CN103951415A - High-voltage-gradient zinc oxide pressure-sensitive resistor and making method thereof - Google Patents
High-voltage-gradient zinc oxide pressure-sensitive resistor and making method thereof Download PDFInfo
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- CN103951415A CN103951415A CN201410128031.5A CN201410128031A CN103951415A CN 103951415 A CN103951415 A CN 103951415A CN 201410128031 A CN201410128031 A CN 201410128031A CN 103951415 A CN103951415 A CN 103951415A
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Abstract
The invention relates to a high-voltage-gradient zinc oxide pressure-sensitive resistor and a making method thereof. The pressure-sensitive resistor comprises 95-99mol% of zinc oxide, and the balance additive; and the additive comprises 0.25-1.20mol% of Sn by SnO2, 0.20-1.00mol% of Sb by Sb2O3, 0.15-0.80mol% of Co by Co3O4, 0.10-0.40mol% of Mn by Mn2O3, 0.10-0.50mol% of Bi by Bi2O3, 0.10-0.50mol% of Ni by NiO, 0.02-0.10mol% of SiO2, 0.075-0.30mol% of B by B2O3, and 0.005-0.20mol% of Al2O3. The method guarantees the excellent electrical performances, reduces the consumption of the additive, and reduces the production cost.
Description
Technical field
The present invention relates to a kind of high voltage gradient zinc oxide varistor and preparation method thereof, particularly a kind of low-cost Zinc-oxide piezoresistor and preparation method thereof, belongs to piezoresistive material preparation field.
Background technology
ZnO varistor is to take ZnO powder as main body, adds other mental compound additives of lot of trace (as Bi
2o
3, Sb
2o
3, MnCO
3, Co
3o
4, Cr
2o
3deng), the heterogeneous semiconductive ceramic element of polycrystalline that at high temperature sintering forms after mixing, moulding.Since its invention, ZnO varistor is, the excellent properties such as response fast, nonlinear factor large, leakage current little, through-current capability strong easily manufactured with it just, in power system and electronic industry, is widely used.
For for the ZnO varistor of multiple additives, it is particularly important that material prescription seems.Wherein the processing treatment of additive is the most key, and the preprocessing of portions additive processing is a kind of processing and treating method of conventional additive.In voltage dependent resistor, additive proportion increases voltage dependent resistor cost compared with conference.
Summary of the invention
The object of the invention is to, make up the deficiencies in the prior art, propose a kind of high voltage gradient zinc oxide varistor and preparation method thereof, when guaranteeing that every electrical property is good, reduce the consumption of additive, reduce production costs.
For achieving the above object, the technical solution used in the present invention is as follows:
A high voltage gradient zinc oxide varistor, is comprised of zinc oxide and additive, and wherein zinc oxide ZnO content is 95～99mol%, and its surplus is additive; It is characterized in that: described additive is elementary composition by Sn, Sb, Co, Mn, Bi, Ni, Si, B and Al, the molecular fraction that each element of interpolation calculates by its oxide form is as follows respectively: SnO
2be 0.25～1.20, Sb
2o
3be 0.20～1.00, Co
3o
4be 0.15～0.80, Mn
2o
3be 0.10～0.40, Bi
2o
3be that 0.10～0.50, NiO is 0.10～0.50, SiO
2be 0.02～0.10, B
2o
3be 0.075～0.30, Al
2o
3be 0.005～0.20.
The preparation method of described high voltage gradient zinc oxide varistor, comprises the steps:
(1) adopt wet chemical method, three kinds in additive raw material Sn, Sb, Co, Mn, Bi and Ni or three kinds are mixed above, obtain polynary nanometer powder;
(2) above-mentioned polynary nanometer powder is mixed with the micropowder of major ingredient zinc oxide ZnO and other additive elements, obtain composite granule;
(3) according to electronic ceramic technology, above-mentioned composite granule is carried out to granulation compressing tablet and makes raw cook, then by raw cook at 900～1100 ℃ of sintering, finally by being obtained described high voltage gradient zinc oxide varistor by silver, silver ink firing.
Wet chemical method described in described step (1) is to adopt sol-gel method or coprecipitation method.
Mixing described in described step (2) is to adopt ball milled.
Described sol-gel method, refer to three kinds in additive raw material Sn, Sb, Co, Mn, Bi and Ni or three kinds are dissolved in respectively in solvent above, mix, stir, add complexing agent, then add ammoniacal liquor or thanomin to regulate pH to 6～11, at 40～80 ℃, heating in water bath is dried to obtain xerogel by colloidal sol at 100～200 ℃ to form stable colloidal sol in 6～20 hours again, finally xerogel is calcined 1～2 hour at 500～800 ℃.
Described coprecipitation method, refer to additive raw material Sn, Sb, Co, Mn, three kinds or three kinds in Bi and Ni are jointly dissolved in appropriate amount of deionized water or ethylene glycol and obtain mixing salt solution above, then prepare precipitant solution, in reaction tank, add deionized water and precipitant solution to regulate pH to 6～11 again, thereby acquisition mother liquor, above-mentioned mixing salt solution and precipitant solution are splashed in mother liquor simultaneously and keep pH to be stabilized in 8～11, being added dropwise to complete rear continuation stirs 1～2 hour at 30～70 ℃, refilter and be precipitated, with deionized water repetitive scrubbing, precipitate 3～5 times, again 80～100 ℃ of oven dry, finally 500～800 ℃ of calcinings 1～2 hour.
Described ball milled, refers to and adopts agate ball or Stainless Steel Ball, the water of usining in planetary ball mill carries out wet-milling as medium, and rotating speed is 400～800rpm, and ratio of grinding media to material is 1: 1～5: 1, and Ball-milling Time is 4～10 hours.
Sintering time described in above-mentioned steps (3) is 1～4 hour.
Compared with prior art, the pressure sensitive voltage of the Zinc-oxide piezoresistor of the unleaded Chrome-free that the present invention obtains is 400～550V/mm, nonlinear factor α > 25, leakage current I
l< 10 μ A, over-all properties is good; Meanwhile, in voltage dependent resistor of the present invention, additive proportion is more generally invented and is reduced approximately 25%, has greatly reduced cost.
Embodiment
Below in conjunction with specific embodiment, the present invention is done to further detailed, complete explanation.
Embodiment 1
The formula of the present embodiment is as follows:
ZnO（99mol%），SnO
2（0.25?mol%），Sb
2O
3（0.20?mol%），Co
3O
4（0.15?mol%），Mn
2O
3?（0.10?mol%），Bi
2O
3（0.10?mol%），NiO（0.10?mol%），SiO
2（0.02?mol%），B
2O
3（0.075?mol%），Al
2O
3（0.005?mol%）。
By Co (CH
3cOO)
24H
2o, Mn (CH
3cOO)
24H
2o and Ni (NO
3)
26H
2o is dissolved in hot water jointly, Bi (NO
3)
35H
2o is dissolved in ethylene glycol, mix, stir, add aqueous citric acid solution, then add thanomin to regulate pH to 10, again at 80 ℃ heating in water bath 20 hours to form stable colloidal sol, colloidal sol is dried to obtain to xerogel at 170 ℃, finally xerogel is obtained to polynary nanometer powder for 2 hours 580 ℃ of calcinings.
By above-mentioned polynary nanometer powder and major ingredient ZnO and additive SnO
2, Sb
2o
3, SiO
2, H
3bO
3and Al (NO
3)
39H
2the micron order additive raw material of O mixes, and adopts agate ball, and the water of usining in planetary ball mill carries out wet-milling as medium, and rotating speed is 500rpm, and ratio of grinding media to material is 1: 1, and Ball-milling Time is 8 hours.The complete powder of ball milling obtains composite granule through oven dry, grinding;
According to electronic ceramic technology, above-mentioned composite granule is carried out to granulation compressing tablet and makes raw cook, then by raw cook 1050 ℃ of sintering 2 hours, finally by draping over one's shoulders silver, silver ink firing, obtain described high voltage gradient zinc oxide varistor.
Test learns that the pressure sensitive voltage of obtained Zinc-oxide piezoresistor is 436V/mm, and nonlinear factor α is 37, leakage current I
lbe 5 μ A.
Embodiment 2
The formula of the present embodiment is as follows:
ZnO（98mol%），SnO
2（0.55?mol%），Sb
2O
3（0.35?mol%），Co
3O
4（0.30?mol%），Mn
2O
3?（0.25?mol%），Bi
2O
3（0.20?mol%），NiO（0.15?mol%），SiO
2（0.04?mol%），B
2O
3（0.15?mol%），Al
2O
3（0.01?mol%）。
By Co (CH
3cOO)
24H
2o, Mn (CH
3cOO)
24H
2o and Ni (NO
3)
26H
2o is dissolved in hot water jointly, SnCl
4, Sb (CH
3cOO)
34H
2o and Bi (NO
3)
35H
2o is dissolved in ethylene glycol, mix, stir, add aqueous citric acid solution, then add ammoniacal liquor to regulate pH to 8, again at 60 ℃ heating in water bath 18 hours to form stable colloidal sol, colloidal sol is dried to obtain to xerogel at 100 ℃, finally xerogel is obtained to polynary nanometer powder for 1 hour 680 ℃ of calcinings.
By above-mentioned polynary nanometer powder and major ingredient ZnO and additive SiO
2, H
3bO
3and Al (NO
3)
39H
2the micron order additive raw material of O mixes, and adopts Stainless Steel Ball, and the water of usining in planetary ball mill carries out wet-milling as medium, and rotating speed is 700rpm, and ratio of grinding media to material is 1: 1, and Ball-milling Time is 6 hours.The complete powder of ball milling obtains composite granule through oven dry, grinding;
?according to electronic ceramic technology, above-mentioned composite granule is carried out to granulation compressing tablet and makes raw cook, then by raw cook 1000 ℃ of sintering 3 hours, finally by draping over one's shoulders silver, silver ink firing, obtain described low-cost Zinc-oxide piezoresistor.
Test learns that the pressure sensitive voltage of obtained Zinc-oxide piezoresistor is 516V/mm, and nonlinear factor α is 26, leakage current I
lbe 9 μ A.
Embodiment 3
The formula of the present embodiment is as follows:
ZnO（96.5mol%），SnO
2（0.90?mol%），Sb
2O
3（0.70?mol%），Co
3O
4（0.55?mol%），Mn
2O
3?（0.35?mol%），Bi
2O
3（0.35?mol%），NiO（0.30?mol%），SiO
2（0.06?mol%），B
2O
3（0.25?mol%），Al
2O
3（0.04?mol%）。
By Co (CH
3cOO)
24H
2o, Mn (CH
3cOO)
24H
2o and Bi
2o
3jointly be dissolved in nitric acid and obtain mixing salt solution, then prepare the K of 1mol/L
2cO
3solution, then add deionized water and K in reaction tank
2cO
3solution is by pH regulator to 9.40 acquisition mother liquor, by above-mentioned mixing salt solution and K
2cO
3solution splashes in mother liquor simultaneously and keeps pH to be stabilized in 9.20 left and right, is added dropwise to complete rear continuation and stirs 1 hour at 40 ℃, refilters and is precipitated, with deionized water repetitive scrubbing, precipitate 3 times, then 100 ℃ of oven dry, finally 580 ℃ of calcinings 2 hours.
By above-mentioned polynary nanometer powder and major ingredient ZnO and additive SnO
2, Sb
2o
3, NiO, SiO
2, H
3bO
3and Al (NO
3)
39H
2the micron order additive raw material of O mixes, and adopts agate ball, and the water of usining in planetary ball mill carries out wet-milling as medium, and rotating speed is 550rpm, and ratio of grinding media to material is 1: 1, and Ball-milling Time is 8 hours.The complete powder of ball milling obtains composite granule through oven dry, grinding;
According to electronic ceramic technology, above-mentioned composite granule is carried out to granulation compressing tablet and makes raw cook, then by raw cook 1050 ℃ of sintering 2 hours, finally by draping over one's shoulders silver, silver ink firing, obtain described low-cost Zinc-oxide piezoresistor.
Test learns that the pressure sensitive voltage of obtained Zinc-oxide piezoresistor is 432V/mm, and nonlinear factor α is 36, leakage current I
lbe 4 μ A.
Embodiment 4
The formula of the present embodiment is as follows:
ZnO（95mol%），SnO
2（1.20?mol%），Sb
2O
3（1.00?mol%），Co
3O
4（0.80?mol%），Mn
2O
3?（0.40?mol%），Bi
2O
3（0.50?mol%），NiO（0.50?mol%），SiO
2（0.10?mol%），B
2O
3（0.30?mol%），Al
2O
3（0.20?mol%）。
By Co (CH
3cOO)
24H
2o, Mn (CH
3cOO)
24H
2o and Bi
2o
3jointly be dissolved in and in nitric acid, obtain mixing salt solution, then measure 100ml ammoniacal liquor, in reaction tank, add deionized water and ammoniacal liquor by pH regulator to 9.60 acquisition mother liquor again, by above-mentioned mixing salt solution with ammoniacal liquor splashes in mother liquor and keep pH to be stabilized in 9.00 left and right simultaneously, be added dropwise to complete rear continuation and stir 2 hours at 60 ℃, refilter and be precipitated, with deionized water repetitive scrubbing, precipitate 5 times, again 80 ℃ of oven dry, finally 680 ℃ of calcinings 1 hour.
By above-mentioned polynary nanometer powder and major ingredient ZnO and additive SnO
2, Sb
2o
3, NiO, SiO
2, H
3bO
3and Al (NO
3)
39H
2the micron order additive raw material of O mixes, and adopts Stainless Steel Ball, and the water of usining in planetary ball mill carries out wet-milling as medium, and rotating speed is 700rpm, and ratio of grinding media to material is 1: 1, and Ball-milling Time is 6 hours.The complete powder of ball milling obtains composite granule through oven dry, grinding;
According to electronic ceramic technology, above-mentioned composite granule is carried out to granulation compressing tablet and makes raw cook, then by raw cook 1000 ℃ of sintering 3 hours, finally by draping over one's shoulders silver, silver ink firing, obtain described high voltage gradient zinc oxide varistor.
Test learns that the pressure sensitive voltage of obtained Zinc-oxide piezoresistor is 411V/mm, and nonlinear factor α is 32, leakage current I
lbe 7 μ A.
The present invention is not only confined to above-mentioned embodiment; persons skilled in the art are according to content disclosed by the invention; can adopt other multiple embodiments to implement the present invention; therefore; every employing project organization of the present invention and thinking; do some simple designs that change or change, all fall into protection scope of the present invention.
Claims (8)
1. a high voltage gradient zinc oxide varistor, is comprised of zinc oxide and additive, and wherein ZnO content is 95～99mol%, and its surplus is additive; It is characterized in that: described additive is elementary composition by Sn, Sb, Co, Mn, Bi, Ni, Si, B and Al, the molecular fraction that each element of interpolation calculates by its oxide form is as follows respectively: SnO
2be 0.25～1.20, Sb
2o
3be 0.20～1.00, Co
3o
4be 0.15～0.80, Mn
2o
3be 0.10～0.40, Bi
2o
3be that 0.10～0.50, NiO is 0.10～0.50, SiO
2be 0.02～0.10, B
2o
3be 0.075～0.30, Al
2o
3be 0.005～0.20.
2. the preparation method of high voltage gradient zinc oxide varistor according to claim 1, comprises the steps:
(1) adopt wet chemical method, three kinds in additive raw material Sn, Sb, Co, Mn, Bi and Ni or three kinds are mixed above, obtain polynary nanometer powder;
(2) above-mentioned polynary nanometer powder is mixed with the micropowder of major ingredient zinc oxide ZnO and other additive elements, obtain composite granule;
(3) according to electronic ceramic technology, above-mentioned composite granule is carried out to granulation compressing tablet and makes raw cook, then by raw cook at 900～1100 ℃ of sintering, finally by draping over one's shoulders silver, silver ink firing, obtain described high voltage gradient zinc oxide varistor.
3. the preparation method of high voltage gradient zinc oxide varistor according to claim 2, is characterized in that: the wet chemical method described in step (1) is to adopt sol-gel method or coprecipitation method.
4. the preparation method of high voltage gradient zinc oxide varistor according to claim 2, is characterized in that: mixing described in step (2) is to adopt ball milled.
5. the preparation method of a kind of high voltage gradient zinc oxide varistor according to claim 3, it is characterized in that: described sol-gel method, refer to three kinds in additive raw material Sn, Sb, Co, Mn, Bi and Ni or three kinds are dissolved in respectively in solvent above, mix, stir, add complexing agent, then add ammoniacal liquor or thanomin to regulate pH to 6～11, again at 40～80 ℃ heating in water bath 6～20 hours to form stable colloidal sol, colloidal sol is dried to obtain to xerogel at 100～200 ℃, finally xerogel is calcined 1～2 hour at 500～800 ℃.
6. the preparation method of a kind of high voltage gradient zinc oxide varistor according to claim 3, it is characterized in that: described coprecipitation method, refer to additive raw material Sn, Sb, Co, Mn, three kinds or three kinds in Bi and Ni are jointly dissolved in appropriate amount of deionized water or ethylene glycol and obtain mixing salt solution above, then prepare precipitant solution, in reaction tank, add deionized water and precipitant solution to regulate pH to 6～11 again, thereby acquisition mother liquor, above-mentioned mixing salt solution and precipitant solution are splashed in mother liquor simultaneously and keep pH to be stabilized in 8～11, being added dropwise to complete rear continuation stirs 1～2 hour at 30～70 ℃, refilter and be precipitated, with deionized water repetitive scrubbing, precipitate 3～5 times, again 80～100 ℃ of oven dry, finally 500～800 ℃ of calcinings 1～2 hour.
7. the preparation method of a kind of high voltage gradient zinc oxide varistor according to claim 4, it is characterized in that: described ball milled, refer to and adopt agate ball or Stainless Steel Ball, the water of usining in planetary ball mill carries out wet-milling as medium, rotating speed is 400～800rpm, ratio of grinding media to material is 1: 1～5: 1, and Ball-milling Time is 4～10 hours.
8. the preparation method of a kind of high voltage gradient zinc oxide varistor according to claim 2, is characterized in that: the sintering time described in step (3) is 1～4 hour.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104478428A (en) * | 2014-11-21 | 2015-04-01 | 四川大学 | Zinc oxide piezoresistor material with high electric potential gradient |
| CN106518049A (en) * | 2016-09-23 | 2017-03-22 | 清华大学 | Manufacturing process for improving voltage gradient of zinc-oxide voltage-sensitive ceramics |
| CN106653256A (en) * | 2017-01-13 | 2017-05-10 | 昆山福烨电子有限公司 | Carbon film resistor with low dielectric constant |
| CN109796202A (en) * | 2019-03-25 | 2019-05-24 | 电子科技大学 | A kind of high-performance low-temperature sintered lamination type piezoresistor material |
| CN111153693A (en) * | 2020-01-03 | 2020-05-15 | 西安恒翔电子新材料有限公司 | Porcelain powder for zinc oxide piezoresistor of lightning protection chip and preparation method thereof |
| CN111508676A (en) * | 2020-04-24 | 2020-08-07 | 国网湖南省电力有限公司 | Small-size distribution network annular zinc oxide resistance card and preparation method thereof |
| CN112851332A (en) * | 2021-01-30 | 2021-05-28 | 西安电子科技大学 | Method for preparing high-voltage gradient zinc oxide piezoresistor by doping coating method |
| 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 |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104478428A (en) * | 2014-11-21 | 2015-04-01 | 四川大学 | Zinc oxide piezoresistor material with high electric potential gradient |
| CN106518049A (en) * | 2016-09-23 | 2017-03-22 | 清华大学 | Manufacturing process for improving voltage gradient of zinc-oxide voltage-sensitive ceramics |
| CN106653256A (en) * | 2017-01-13 | 2017-05-10 | 昆山福烨电子有限公司 | Carbon film resistor with low dielectric constant |
| CN109796202A (en) * | 2019-03-25 | 2019-05-24 | 电子科技大学 | A kind of high-performance low-temperature sintered lamination type piezoresistor material |
| CN111153693A (en) * | 2020-01-03 | 2020-05-15 | 西安恒翔电子新材料有限公司 | Porcelain powder for zinc oxide piezoresistor of lightning protection chip and preparation method thereof |
| CN111508676A (en) * | 2020-04-24 | 2020-08-07 | 国网湖南省电力有限公司 | Small-size distribution network annular zinc oxide resistance card and preparation method thereof |
| CN111508676B (en) * | 2020-04-24 | 2021-08-24 | 国网湖南省电力有限公司 | Small-size distribution network annular zinc oxide resistance card and preparation method thereof |
| CN112851332A (en) * | 2021-01-30 | 2021-05-28 | 西安电子科技大学 | Method for preparing high-voltage gradient zinc oxide piezoresistor by doping coating method |
| 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 |
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| Publication number | Publication date |
|---|---|
| CN103951415B (en) | 2016-04-27 |
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