (PVA) as caking agent, dry-pressing becomes the green compact of Φ 15 mm, thickness 1.5 mm.Green compact are positioned in stove and are slowly warming up to 400 DEG C of insulation 1 h and carry out binder removal, then are warming up to 1150 DEG C, cool to room temperature with the furnace after heat preservation sintering 2 h, and in 870 DEG C of insulation 0.5 h by silver electrode.The zinc oxide varistor valve of gained is through performance test, and voltage gradient is 920 V/mm, and nonlinear factor is 33, and leakage current is 1.9 μ A.
Embodiment 6
The formula of the present embodiment is as follows:
Nano-ZnO 94.0%, micron Bi
2o
30.8%, Sb
2o
32.0%, Cr
2o
30.7%, Co
2o
30.7%, MnO
20.7%, Er
2o
30.55%, Pr
6o
110.45%, CeO
20.1%;
Add in agate grinding pot after the micron powder of multielement additive is proportionally weighed mixing, add dehydrated alcohol or acetone makes lubricant, wet ball grinding 4 h in planetary ball mill, the amount adding dehydrated alcohol or acetone is limited with mixed powder sufficient lubrication.Nano-zinc oxide powder is added by proportioning, wet ball grinding 24 h in additive powder upon mixing.Powder is dried at temperature 70 DEG C, and at 450 DEG C of pre-burning 1 h.Add 4%(massfraction after powder pre-burning) polyvinyl alcohol (PVA) as caking agent, dry-pressing becomes the green compact of Φ 15 mm, thickness 1.5 mm.Green compact are positioned in stove and are slowly warming up to 400 DEG C of insulation 1 h and carry out binder removal, then are warming up to 1200 DEG C, cool to room temperature with the furnace after heat preservation sintering 2 h, and in 870 DEG C of insulation 0.5 h by silver electrode.The zinc oxide varistor valve of gained is through performance test, and voltage gradient is 850 V/mm, and nonlinear factor is 37, and leakage current is 1.2 μ A.
Claims (2)
1. a high-potential gradient zinc oxide piezoresistive material, is characterized in that taking Nano-class zinc oxide as material of main part, and add micron order additive, concrete component comprises:
Nano level ZnO 94.0 ~ 97.0%
Micron order additive Bi
2o
30.35 ~ 0.8%
Sb
2O
31.0~2.0%
Cr
2O
3 0.4~0.7%
Co
2O
3 0.35~0.7%
MnO
20.5~0.7%
Rare earth oxide 0.02 ~ 1.1%
Wherein, rare earth oxide is Pr
6o
11, La
2o
3, Y
2o
3, Sm
2o
3, Nd
2o
3, CeO
2, Eu
2o
3, Dy
2o
3, Er
2o
3in 2 ~ 3 kinds.
2. high potential gradient pressure-sensitive resistive material preparation method as claimed in claim 1, its concrete steps are as follows:
(1) ball mill mixing
The micron powder of multielement additive is proportionally weighed, be placed in agate tank, add dehydrated alcohol or acetone makes lubricant, wet ball grinding 2 ~ 4 h in planetary ball mill, add nano-zinc oxide powder in proportion again, wet ball grinding 24 h, adds dehydrated alcohol or acetone is limited with mixed powder sufficient lubrication;
(2) oven dry, pre-burning
Mixed powder after ball milling through 60 ~ 80 DEG C of oven dry, and at 400 ~ 450 DEG C of pre-burning 1 ~ 2 h;
(3) granulation, shaping
Add 3 ~ 6 wt% polyvinyl alcohol (PVA) granulations afterwards, pressing machine is shaping, disk is of a size of Φ 15 mm, thickness 1.5 mm;
(4) sinter
Adopt continuous tunnel furnace or box-type furnace, temperature, at 400 DEG C of insulation 1 h binder removals, is then incubated 2 h in 1100 ~ 1200 DEG C;
(5) by silver electrode
Adopt continuous tunnel furnace or box-type furnace, 850 ~ 870 DEG C of temperature 0.5 ~ 1 h.
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|---|---|---|---|
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|---|---|---|---|
| CN201410673596.1A CN104478428B (en) | 2014-11-21 | 2014-11-21 | Zinc oxide piezoresistor material with high electric potential gradient |
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| CN104478428B CN104478428B (en) | 2017-02-22 |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105139986A (en) * | 2015-09-23 | 2015-12-09 | 南京先正电子有限公司 | Explosion-proof type zinc oxide piezoresistor and preparation method thereof |
| CN105272208A (en) * | 2015-11-07 | 2016-01-27 | 汕头高新区松田实业有限公司 | Zinc oxide piezoresistor dielectric material and preparation method thereof |
| CN106024231A (en) * | 2016-05-27 | 2016-10-12 | 辰硕电子(九江)有限公司 | Preparation method of zinc oxide piezoresistor ceramic chip |
| CN107021751A (en) * | 2017-04-10 | 2017-08-08 | 湖北工业大学 | A kind of high-potential gracient arrester zinc oxide piezoresistor ceramic |
| CN108264343A (en) * | 2018-02-07 | 2018-07-10 | 合肥安力电力工程有限公司 | A kind of modified nano zinc oxide piezoresistive material and preparation method thereof |
| 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 |
| CN108774061A (en) * | 2018-06-26 | 2018-11-09 | 东莞市瓷谷电子科技有限公司 | A kind of high-performance zinc oxide pressure-sensitive resistor medium material and preparation method thereof |
| CN108794036A (en) * | 2018-05-23 | 2018-11-13 | 宁夏中科天际防雷研究院有限公司 | A kind of lightning protection electrical chip and its preparation method and application based on zinc oxide |
| CN109734435A (en) * | 2018-11-19 | 2019-05-10 | 西安交通大学 | A kind of Nanocrystalline Zno-based Varistor material and preparation method |
| CN110423110A (en) * | 2019-09-01 | 2019-11-08 | 烟台大学 | A kind of ultra-high non-linear ZnO-Bi2O3Base voltage-sensitive ceramic and preparation method thereof |
| CN116835975A (en) * | 2023-07-05 | 2023-10-03 | 广东电网有限责任公司 | ZnO polycrystalline ceramic with high breakdown field strength, preparation method and cable sheath protector |
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| CN103951415A (en) * | 2014-04-01 | 2014-07-30 | 西安电子科技大学 | High-voltage-gradient zinc oxide pressure-sensitive resistor and making method thereof |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105139986A (en) * | 2015-09-23 | 2015-12-09 | 南京先正电子有限公司 | Explosion-proof type zinc oxide piezoresistor and preparation method thereof |
| CN105139986B (en) * | 2015-09-23 | 2018-04-03 | 南京先正电子股份有限公司 | Explosion-proof type zinc oxide varistor and preparation method thereof |
| CN105272208A (en) * | 2015-11-07 | 2016-01-27 | 汕头高新区松田实业有限公司 | Zinc oxide piezoresistor dielectric material and preparation method thereof |
| CN105272208B (en) * | 2015-11-07 | 2018-04-27 | 汕头高新区松田实业有限公司 | A kind of zinc oxide varistor dielectric material and preparation method thereof |
| CN106024231A (en) * | 2016-05-27 | 2016-10-12 | 辰硕电子(九江)有限公司 | Preparation method of zinc oxide piezoresistor ceramic chip |
| CN106024231B (en) * | 2016-05-27 | 2018-07-10 | 辰硕电子(九江)有限公司 | A kind of preparation method of zinc oxide varistor tile |
| CN107021751A (en) * | 2017-04-10 | 2017-08-08 | 湖北工业大学 | A kind of high-potential gracient arrester zinc oxide piezoresistor ceramic |
| CN108264343A (en) * | 2018-02-07 | 2018-07-10 | 合肥安力电力工程有限公司 | A kind of modified nano zinc oxide piezoresistive material and preparation method thereof |
| 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 |
| CN108794036A (en) * | 2018-05-23 | 2018-11-13 | 宁夏中科天际防雷研究院有限公司 | A kind of lightning protection electrical chip and its preparation method and application based on zinc oxide |
| CN108774061A (en) * | 2018-06-26 | 2018-11-09 | 东莞市瓷谷电子科技有限公司 | A kind of high-performance zinc oxide pressure-sensitive resistor medium material and preparation method thereof |
| CN108774061B (en) * | 2018-06-26 | 2021-06-01 | 东莞市瓷谷电子科技有限公司 | High-performance zinc oxide piezoresistor dielectric material and preparation method thereof |
| CN109734435A (en) * | 2018-11-19 | 2019-05-10 | 西安交通大学 | A kind of Nanocrystalline Zno-based Varistor material and preparation method |
| CN110423110A (en) * | 2019-09-01 | 2019-11-08 | 烟台大学 | A kind of ultra-high non-linear ZnO-Bi2O3Base voltage-sensitive ceramic and preparation method thereof |
| CN110423110B (en) * | 2019-09-01 | 2021-11-05 | 烟台大学 | Ultrahigh nonlinear ZnO-Bi2O3Base pressure sensitive ceramic and preparation method thereof |
| CN116835975A (en) * | 2023-07-05 | 2023-10-03 | 广东电网有限责任公司 | ZnO polycrystalline ceramic with high breakdown field strength, preparation method and cable sheath protector |
| CN116835975B (en) * | 2023-07-05 | 2024-05-14 | 广东电网有限责任公司 | ZnO polycrystalline ceramic with high breakdown field strength, preparation method and cable sheath protector |
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