CN102020463A - Zinc oxide piezoresistor material and preparing method thereof - Google Patents
Zinc oxide piezoresistor material and preparing method thereof Download PDFInfo
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- CN102020463A CN102020463A CN 201010538897 CN201010538897A CN102020463A CN 102020463 A CN102020463 A CN 102020463A CN 201010538897 CN201010538897 CN 201010538897 CN 201010538897 A CN201010538897 A CN 201010538897A CN 102020463 A CN102020463 A CN 102020463A
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Abstract
The present invention discloses a zinc oxide piezoresistor material comprising the following raw materials: ZnO, Bi2O3, Sb2O3, Co2O3, Cr2O3, MnCO3, NiO, Al2O3 and oxides of boron, wherein, calculating according to B2O3, the weight ratio of the oxide of boron to ZnO is 2.1-20:100; the percentages by mole of ZnO, Bi2O3, Sb2O3, Co2O3, Cr2O3, MnCO3, NiO and Al2O3 are respectively 90.5%-96.5%, 0.3%-5%, 0.1%-3%, 0.1-2%, 0.1%-1%, 0.2%-2%, 0.1%-1% and 0.005%-0.05%; and voltage-dependent combination performance of the material is good. The present invention further discloses a preparing method of the material; the method has the advantages of simple technology and low cost, and the method is suitable for industrialized production.
Description
Technical field
The present invention relates to the piezoresistive material technical field, be specifically related to a kind of high non-linearity zinc oxide piezoresistive material and preparation method thereof.
Background technology
Zinc-oxide piezoresistor has enjoyed researcher's attention always, and is used widely in the arrester of countries in the world owing to its excellent pressure-sensitive character since coming out.Common zinc oxide piezoresistive material all is take ZnO as main component, by adding Bi
2O
3, Sb
2O
3, Mn
O2, Co
2O
3, Cr
2O
3The sintered body that forms by the manufacturing of ordinary electronic ceramic process Deng metal oxide (generally containing the 8-10 kind) (or pottery).These additives can be divided three classes by the mechanism of action: (1) accelerating oxidation zinc voltage-sensitive ceramic forms the additive of grain boundary structure, such as Bi
2O
3, BaO, SrO, PbO, Pr
2O
3To promote liquid-phase sintering and form trap and surface state and that zinc oxide piezoresistive material is had is non-linear Deng, their main impacts; (2) improve the additive of zinc oxide pressure-sensitive ceramic electric property nonlinear characteristic, such as MnO, Co
2O
3, Cr
2O
3, Al
2O
3Deng, their part provides carrier for the solid solution of donor impurity institute in ZnO crystal grain, and remainder then forms trap and acceptor state and has improved the height of potential barrier at crystal boundary; (3) additive of raising reliability is such as Sb
2O
3, SiO
2, NiO, CeO
2With a small amount of frit, their Main Function is to improve zinc oxide pressure-sensitive ceramic to the stability of the impact of voltage load and environment (such as temperature and humidity).
According to the difference of additive, Zinc-oxide piezoresistor generally is divided into different material systems, and wherein most widely used is ZnO-Bi
2O
3-Sb
2O
3Be piezoresistive material, remove Bi in this material system
2O
3, Sb
2O
3As outside the additive, a small amount of MnO, Co have also been added
2O
3, NiO, Cr
2O
3Deng transition metal oxide.ZnO-Bi
2O
3-Sb
2O
3The microstructure that is piezoresistive material is made up of grain and grain boundary two parts, and wherein crystal grain is the zinc oxide phase mutually, and Grain-Boundary Phase generally comprises rich bismuth mutually and zinc antimony Spinel; This material system has the preferably quick combination property of voltage, but sintering temperature is higher, and high sintering temperature makes ceramics generation deformation first easily, affects the coating quality of ceramics electrode, thereby has influence on ratio defective product, second makes easily low-melting component (Bi
2O
3, Sb
2O
3) excessive volatilization, cause the quick parameter of device voltage to descend.For appropriateness reduces sintering temperature, disclose among the Chinese patent application CN02122851.5 in the zinc oxide pressure-sensitive material and to have added some and help the oxide compound of grain growing, be characterized in: add small amounts titanium or boron oxide, wherein the addition of titanium oxide is no more than 5% of zinc oxide weight, and the addition of boron oxide is no more than 1% of zinc oxide weight; Its adding mode is modulated into powder for earlier titanium oxide or boron oxide and other additive being mixed together pre-burning, and then the powder that is modulated into and zinc oxide mixed to reburn forms porcelain.Though this method sintering temperature lowers but the preparation process relative complex to some extent, and the optimization of the quick parameter of its main several voltage (nonlinear factor, leakage current, electric current discharge capacity and through-flow back pressure sensitive voltage velocity of variation) is also undesirable.
Summary of the invention
The invention provides a kind of over-all properties zinc oxide piezoresistive material superior, with low cost.
The present invention also provides a kind of preparation method of zinc oxide piezoresistive material, and this method preparation technology is simple, cost is low, is suitable for suitability for industrialized production.
A kind of zinc oxide piezoresistive material is made by following raw material: ZnO, Bi
2O
3, Sb
2O
3, Co
2O
3, Cr
2O
3, MnCO
3, NiO, Al
2O
3Oxide with boron;
Wherein, the oxide of boron is with B
2O
3The weight ratio of counting with ZnO that converts is 2.1～20: 100;
ZnO, Bi
2O
3, Sb
2O
3, Co
2O
3, Cr
2O
3, MnCO
3, NiO and Al
2O
3In the molar percentage of each raw material consist of: 90.5%～96.5%ZnO, 0.3%～5%Bi
2O
3, 0.1%～3%Sb
2O
3, 0.1%～2%Co
2O
3, 0.1%～1%Cr
2O
3, 0.2%～2%MnCO
3, 0.1%～1%NiO and 0.005%～0.05%Al
2O
3
The present invention is at ZnO-Bi
2O
3-Sb
2O
3Be that the piezoresistive material major ingredient (is ZnO, Bi
2O
3, Sb
2O
3, Co
2O
3, Cr
2O
3, MnCO
3, NiO and Al
2O
3) in to add an amount of low-melting compound be the oxide of boron, its mechanism of action is: the oxide of boron is not only better compatible with the raw material of other zinc oxide piezoresistive material, and the effectively growth of accelerating oxidation zinc crystal grain in sintering process of the oxide of low-melting boron, simultaneously by with Bi
2O
3Improve the microstructure of zinc oxide piezoresistive material with the reaction of ZnO, obtain containing in the microstructure boron bismuth glass and Firebrake ZB mutually and the good zinc oxide piezoresistive material of the quick combination property of voltage.
Contain boron bismuth glass and zinc borate in the microtexture of described zinc oxide piezoresistive material mutually.
In order to reach better invention effect, preferred boron trioxide of the oxide compound of described boron or boric acid.
The preparation method of described zinc oxide piezoresistive material comprises step:
With ZnO, Bi
2O
3, Sb
2O
3, Co
2O
3, Cr
2O
3, MnCO
3, NiO, Al
2O
3Through wet ball grinding, drying, extrusion forming and sintering, make zinc oxide piezoresistive material after mixing with the oxide of boron.
The condition optimization of described wet ball grinding is: with the deionized water solvent, and ball milling 2.5 hours～5 hours.
Described exsiccant condition optimization was: 80 ℃～95 ℃ dryings 10 hours～15 hours.
Described agglomerating condition optimization is: be warming up to 800 ℃～1100 ℃ insulations 2.5 hours～5 hours with 120 ℃/hour～160 ℃/hour temperature rise rates.
Zinc oxide piezoresistive material of the present invention has high voltage gradient (V
1mA〉=250V/mm) and the good quick over-all properties of voltage.It particularly has crucial application potential aspect the high-voltage arrester in the line protection field.
Compared with prior art, the present invention has following advantage:
Zinc oxide piezoresistive material of the present invention has the quick over-all properties of good voltage, and (1) this zinc oxide piezoresistive material has proper voltage gradient, high nonlinear factor and low leakage current density: at the potential gradient V of 800 ℃ of-1100 ℃ of these zinc oxide piezoresistive materials of agglomerating
1mA=250～380V/mm, nonlinear factor α be greater than 60, leakage current 0.75V
1mADown less than 0.3 μ A; Proper voltage gradient, high nonlinear factor and low leakage current density make it not only power consumption are little in actual applications, power consumption is low, are difficult to simultaneously take place destroyed by the heating that causes own out of control.(2) this zinc oxide piezoresistive material has high electric current discharge capacity and low pressure sensitive voltage velocity of variation: at the electric current discharge capacity (twice pulse test of 8/20 μ S waveform of stipulating among the GB-10193) of 800 ℃ of-1100 ℃ of these zinc oxide piezoresistive materials of agglomerating (is example with diameter 35mm disk) greater than 950A/cm
3, through-flow back pressure sensitive voltage V
1mAVelocity of variation is ± (2.0～4.0) %; High discharge capacity and low pressure sensitive voltage velocity of variation make it significantly improve in surge receptivity and the stability of handling lightning impulse, igniter shock, get rid of when bearing impact isopulse heavy current impact.(3) this zinc oxide piezoresistive material has good ageing-resistant performance: at the ageing-resistant coefficient of 800 ℃ of-1100 ℃ of these zinc oxide piezoresistive materials of agglomerating less than 0.85.
When preparing, zinc oxide piezoresistive material of the present invention only needs once sintered forming after all raw material uniform mixing, ball milling, the extrusion forming, preparation method's technology is simple, need not special equipment and control, the cycle is short, sintering temperature is lower, easy to operate, and the very easy acquisition of required raw material, with low cost, be suitable for suitability for industrialized production.
Description of drawings
Fig. 1 is the powder X-ray RD thing phase collection of illustrative plates of zinc oxide piezoresistive material among the embodiment 1; Wherein, X-coordinate is 2 θ angles, and ordinate zou is relative intensity (intensity);
Fig. 2 is the powder X-ray RD thing phase collection of illustrative plates of Comparative Examples material (being implementation column 4 made samples among the Chinese patent application CN02122851.5); Wherein, X-coordinate is 2 θ angles, and ordinate zou is relative intensity (intensity).
Embodiment
The present invention mainly is at ZnO-Bi
2O
3-Sb
2O
3-Co
2O
3-Cr
2O
3-MnCO
3-NiO-Al
2O
3Add an amount of low melting point boron oxide compound in the major ingredient, make and the preferably low melting point boron oxide compound effectively growth of accelerating oxidation zinc crystal grain in sintering process of zinc oxide piezoresistive material compatibility, simultaneously by with Bi
2O
3Improve microstructure with the reaction of ZnO.The present invention is further described below in conjunction with embodiment.
Embodiment 1
The principal component material is made up of the raw material of following molar percentage: 94.5mol%ZnO, 1.18mol%Bi
2O
3, 0.1mol%Sb
2O
3, 2mol%Co
2O
3, 0.1mol%Cr
2O
3, 2mol%MnCO
3, 0.1mol%NiO and 0.02mol%Al
2O
3Boron oxide compound is boric acid, and the consumption of boric acid is with B
2O
3The weight ratio of zinc oxide is 3: 100 in conversion meter and the principal component material.
By above-mentioned consumption boric acid and principal component material are mixed afterwards with deionized water and zirconium ball ball milling 3 hours in planetary ball mill, 90 ℃ obtained the Zinc-oxide piezoresistor powder in lower dry 12 hours then.The Zinc-oxide piezoresistor powder is added the molding that is pressed into the disk shape, place air atmosphere to be warming up to 1050 ℃ with 150 ℃/hour temperature rise rate, be incubated that furnace cooling obtains zinc oxide piezoresistive material (being sintered compact) after 3 hours, the test portion of this zinc oxide piezoresistive material is of a size of thickness 10mm, diameter 35mm.
Above-mentioned zinc oxide piezoresistive material is polished on 1200 order SiC sand paper, then it is cleaned in alcohol with ultrasonic wave, obtain sample.After coating electrode silver plasm equably on the upper and lower surface of sample, put into resistance furnace, silver ink firing under 300 ℃ of conditions, be incubated 30 minutes, grid for welding lead-in wire on the electrode silver plasm face that burns till obtains zinc oxide varistor again, is used to measure the electrical property of above-mentioned zinc oxide piezoresistive material.Relevant test method among GB/T16528-1996 and the GB 11032-2000 is adopted in the test of electrical property.
The electric performance test result is: this zinc oxide piezoresistive material potential gradient V
1mABe 280V/mm, nonlinear factor α reaches 70, leakage current 0.75V
1mALess than 0.1 μ A, electric current discharge capacity (twice pulse test of 8/20 μ S waveform of stipulating among the GB-10193) is greater than 1000A/cm3 down, and through-flow back pressure sensitive voltage V1mA velocity of variation is ± 2.0%; The ageing-resistant coefficient of material is less than 0.8.
The electric performance test result shows that this zinc oxide piezoresistive material not only has high nonlinear factor and low leakage current density but also has high electric current discharge capacity, low pressure sensitive voltage velocity of variation and low ageing-resistant coefficient, the quick excellent of its integrated voltage.
Simultaneously, the powder X-ray RD analytical results of this zinc oxide pressure-sensitive material shows that this zinc oxide pressure-sensitive material compares it and also exist obviously different with Zinc oxide pressure sensitive (as: implementation column 4 made samples among the Chinese patent application CN02122851.5) in the past in the phase composite of microcosmic thing.
The powder X-ray RD analytical results of this zinc oxide piezoresistive material and Comparative Examples material (implementation column 4 made samples among the Chinese patent application CN02122851.5) as depicted in figs. 1 and 2.
Comparison diagram 1 and Fig. 2, as can be known: the zinc oxide pressure-sensitive material among the Chinese patent application CN02122851.5 has different microtextures with zinc oxide pressure-sensitive material of the present invention, do not have the zinc borate phase in the microtexture of the zinc oxide pressure-sensitive material among the Chinese patent application CN02122851.5, and zinc oxide pressure-sensitive material of the present invention contains certain zinc borate phase.Contain certain bismuth oxide phase in the microstructure of the zinc oxide pressure-sensitive material among the Chinese patent application CN02122851.5 simultaneously, and not having the bismuth oxide phase in the microstructure of zinc oxide pressure-sensitive material of the present invention, the bismuth oxide that adds in this material has reacted with the oxide of the boron that adds in preparation process and has formed the boron bismuth glass.The performance of zinc oxide pressure-sensitive material of the present invention and microstructure presentation of results: the oxide of the low melting point boron that adds among the present invention effectively growth of accelerating oxidation zinc crystal grain reduces sintering temperature, and can by with Bi
2O
3Improve the microstructure of zinc oxide piezoresistive material with the reaction of ZnO, obtain containing in the microstructure boron bismuth glass and Firebrake ZB mutually and the good zinc oxide piezoresistive material of the quick combination property of voltage.
Embodiment 2
The principal component material is made up of the raw material of following molar percentage: 96.5mol%ZnO, 0.3mol%Bi
2O
3, 0.895mol%Sb
2O
3, 0.1mol%Co
2O
3, 1mol%Cr
2O
3, 0.2mol%MnCO
3, 1mol%NiO and 0.005mol%Al
2O
3Boron oxide compound is diboron trioxide, and the consumption of diboron trioxide is with B
2O
3The weight ratio of zinc oxide is 2.1: 100 in conversion meter and the principal component material.
By above-mentioned consumption diboron trioxide and principal component material are mixed afterwards with deionized water and zirconium ball ball milling 3 hours in planetary ball mill, 95 ℃ obtained the Zinc-oxide piezoresistor powder in lower dry 12 hours then.The Zinc-oxide piezoresistor powder is added the molding that is pressed into the disk shape, place air atmosphere to be warming up to 1100 ℃ with 120 ℃/hour temperature rise rate, be incubated that furnace cooling obtains zinc oxide piezoresistive material (being sintered compact) after 3 hours, the test portion of this zinc oxide piezoresistive material is of a size of thickness 10mm, diameter 35mm.
The preparation of zinc oxide varistor is with embodiment 1.Measure the electrical property of above-mentioned zinc oxide piezoresistive material.Relevant test method among GB/T16528-1996 and the GB 11032-2000 is adopted in the test of electrical property.
The electric performance test result is: this zinc oxide piezoresistive material potential gradient V
1mABe 250V/mm, nonlinear factor α reaches 62, leakage current 0.75V
1mALess than 0.3 μ A, electric current discharge capacity (twice pulse test of 8/20 μ S waveform of stipulating among the GB-10193) is greater than 950A/cm down
3, through-flow back pressure sensitive voltage V
1mAVelocity of variation is ± 3.0%; The ageing-resistant coefficient of material is less than 0.85.The electric performance test result shows that this zinc oxide piezoresistive material not only has high nonlinear factor and low leakage current density but also has high electric current discharge capacity, low pressure sensitive voltage velocity of variation and low ageing-resistant coefficient, the quick excellent of its integrated voltage.Simultaneously, the powder X-ray RD analysis result of this zinc oxide piezoresistive material illustrates and contains certain boron bismuth glass and Firebrake ZB in its microstructure mutually.
Embodiment 3
The principal component material is made up of the raw material of following molar percentage: 92.5mol%ZnO, 5mol%Bi
2O
3, 0.55mol%Sb
2O
3, 0.5mol%Co
2O
3, 0.5mol%Cr
2O
3, 0.5mol%MnCO
3, 0.4mol%NiO and 0.05mol%Al
2O
3Boron oxide compound is boric acid, and the consumption of boric acid is with B
2O
3The weight ratio of zinc oxide is 10: 100 in conversion meter and the principal component material.
By above-mentioned consumption boric acid and principal component material are mixed afterwards with deionized water and zirconium ball ball milling 3 hours in planetary ball mill, 85 ℃ obtained the Zinc-oxide piezoresistor powder in lower dry 12 hours then.The Zinc-oxide piezoresistor powder is added the molding that is pressed into the disk shape, place air atmosphere to be warming up to 800 ℃ with 160 ℃/hour temperature rise rate, be incubated that furnace cooling obtains zinc oxide piezoresistive material (being sintered compact) after 5 hours, the test portion of this zinc oxide piezoresistive material is of a size of thickness 10mm, diameter 35mm.
The preparation of zinc oxide varistor is with embodiment 1.Measure the electrical property of above-mentioned zinc oxide piezoresistive material.Relevant test method among GB/T16528-1996 and the GB 11032-2000 is adopted in the test of electrical property.
The electric performance test result is: this zinc oxide piezoresistive material potential gradient V
1mABe 380V/mm, nonlinear factor α reaches 68, leakage current 0.75V
1mALess than 0.2 μ A, electric current discharge capacity (twice pulse test of 8/20 μ S waveform of stipulating among the GB-10193) is greater than 950A/cm down
3, through-flow back pressure sensitive voltage V
1mAVelocity of variation is ± 4.0%; The ageing-resistant coefficient of material is less than 0.85.The electric performance test result shows that this zinc oxide piezoresistive material not only has high nonlinear factor and low leakage current density but also has high electric current discharge capacity, low pressure sensitive voltage velocity of variation and low ageing-resistant coefficient, the quick excellent of its integrated voltage.Simultaneously, the powder X-ray RD analysis result of this zinc oxide piezoresistive material illustrates and contains certain boron bismuth glass and Firebrake ZB in its microstructure mutually.
Embodiment 4
The principal component material is made up of the raw material of following molar percentage: 90.5mol%ZnO, 4.5mol%Bi
2O
3, 3.0mol%Sb
2O
3, 0.5mol%Co
2O
3, 0.5mol%Cr
2O
3, 0.5mol%MnCO
3, 0.48mol%NiO and 0.02mol%Al
2O
3Boron oxide compound is diboron trioxide, and the consumption of diboron trioxide is with B
2O
3The weight ratio of zinc oxide is 20: 100 in conversion meter and the principal component material.
By above-mentioned consumption diboron trioxide and principal component material are mixed afterwards with deionized water and zirconium ball ball milling 3 hours in planetary ball mill, 90 ℃ obtained the Zinc-oxide piezoresistor powder in lower dry 12 hours then.The Zinc-oxide piezoresistor powder is added the molding that is pressed into the disk shape, place air atmosphere to be warming up to 900 ℃ with 150 ℃/hour temperature rise rate, be incubated that furnace cooling obtains zinc oxide piezoresistive material (being sintered compact) after 5 hours, the test portion of this zinc oxide piezoresistive material is of a size of thickness 10mm, diameter 35mm.
The preparation of zinc oxide varistor is with embodiment 1.Measure the electrical property of above-mentioned zinc oxide piezoresistive material.Relevant test method among GB/T16528-1996 and the GB 11032-2000 is adopted in the test of electrical property.
The electric performance test result is: this zinc oxide piezoresistive material potential gradient V
1mABe 350V/mm, nonlinear factor α reaches 65, leakage current 0.75V
1mALess than 0.2 μ A, electric current discharge capacity (twice pulse test of 8/20 μ S waveform of stipulating among the GB-10193) is greater than 950A/cm down
3, through-flow back pressure sensitive voltage V
1mAVelocity of variation is ± 2.0%; The ageing-resistant coefficient of material is less than 0.85.The electric performance test result shows that this zinc oxide piezoresistive material not only has high nonlinear factor and low leakage current density but also has high electric current discharge capacity, low pressure sensitive voltage velocity of variation and low ageing-resistant coefficient, the quick excellent of its integrated voltage.Simultaneously, the powder X-ray RD analysis result of this zinc oxide piezoresistive material illustrates and contains certain boron bismuth glass and Firebrake ZB in its microstructure mutually.
Claims (7)
1. a zinc oxide piezoresistive material is made by following raw material: ZnO, Bi
2O
3, Sb
2O
3, Co
2O
3, Cr
2O
3, MnCO
3, NiO, Al
2O
3Oxide with boron;
Wherein, the oxide of boron is with B
2O
3The weight ratio of counting with ZnO that converts is 2.1～20: 100;
ZnO, Bi
2O
3, Sb
2O
3, Co
2O
3, Cr
2O
3, MnCO
3, NiO and Al
2O
3In the molar percentage of each raw material consist of: 90.5%～96.5%ZnO, 0.3%～5%Bi
2O
3, 0.1%～3%Sb
2O
3, 0.1%～2%Co
2O
3, 0.1%～1%Cr
2O
3, 0.2%～2%MnCO
3, 0.1%～1%NiO and 0.005%～0.05%Al
2O
3
2. zinc oxide piezoresistive material as claimed in claim 1 is characterized in that, the oxide compound of described boron is boron trioxide or boric acid.
3. zinc oxide piezoresistive material as claimed in claim 1 is characterized in that, contains boron bismuth glass and zinc borate in the microtexture of described zinc oxide piezoresistive material mutually.
4. as the preparation method of each described zinc oxide piezoresistive material of claim 1～3, comprise step:
With ZnO, Bi
2O
3, Sb
2O
3, Co
2O
3, Cr
2O
3, MnCO
3, NiO, Al
2O
3Through wet ball grinding, drying, extrusion forming and sintering, make zinc oxide piezoresistive material after mixing with the oxide of boron.
5. the preparation method of zinc oxide piezoresistive material as claimed in claim 4 is characterized in that, the condition of described wet ball grinding is: with the deionized water solvent, and ball milling 2.5 hours～5 hours.
6. the preparation method of zinc oxide piezoresistive material as claimed in claim 4 is characterized in that, described exsiccant condition is: 80 ℃～95 ℃ dryings 10 hours～15 hours.
7. the preparation method of zinc oxide piezoresistive material as claimed in claim 4 is characterized in that, described agglomerating condition is: be warming up to 800 ℃～1100 ℃ insulations 2.5 hours～5 hours with 120 ℃/hour～160 ℃/hour temperature rise rates.
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