CN104150897B - High energy high potential gradient type tindioxide piezoresistor composite powder and preparation method - Google Patents
High energy high potential gradient type tindioxide piezoresistor composite powder and preparation method Download PDFInfo
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- CN104150897B CN104150897B CN201410446361.9A CN201410446361A CN104150897B CN 104150897 B CN104150897 B CN 104150897B CN 201410446361 A CN201410446361 A CN 201410446361A CN 104150897 B CN104150897 B CN 104150897B
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- tindioxide
- titanium dioxide
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Abstract
The present invention relates to a kind of high energy high potential gradient type tindioxide piezoresistor composite powder and preparation method, each component of this matrix material is by SnO
2, Co
2o
3, TiO
2, Sb
2o
5, Nb
2o
5, Pr
6o
11, Y
2o
3make, adopt in the tindioxide powder of submicron order, mix titanium dioxide, antimony peroxide, cobalt sesquioxide, Niobium Pentxoxide, 11 oxidation six praseodymiums, yttrium oxides, wherein, 11 oxidation six praseodymiums and yttrium oxide are as potential gradient toughener, titanium dioxide and antimony peroxide are mono-dispersed nano grade particles, nanometer antimony peroxide can react with tindioxide and changes Spinel into and be uniformly distributed in crystal boundary in sintering process, pricks nail effect suppress tindioxide anisotropic grain growth by crystal boundary.Also can be used to the adding of antimony peroxide the median size controlling crystal grain, the grain and grain boundary density in unit volume is strengthened, the finished product are had, and energy density is large, potential gradient is high, leakage current is little, produce the features such as consistence is better in batches.This preparation method is simple, controlled, can be used for mass industrialized production.
Description
Technical field
The present invention relates to a kind of high energy, high potential gradient type tindioxide piezoresistor composite powder and preparation method thereof, belongs to electronic ceramic preparation and applied technical field.
Background technology
Voltage dependent resistor powder is the starting material material for making piezoresistor.Piezoresistor is a kind of votage limit type protection device resistance device with nonlinear wind vibration, is mainly used in carrying out voltage clamping when circuit bears overvoltage, absorbs unnecessary electric current to protect susceptible device susceptor.Utilize the nonlinear wind vibration of piezoresistive material, when superpotential appears at two interpolars of piezoresistor, piezoresistor by voltage clamp to a relatively-stationary magnitude of voltage, thus can realize the protection to late-class circuit.In certain temperature and specific voltage range, the rising sharply with the rising of voltage of the electric current of piezoresistor, its resistance value sharply declines with the rising of voltage, has nonlinear wind vibration.Piezoresistor by the absorption of pulse voltage, surge voltage, induced lightening voltage, switching overvoltage, thus protects electron device, electronic circuit, electronics, electrical equipment from the impact of abnormal voltage effectively.
Zinc oxide is traditional piezoresistive material, and zinc oxide varistor has the features such as nonlinear factor is large, leakage current is little, through-current capability is strong, the time of response is fast, is widely used in using electrical domain.Zinc oxide voltage dependent resistor is divided into again low-pressure type voltage dependent resistor and high energy type voltage dependent resistor.The voltage gradient of now general high energy type zinc oxide pressure sensitive, generally at 120 ~ 200V/mm, is difficult to the service requirements meeting noble potential applied environment.Therefore, improve voltage gradient and the nonlinear factor (reduction residual voltage ratio) of high energy type voltage dependent resistor, i.e. development of new high pressure, high energy type voltage dependent resistor, become the direction of voltage dependent resistor exploitation.
In prior art, for sintering high energy, the composite granule of high potential gradient type Zinc-oxide piezoresistor mixes a small amount of Bi by certain molar percentage in Zinc oxide powder base-material
20
3, Ti0
2, Co
20
3, Ni
20
3, Sn02, Y
2o
3deng additive, then this powder is made through techniques such as mixing and ball milling, granulation, shaping, sintering.Traditional technology uses pre-ball milled by additive co-grinding, reduces their particle diameter, and then mixed with main base-material by the additive of pre-milled.If but add the uneven general different growth that can cause crystal grain, produce microstructural flaws, thus make voltage dependent resistor on electrical property, show the decline of potential gradient and energy density.Piezoresistive wafer destroys mainly because the ununiformity of resistor disc internal microstructure causes distribution of current uneven, and resistor disc inside produces thermal stresses, makes it burst and punctures, and therefore improving microscopic uniformity is the basic of raising resistor disc energy tolerance density.Even if but adopt current state-of-the-art high speed stirred ball mill or sand mill, also can only by the particle size reduction of additive to about 0.20 μm.The granularity of this size range and main base-material zinc oxide is more or less the same, and therefore use this method can not continue the uniform doping improving additive, the electrical property of voltage dependent resistor also can not be greatly improved.Therefore, adopt new material prescription, high energy that preparation method develops excellent performance, the zinc oxide material of high potential gradient, or novel non-oxide zinc piezoresistive material has great importance.
Summary of the invention:
The object of the invention is, provide a kind of high energy high potential gradient type tindioxide piezoresistor composite powder and preparation method, each component of this matrix material is by SnO
2, Co
2o
3, TiO
2, Sb
2o
5, Nb
2o
5, Pr
6o
11, Y
2o
3make, adopt in the tindioxide powder of submicron order, mix titanium dioxide, antimony peroxide, cobalt sesquioxide, Niobium Pentxoxide, 11 oxidation six praseodymiums, yttrium oxides, wherein, 11 oxidation six praseodymiums and yttrium oxide are as potential gradient toughener, titanium dioxide and antimony peroxide are mono-dispersed nano grade particles, nanometer antimony peroxide can react with tindioxide and changes Spinel into and be uniformly distributed in crystal boundary in sintering process, pricks nail effect suppress tindioxide anisotropic grain growth by crystal boundary.Also can be used to the adding of antimony peroxide the median size controlling crystal grain, the grain and grain boundary density in unit volume is strengthened, the finished product are had, and energy density is large, potential gradient is high, leakage current is little, produce the features such as consistence is better in batches.This preparation method is simple, controlled, can be used for mass industrialized production.
A kind of high energy high potential gradient type tindioxide piezoresistor composite powder of the present invention, each component of this composite granule is by molar percentage SnO
295.6-97.85mol%, Co
2o
30.9-1.5mol%, TiO
20.1-1mol%, Sb
2o
50.05-0.5%, Nb
2o
50.1-0.4mol%, Pr
6o
110.5mol%, Y
2o
30.5mol% makes.
The preparation method of described high energy high potential gradient type tindioxide piezoresistor composite powder, follows these steps to carry out:
A, in ball mill, titanium dioxide nanoparticle 0.1%-1mol%, cobalt sesquioxide 0.9%-1.5mol% powder, Niobium Pentxoxide 0.1%-0.4mol% powder, 11 oxidation six praseodymium 0.5mol% and yttrium oxide 0.5mol% are mixed, ball milling 3-6 hour, makes mixture;
Add tindioxide 95.6-97.85mol% powder and the nanometer antimony peroxide particle 0.05%-0.5mol% of submicron order in b, the mixture that obtained by step a, then through ball milling 1-3 hour, make mixture;
C, the mixture obtained by step b are dried, and sieve, obtain the powder of mixture;
Sinter 3-6 hour at being positioned over temperature 800-1300 DEG C in d, the mixture powder that obtained by step c, obtain Nanocrystalline Zno-based Varistor composite powder material;
Titanium dioxide granule in step a is mono-dispersed nano grade particles, mixes in composite granule with the form of the water-sol.
Content of titanium dioxide in Nanometer Titanium Dioxide Hydrosol in step a is 10wt%-30wt%.
Antimony peroxide particle in step b is mono-dispersed nano grade particles, mixes in composite granule with the form of the water-sol containing antimony peroxide particle.
Antimony peroxide content in nanometer antimony pentoxide hydrosol in step b is 10wt%-30wt%.
A kind of high energy high potential gradient type tindioxide piezoresistor composite powder of the present invention, it take tindioxide as principal phase, add the sintering powder body material after other rare-earth oxide modified some, tindioxide piezoresistive material has that doping is few, doping loss is little and thermal conductivity advantages of higher, and in electronics, power system, application prospect is fine.
A kind of high energy high potential gradient type tindioxide piezoresistor composite powder of the present invention, nanometer antimony peroxide is added in formula, can react with tindioxide in sintering process and generate Spinel, this Spinel can be uniformly distributed in crystal boundary, tindioxide grain growing is suppressed by Grain boundary pinning effect, increase the grain boundary density in material, make grain growing more even.Antimony peroxide and titanium dioxide are the crucial additives suppressing tindioxide grain growing, and adding proportion is very little.Its nanoparticle is added with the form of the water-sol, coacervate can not be formed, ensure that the monodisperse status of its particle of nanometer, thus ensure that the Spinel generated is evenly distributed in crystal boundary, this technique ensures that rare earth oxide plays the prerequisite of maximum modification effect.
A kind of high energy high potential gradient type tindioxide piezoresistor composite powder of the present invention, efficient electric potential gradient toughener Praseodymium trioxide and yttrium oxide is also add in formula, it can the grain-size of remarkable refinement tin dioxide material, improve the grain and grain boundary density in material, improve the potential gradient of material.
Compared with prior art; the high energy high potential gradient type tindioxide piezoresistor composite powder that the present invention is rare earth modified; component is simple; the easy controllable precise of doped with rare-earth elements; antimony peroxide and titanium dioxide is added by the mode of water-sol nanoparticle; potential gradient toughener Praseodymium trioxide and yttrium oxide is added by the mode of powder; optimize material mixture ratio; improve energy force density and the potential gradient of tindioxide piezoresistive material; significantly improve its electric property, the miniaturization for voltage dependent resistor product has very positive meaning.
The voltage dependent resistor product that the tindioxide piezoresistor composite powder obtained by the method for the invention is repressed, sintering is made has the advantage that energy density is large, potential gradient is high, leakage current is little, voltage gradient regulation range large and batch production consistence is good.
Accompanying drawing explanation
Scanning electron microscope (SEM) photo of Fig. 1 tindioxide voltage dependent resistor obtained by the embodiment of the present invention 1;
X-ray diffraction (XRD) collection of illustrative plates of Fig. 2 tindioxide piezoresistor composite powder material obtained by the embodiment of the present invention 1;
Embodiment
Embodiment 1
In ball mill, titanium dioxide nanoparticle 0.1mol%, cobalt sesquioxide powder 0.9mol%, Niobium Pentxoxide powder 0.1mol%, 11 oxidation six praseodymium powder 0.5mol%, yttrium oxide powder 0.5mol% are mixed, ball milling 4 hours, make mixture, wherein titanium dioxide granule is mono-dispersed nano grade particles, mix in composite granule with the form of the water-sol, the content of titanium dioxide in the water-sol is 10w%;
Tindioxide powder 97.85mol% and the nanometer antimony peroxide particle 0.05mol% of submicron order will be added in the mixture obtained, again through ball milling 2 hours, make mixture, wherein nanometer antimony peroxide particle is mono-dispersed nano grade particles, mix in composite granule with the form of the water-sol, the antimony peroxide content in the water-sol is 10w%;
The mixture obtained is dried, sieves, the powder of the mixture obtained;
Sinter 6 hours at again the powder of the mixture obtained being positioned over temperature 800 DEG C, obtain tindioxide piezoresistor composite powder material;
The tindioxide piezoresistor composite powder of preparation is pressed into ceramic body according to a conventional method, then ceramic body is sintered 5 hours at temperature 1150 DEG C, obtain tindioxide voltage dependent resistor.
Embodiment 2
In ball mill, titanium dioxide nanoparticle 1mol%, cobalt sesquioxide powder 1.5mol%, Niobium Pentxoxide powder 0.4mol%, 11 oxidation six praseodymium powder 0.5mol% and yttrium oxide powder 0.5mol% are mixed, ball milling 3 hours,
Make mixture, wherein titanium dioxide granule is mono-dispersed nano grade particles, mixes in composite granule with the form of the water-sol, and the content of titanium dioxide in the water-sol is 30w%;
Tindioxide powder 95.6mol% and the nanometer antimony peroxide particle 0.5mol% of submicron order will be added in the mixture obtained, again through ball milling 1 hour, make mixture, wherein antimony peroxide particle is mono-dispersed nano grade particles, mix in composite granule with the form of the water-sol, the antimony peroxide content in the water-sol is 30w%;
The mixture obtained is dried, sieves, obtain the powder of mixture;
Sinter 3 hours at again the powder of the mixture obtained being positioned over temperature 1300 DEG C, obtain tindioxide piezoresistor composite powder material;
The tindioxide piezoresistor composite powder of preparation is pressed into ceramic body according to a conventional method, then ceramic body is sintered 5 hours at temperature 1150 DEG C, obtain tindioxide voltage dependent resistor.
Embodiment 3
In ball mill, titanium dioxide nanoparticle 0.1mol%, cobalt sesquioxide powder 1.5mol%, Niobium Pentxoxide powder 0.4mol%, 11 oxidation six praseodymium powder 0.5mol% and yttrium oxide powder 0.5mol% are mixed, ball milling 6 hours, make mixture, wherein titanium dioxide granule is mono-dispersed nano grade particles, mix in composite granule with the form of the water-sol, the content of titanium dioxide in the water-sol is 15w%;
Tindioxide 96.5mol% powder and the nanometer antimony peroxide particle 0.5mol% of submicron order will be added in the mixture obtained, again through ball milling 3 hours, make mixture, wherein antimony peroxide particle is mono-dispersed nano grade particles, mix in composite granule with the form of the water-sol, the antimony peroxide content in the water-sol is 20w%;
The mixture obtained is dried, sieves, obtain the powder of mixture;
Sinter 4 hours at again the powder of the mixture obtained being positioned over temperature 1100 DEG C, obtain tindioxide piezoresistor composite powder material;
The tindioxide piezoresistor composite powder of preparation is pressed into ceramic body according to a conventional method, then ceramic body is sintered 5 hours at temperature 1150 DEG C, obtain tindioxide voltage dependent resistor.
Embodiment 4
In ball mill, titanium dioxide nanoparticle 0.5mol%, cobalt sesquioxide powder 1.2mol%, Niobium Pentxoxide powder 0.3mol%, 11 oxidation six praseodymium powder 0.2mol% and yttrium oxide powder 0.1mol% are mixed, ball milling 5 hours, make mixture, wherein titanium dioxide granule is mono-dispersed nano grade particles, mix in composite granule with the form of the water-sol, the content of titanium dioxide in the water-sol is 20w%;
Tindioxide 97.6mol% powder and the nanometer antimony peroxide particle 0.1mol% water-sol of submicron order will be added in the mixture obtained, again through ball milling 2 hours, make mixture, wherein antimony peroxide particle is mono-dispersed nano grade particles, mix in composite granule with the form of the water-sol, the antimony peroxide content in the water-sol is 15w%;
The mixture obtained is dried, sieves, obtain the powder of mixture;
Sinter 5 hours at again the powder obtaining mixture being positioned over temperature 900 DEG C, obtain tindioxide piezoresistor composite powder material;
The tindioxide piezoresistor composite powder of preparation is pressed into ceramic body according to a conventional method, then ceramic body is sintered 5 hours at temperature 1150 DEG C, obtain tindioxide voltage dependent resistor.
Embodiment 5 (contrast 1)
In ball mill, by Nano titanium dioxide powder 0.1mol%, cobalt sesquioxide powder 0.9mol%, Niobium Pentxoxide powder 0.1mol%, 11 oxidation six praseodymium powder 0.5mol%, the mixing of yttrium oxide powder 0.5mol% powder, ball milling 4 hours, makes mixture;
To in the mixture obtained, add tindioxide 97.85mol% powder and the nano level antimony peroxide powder 0.05mol% of submicron order, then through ball milling 2 hours, make mixture;
The mixture obtained is dried, sieves, obtain the powder of mixture;
Sinter 6 hours at the powder obtaining mixture being positioned over temperature 800 DEG C, obtain tindioxide piezoresistor composite powder material;
The tindioxide piezoresistor composite powder of preparation is pressed into ceramic body according to a conventional method, then ceramic body is sintered 5 hours at temperature 1150 DEG C, obtain tindioxide voltage dependent resistor.
Embodiment 6 (contrast 2)
In ball mill, by AR micro-scale titanium dioxide powder 0.1mol%, cobalt sesquioxide powder 0.9mol%, Niobium Pentxoxide powder 0.1mol%, 11 oxidation six praseodymium powder 0.5mol%, the mixing of yttrium oxide powder 0.5mol% powder, ball milling 4 hours, makes mixture;
To in the mixture obtained, add tindioxide 97.85mol% powder and the AR micron order antimony peroxide 0.05mol% powder of submicron order, then through ball milling 2 hours, make mixture;
The mixture obtained is dried, sieves, obtain the powder of mixture;
Sinter 6 hours at the powder obtaining mixture being positioned over temperature 800 DEG C, obtain tindioxide piezoresistor composite powder material;
The tindioxide piezoresistor composite powder of preparation is pressed into ceramic body according to a conventional method, then ceramic body is sintered 5 hours at temperature 1150 DEG C, obtain tindioxide voltage dependent resistor.
Embodiment 7
Voltage dependent resistor embodiment 1 and embodiment 5, embodiment 6 prepared adopts varistor tester to carry out performance test to it, and test result is as shown in table 1:
Table 1:
| Numbering | Potential gradient (V/mm) | Pressure sensitive voltage plastisied dispersion % | Leakage current density μ A/cm 2 | Energy density (J/cm 3) |
| Embodiment 1 | 732 | 3.4 | 0.82 | 1022 |
| Embodiment 5 | 403 | 9.8 | 1.432 | 685 |
| Embodiment 6 | 256 | 20.1 | 2.3 | 483 |
Test result as can be seen from table 1, high energy made by embodiment 1, noble potential tindioxide voltage dependent resistor, its voltage gradient, energy density, leakage current, homogeneity of product in, be all better than adopting the voltage dependent resistor product that traditional method adds nano level or micron order antimony peroxide, titania powder is produced.Illustrate that adding modified oxide with the form of nano-sized hydrosol is prepare a kind of effective method of high-performance tindioxide voltage dependent resistor powder.
Claims (1)
1. a preparation method for high energy high potential gradient type tindioxide piezoresistor composite powder, is characterized in that each component of this composite granule is by molar percentage SnO
295.6-97.85mol%, Co
2o
30.9-1.5mol%, TiO
20.1-1mol%, Sb
2o
50.05-0.5%, Nb
2o
50.1-0.4mol%, Pr
6o
110.5mol%, Y
2o
30.5mol% makes, and concrete operations follow these steps to carry out:
A, in ball mill, titanium dioxide nanoparticle 0.1%-1mol%, cobalt sesquioxide powder 0.9%-1.5mol%, Niobium Pentxoxide powder 0.1%-0.4mol%, 11 oxidation six praseodymium powder 0.5mol% and yttrium oxide powder 0.5mol% are mixed, ball milling 3-6 hour, make mixture, wherein titanium dioxide granule is mono-dispersed nano grade particles, mix in composite granule with the form of Nanometer Titanium Dioxide Hydrosol, the content of titanium dioxide in Nanometer Titanium Dioxide Hydrosol is 10wt%-30wt%;
Tindioxide powder 95.6-97.85mol% and the nanometer antimony peroxide particle 0.05%-0.5mol% of submicron order is added in b, the mixture that obtained by step a, again through ball milling 1-3 hour, make mixture, wherein antimony peroxide particle is mono-dispersed nano grade particles, mix in composite granule with the form of the water-sol containing antimony peroxide particle, the antimony peroxide content amount in nanometer antimony pentoxide hydrosol is 10wt%-30wt%;
C, the mixture obtained by step b are dried, and sieve, obtain the powder of mixture;
D, the mixture powder obtained by step c sinter 3-6 hour at being positioned over temperature 800-1300 DEG C, obtain high energy high potential gradient type tindioxide piezoresistor composite powder.
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Citations (3)
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| CN101197203A (en) * | 2007-11-30 | 2008-06-11 | 华南理工大学 | Tin oxide piezoresistance material and method for producing the same |
| JP5129107B2 (en) * | 2008-05-16 | 2013-01-23 | 旭化成イーマテリアルズ株式会社 | Polyamic acid varnish composition, polyimide resin and metal-polyimide composite |
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| CN101197203A (en) * | 2007-11-30 | 2008-06-11 | 华南理工大学 | Tin oxide piezoresistance material and method for producing the same |
| JP5129107B2 (en) * | 2008-05-16 | 2013-01-23 | 旭化成イーマテリアルズ株式会社 | Polyamic acid varnish composition, polyimide resin and metal-polyimide composite |
| CN103880411A (en) * | 2014-02-26 | 2014-06-25 | 江苏世星电子科技有限公司 | High-gradient rare earth modified stannic oxide pressure-sensitive resistance material and preparation method thereof |
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| The influence of yttrium on a typical SnO2 varistor system: Microstructural and electrical features;R. Parra et al.;《Materials Chemistry and Physics》;20051231;第94卷;第347页至第352页 * |
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