CN1801409A - Method for preparing high-potential gradient zinc oxide piezoresistive material by low-temperature sintering - Google Patents
Method for preparing high-potential gradient zinc oxide piezoresistive material by low-temperature sintering Download PDFInfo
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Abstract
The preparation method for high-potential gradient ZnO piezoresistor material comprises: with high-energy ball grinding technology, adding rare earth oxides included Bi2O3, Sb2O3, Cr2O3, Co2O3, MnO2, and Y2O3; sintering at 800Deg, and obtaining the product. The advantages of this invention comprises: simple process technology, low sintering temperature, fit to traditional device, well properties of the product, 5.50-5.64g/cm3 density, 1845.66-2233.33V/mm voltage-sensitive potential gradient, 21.3-25.8 nonlinear index, and 1.55-10.2muA drain current (given 0.75V1mA).
Description
Technical field
The present invention relates to a kind of method for preparing high-potential gradient zinc oxide piezoresistive material, belong to piezoresistive material manufacturing technology field.
Background technology
Zinc oxide piezoresistive material has excellent volt-ampere characteristic, is widely used in the manufacturing arrester valve piece made.For realizing the miniaturization and the lightness of arrester valve piece made, reduce manufacturing cost, the exploitation high-potential gracient is a development trend
[1]Viswanath
[2]The superfine nano powder that uses colloidal suspension and centrifugal separation to obtain, the Zinc-oxide piezoresistor of preparing electric potential gradient up to 3000V/mm 750 ℃ of sintering temperatures.Duran
[3]The nano powder that also utilizes chemical method to make, having prepared electric potential gradient under 900 ℃ and 825 ℃ of double sintering temperature is the Zinc-oxide piezoresistor of 2000V/mm.Last two kinds of methods all exist complex process, shortcoming that cost is high, are difficult to form large-scale production.Oh
[4]Adopt non-oxidation bismuth meal end sintering for the first time, be coated with the way of double sintering again behind the bismuth oxide-containing slurry, the zinc oxide electric potential gradient of exploitation is 500-900V/mm, but sintering temperature height (once sintered 1200-1350 ℃, secondary is 1000-1200 ℃).Fah
[5]Then adopt high-energy ball milling method, powder is refined to about 17nm near industrialization technology, first single shaft compacting, isostatic compaction is reduced to sintering temperature under 1100 ℃ again, has prepared the zinc oxide piezoresistive material that electric potential gradient reaches 440V/mm.Alamdari
[6]Adopt the additive high-energy ball milling different with Fah, the electric potential gradient of the zinc oxide piezoresistive materials of preparation is 1550V/mm under 1000 ℃.But both temperature are still higher, and equal pressing forming technology increases cost.Bernik
[7]By adding rare earth oxide Y
2O
3, make the zinc oxide grain size be reduced to 5.4 μ m from 11.3, electric potential gradient is promoted to 274V/mm from 150.Nahm
[8]Also by in containing Pr zinc oxide system, adding Y
2O
3, make electric potential gradient be increased to 748.1V/mm from 39.4.But not only the electric potential gradient absolute value is low for the two, and sintering temperature too high (all greater than 1200 ℃).
List of references
[1] basic research of Li Sheng great waves .ZnO piezoresistive wafer and technical development dynamic [J]. electromagnetism lightning arrester, 1998, (3): 42-48.
[2]R.N.Viswanath，S.Ramasamy，R.Ramamoorthy，etal.Preparation and characterization ofnanocrystalline ZnO based materials for varistor applications[J].Nanostructuredmaterials，1995，6：993-996.
[3]P.Duran，F.Capel，J.Tartaj，C.Moure.Effects of low-temperature annealing on the microstructureand electrical properties of doped-ZnO varistors[J].Key EngineeringMaterials，2002，206-213：1389-1392.
[4]Myung H.Oh，Kyung J，Lee，In J.Chung，etal.Fabrication method for high voltage zinc oxidevaristor[P].U.S.：5004573，Apr.2，1991.
[5]C.P.Fah，，J.Wang.Effect of high-energy mechanical activation on the microstructure andelectrical properties of ZnO-based varistors[J]，Solid State lonics，2000，132：107-117.
[6]H.D.Alamdari，S.Boily，M.Blouin，etal.High energy ball milled nanocrystalline ZnOvaristors[J].Materials Science Forum，2000，343-346：909-917.
[7]S.Bernik，S.Macek，B.Ai.Microstructural and electrical characteristics of Y
2O
3-dopedZnO-Bi
2O
3-based varistor ceramics[J].Journal of the European CeramicSociety，2001，21：1875-1878.
[8]C-W Nahm，B-C Shin，B-H Min.Microstructure and electrical properties of Y
2O
3-dopedZnO-Pr
6O
11-based varistor ceramics[J].Materials Chemistry and Physics，2003，82：157-164.
Summary of the invention
The technical problem to be solved in the present invention is to release a kind of method for preparing high-potential gradient zinc oxide piezoresistive material.This method has simple, the easy operating of technology, the not high and low advantage of production cost to equipment requirements.The properties of product of this method preparation are good, and electric potential gradient height, density are big, even tissue, non linear coefficient are higher, have following electrical performance indexes: electric potential gradient 1800～2200V/mm, and nonlinear exponent 21.3～25.8, leakage current is less than 10 μ A.
The present invention is resolved above-mentioned technical problem by following technical scheme: adopt high-energy ball-milling process, by add rare earth oxide in zinc oxide (ZnO): bismuth oxide (Bi
2O
3), antimonous oxide (Sb
2O
3), chrome green (Cr
2O
3), cobalt sesquioxide (Co
2O
3), manganese dioxide (MnO
2) and yttria (Y
2O
3), at 800 ℃ of following sintering, prepare high-potential gradient zinc oxide piezoresistive material.
Now describe technical scheme of the present invention in detail.
A kind of method for preparing high-potential gradient zinc oxide piezoresistive material is characterized in that, comprises following operating procedure:
The wet-milling of first step high energy
Get and be purchased micron order zinc oxide, bismuth oxide, antimonous oxide, chrome green, cobalt sesquioxide, manganese dioxide and yttria powder, press zinc oxide: bismuth oxide: antimonous oxide: chrome green: cobalt sesquioxide: manganese dioxide: the molar percentage of yttria=(96.5-X): 0.7: 1.0: 0.5: 0.8: 0.5: the mixed of X, X=0.02～0.10 wherein, put into high energy ball mill, with rotating speed 450～550rpm, ball powder ratio 20: 1, wet-milling in absolute ethyl alcohol, the wet-milling time is 3～7 hours, from high energy ball mill, take out, 150～250 ℃ of oven dry down obtain dry mixed powder in resistance furnace;
The high energy dry grinding of second step
The mixed powder of the drying that the first step is made is put into high energy ball mill, is 20: 1 with rotating speed 450～550rpm, ball powder ratio, dry grinding, and the dry grinding time is 0.5～1.5 hour, takes out from high energy ball mill, obtains uniform nanometer mixed powder;
The 3rd one-step forming
With uniform nanometer mixed powder compression moulding under 10～40 t hydraulic press that second step made, get the standard specimen of φ 10.0 * 2.0mm;
The 4th step burnt till
The 3rd standard specimen that make of step is put into resistance furnace, and 800 ℃ of following sintering 2 hours heat up in the stove and rate of temperature fall is 5 ℃/min, obtain the sintering standard specimen;
The 5th step was coated with electrode silver plasm
Go on foot on two end faces of the sintering standard specimen that makes the 4th, coat electrode silver plasm, put into resistance furnace, 600 ℃ are incubated 15 minutes down, cool to room temperature with the furnace, obtain the sintering standard specimen that end face scribbles electrode silver plasm;
The 6th step soldering contact conductor
Scribble soldering contact conductor on the end face of sintering standard specimen of electrode silver plasm at the 5th end face that make of step, finished product, high-potential gradient zinc oxide piezoresistive material.
The performance index that finished product of the present invention has: density is 5.50～5.64g/cm
3Pressure-sensitive current potential (V
1mA) gradient is 1845.66～2233.33V/mm; Nonlinear exponent is 21.3～25.8; Leakage current (0.75V1
MABe 1.55～10.2 μ A down).
Technical scheme of the present invention is further characterized in that in the first step, high energy ball mill is a planetary high-energy ball mill, adopts wear-resisting ball of steel and nylon jar, and rotating speed is 500rpm, and the wet-milling time is 5 hours, and the furnace temperature of resistance furnace is 200 ℃.
Technical scheme of the present invention is further characterized in that in second step, high energy ball mill is a planetary high-energy ball mill, adopts wear-resisting ball of steel and nylon jar, and rotating speed is 500rpm, and the dry grinding time is 1 hour.
Technical scheme of the present invention is further characterized in that, in the 3rd step, and the compression moulding under 25 t hydraulic press of nanometer mixed powder.
Technical scheme of the present invention is further characterized in that in the first step, high energy ball mill is a planetary high-energy ball mill, adopt wear-resisting ball of steel and nylon jar, rotating speed is 500rpm, and the wet-milling time is 5 hours, the furnace temperature of resistance furnace is 200 ℃, in second step, high energy ball mill is a planetary high-energy ball mill, adopts wear-resisting ball of steel and nylon jar, rotating speed is 500rpm, the dry grinding time is 1 hour, in the 3rd step, and the compression moulding under 25 t hydraulic press of nanometer mixed powder.
The present invention has following outstanding advantage:
(1) high-energy ball milling increases grain refinement, low temperature active; Add an amount of Y
2O
3, can not only stop growing up of ZnO crystal grain, and can also improve the nonlinear exponent of finished product.More than two measures guaranteed that material behind 800 ℃ of sintering, had both had high-potential gracient, have the higher non-linearity index again.
(2) compare with traditional handicraft, sintering temperature reduces significantly, only is 800 ℃.
(3) traditional pre-burning and granulating working procedure have been saved in work simplification.
(4) not high to equipment requirements, legacy equipment can meet the demands.
Subordinate list and explanation thereof
Table 1 is the prescription of high-potential gradient zinc oxide piezoresistive material of the present invention.
Table 1
| Constituent element | ZnO | Bi 2O 3 | Sb 2O 3 | Cr 2O 3 | Co 2O 3 | MnO 2 | Y 2O 3 |
| Mole, % | 96.5-X | 0.7 | 1.0 | 0.5 | 0.8 | 0.5 | X＝0.02～0.10 |
Table 2 is high-potential gradient zinc oxide piezoresistive materials of preparing of the present invention and the performance comparison of external same type of material.
Table 2
| Material | Comparison other | Relative density (%) | Electric potential gradient (V/mm) | Nonlinear exponent | Firing temperature (℃) |
| Zinc-oxide piezoresistor | Nahm adds Y 2O 3Method | 95.67 | 748.1 | 51.2 | 1350 |
| Zinc-oxide piezoresistor | The Alamdari high-energy ball milling method | 99.95 | 1550 | 59 | 1000 |
| Zinc-oxide piezoresistor | The present invention | 99.82 | 2233.33 | 25.8 | 800 |
Embodiment
Embodiment 1
Get and be purchased micron order zinc oxide (ZnO), bismuth oxide (Bi
2O
3), antimonous oxide (Sb
2O
3), chrome green (Cr
2O
3), cobalt sesquioxide (Co
2O
3), manganese dioxide (MnO
2) and yttria (Y
2O
3) powder, mix by following prescription, put into planetary high-energy ball mill, adopt wear-resisting ball of steel and nylon jar, rotating speed 550rpm, ball powder ratio 20: 1, wet-milling is after 3 hours in absolute ethyl alcohol, from spherical tank, take out, 150 ℃ of oven dry in resistance furnace, recipe calculation: with X=0.02 substitution following formula, zinc oxide: bismuth oxide: antimonous oxide: chrome green: cobalt sesquioxide: manganese dioxide: the molar percentage of yttria=(96.5-X): 0.7: 1.0: 0.5: 0.8: 0.5: X, must fill a prescription zinc oxide: bismuth oxide: antimonous oxide: chrome green: cobalt sesquioxide: manganese dioxide: the molar percentage of yttria=96.48: 0.7: 1.0: 0.5: 0.8: 0.5: 0.02.With the oven dry mixed powder under identical ball milling condition, dry grind after 0.5 hour, from spherical tank, take out.Mixed powder is pressed into φ 10 * 2.0mm standard specimen under 10 t hydraulic press.Standard specimen is put into resistance furnace,, heat up in the stove and rate of temperature fall is 5 ℃/min in 800 ℃ of following sintering 2 hours.After burning till on the upper and lower surface of standard specimen, coating electrode silver plasm equably, put into resistance furnace, be incubated 15 minutes down at 600 ℃, cool to room temperature with the furnace.On the electrode silver plasm face that burns till, the soldering contact conductor obtains high-potential gradient zinc oxide piezoresistive material.Its density is 5.57g/cm
3, pressure-sensitive current potential (V
1mA) gradient is 1845.66V/mm, nonlinear exponent is 25.8, leakage current (0.75V
1mABe 3.35 μ A down).
Embodiment 2
Get and be purchased micron order zinc oxide (ZnO), bismuth oxide (Bi
2O
3), antimonous oxide (Sb
2O
3), chrome green (Cr
2O
3), cobalt sesquioxide (Co
2O
3), manganese dioxide (MnO
2) and yttria (Y
2O
3) powder, mix by following prescription, put into planetary high-energy ball mill, adopt wear-resisting ball of steel and nylon jar, rotating speed 500rpm, ball powder ratio 20: 1, wet-milling is after 5 hours in absolute ethyl alcohol, from spherical tank, take out, 200 ℃ of oven dry in resistance furnace, recipe calculation: with X=0.08 substitution following formula, zinc oxide: bismuth oxide: antimonous oxide: chrome green: cobalt sesquioxide: manganese dioxide: the molar percentage of yttria=(96.5-X): 0.7: 1.0: 0.5: 0.8: 0.5: X, must fill a prescription zinc oxide: bismuth oxide: antimonous oxide: chrome green: cobalt sesquioxide: manganese dioxide: the molar percentage of yttria=96.42: 0.7: 1.0: 0.5: 0.8: 0.5: 0.08.With the oven dry mixed powder under identical ball milling condition, dry grind after 1 hour, from spherical tank, take out.Mixed powder is pressed into φ 10 * 2.0mm standard specimen under 25 t hydraulic press.Standard specimen is put into resistance furnace,, heat up in the stove and rate of temperature fall is 5 ℃/min in 800 ℃ of following sintering 2 hours.After burning till on the upper and lower surface of standard specimen, coating electrode silver plasm equably, put into resistance furnace, be incubated 15 minutes down at 600 ℃, cool to room temperature with the furnace.On the electrode silver plasm face that burns till, the soldering contact conductor obtains high-potential gradient zinc oxide piezoresistive material.Its density is 5.55g/cm
3, pressure-sensitive current potential (V
1mA) gradient is 2110.45V/mm, nonlinear exponent is 24.3, leakage current (0.75V
1mABe 1.55 μ A down).
Embodiment 3
Get and be purchased micron order zinc oxide (ZnO), bismuth oxide (Bi
2O
3), antimonous oxide (Sb
2O
3), chrome green (Cr
2O
3), cobalt sesquioxide (Co
2O
3), manganese dioxide (MnO
2) and yttria (Y
2O
3) powder, mix by following prescription, put into planetary high-energy ball mill, adopt wear-resisting ball of steel and nylon jar, rotating speed 450rpm, ball powder ratio 20: 1, wet-milling is after 7 hours in absolute ethyl alcohol, from spherical tank, take out, 250 ℃ of oven dry in resistance furnace, recipe calculation: with X=0.1 substitution following formula, zinc oxide: bismuth oxide: antimonous oxide: chrome green: cobalt sesquioxide: manganese dioxide: the molar percentage of yttria=(96.5-X): 0.7: 1.0: 0.5: 0.8: 0.5: X, must fill a prescription zinc oxide: bismuth oxide: antimonous oxide: chrome green: cobalt sesquioxide: manganese dioxide: the molar percentage of yttria=96.4: 0.7: 1.0: 0.5: 0.8: 0.5: 0.1.With the oven dry mixed powder under identical ball milling condition, dry grind after 1 hour, from spherical tank, take out.Mixed powder is pressed into φ 10 * 2.0mm standard specimen under 40 t hydraulic press.Standard specimen is put into resistance furnace,, heat up in the stove and rate of temperature fall is 5 ℃/min in 800 ℃ of following sintering 2 hours.After burning till on the upper and lower surface of standard specimen, coating electrode silver plasm equably, put into resistance furnace, be incubated 15 minutes down at 600 ℃, cool to room temperature with the furnace.On the electrode silver plasm face that burns till, the soldering contact conductor obtains high-potential gradient zinc oxide piezoresistive material.Its density is 5.50g/cm
3, pressure-sensitive current potential (V
1mA) gradient is 2233.33V/mm, nonlinear exponent is 21.3, leakage current (0.75V
1mABe 1.64 μ A down).
Claims (5)
1, a kind of method for preparing high-potential gradient zinc oxide piezoresistive material is characterized in that, comprises following operating procedure:
The wet-milling of first step high energy
Get and be purchased micron order zinc oxide, bismuth oxide, antimonous oxide, chrome green, cobalt sesquioxide, manganese dioxide and yttria powder, press zinc oxide: bismuth oxide: antimonous oxide: chrome green: cobalt sesquioxide: manganese dioxide: the molar percentage of yttria=(96.5-X): 0.7: 1.0: 0.5: 0.8: 0.5: the mixed of X, X=0.02～0.10 wherein, put into high energy ball mill, with rotating speed 450～550rpm, ball powder ratio 20: 1, wet-milling in absolute ethyl alcohol, the wet-milling time is 3～7 hours, from high energy ball mill, take out, 150～250 ℃ of oven dry down obtain dry mixed powder in resistance furnace;
The high energy dry grinding of second step
The mixed powder of the drying that the first step is made is put into high energy ball mill, is 20: 1 with rotating speed 450～550rpm, ball powder ratio, dry grinding, and the dry grinding time is 0.5～1.5 hour, takes out from high energy ball mill, obtains uniform nanometer mixed powder;
The 3rd one-step forming
With uniform nanometer mixed powder compression moulding under 10～40 t hydraulic press that second step made, get the standard specimen of φ 10.0 * 2.0mm;
The 4th step burnt till
The 3rd standard specimen that make of step is put into resistance furnace, and 800 ℃ of following sintering 2 hours heat up in the stove and rate of temperature fall is 5 ℃/min, obtain the sintering standard specimen;
The 5th step was coated with electrode silver plasm
Go on foot on two end faces of the sintering standard specimen that makes the 4th, coat electrode silver plasm, put into resistance furnace, 600 ℃ are incubated 15 minutes down, cool to room temperature with the furnace, obtain the sintering standard specimen that end face scribbles electrode silver plasm;
The end face that the 6th step soldering contact conductor made in the 5th step scribbles soldering contact conductor on the end face of sintering standard specimen of electrode silver plasm, finished product, high-potential gradient zinc oxide piezoresistive material.
2, the method for preparing high-potential gradient zinc oxide piezoresistive material according to claim 1, it is characterized in that, in the first step, high energy ball mill is a planetary high-energy ball mill, adopt wear-resisting ball of steel and nylon jar, rotating speed is 500rpm, and the wet-milling time is 5 hours, and the furnace temperature of resistance furnace is 200 ℃.
3, the method for preparing high-potential gradient zinc oxide piezoresistive material according to claim 1 is characterized in that, in second step, high energy ball mill is a planetary high-energy ball mill, adopt wear-resisting ball of steel and nylon jar, rotating speed is 500rpm, and the dry grinding time is 1 hour.
4, the method for preparing high-potential gradient zinc oxide piezoresistive material according to claim 1 is characterized in that, in the 3rd step, and the compression moulding under 25 t hydraulic press of nanometer mixed powder.
5, the method for preparing high-potential gradient zinc oxide piezoresistive material according to claim 1, it is characterized in that, in the first step, high energy ball mill is a planetary high-energy ball mill, adopt wear-resisting ball of steel and nylon jar, rotating speed is 500rpm, the wet-milling time is 5 hours, and the furnace temperature of resistance furnace is 200 ℃, in second step, high energy ball mill is a planetary high-energy ball mill, adopt wear-resisting ball of steel and nylon jar, rotating speed is 500rpm, and the dry grinding time is 1 hour, in the 3rd step, the compression moulding under 25 t hydraulic press of nanometer mixed powder.
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