CN104150896A - High-through-flow small-sized zinc oxide varistor dielectric material and preparation method thereof - Google Patents
High-through-flow small-sized zinc oxide varistor dielectric material and preparation method thereof Download PDFInfo
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- CN104150896A CN104150896A CN201410389495.1A CN201410389495A CN104150896A CN 104150896 A CN104150896 A CN 104150896A CN 201410389495 A CN201410389495 A CN 201410389495A CN 104150896 A CN104150896 A CN 104150896A
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Abstract
The invention relates to a high-through-flow small-sized zinc oxide varistor dielectric material and a preparation method thereof. The high-through-flow small-sized zinc oxide varistor dielectric material comprises a major component, a first auxiliary component and a second auxiliary component, wherein the major component comprises 100 mol of ZnO; the first auxiliary component comprises Sb2O3, Co2O3, Bi2O3, MnO2, Cr2O3 and Ni2O3, each of which is 0.05-1.3 mol; the second auxiliary component comprises Al2O3, boric acid and AgNO3, each of which is 0.05-0.6 mol. A varistor prepared from the high-through-flow small-sized zinc oxide varistor dielectric material is smaller in size, and the pulse impact resistance is greatly improved; the nonlinear coefficient of the acquired high-through-flow small-sized zinc oxide varistor dielectric material is more than 50; the pulse impact resistance of the high-through-flow small-sized zinc oxide varistor dielectric material is high.
Description
Technical field
The present invention relates to a kind of dielectric material of resistor, relate in particular to a kind of high throughflow miniaturization zinc oxide varistor dielectric material and preparation method thereof.
Background technology
Zinc oxide piezoresistive material can be used for manufacturing high-energy zinc oxide varistor, and this resistor disc can be used for manufacturing thunder arrester or piezoresistor, is applied to absorb abnormal overvoltage with protection circuit system in power electronic circuits.Often can be because thunderbolt load switching causes circuit abnormal overvoltage in power electronic circuits, zinc oxide material has absorbed for power electronic circuits in a large number or has suppressed abnormal overvoltage, and protection power electronic equipment exempts from destruction.
At present, on market in disclosed Zinc-oxide piezoresistor, the shared quality overall proportion of main component zinc oxide is 87～91%, the quality overall proportion of other additive accounts for 9～13%, Zinc-oxide piezoresistor industry personage clearly knows, the size of product through-current capability is decided by ceramics size, market requires more and more higher to product size now, miniaturization product is progressively by the market requirement, in market competition very fierce today, in the face of the pressure to product size on market, the application of Zinc-oxide piezoresistor and popularization all will be subject to great negative impact, high throughflow miniaturization zinc oxide varistor in view of this consideration, guaranteeing under the condition that pulse shock tolerance is good, the invention of miniaturization Zinc-oxide piezoresistor dielectric material is the inevitable product of market development.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of high throughflow miniaturization zinc oxide varistor dielectric material and preparation method thereof, the piezoresistor of being made by this high throughflow miniaturization zinc oxide varistor dielectric material has high impulse and impacts tolerance, the advantage that volume is little.The technical scheme adopting is as follows:
A high throughflow miniaturization Zinc-oxide piezoresistor dielectric material, is characterized in that: comprise principal constituent, the first minor component and the second minor component, each content forming is as follows:
Principal constituent comprises ZnO, and the content of ZnO is 100mol;
The first minor component comprises Sb
2o
3, Co
2o
3, Bi
2o
3, MnO
2, Cr
2o
3, Ni
2o
3, the content of each component is 0.05～1.3mol;
The second minor component comprises Al
2o
3, boric acid, AgNO
3, the content of each component is 0.05～0.6 mol.
In formula, the content of Ag glass is generally 0.05～0.6 mol, so being 1.26 Ag+, the ionic radius of Ag+ is difficult to enter ZnO crystal grain inside, only may be present in grain boundary segregation layer, monovalent ion have reduce and clamp down on fermi level EFB(Chinese) effect, be a kind of crystal boundary stablizer, so monovalent ion Ag+ can improve non-linear a value, reduce through-flow velocity of variation, in Zinc-oxide piezoresistor dielectric material after sintering, contain Sb
2o
3, Co
2o
3, Bi
2o
3, MnO
2, Cr
2o
3, Ni
2o
3with a small amount of Al
2o
3, boric acid, AgNO
3, its Ag glass form can with Zinc-oxide piezoresistor porcelain each mutually well molten and, be conducive to Ag+ and be uniformly distributed in porcelain body, Ag glass is conducive to aging resistance, because of it, clamp down on fermi level and suppressed ion migration, make state-of-charge dipole reduced number, thereby extend work-ing life.B in formula
2o
3content be generally 0.05～0.6 mol, B
2o
3be the oxide compound that can form separately glass that a kind of surface can be extremely low, in sintering process, B2O3 easily and Bi
2o
3, Sb
2o
3generate fine and close glassy phase with calking zine ion, this glassy phase moves to surface under the effect of vapour pressure, fills because of Bi
2o
3, Sb
2o
3the pore that volatilizees and generate, in process of cooling, it can form good engagement between crystal grain and spinel, has reduced grain boundary defects concentration, so it has the effect of the moisture absorption of preventing and the through-flow velocity of variation of change.Owing to there is more ZnO in frit, can stop the Zn ion on ZnO crystal grain point to spread in crystal grain layer, thereby the concentration of Zn ion is higher in crystal grain, grain resistance value is low, so large current non-linear is better, this glass fusing point is low, is conducive to increase liquid content and Bi
2o
3the abundant solid solution of being respectively on good terms, at high temperature increased Mn, Cr, the content of Co plasma in liquid phase, making has the segregation in high resistant interfacial layer of more ion in process of cooling, reinforces and has improved potential barrier.Therefore, the made voltage dependent resistor of this high throughflow miniaturization Zinc-oxide piezoresistor dielectric material, not only increased substantially pulse shock tolerance, and product size is less; Also can be by regulating the chemical constitution ratio of material to obtain high throughflow miniaturization zinc oxide piezoresistor ceramic material; The high throughflow miniaturization Zinc-oxide piezoresistor dielectric material nonlinear factor obtaining is greater than 50; Manufacture craft is simple, makes and synchronizes with conventional Zinc-oxide piezoresistor; High throughflow miniaturization zinc oxide piezoresistor ceramic material pulse shock tolerance is strong, is expected to be applied to the lightning protection overvoltage protection of electric lightning or other power electronic circuits.
In this formula, introduce Al
2o
3, boric acid, AgNO
3improved the current density in product unit surface, the pulse shock tolerance of zinc oxide varistor is decided by the cross-sectional area of product, in the pulse shock tolerance situation of regulation, thereby the current density that improves product unit cross-sectional area just can be dwindled product cross-sectional area and reached product miniaturization production.
As preferred version of the present invention, described Al
2o
3with Al(NO
3) form introducing.
As preferred version of the present invention, described MnO
2with Mn
3o
4, MnO
2or MnCO
3form is introduced.
As preferred version of the present invention, described Co
2o
3with Co
3o
4, or the carbonate that contains cobalt element or organic salt introducing.
A preparation method for high throughflow miniaturization Zinc-oxide piezoresistor dielectric material, is characterized in that comprising the steps:
(1) preparation of additive slip: according to proportioning, take the first minor component Sb
2o
3, Co
2o
3, Bi
2o
3, MnO
2, Cr
2o
3, Ni
2o
3, and the second minor component Al
2o
3, boric acid, AgNO
3, add appropriate pure water and dispersion agent to carry out high-speed stirring or ball milling, each component is fully mixed, make additive slip;
(2) preparation of spraying slip: add principal constituent ZnO to additive slip the inside, fully stir or ball milling, and add polyvinyl alcohol solution to make spraying slip; Through 3 hours high-speed stirring or ball milling, at the proportion of spraying slip, be 1.5～2.2, and viscosity is while being 40～200cps, starts to prepare mist projection granulating;
Proportion at spraying slip is 1.5～2.2, and in the viscosity situation that is 40～200cps, in spraying slurry each component can be dispersed, mix, can layering, make the content of each composition in the granulation powder of gained in subsequent step (3) even, improve the quality of product.
(3) preparation of pelletizing: adopt spray-drying tower by step (2) gained spraying slip spray drying granulation;
(4) dry-pressing formed: the granulation powder of step (3) gained, through dry-pressing formed, is made to disc-shaped blank on demand;
(5) sintering: by dry-pressing formed blank, after getting rid of polyvinyl alcohol colloid, in temperature, be sintering under 1100～1280 ℃ of conditions, remove moisture, ammonium salt dispersion agent and and remaining polyvinyl alcohol, obtain high throughflow miniaturization zinc oxide piezoresistor ceramic sheet.
As preferred version of the present invention, the dispersion agent in described step (1) is ammonium salt dispersion agent.
As the further preferred version of the present invention, described ammonium salt dispersion agent account for the first minor component and the second minor component total mass 0.8～1.5%.
As preferred version of the present invention, in described step (2), in the mixture of principal constituent, the first minor component and the second minor component, in every 100 grams of mixtures, add the polyvinyl alcohol solution containing 0.9～1.5 gram of solid polyethylene alcohol.
Compared with prior art, tool has the following advantages in the present invention:
The made voltage dependent resistor of this high throughflow miniaturization Zinc-oxide piezoresistor dielectric material, size is not only less, and has increased substantially pulse shock tolerance; Also can be by regulating the chemical constitution ratio of material to obtain high throughflow miniaturization zinc oxide piezoresistor ceramic material; The high throughflow miniaturization Zinc-oxide piezoresistor dielectric material nonlinear factor obtaining is greater than 50; Manufacture craft is simple, makes and synchronizes with conventional Zinc-oxide piezoresistor; High throughflow miniaturization zinc oxide piezoresistor ceramic material pulse shock tolerance is strong, is expected to be applied to the lightning protection overvoltage protection of electric lightning or other power electronic circuits.
Accompanying drawing explanation
Fig. 1 is the schema of manufacture method of the present invention;
Fig. 2 respectively organizes sample size schematic diagram;
Fig. 3 respectively organizes sample unit for electrical property parameters schematic diagram.
Embodiment
Below in conjunction with accompanying drawing and the preferred embodiment of the present invention, be described further.
Embodiment mono-
This high throughflow miniaturization Zinc-oxide piezoresistor dielectric material, comprises principal constituent, the first minor component and the second minor component, and each content forming is as follows:
Principal constituent comprises ZnO, and the content of ZnO is 100mol;
The first minor component comprises Sb
2o
3, Co
2o
3, Bi
2o
3, MnO
2, Cr
2o
3, Ni
2o
3, the content of each component is 0.05mol;
The second minor component comprises Al
2o
3, boric acid, AgNO
3, the content of each component is 0.05 mol.
In a kind of concrete scheme, above-mentioned Al
2o
3with Al(NO
3) form introducing.
In a kind of concrete scheme, above-mentioned MnO
2with Mn
3o
4, MnO
2or MnCO
3form is introduced.
In a kind of concrete scheme, above-mentioned Co
2o
3with Co
3o
4, or the carbonate that contains cobalt element or organic salt introducing.
As shown in Figure 1, the preparation method of this high throughflow miniaturization Zinc-oxide piezoresistor dielectric material, comprises the steps:
(1) preparation of additive slip: according to proportioning, take the first minor component Sb
2o
3, Co
2o
3, Bi
2o
3, MnO
2, Cr
2o
3, Ni
2o
3, and the second minor component Al
2o
3, boric acid, AgNO
3add appropriate pure water and ammonium salt dispersion agent, the mass ratio of pure water and ZnO is 0.7:1, ammonium salt dispersion agent account for the first minor component and the second minor component total mass 1%(0.8～1.5% can), then carry out high-speed stirring or ball milling, each component is fully mixed, and make median size be less than 1 μ m, make additive slip;
(2) preparation of spraying slip: add principal constituent ZnO to additive slip the inside, fully stir or ball milling, and add polyvinyl alcohol solution to make spraying slip, in the mixture of principal constituent, the first minor component and the second minor component, in every 100 grams of mixtures, add containing 1 gram of solid polyethylene alcohol (0.9～1.5 gram can) polyvinyl alcohol solution; Through 3 hours high-speed stirring or ball milling, the proportion of spraying slip be 1.8(1.5～2.2 can), and viscosity be 100(40～200cps can) time, start to prepare mist projection granulating;
(3) preparation of pelletizing: adopt spray-drying tower by step (2) gained spraying slip spray drying granulation;
(4) dry-pressing formed: the granulation powder of step (3) gained, through dry-pressing formed, is made to disc-shaped blank on demand;
(5) sintering: by dry-pressing formed blank after getting rid of polyvinyl alcohol colloid, in temperature, it is sintering under 1150 ℃ of (1100～1280 ℃ can) conditions, remove moisture, ammonium salt dispersion agent and and remaining polyvinyl alcohol, obtain high throughflow miniaturization zinc oxide piezoresistor ceramic sheet.
Embodiment bis-
In the situation that other parts are all identical with embodiment mono-, its difference is that the content of each component in the first minor component, the second minor component is different: each component S b in the first minor component
2o
3, Co
2o
3, Bi
2o
3, MnO
2, Cr
2o
3, Ni
2o
3content be 1.3mol; Each component Al in the second minor component
2o
3, boric acid, AgNO
3content be 0.6mol.
Embodiment tri-
In the situation that other parts are all identical with embodiment mono-, its difference is that the content of each component in the first minor component, the second minor component is different: each component S b in the first minor component
2o
3, Co
2o
3, Bi
2o
3, MnO
2, Cr
2o
3, Ni
2o
3content be 0.7mol; Each component Al in the second minor component
2o
3, boric acid, AgNO
3content be 0.3mol.
Embodiment tetra-
In the situation that other parts are all identical with embodiment mono-, its difference is that the content of each component in the first minor component, the second minor component is different: Sb in the first minor component
2o
3, Co
2o
3content be 0.1mol, Bi
2o
3, MnO
2content be 0.5mol, Cr
2o
3, Ni
2o
3content be 1.1mol; Al in the second minor component
2o
3content be 0.3mol, the content of boric acid is 0.08mol, AgNO
3content be 0.4mol.
According to above embodiment mono-to embodiment tetra-, make respectively 4 groups of zinc oxide piezoresistor ceramic sheet samples (black porcelain body), in zinc oxide piezoresistor ceramic sheet sample (black porcelain body) both ends of the surface, stamp silver electrode paste, through 590 ℃ of reduction, obtain argent electrode layer, make totally four groups of voltage dependent resistor prints, be labeled as successively test one, test two, test three and test four.
In addition, according to prior art, make one group of other voltage dependent resistor print, be labeled as comparative sample.
The size of the zinc oxide piezoresistor ceramic sheet (black magnet) of comparative sample and test one, test two, test three, test four as shown in Figure 2.
Then, in above five groups of voltage dependent resistor print two sides metal electrodes welding after tinned lead, by after print heating by porcelain body dip-coating epoxy resin weld, and by 150 ℃ curing 90 minutes, make electric performance test sample.
Adopt the Taibei to admire the special tester of section's TTK voltage dependent resistor, record five groups of three parameters that test is relevant.
Bearing pulsed current impact capacity is the key that piezoresistive element can obtain practical application.Sample pulse testing waveform of the present invention is 8/20 μ S simulation lightning wave, peak point current target value is 6000A(PANASONIC 2003 standards), the pressure sensitive voltage of test sample product before and after pulse shock test, calculate pressure sensitive voltage velocity of variation, and observe and decide sample bears the surface structure after pulse shock, if pressure sensitive voltage V1.0mA velocity of variation is in ± 10%, and after sample bears pulse shock, surface structure has no destruction, judge that this sample bears pulse shock performance qualified, otherwise judge that this sample was for losing efficacy.
Fig. 3 lists the electric performance test result that corresponding diagram 1 is respectively organized sample, " minimum a value, the front maximum leakage current of pulse shock before pulse shock " listed in Fig. 3, for the mean value of every group of data recording before pulse testing, " pulse shock failure rate " data are every group of failure number impacting in sum.
In Fig. 2 and Fig. 3, the contrast of test one, test two, test three, test four and comparative sample, the made voltage dependent resistor of zinc oxide piezoresistor ceramic sheet of producing by the present invention, less than the product of prior art dimensionally, through-flow tolerance increases substantially.
In addition; it should be noted that, the specific embodiment described in this specification sheets, its each several part titles etc. can be different; all equivalence or simple change of doing according to described structure, feature and the principle of patent design of the present invention, are included in the protection domain of patent of the present invention.Those skilled in the art can make various modifications or supplement or adopt similar mode to substitute described specific embodiment; only otherwise depart from structure of the present invention or surmount this scope as defined in the claims, all should belong to protection scope of the present invention.
Claims (8)
1. a high throughflow miniaturization Zinc-oxide piezoresistor dielectric material, is characterized in that: comprise principal constituent, the first minor component and the second minor component, each content forming is as follows:
Principal constituent comprises ZnO, and the content of ZnO is 100mol;
The first minor component comprises Sb
2o
3, Co
2o
3, Bi
2o
3, MnO
2, Cr
2o
3, Ni
2o
3, the content of each component is 0.05～1.3mol;
The second minor component comprises Al
2o
3, boric acid, AgNO
3, the content of each component is 0.05～0.6 mol.
2. high throughflow miniaturization Zinc-oxide piezoresistor dielectric material as claimed in claim 1, is characterized in that: described Al
2o
3with Al(NO
3) form introducing.
3. high throughflow miniaturization Zinc-oxide piezoresistor dielectric material as claimed in claim 1, is characterized in that: described MnO
2with Mn
3o
4, MnO
2or MnCO
3form is introduced.
4. high throughflow miniaturization Zinc-oxide piezoresistor dielectric material as claimed in claim 1, is characterized in that: described Co
2o
3with Co
3o
4, or the carbonate that contains cobalt element or organic salt introducing.
5. the preparation method of high throughflow miniaturization Zinc-oxide piezoresistor dielectric material as claimed in claim 1, is characterized in that comprising the steps:
(1) preparation of additive slip: according to proportioning, take the first minor component Sb
2o
3, Co
2o
3, Bi
2o
3, MnO
2, Cr
2o
3, Ni
2o
3, and the second minor component Al
2o
3, boric acid, AgNO
3, add appropriate pure water and dispersion agent to carry out high-speed stirring or ball milling, each component is fully mixed, make additive slip;
(2) preparation of spraying slip: add principal constituent ZnO to additive slip the inside, fully stir or ball milling, and add polyvinyl alcohol solution to make spraying slip; Through 3 hours high-speed stirring or ball milling, at the proportion of spraying slip, be 1.5～2.2, and viscosity is while being 40～200cps, starts to prepare mist projection granulating;
(3) preparation of pelletizing: adopt spray-drying tower by step (2) gained spraying slip spray drying granulation;
(4) dry-pressing formed: the granulation powder of step (3) gained, through dry-pressing formed, is made to disc-shaped blank on demand;
(5) sintering: by dry-pressing formed blank, after getting rid of polyvinyl alcohol colloid, in temperature, be sintering under 1100～1280 ℃ of conditions, remove moisture, ammonium salt dispersion agent and and remaining polyvinyl alcohol, obtain high throughflow miniaturization zinc oxide piezoresistor ceramic sheet.
6. the preparation method of high throughflow miniaturization Zinc-oxide piezoresistor dielectric material as claimed in claim 5, is characterized in that: the dispersion agent in described step (1) is ammonium salt dispersion agent.
7. the preparation method of high throughflow miniaturization Zinc-oxide piezoresistor dielectric material as claimed in claim 6, is characterized in that: described ammonium salt dispersion agent account for the first minor component and the second minor component total mass 0.8～1.5%.
8. the preparation method of high throughflow miniaturization Zinc-oxide piezoresistor dielectric material as claimed in claim 5, it is characterized in that: in described step (2), in the mixture of principal constituent, the first minor component and the second minor component, in every 100 grams of mixtures, add the polyvinyl alcohol solution containing 0.9～1.5 gram of solid polyethylene alcohol.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104681223A (en) * | 2014-12-29 | 2015-06-03 | 广西新未来信息产业股份有限公司 | Lightning and surge protection composite pressure sensitive resistor and manufacturing 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 |
| CN105906339A (en) * | 2016-04-20 | 2016-08-31 | 宝鸡瑞丰电子科技有限公司 | Large-through-current medium-voltage ZnO pressure-sensitive resistance ceramic material and preparation method thereof |
| CN107021750A (en) * | 2017-03-24 | 2017-08-08 | 合肥羿振电力设备有限公司 | A kind of high sensitivity Zinc-oxide piezoresistor |
| CN109956744A (en) * | 2017-12-22 | 2019-07-02 | 东莞碧克电子有限公司 | High-performance varistor of primary protection and preparation method thereof |
| CN110563457A (en) * | 2019-09-05 | 2019-12-13 | 华南理工大学 | nitrogen ion doped zinc oxide-based piezoresistor and preparation method thereof |
| CN111029071A (en) * | 2019-12-31 | 2020-04-17 | 常州泰捷防雷科技有限公司 | Preparation method of medium-voltage gradient zinc oxide piezoresistor MOV chip |
| CN111181143A (en) * | 2020-02-18 | 2020-05-19 | 北京捷安通达科贸有限公司 | Transient impulse voltage suppressor |
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| CN101350239A (en) * | 2007-07-16 | 2009-01-21 | 深圳振华富电子有限公司 | Stacking slice type piezoresistor and manufacturing method thereof |
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| CN101350239A (en) * | 2007-07-16 | 2009-01-21 | 深圳振华富电子有限公司 | Stacking slice type piezoresistor and manufacturing method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104681223A (en) * | 2014-12-29 | 2015-06-03 | 广西新未来信息产业股份有限公司 | Lightning and surge protection composite pressure sensitive resistor and manufacturing method thereof |
| CN104681223B (en) * | 2014-12-29 | 2018-07-13 | 广西新未来信息产业股份有限公司 | A kind of compound piezoresistor of lightning protection surge 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 |
| CN105906339A (en) * | 2016-04-20 | 2016-08-31 | 宝鸡瑞丰电子科技有限公司 | Large-through-current medium-voltage ZnO pressure-sensitive resistance ceramic material and preparation method thereof |
| CN105906339B (en) * | 2016-04-20 | 2019-02-12 | 宝鸡瑞丰电子科技有限公司 | A kind of through-flow middle pressure ZnO varistor porcelain and preparation method thereof greatly |
| CN107021750A (en) * | 2017-03-24 | 2017-08-08 | 合肥羿振电力设备有限公司 | A kind of high sensitivity Zinc-oxide piezoresistor |
| CN109956744A (en) * | 2017-12-22 | 2019-07-02 | 东莞碧克电子有限公司 | High-performance varistor of primary protection and preparation method thereof |
| CN110563457A (en) * | 2019-09-05 | 2019-12-13 | 华南理工大学 | nitrogen ion doped zinc oxide-based piezoresistor and preparation method thereof |
| CN111029071A (en) * | 2019-12-31 | 2020-04-17 | 常州泰捷防雷科技有限公司 | Preparation method of medium-voltage gradient zinc oxide piezoresistor MOV chip |
| CN111181143A (en) * | 2020-02-18 | 2020-05-19 | 北京捷安通达科贸有限公司 | Transient impulse voltage suppressor |
| CN111181143B (en) * | 2020-02-18 | 2023-07-25 | 慈溪市万能电子有限公司 | Transient pulse voltage suppressor |
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