CN101555130A - Low-pressure pressure-sensitive ceramic material and preparation method thereof - Google Patents

Low-pressure pressure-sensitive ceramic material and preparation method thereof Download PDF

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Publication number
CN101555130A
CN101555130A CNA2009101140906A CN200910114090A CN101555130A CN 101555130 A CN101555130 A CN 101555130A CN A2009101140906 A CNA2009101140906 A CN A2009101140906A CN 200910114090 A CN200910114090 A CN 200910114090A CN 101555130 A CN101555130 A CN 101555130A
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pressure
mno
tio
ceramic material
sensitive ceramic
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王宁章
马玉田
沙沙
秦国宾
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Guangxi University
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Guangxi University
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Abstract

The invention relates to a low-pressure pressure-sensitive ceramic material and a preparation method thereof. The material comprises a component A and a component B and contents thereof by mass percent are as follows: A comprises 57.4 percent of SrO, 40.7 percent of TiO2, 0.7 percent of Nb2O5, 0.8 percent of CeO2 and 0.4 percent of MnO; and B comprises 92.4 percent of Al2O3, 0.1 percent of Co2O3, 3.5 percent of MnO, 2.5 percent of Cr2O3, 0.3 percent of SiO2 and 1.5 percent of TiO2; pure reagents are taken according to a mass ratio of the component A and the component B being equal to 4:6 to 6:4, subjected to mixing, ball milling, drying, pelleting and sintering in a vacuum graphite oven at the temperature of 1305 to 1500 DEG C after being pressed and formed, and are cooled with the oven or cooled with the oven after being kept at constant temperature for 1 to 3h; surface treatment and cleaning are conducted to a sample after sintering, and the pressure-sensitive ceramic material with C=0.02 to 22muF, epsilon=1.7*10<5> to 1.5*10<8>, U1mA=0.6 to 6.3V, U10mA=1.8 to 11.6V and alpha=2.1 to 5.1 is obtained after put through electrode; and the preparation method is simple, safe and reliable.

Description

A kind of low-pressure pressure-sensitive ceramic material and preparation method thereof
One, technical field
The present invention relates to a kind of low-pressure pressure-sensitive ceramic material and preparation method thereof, belong to electric elements and material manufacturing technology field thereof
Two, technical background
Along with the miniaturization of electronic product, integrated, low pressure development, increasing to the demand of low-pressure pressure-sensitive ceramic material.Voltage-sensitive ceramic has capacity effect and piezo resistance effect, can play the dual function of overvoltage protection and filtering noise.At present the ZnO voltage-sensitive ceramic is most widely used general, and its static capacity is too small, specific inductivity is little (about 10 3About), pressure sensitive voltage low inadequately (>20V/mm), be difficult to make the voltage dependent resistor of several volts.SrTiO 3Contrast ZnO pressure-sensitive ceramic material not only has good non-ohmic behavior, but also has static capacity big (be ZnO 3-10 doubly).Particularly in low-pressure field, its electrical capacity is that the ZnO voltage-sensitive ceramic hardly matches greater than 0.01 μ F.Along with SrTiO 3The expansion of the breadth and depth that voltage-sensitive ceramic is used is to SrTiO 3The performance requriements of pressure-sensitive ceramic material also improves constantly.Because the voltage-sensitive ceramic performance depends on the constituent structure and the preparation technology of material.So some rare earth oxides and improvement preparation technology come the good SrTiO of obtained performance by mixing 3Pressure-sensitive ceramic material.
SrTiO 3The once-firing method is adopted in the production of voltage-sensitive ceramic now mostly, and its technology is simpler than traditional double firing process.But such material must be in reducing atmosphere sintering, just can make the abundant semiconductor of crystal grain, thereby also must make the crystal boundary insulating of SrTiO3 voltage-sensitive ceramic obtain pressure-sensitive character through oxidizing thermal treatment.In the production process, reducing atmosphere is usually by N 2+ H 2Provide, this has not only increased the difficulty of preparation cost and technology controlling and process, and also has safety issue in preparation process.So be conceived to SrTiO 3The voltage-sensitive ceramic large-scale application, it is significant to seek simpler and safer preparation method.
Three, summary of the invention
The purpose of this invention is to provide a kind of low-pressure pressure-sensitive ceramic material and preparation method thereof.This preparation method can prepare a kind of low pressure, the pressure-sensitive ceramic material of better performances, and preparation technology is simple, and safety performance is reliable.
The present invention achieves the above object by the following technical programs: a kind of low-pressure pressure-sensitive ceramic material, described material contain A, B two components and content and are by mass percentage:
A、57.4%SrO+40.7%TiO 2+0.7%Nb 2O 5+0.8%CeO 2+0.4%MnO
B、92.4%Al 2O 3+0.1%Co 2O 3+3.5%MnO+2.5%Cr 2O 3+0.3%SiO 2+1.5%TiO 2
Above-mentioned A, B two components are pressed mass ratio mixed in 4: 6~6: 4.
Another technical scheme is that described material contains A, B two components and content and is by mass percentage:
A、57.4%SrO+40.7%TiO 2+0.7%Nb 2O 5+0.8%CeO 2+0.4%MnO
B、92.4%Al 2O 3+0.1%Co 2O 3+3.5%MnO+2.5%Cr 2O 3+0.3%SiO 2+1.5%TiO 2
Above-mentioned A, B two components are pressed mass ratio mixes at 4: 6
Another technical scheme is that described material contains A, B two components and content and is by mass percentage:
A:57.4%SrO+40.7%TiO 2+0.7%Nb 2O 5+0.8%CeO 2+0.4%MnO
B:92.4%Al 2O 3+0.1%Co 2O 3+3.5%MnO+2.5%Cr 2O 3+0.3%SiO 2+1.5%TiO 2
Press mass ratio at above-mentioned A, B composition mixes at 5: 5.
Another technical scheme is that described material contains A, B two components and content (mass ratio) and is:
A:57.4%SrO+40.7%TiO 2+0.7%Nb 2O 5+0.8%CeO 2+0.4%MnO
B:92.4%Al 2O 3+0.1%Co 2O 3+3.5%MnO+2.5%Cr 2O 3+0.3%SiO 2+1.5%TiO 2
Press mass ratio in above-mentioned A, B two components mixes at 5.5: 4.5.
Another technical scheme is that described material contains A, B two components and content (mass ratio) and is:
A:57.4%SrO+40.7%TiO 2+0.7%Nb 2O 5+0.8%CeO 2+0.4%MnO
B:92.4%Al 2O 3+0.1%Co 2O 3+3.5%MnO+2.5%Cr 2O 3+0.3%SiO 2+1.5%TiO 2
Press mass ratio in above-mentioned A, B two components mixes at 6: 4.
Prepare the method for described low-pressure pressure-sensitive ceramic material, comprise batch mixing, ball milling, drying, granulation, compression moulding is characterized in that, described batch mixing is to contain A, B two components and content to be by mass percentage:
A、57.4%SrO+40.7%TiO 2+0.7%Nb 2O 5+0.8%CeO 2+0.4%MnO
B、92.4%Al 2O 3+0.1%Co 2O 3+3.5%MnO+2.5%Cr 2O 3+0.3%SiO 2+1.5%TiO 2
According to A, B two constituent masses ratio is that 4: 6~6: 4 ratio takes by weighing above-mentioned analytical reagent, mix, be prepared into sample by abovementioned steps, be placed in the Vacuum graphite oven in 1305~1500 ℃ of following sintering, furnace cooling or be incubated 1~3h after furnace cooling, the sample that burns till top electrode after surface treatment is cleaned makes described pressure-sensitive ceramic material.
Concrete preparation method's step is as follows:
1, be that 4: 6~6: 4 ratio takes by weighing above-mentioned analytical reagent according to A, B two constituent masses ratio, mix back ball milling 2~4h in planetary ball mill,
It is 2, first that suppressing thickness with TDP-1.5 one-shot shaper after the 200 purpose sieve granulations excessively is the sample of 1~2mm disc with the dry 6~8h in loft drier of the batch mixing behind the ball milling,
3, sample is placed in the Vacuum graphite oven at 1305~1500 ℃ of sintering, furnace cooling or be incubated 1~3h after furnace cooling, the sample that burns till top electrode after surface treatment is cleaned promptly obtains described pressure-sensitive ceramic material.
4, under 1000Hz, test room temperature electric capacity with 2693C type LCR digital electric bridge, and calculate specific inductivity.With TH2687C type leakage current tester, the pressure sensitive voltage of test gained pressure-sensitive ceramic material calculates nonlinear factor.
The present invention has the following advantages and active effect:
1, sintering temperature is wide, and production technique is simple, and is safe and reliable.
2, can produce specific inductivity under this technology is that electric capacity is C=0.02~22 μ F, ε=1.7 * 10 5~1.5 * 10 8, pressure sensitive voltage is U 1mA=0.6~6.3V, U 10mA=1.8~11.6V, nonlinear factor are the pressure-sensitive ceramic material of a=2.1~5.1.
Four, embodiment
Embodiment 1
The component of described material and content mass ratio are:
A、57.4%SrO+40.7%TiO 2+0.7%Nb 2O 5+0.8%CeO 2+0.4%MnO
B、92.4%Al 2O 3+0.1%Co 2O 3+3.5%MnO+2.5%Cr 2O 3+0.3%SiO 2+1.5%TiO 2
In two groups of constituent mass ratios of A, B is that 4: 6 ratio takes by weighing reagent, batch mixing, through ball milling, drying, granulation, moulding, the sample of moulding is placed on Vacuum graphite oven in 1500 ℃ of sintering, furnace cooling, top electrode after surface treatment is cleaned, the performance perameter of test gained pressure-sensitive ceramic material: capacitor C is 0.8 μ F, and DIELECTRIC CONSTANT is 9.9 * 10 6, pressure sensitive voltage U 1mA=0.6V, U 10mA=1.8V, nonlinear factor a=2.1.
Embodiment 2
The component of described material and content mass ratio are:
A、57.4%SrO+40.7%TiO 2+0.7%Nb 2O 5+0.8%CeO 2+0.4%MnO
B、92.4%Al 2O 3+0.1%Co 2O 3+3.5%MnO+2.5%Cr 2O 3+0.3%SiO 2+1.5%TiO 2
In two groups of constituent mass ratios of A, B is that 4: 6 ratio takes by weighing reagent, batch mixing, through ball milling, drying, granulation, moulding, the sample of moulding is placed on Vacuum graphite oven in 1350 ℃ of sintering, furnace cooling behind the insulation 2h, top electrode after surface treatment is cleaned, the performance perameter of test gained pressure-sensitive ceramic material: capacitor C is 22 μ F, and DIELECTRIC CONSTANT is 1.5 * 10 8, pressure sensitive voltage U 1mA=6.3V, U 10mA=11.6V, nonlinear factor a=3.8.
Embodiment 3
Another component and the content mass ratio of described material are:
A、57.4%SrO+40.7%TiO 2+0.7%Nb 2O 5+0.8%CeO 2+0.4%MnO
B、92.4%Al 2O 3+0.1%Co 2O 3+3.5%MnO+2.5%Cr 2O 3+0.3%SiO 2+1.5%TiO 2
In two groups of constituent mass ratios of A, B is that 5.5: 4.5 ratio takes by weighing reagent, batch mixing, through ball milling, drying, granulation, moulding, the sample of moulding is placed on Vacuum graphite oven in 1320 ℃ of sintering, furnace cooling behind the insulation 3h, top electrode after surface treatment is cleaned, the performance perameter of test gained pressure-sensitive ceramic material: capacitor C is 0.05 μ F, and DIELECTRIC CONSTANT is 6.1 * 10 5, pressure sensitive voltage U 1mA=2.8V, U 10mA=4.4V, nonlinear factor a=5.1.
Embodiment 4
Another component and the content mass ratio of described material are:
A、57.4%SrO+40.7%TiO 2+0.7%Nb 2O 5+0.8%CeO 2+0.4%MnO
B、92.4%Al 2O 3+0.1%Co 2O 3+3.5%MnO+2.5%Cr 2O 3+0.3%SiO 2+1.5%TiO 2
In two groups of constituent mass ratios of A, B is that 5: 5 ratio takes by weighing reagent, batch mixing, through ball milling, drying, granulation, moulding, the sample of moulding is placed on Vacuum graphite oven in 1305 ℃ of sintering, furnace cooling, top electrode after surface treatment is cleaned, the performance perameter of test gained pressure-sensitive ceramic material: capacitor C is 0.09 μ F, and DIELECTRIC CONSTANT is 6.3 * 10 5, pressure sensitive voltage U 1mA=4.9V, U 10mA=8.5V, nonlinear factor a=4.2.
Embodiment 5
Another component and the content mass ratio of described material are:
A、57.4%SrO+40.7%TiO 2+0.7%Nb 2O 5+0.8%CeO 2+0.4%MnO
B、92.4%Al 2O 3+0.1%Co 2O 3+3.5%MnO+2.5%Cr 2O 3+0.3%SiO 2+1.5%TiO 2
In two groups of constituent mass ratios of A, B is that 4: 6 ratio takes by weighing reagent, batch mixing, through ball milling, drying, granulation, moulding, the sample of moulding is placed on Vacuum graphite oven in 1335 ℃ of sintering, furnace cooling behind the insulation 1h, top electrode after surface treatment is cleaned, the performance perameter of test gained pressure-sensitive ceramic material: capacitor C is 0.02 μ F, and DIELECTRIC CONSTANT is 1.7 * 10 5, pressure sensitive voltage U 1mA=4.8V, U 10mA=9.7V, nonlinear factor a=3.3.
Embodiment 6
Another component and the content mass ratio of described material are:
A、57.4%SrO+40.7%TiO 2+0.7%Nb 2O 5+0.8%CeO 2+0.4%MnO
B、92.4%Al 2O 3+0.1%Co 2O 3+3.5%MnO+2.5%Cr 2O 3+0.3%SiO 2+1.5%TiO 2
In two groups of constituent mass ratios of A, B is that 5: 5 ratio takes by weighing reagent, batch mixing, through ball milling, drying, granulation, moulding, the sample of moulding is placed on Vacuum graphite oven in 1500 ℃ of sintering, furnace cooling, top electrode after surface treatment is cleaned, the performance perameter of test gained pressure-sensitive ceramic material: capacitor C is 1.6 μ F, and DIELECTRIC CONSTANT is 1.2 * 10 7, pressure sensitive voltage U 1mA=2.3V, U 10mA=3.8V, nonlinear factor a=4.6.

Claims (6)

1, a kind of low-pressure pressure-sensitive ceramic material is characterized in that, described material contains A, B two components and content and is by mass percentage:
A、57.4%SrO+40.7%TiO 2+0.7%Nb 2O 5+0.8%CeO 2+0.4%MnO
B、92.4%Al 2O 3+0.1%Co 2O 3+3.5%MnO+2.5%Cr 2O 3+0.3%SiO 2+1.5%TiO 2
Above-mentioned A, B two components are pressed mass ratio mixed in 4: 6~6: 4.
2, low-pressure pressure-sensitive ceramic material according to claim 1 is characterized in that, described material contains A, B two components and content and is by mass percentage:
A、57.4%SrO+40.7%TiO 2+0.7%Nb 2O 5+0.8%CeO 2+0.4%MnO
B、92.4%Al 2O 3+0.1%Co 2O 3+3.5%MnO+2.5%Cr 2O 3+0.3%SiO 2+1.5%TiO 2
Above-mentioned A, B two components are pressed mass ratio mixes at 4: 6
3, low-pressure pressure-sensitive ceramic material according to claim 1 is characterized in that, described material contains A, B two components and content and is by mass percentage:
A:57.4%SrO+40.7%TiO 2+0.7%Nb 2O 5+0.8%CeO 2+0.4%MnO
B:92.4%Al 2O 3+0.1%Co 2O 3+3.5%MnO+2.5%Cr 2O 3+0.3%SiO 2+1.5%TiO 2
Press mass ratio at above-mentioned A, B composition mixes at 5: 5.
4, low-pressure pressure-sensitive ceramic material according to claim 1 is characterized in that, described material contains A, B two components and content by mass percentage by being:
A:57.4%SrO+40.7%TiO 2+0.7%Nb 2O 5+0.8%CeO 2+0.4%MnO
B:92.4%Al 2O 3+0.1%Co 2O 3+3.5%MnO+2.5%Cr 2O 3+0.3%SiO 2+1.5%TiO 2
Press mass ratio in above-mentioned A, B two components mixes at 5.5: 4.5.
5, low-pressure pressure-sensitive ceramic material according to claim 1 is characterized in that, described material contains A, B two components and content and is by mass percentage:
A:57.4%SrO+40.7%TiO 2+0.7%Nb 2O 5+0.8%CeO 2+0.4%MnO
B:92.4%Al 2O 3+0.1%Co 2O 3+3.5%MnO+2.5%Cr 2O 3+0.3%SiO 2+1.5%TiO 2
Press mass ratio in above-mentioned A, B two components mixes at 6: 4.
6, prepare the method for the described low-pressure pressure-sensitive ceramic material of claim 1, comprise batch mixing, ball milling, drying, granulation, moulding is characterized in that, described batch mixing is to contain A, B two components and content to be by mass percentage:
A、57.4%SrO+40.7%TiO 2+0.7%Nb 2O 5+0.8%CeO 2+0.4%MnO
B、92.4%Al 2O 3+0.1%Co 2O 3+3.5%MnO+2.5%Cr 2O 3+0.3%SiO 2+1.5%TiO 2
According to A, B two constituent masses ratio is that 4: 6~6: 4 ratio takes by weighing above-mentioned analytical reagent, mix, be prepared into sample by abovementioned steps, be placed in the Vacuum graphite oven in 1305~1500 ℃ of following sintering, furnace cooling or be incubated 1~3h after furnace cooling, the sample that burns till top electrode after surface treatment is cleaned makes described pressure-sensitive ceramic material.
CNA2009101140906A 2009-05-22 2009-05-22 Low-pressure pressure-sensitive ceramic material and preparation method thereof Pending CN101555130A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112174659A (en) * 2020-10-09 2021-01-05 新昌中国计量大学企业创新研究院有限公司 Strontium titanate piezoresistor and preparation method thereof
CN112321296A (en) * 2020-10-23 2021-02-05 中国科学院上海硅酸盐研究所 Bismuth-free zinc oxide piezoresistor ceramic chip and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112174659A (en) * 2020-10-09 2021-01-05 新昌中国计量大学企业创新研究院有限公司 Strontium titanate piezoresistor and preparation method thereof
CN112321296A (en) * 2020-10-23 2021-02-05 中国科学院上海硅酸盐研究所 Bismuth-free zinc oxide piezoresistor ceramic chip and preparation method thereof

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Open date: 20091014