CN104150897A - High-energy high-potential-gradient type tin dioxide piezoresistor composite powder and preparation method - Google Patents
High-energy high-potential-gradient type tin dioxide piezoresistor composite powder and preparation method Download PDFInfo
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- CN104150897A CN104150897A CN201410446361.9A CN201410446361A CN104150897A CN 104150897 A CN104150897 A CN 104150897A CN 201410446361 A CN201410446361 A CN 201410446361A CN 104150897 A CN104150897 A CN 104150897A
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Abstract
The invention relates to high-energy high-potential-gradient type tin dioxide piezoresistor composite powder and a preparation method. The composite powder is prepared from the following components: SnO2, Co2O3, TiO2, Sb2O5, Nb2O5, Pr6O11 and Y2O3 and titanium dioxide, antimony pentoxide, cobaltic oxide, niobium pentoxide, praseodymium oxide and yttria are doped in submicron-class tin dioxide powder, wherein praseodymium oxide and yttria are used as potential gradient reinforcing agents; both titanium dioxide and antimony pentoxide are monodispersed nano particles; nano antimony pentoxide can react with tin dioxide in the sintering process to be converted into a spinel phase and is uniformly distributed in a crystal boundary; by a crystal boundary pinning effect, abnormal grain growth of tin dioxide crystal grains is inhibited. Addition of antimony pentoxide also can be used for controlling the average particle size of the crystal grains, so that crystal grain and crystal boundary densities in unit volume are reinforced and the final product has the characteristics of high energy density, high potential gradient, small leakage current, good batch production consistency and the like. The preparation method is simple and controllable and can be used for mass industrial 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 non-linear volt-ampere characteristic, is mainly used in the time that circuit bears overvoltage, carrying out voltage clamping, absorbs unnecessary electric current with protection susceptible device susceptor.Utilize the non-linear volt-ampere characteristic of piezoresistive material, when superpotential appears at two interpolars of piezoresistor, piezoresistor can be by voltage clamp to relatively-stationary magnitude of voltage, thereby realizes 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 non-linear volt-ampere characteristic.Piezoresistor passes through the absorption of pulse voltage, surge voltage, induction lightening pressure, switching overvoltage, thereby effectively protects electron device, electronic circuit, electronics, consumer to avoid the impact of abnormal voltage.
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 meet the service requirements of 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, becomes the direction that voltage dependent resistor is developed.
In prior art, for sintering high energy, the composite granule of high potential gradient type Zinc-oxide piezoresistor is to mix 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, moulding, sintering.Traditional technology is to use pre-ball milled by additive co-grinding, reduces their particle diameter, and then the additive of pre-milled is mixed with main base-material.If but add the uneven general different growth that can cause crystal grain, produce microtexture defect, thereby make voltage dependent resistor on electrical property, show the decline of potential gradient and energy density.It is mainly because the ununiformity of resistor disc internal microstructure causes distribution of current inhomogeneous that piezoresistive wafer destroys, and the inner thermal stresses that produces of resistor disc, bursts it and puncture, and therefore improving microscopic uniformity is improve resistor disc energy tolerance density basic.Even but adopt current state-of-the-art high speed stirred ball mill or sand mill, also can only be by the particle size reduction of additive to 0.20 μ m left and right.The granularity of this size range and main base-material zinc oxide is more or less the same, and therefore uses this method can not continue to improve the uniform doping of additive, and the electrical property of voltage dependent resistor also can not be greatly improved.Therefore, adopt new material prescription, preparation method to develop the high energy of 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, a kind of high energy high potential gradient type tindioxide piezoresistor composite powder and preparation method are provided, and the 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 and in the tindioxide powder of submicron order, mix titanium dioxide, antimony peroxide, cobalt sesquioxide, Niobium Pentxoxide, 11 oxidation six praseodymiums, yttrium oxide, 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.Antimony peroxide add the median size that also can be used to control crystal grain, the grain and grain boundary density in unit volume is strengthened, make the finished product there is the features such as energy density is large, potential gradient is high, leakage current is little, batch production consistence is better.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, the 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;
In b, mixture that step a is obtained, add tindioxide 95.6-97.85mol% powder and the nanometer antimony peroxide particle 0.05%-0.5mol% of submicron order, then through ball milling 1-3 hour, make mixture;
C, the mixture that step b is obtained are dried, and sieve, and obtain the powder of mixture;
In d, mixture powder that step c is obtained, be positioned over sintering 3-6 hour at temperature 800-1300 DEG 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 that contains 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 is taking tindioxide as principal phase, add the sintering powder body material after some other rare-earth oxide modified, 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, in formula, increase nanometer antimony peroxide, in sintering process, can react with tindioxide and generate Spinel, this Spinel can be uniformly distributed in crystal boundary, suppress tindioxide grain growing by Grain boundary pinning effect, increase the crystal boundary density in material, make grain growing more even.Antimony peroxide and titanium dioxide are the crucial additives that suppresses tindioxide grain growing, and adding proportion is very little.Its nanoparticle is added with the form of the water-sol, can not form coacervate, ensure the monodisperse status of its particle of nanometer, the equal Uniform thereby the Spinel that guarantee generates distributes in crystal boundary, this technique is the prerequisite that ensures rare earth oxide performance 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 in formula, are also increased, it is the grain-size of refinement tin dioxide material significantly, 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; doped with rare-earth elements is easily accurately controlled; add antimony peroxide and titanium dioxide by the mode of water-sol nanoparticle; add potential gradient toughener Praseodymium trioxide and yttrium oxide by the mode of powder; optimize material mixture ratio; energy force density and the potential gradient of tindioxide piezoresistive material are improved; obviously improve its electric property, had very positive meaning for the miniaturization of voltage dependent resistor product.
The voltage dependent resistor product that tindioxide piezoresistor composite powder is repressed, sintering is made obtaining by the method for the invention has advantages of that energy density is large, potential gradient is high, leakage current is little, voltage gradient regulation range large and batch production high conformity.
Brief description of the drawings
Fig. 1 is scanning electron microscope (SEM) photo of the obtained tindioxide voltage dependent resistor of the embodiment of the present invention 1;
Fig. 2 is X-ray diffraction (XRD) collection of illustrative plates of the obtained tindioxide piezoresistor composite powder of the embodiment of the present invention 1 material;
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 obtaining, 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 obtaining is dried, sieve, the powder of the mixture obtaining;
Again the powder of the mixture obtaining is positioned at 800 DEG C of temperature to sintering 6 hours, obtains tindioxide piezoresistor composite powder material;
The tindioxide piezoresistor composite powder of preparation is pressed into ceramic body according to a conventional method, then by ceramic body sintering 5 hours at 1150 DEG C of temperature, obtains 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 obtaining, 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 obtaining is dried, sieve, obtain the powder of mixture;
Again the powder of the mixture obtaining is positioned at 1300 DEG C of temperature to sintering 3 hours, obtains tindioxide piezoresistor composite powder material;
The tindioxide piezoresistor composite powder of preparation is pressed into ceramic body according to a conventional method, then by ceramic body sintering 5 hours at 1150 DEG C of temperature, obtains 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 obtaining, 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 obtaining is dried, sieve, obtain the powder of mixture;
Again the powder of the mixture obtaining is positioned at 1100 DEG C of temperature to sintering 4 hours, obtains tindioxide piezoresistor composite powder material;
The tindioxide piezoresistor composite powder of preparation is pressed into ceramic body according to a conventional method, then by ceramic body sintering 5 hours at 1150 DEG C of temperature, obtains 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 obtaining, 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 obtaining is dried, sieve, obtain the powder of mixture;
Again the powder that obtains mixture is positioned at 900 DEG C of temperature to sintering 5 hours, obtains tindioxide piezoresistor composite powder material;
The tindioxide piezoresistor composite powder of preparation is pressed into ceramic body according to a conventional method, then by ceramic body sintering 5 hours at 1150 DEG C of temperature, obtains tindioxide voltage dependent resistor.
Embodiment 5 (contrast 1)
In ball mill, Nano titanium dioxide powder 0.1mol%, cobalt sesquioxide powder 0.9mol%, Niobium Pentxoxide powder 0.1mol%, 11 oxidation six praseodymium powder 0.5mol%, yttrium oxide powder 0.5mol% powder are mixed, ball milling 4 hours, makes mixture;
To in the mixture obtaining, 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 obtaining is dried, sieve, obtain the powder of mixture;
The powder that obtains mixture is positioned at 800 DEG C of temperature to sintering 6 hours, obtains tindioxide piezoresistor composite powder material;
The tindioxide piezoresistor composite powder of preparation is pressed into ceramic body according to a conventional method, then by ceramic body sintering 5 hours at 1150 DEG C of temperature, obtains tindioxide voltage dependent resistor.
Embodiment 6 (contrast 2)
In ball mill, AR micron order titanium dioxide powder 0.1mol%, cobalt sesquioxide powder 0.9mol%, Niobium Pentxoxide powder 0.1mol%, 11 oxidation six praseodymium powder 0.5mol%, yttrium oxide powder 0.5mol% powder are mixed, ball milling 4 hours, makes mixture;
To in the mixture obtaining, 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 obtaining is dried, sieve, obtain the powder of mixture;
The powder that obtains mixture is positioned at 800 DEG C of temperature to sintering 6 hours, obtains tindioxide piezoresistor composite powder material;
The tindioxide piezoresistor composite powder of preparation is pressed into ceramic body according to a conventional method, then by ceramic body sintering 5 hours at 1150 DEG C of temperature, obtains tindioxide voltage dependent resistor.
Embodiment 7
Voltage dependent resistor prepared by embodiment 1 and embodiment 5, embodiment 6 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 from table 1 can be found out, the high energy that embodiment 1 is made, noble potential tindioxide voltage dependent resistor, it is all better than adopting traditional method to add the voltage dependent resistor product that nano level or micron order antimony peroxide, titania powder are produced aspect voltage gradient, energy density, leakage current, homogeneity of product.Illustrate that adding modified oxide with the form of nano-sized hydrosol is to prepare a kind of effective method of high-performance tindioxide voltage dependent resistor powder.
Claims (6)
1. a high energy high potential gradient type tindioxide piezoresistor composite powder, is characterized in that the 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.
2. a preparation method for high energy high potential gradient type tindioxide piezoresistor composite powder as described in claim 1, is characterized in that following these steps to carrying 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, makes mixture;
In b, mixture that step a is obtained, add tindioxide powder 95.6-97.85mol% and nanometer antimony peroxide particle 0. 05%-0.5mol% of submicron order, then through ball milling 1-3 hour, make mixture;
C, the mixture that step b is obtained are dried, and sieve, and obtain the powder of mixture;
D, the mixture powder that step c is obtained are positioned over sintering 3-6 hour at temperature 800-1300 DEG C, obtain high energy high potential gradient type tindioxide piezoresistor composite powder.
3. preparation method according to claim 2, is characterized in that the titanium dioxide granule in step a is mono-dispersed nano grade particles, mixes in composite granule with the form of Nanometer Titanium Dioxide Hydrosol.
4. Nanometer Titanium Dioxide Hydrosol according to claim 3, is characterized in that the content of titanium dioxide in Nanometer Titanium Dioxide Hydrosol is 10wt%-30wt%.
5. preparation method according to claim 2, is characterized in that the antimony peroxide particle in step b is mono-dispersed nano grade particles, mixes in composite granule with the form of the water-sol that contains antimony peroxide particle.
6. nanometer antimony pentoxide hydrosol according to claim 2, is characterized in that the antimony peroxide content amount in nanometer antimony pentoxide hydrosol is 10wt%-30wt%.
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