CN101531507B - High energy type zinc oxide piezoresistor composite powder and method for manufacturing piezoresistor - Google Patents
High energy type zinc oxide piezoresistor composite powder and method for manufacturing piezoresistor Download PDFInfo
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- CN101531507B CN101531507B CN2009100490870A CN200910049087A CN101531507B CN 101531507 B CN101531507 B CN 101531507B CN 2009100490870 A CN2009100490870 A CN 2009100490870A CN 200910049087 A CN200910049087 A CN 200910049087A CN 101531507 B CN101531507 B CN 101531507B
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Abstract
The invention discloses high energy zinc oxide piezoresistor composite powder. The powder is prepared by doping titanium dioxide, antimony peroxide, dibismuth trioxide, cobalt sesquioxide, manganous carbonate, nickel sesquioxide and aluminum nitrate into submicron grade zinc oxide powder according to a certain molar percentage, wherein the titanium dioxide and the antimony peroxide are monodisperse nanometer grains; the nanometer antimony peroxide can react with the dibismuth trioxide and the zinc oxide in a sintering process to be converted into spinelle phase and evenly distributed in a grain boundary, thereby inhibiting anisotropic growth of zinc oxide grains through grain boundary pinning effect; and addition of the antimony peroxide can be used for controlling the average grain diameter of the grain, so that a finished product has large energy density, low residual voltage ratio, small drain current, large regulation range of voltage gradient and good consistency of batch production. The invention also discloses a method for manufacturing the high energy zinc oxide piezoresistor, which is to dope the nanometer titanium dioxide grains and the nanometer antimony peroxide grains into the composite powder in sequence in a mode of hydrosol.
Description
Technical field
The present invention relates to a kind of high energy type zinc oxide piezoresistor composite powder, and the method for making this high energy type zinc oxide piezoresistor.
Background technology
From the angle of prescription, Zinc-oxide piezoresistor is divided into ZnO-Bi
2O
3-Sb
2O
3System and ZnO-Bi
2O
3-TiO
2Be two big classes.
Wherein, ZnO-Bi
2O
3-Sb
2O
3Be that voltage dependent resistor is called the high-pressure type voltage dependent resistor again, the universal piezoresistor, surge protector that mainly comprises pressure sensitive voltage 180～1800V is with voltage dependent resistor and gapless metal-oxide lighting arrester piezoresistive wafer.Be characterized in grain-size little (mean diameter 8～20 μ m), voltage gradient height (150～400V/mm), low (the current density 30A/cm of limit voltage ratio under the big electric current
2Under limit voltage ratio 1.50～1.84, current density 2kA/cm
2Under limit voltage ratio≤2.3～2.8), (2≤ms) overvoltage surge has the ideal protective capacities, and energy density is less, has only 50～300J/cm to narrow pulsewidth
3About.Therefore, it is mainly used in operating voltage greater than very short (0.01～2ms) Lightning Over-voltage protection discharge time in the electronic instrument, low-voltage distribution system and the high pressure electrical power trans mission/distribution system that exchange 100V or direct current 150V.
ZnO-Bi
2O
3-TiO
2The characteristics that are voltage dependent resistor be grain-size big (mean diameter 40～100 μ m), voltage gradient low (25～50V/mm), limit voltage ratio height (the current density 30A/cm under the big electric current
2Under limit voltage ratio 1.80～2.25, current density 2kA/cm
2Under limit voltage ratio 3.8～5.0).
ZnO-Bi
2O
3-TiO
2Be that voltage dependent resistor is divided into low-pressure type voltage dependent resistor and high energy type voltage dependent resistor again.Wherein, technological standard system, the Application Areas of low-pressure type voltage dependent resistor and high-pressure type voltage dependent resistor are basic identical.And the high energy type voltage dependent resistor is mainly used in the long (absorption of magnetic field energy in 50～1000ms) switching overvoltage protection and inductance element discharge time; move energy, large synchronous generator rotor demagnetization, middle great power conversion circuit system operation overvoltage protection etc. as superconducting coil, its definition and measuring method with the technical indicator of low-pressure type voltage dependent resistor is all different.
On structure, profile, the ceramics diameter of low-pressure type voltage dependent resistor is generally 5～20mm, and thickness is generally 0.5～2.0mm; The ceramics diameter of high energy type voltage dependent resistor is generally 56～88mm, and thickness is generally 10～30mm.On technical indicator, the core technology index of low-pressure type voltage dependent resistor is the limit voltage ratio under peak inrush current under the 8/20 standard lightning current wave and this waveform; The core technology index of high energy type voltage dependent resistor is the limit voltage ratio under energy density under the delta current ripple and this waveform.The energy capacity height of high energy type voltage dependent resistor, but high-rate performance is not ideal enough, the residual voltage ratio of minor diameter element is higher, often do not reach the pressure limiting requirement, therefore, improve the voltage gradient and the nonlinear factor (reduction residual voltage ratio) of high energy type voltage dependent resistor, promptly develop high pressure high energy type voltage dependent resistor, become the direction of voltage dependent resistor exploitation.
In the prior art, the composite granule that is used for the sintering high energy type zinc oxide piezoresistor is to mix a spot of Bi at the ZnO matrix of powder material by certain molar percentage
2O
3, TiO
2, Co
2O
3, MnCO
3, Ni
2O
3, SnO
2, SrCO
3, BaCO
3Deng additive, again this powder is made through technologies such as mixing and ball milling, granulation, moulding, sintering.
Wherein, TiO
2Be that (adding proportion is about 0.2～2mol%) for the crystal grain growth substance of most critical, but if add the uneven general different growth that can cause ZnO crystal grain, produce the microtexture defective, thereby make voltage dependent resistor on electrical property, show the rising of limit voltage ratio and the decline of energy density.Analysis revealed, TiO
2The ununiformity of adding is one of further key factor that improves of performance that hinders the high energy piezoresistive wafer.
Traditional technology is to use pre-ball milled that additive is mixed and pulverizes, and reduce their particle diameter, and then the additive that pre-grinding is good mixes with main base-material.Even but adopt present state-of-the-art high speed stirred ball mill or sand mill, also additive particle size can only be reduced to 0.15～0.20 μ m.The granularity of this size range and main base-material ZnO is more or less the same, and therefore uses this method can not continue to improve the uniform doping of additive, and the performance of high energy type voltage dependent resistor also can not be greatly improved.
After nineteen ninety-five, someone's nano level main base-material and nanometer additive modifying function that begins one's study to Zinc-oxide piezoresistor.As the patent No. is the addition means that the patent of invention of ZL99120639.8 discloses a kind of nanoparticle, is to add dispersion agent earlier to nano-TiO
2Powder body material carries out pre-dispersed, and then mixes with other submicron order powder, makes Zinc-oxide piezoresistor at last.But because the surface exists more than 30 active group that character is different, the bonding force in the coacervate between the nanoparticle is very strong, and is pre-dispersed for up to 30 hours, and also can only be with TiO
2Part coacervate in the nano-powder separates, and can not realize the doping of nanoparticle with the single particle form.And in sintering process, the outer atom of coacervate spreads in a large number, cause the incorgruous of local grain to grow up, and its internal contraction becomes bigger particle, also can form pore isostructuralism defective during contraction, makes the unstable properties of voltage dependent resistor.Because the existence of these unfavorable factors, aforesaid method is not applied in actual production.
Publication number is that the patent of invention of CN1614720 discloses a kind of employing liquid phase medium and comes nano-TiO
2Particle carries out dispersive technology, and this method adopts liquid phase synthetic dispersed nano TiO
2Mutually compound with other common micron-sized powder materials, make nano-TiO
2Particle can be in system uniform distribution and do not have coacervate fully.
But nano-TiO
2Even additive distributes very evenly, can not avoid ZnO crystal grain fully＜1010 in system〉and＜different growth on 2110〉crystalline orientation.This be since the different growth of ZnO crystal grain except with TiO
2Mix inhomogeneous relevant outside, also with adhered to TiO
2The surface orientation of particulate ZnO crystal grain is relevant, therefore only improves TiO
2Adulterated uniformity coefficient also can not solve the different growth problem of ZnO crystal grain in sintering fully.
Summary of the invention
One of purpose of the present invention is to provide a kind of high energy type zinc oxide piezoresistor composite powder, the less generation different growth of this composite granule ZnO crystal grain in sintering process, and the high energy type zinc oxide piezoresistor performance that sintering forms is better.
For achieving the above object, the present invention has taked following technical scheme:
A kind of high energy type zinc oxide piezoresistor composite powder, this composite granule are to mix following each component by mole per-cent in the Zinc oxide powder of submicron order:
Titanium dioxide 0.2%～2%;
Antimony peroxide 0.05%～0.5%;
Bismuthous oxide bismuth trioxide 0.2%～1.0%;
Cobalt sesquioxide 0.9%～1.5%;
Manganous carbonate 0.3%～0.8%;
Nickel sesquioxide 0.1%～0.4%;
Aluminum nitrate 0.001%～0.01%;
Wherein, titanium dioxide and antimony peroxide are the mono-dispersed nano grade particles.
The particle diameter of described titanium dioxide granule is less than 20 nanometers, mixes in the described composite granule with the form of the water-sol that contains titanium dioxide granule.
Described antimony peroxide particle grain size is mixed in the described composite granule with the form that contains the antimony peroxide particulate water-sol less than 50 nanometers.
Also be mixed with the following component of molar percentage in the described powder:
Barium carbonate 0.05%～0.1%;
Tindioxide 0.5%～0.9%;
Strontium carbonate powder 0.005%～0.009%;
Lead borate 0.02～0.05%;
Silver Nitrate 0.001%～0.005%.
The high energy type zinc oxide piezoresistor composite powder of implementing according to technique scheme has following advantage:
1, in prescription, increased nanometer antimony peroxide (Sb
2O
5), in sintering process, it can with the bismuthous oxide bismuth trioxide (Bi in the system
2O
3) and zinc oxide (ZnO) reaction generation Zn
2Bi
3Sb
3O
14The Jiao Lvshi phase, Jiao Lvshi changes Zn into about 850
7Sb
2O
12Spinel phase, this spinel are uniformly distributed in the crystal boundary mutually, prick the nail effect by crystal boundary and suppress ZnO crystal grain different growth, make the growth of ZnO crystal grain of ceramics inside more even.
2, can also be by regulating Sb
2O
5Add-on control the median size of ZnO crystal grain, make the adjusting of voltage gradient more flexible, can obtain higher voltage gradient.Therefore under the prerequisite that guarantees equal pressure sensitive voltage, sheet footpath and energy tolerance, suitably increase nanometer Sb
2O
5Adding proportion, can reduce the product thickness and the volume of high energy type voltage dependent resistor, improve the energy density of product.
In sum, the voltage dependent resistor product that adopts this composite granule sintering to make has the advantage that energy density is big, limit voltage ratio (residual voltage ratio) is low, leakage current is little, the voltage gradient regulation range is big and produce high conformity in batches.
Two of purpose of the present invention is to provide a kind of manufacture method of high energy type zinc oxide piezoresistor, and the growth of ZnO crystal grain is regular in the high energy type zinc oxide piezoresistor of making by this method, performance is better.
For achieving the above object, the present invention has taked following technical scheme:
A kind of manufacture method of high energy type zinc oxide piezoresistor comprises following steps:
The preparation of step 1, composite granule:
A, in ball mill, the nano titanium oxide water-sol and bismuthous oxide bismuth trioxide powder, cobalt sesquioxide powder, manganous carbonate powder and nickel sesquioxide powder by the following prescription mixing and ball milling of mole per-cent 1～4 hour, are made mixture one:
Titanium dioxide 0.2%～2%;
Bismuthous oxide bismuth trioxide 0.2%～1.0%;
Cobalt sesquioxide 0.9%～1.5%;
Manganous carbonate 0.3%～0.8%;
Nickel sesquioxide 0.1%～0.4%;
B, add the Zinc oxide powder and the nanometer antimony peroxide water-sol of submicron order in said mixture one, through ball milling 0.5～2 hour, make mixture two again, wherein the molar percentage of antimony peroxide is 0.05%～0.5%;
C, add additive agent electrolytes such as tackiness agent, releasing agent and aluminum nitrate in said mixture two, ball milling discharging after 20～40 minutes again, drying, granulation become high energy type zinc oxide piezoresistor composite powder;
Step 2, with above-mentioned composite granule compression moulding, sintering is made high energy type zinc oxide piezoresistor.
In the described nano titanium oxide water-sol: the content of titanium dioxide is that 1wt%～10wt%, particle grain size are less than 20 nanometers.
In the described nanometer antimony peroxide water-sol: the content of antimony peroxide is that 40wt%～50wt%, particle grain size are less than 50 nanometers.
Described binding agent is polyvinyl alcohol or polyoxyethylene glycol binding agent, and quality accounts for 0.3%～1% of described composite granule.
Described releasing agent is the stearic acid releasing agent, and quality accounts for the 0.3wt%～1wt% of described composite granule.
In the described step 2, sintering temperature is 1100 ℃～1300 ℃.
The manufacture method of the high energy type zinc oxide piezoresistor of implementing according to technique scheme has following advantage:
1, antimony peroxide (Sb
2O
5) be to suppress ZnO crystal grain at TiO
2The crucial additive of eigenmode different growth takes place down in effect, and adding proportion is very little.The form of its nanoparticle with the water-sol added, can not form coacervate, guaranteed nanometer Sb
2O
5The particulate list disperses, thus the Zn that assurance is generated
2Bi
3Sb
3O
14Jiao Lvshi phase and Zn
7Sb
2O
12Spinel is evenly distributed in crystal boundary,
2, for fear of nanometer Sb
2O
5Particle and nano-TiO
2Particle directly meet and precipitate or they and other additive agent electrolytes between the ionogen coagulation takes place and lose nano effect; after needing that these two kinds of particles are added system at twice and mixing with the solid particulate of other submicron orders; add additive agent electrolyte again, this technology is to guarantee nanometer Sb
2O
5Particle and nano-TiO
2Particle is brought into play the prerequisite of maximum nano modification effect.
Embodiment
Below in conjunction with embodiment the specific embodiment of the present invention is described:
The manufacture method of powder is identical in Comparative Examples 1, Comparative Examples 2, the Comparative Examples 3, and the prescription that all reaches as follows in the table 1 (seeing this specification sheets last page) is separately finished:
A, in ball mill, with the prescription mixing and ball milling 2 hours that the nano titanium oxide water-sol and bismuthous oxide bismuth trioxide, cobalt sesquioxide, manganous carbonate, nickel sesquioxide, barium carbonate, tindioxide, lead borate, Strontium carbonate powder are pressed table 1, make mixture one.
B, the content that adds zinc oxide and antimony peroxide by the prescription of table 1 in said mixture one are the nanometer antimony peroxide water-sol (not adding antimony peroxide in the Comparative Examples 1,2,3) of 45wt%, through ball milling 1 hour, make mixture two again.
C, the prescription of pressing table 1 in said mixture two add aluminum nitrate, Silver Nitrate, and account for 0.7% the polyvinyl alcohol adhesive of making back composite granule total mass and account for 0.5% the stearic acid releasing agent of making back composite granule total mass, ball milling discharging after 25 minutes again, drying, granulation become high energy type zinc oxide piezoresistor composite powder.
The above-mentioned composite granule compression moulding that will make at last sinters high energy type zinc oxide piezoresistor under 1100 ℃～1300 ℃.The highest sintering temperature is 1270 degrees centigrade, is incubated 2 hours.350 of disks that are of a size of Φ 84mm * 10mm after 4 groups of samples all are pressed into and fire carry out performance test, and test result is as shown in table 2.
Table 2:
| Voltage gradient (V/mm) | Pressure sensitive voltage plastisied dispersion (%) | Leakage current (μ A) | Limit voltage ratio | Energy density (J/cm 3) | |
| Comparative Examples 1 | 35.4 | 9.13 | 9.50～13.2 | 1.35～1.41 | 557～585 |
| Comparative Examples 2 | 37.3 | 23.5 | 3.2～123 | 1.36～1.67 | 4.82～576 |
| Comparative Examples 3 | 44.5 | 13.6 | 48.2～76.8 | 1.58～1.66 | 382～415 |
| Embodiment 1 | 88.5 | 2.14 | 5.1～7.5 | 1.33～1.35 | 986～997 |
Annotate 1: the pressure sensitive voltage plastisied dispersion is the square root of the variance of each sample pressure sensitive voltage value and the ratio of its mean value;
Annotate 2: leakage current is unified under 75% ratio-voltage and measures;
Annotate 3: limit voltage ratio records under 300A;
Annotate 4: energy density is a sample when absorbing the magnetic field energy that the 1H inductance discharges, and the energy that absorbed before the thermal breakdown and the ratio of sample volume take place.
Test result from table 2 as can be seen, the high energy type zinc oxide piezoresistor that embodiment 1 is made, aspect its regulation range, macro-energy density, leakage current, limit voltage ratio, the homogeneity of product, all be much better than and adopt traditional method, add nano-powder TiO in voltage gradient
2, single interpolation nano-TiO
2The high energy type voltage dependent resistor that water-sol method is produced.
As mentioned above, we are illustrated according to aim of the present invention fully, but the present invention is not limited to the foregoing description and implementation method.The practitioner of correlative technology field can carry out different variations and enforcement in the scope of technological thought permission of the present invention.
Table 1:
(in embodiment and each Comparative Examples, the raw material of same composition is same batch)
Claims (10)
1. high energy type zinc oxide piezoresistor composite powder, it is characterized in that: this composite granule is to mix following each component by mole per-cent in the Zinc oxide powder of submicron order:
Titanium dioxide 0.2%～2%;
Antimony peroxide 0.05%～0.5%;
Bismuthous oxide bismuth trioxide 0.2%～1.0%;
Cobalt sesquioxide 0.9%～1.5%;
Manganous carbonate 0.3%～0.8%;
Nickel sesquioxide 0.1%～0.4%;
Aluminum nitrate 0.001%～0.01%;
Wherein, titanium dioxide and antimony peroxide are the mono-dispersed nano grade particles.
2. high energy type zinc oxide piezoresistor composite powder according to claim 1 is characterized in that: the particle diameter of described titanium dioxide granule is less than 20 nanometers, mixes in the described composite granule with the form of the water-sol that contains titanium dioxide granule.
3. high energy type zinc oxide piezoresistor composite powder according to claim 1 is characterized in that: described antimony peroxide particle grain size is mixed in the described composite granule with the form that contains the antimony peroxide particulate water-sol less than 50 nanometers.
4. high energy type zinc oxide piezoresistor composite powder according to claim 1 is characterized in that: also be mixed with the following component of molar percentage in the described powder:
Barium carbonate 0.05%～0.1%;
Tindioxide 0.5%～0.9%;
Strontium carbonate powder 0.005%～0.009%;
Lead borate 0.02～0.05%;
Silver Nitrate 0.001%～0.005%.
5. the manufacture method of a high energy type zinc oxide piezoresistor is characterized in that: comprise following steps:
The preparation of step 1, composite granule:
A, in ball mill, the nano titanium oxide water-sol and bismuthous oxide bismuth trioxide powder, cobalt sesquioxide powder, manganous carbonate powder and nickel sesquioxide powder by the following prescription mixing and ball milling of mole per-cent 1～4 hour, are made mixture one:
Titanium dioxide 0.2%～2%;
Bismuthous oxide bismuth trioxide 0.2%～1.0%;
Cobalt sesquioxide 0.9%～1.5%;
Manganous carbonate 0.3%～0.8%;
Nickel sesquioxide 0.1%～0.4%;
B, add the Zinc oxide powder and the nanometer antimony peroxide water-sol of submicron order in said mixture one, through ball milling 0.5～2 hour, make mixture two again, wherein the molar percentage of antimony peroxide is 0.05%～0.5%;
C, in said mixture two, add tackiness agent, releasing agent and aluminum nitrate additive agent electrolyte, ball milling discharging after 20～40 minutes again, drying, granulation become high energy type zinc oxide piezoresistor composite powder;
Step 2, with above-mentioned composite granule compression moulding, sintering is made high energy type zinc oxide piezoresistor.
6. the manufacture method of high energy type zinc oxide piezoresistor according to claim 5, it is characterized in that: in the described nano titanium oxide water-sol: the content of titanium dioxide is that 1wt%～10wt%, particle grain size are less than 20 nanometers.
7. the manufacture method of high energy type zinc oxide piezoresistor according to claim 5, it is characterized in that: in the described nanometer antimony peroxide water-sol: the content of antimony peroxide is that 40wt%～50wt%, particle grain size are less than 50 nanometers.
8. the manufacture method of high energy type zinc oxide piezoresistor according to claim 5, it is characterized in that: described binding agent is polyvinyl alcohol or polyoxyethylene glycol binding agent, and quality accounts for 0.3%～1% of described composite granule.
9. the manufacture method of high energy type zinc oxide piezoresistor according to claim 5, it is characterized in that: described releasing agent is the stearic acid releasing agent, and quality accounts for the 0.3wt%～1wt% of described composite granule.
10. the manufacture method of high energy type zinc oxide piezoresistor according to claim 5, it is characterized in that: in the described step 2, sintering temperature is 1100 ℃～1300 ℃.
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| CN102515740A (en) * | 2011-11-29 | 2012-06-27 | 中国科学院过程工程研究所 | High energy type zinc oxide piezoresistor material and preparation method thereof |
| EP2645380A1 (en) * | 2012-03-30 | 2013-10-02 | Inael Electrical Systems, S.A. | A method for obtaining doped zinc oxide varistors, the product obtained by said method and its use |
| CN102723157A (en) * | 2012-06-14 | 2012-10-10 | 扬州发运电气有限公司 | Manufacturing method for medium-voltage high-energy zinc oxide resistor disc |
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| CN107082635B (en) * | 2017-04-24 | 2020-02-18 | 新昌县恩喜电器有限公司 | Piezoresistor with low residual voltage ratio and application thereof |
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