CN109796202A - A kind of high-performance low-temperature sintered lamination type piezoresistor material - Google Patents
A kind of high-performance low-temperature sintered lamination type piezoresistor material Download PDFInfo
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- CN109796202A CN109796202A CN201910227097.2A CN201910227097A CN109796202A CN 109796202 A CN109796202 A CN 109796202A CN 201910227097 A CN201910227097 A CN 201910227097A CN 109796202 A CN109796202 A CN 109796202A
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Abstract
The present invention relates to a kind of high stability low-temperature sintering lamination type piezoresistor materials, belong to technical field of electronic materials.The present invention is to ZnO-Bi2O3Base low-temperature sintered piezoresistive material, passes through Ta2O5With the addition of BBSZ glass, mass transport process is accelerated using liquid phase sintering mechanism, the sintered density of material is further improved, reduces the sintering temperature of material.Thus material passes through slice type piezoresistor prepared by lamination sheet type capacitor manufacturing process, its pressure-sensitive character with high stable, sintering temperature is low (850 DEG C~925 DEG C), nonlinear factor height (>=86.26), leakage current is small, has a good application prospect.
Description
Technical field
The invention belongs to technical field of electronic materials, and in particular to a kind of high-performance low-temperature sintered lamination type piezoresistor
Material.
Background technique
Varistor is a kind of resistance device with nonlinear wind vibration, be mainly used for circuit bear over-voltage when into
Row voltage clamping absorbs extra electric current to protect Sensitive Apparatus.The wherein slice type piezoresistor of laminated construction, because of its size
The advantages that small, fast response time, big energy ability to bear, at the same can satisfy electronic component to planarization, it is integrated with it is micro-
The growth requirement of type is widely used in the fields such as Aeronautics and Astronautics, electric power, mobile communication, automotive electronics, household electrical appliance, tool
There is good development prospect.
Currently, the inorganic material for manufacturing lamination type piezoresistor of comparative maturity mainly has ZnO- base, TiO2Base
And SnO2Base voltage sensitive resistor material etc..ZnO- base voltage sensitive resistor material has excellent nonlinear factor (α > 50), small electric leakage
The advantages that stream, performance are stable, preparation process is simple, application is more wide, is mainly used as overvoltage protection, electrostatic protection, absorbs wave
Gush Energy device.TiO2Base voltage sensitive resistor material electric potential gradient is lower, thus (pressure sensitive voltage is in 20V or less) in low-pressure field
There is certain application, but the problems such as that there is nonlinear factors is relatively low, stability is poor, repeatability is bad.SnO2Base is pressure-sensitive
Resistance material electric potential gradient is high, can prepare the varistor of high gradient, but there are raw material valuableness, and the not high (α of nonlinear factor
Generally less than 25) the disadvantages of.
In order to further increase the application of material, many people are to TiO2Base voltage sensitive resistor material and SnO2Base voltage sensitive resistor
Material has carried out study on the modification, such as " the mixing influence of the tantalum to titanium dioxide varistor performance " of Li Changpeng, Gong Yunyun
《TiO2The preparation of base voltage-sensitive ceramic and its doping vario-property research ", " TiO of Li Wenge etc.2Base voltage sensitive resistor material and high compression ring
The preparation method of shape piezoresistor ", " SrCO that CN107555985A, king be self-important to be given etc.3SnO caused by adulterating2Varistor
Size effect ", " SnO of He Jianfeng2The research of piezoresistive material doping vario-property " etc..Research finds Ta2O5In TiO2Base
Piezoresistive material and SnO2Has non-linear I-V response in base voltage sensitive resistor material, so that it be made to generate preferably pressure-sensitive spy
Property, and Ta2O5Doping TiO also can be improved2Base voltage sensitive resistor material densified sintering product, to improve its performance.
But about Ta2O5Adulterate ZnO-Bi2O3Base voltage sensitive resistor material yet there are no report, and the doping vario-property of congeners is more
Using Nb2O5And its it is composite mixed." shadow of (Nb, Mg, the Al) multi-element doping to ZnO pressure sensitive electrical properties of such as Chen Hongcun
Ring ", Nb2O5Doping ZnO- base voltage sensitive resistor material be remarkably improved the barrier height of varistor, improve the non-of varistor
Linearly；In addition Nb2O5Doping can also reduce ZnO grain resistance rate, and control lattice distortion improves ZnO- base voltage sensitive resistor pulse
Electric current tolerance and anti-aging property, such as " Y3+、Nb5+Compound donor doping ZnO voltage-sensitive ceramic and preparation method ",
CN106946561A、《In3+、Nb5+Compound donor doping ZnO voltage-sensitive ceramic and preparation method ", CN106946562A.But this two
The sintering temperature of kind based varistor is all up to 1200 DEG C, and high sintering temperature needs the interior electrode slurry high using palladium content
Material, higher cost, the low-temperature sintering of varistor are conducive to the reduction of cost, and compatible with the casting technique in later period.
At present in terms of the low-temperature sintering for realizing ZnO- base voltage sensitive resistor material, mainly pass through addition low-temperature sintering addition
Agent realizes, such as B2O3、V2O5、Bi2O3Deng.Such as CN1564270A " low-temperature sintering ZnO multilayer chip varistor and its manufacture
Method " a kind of sinter additives are disclosed, mainly by Bi2O3、Sb2O3、B2O3、TiO2Composition；CN03964837A, it is " a kind of pressure-sensitive
Ceramic resistor " mainly pass through while adding V2O5And TiO2To ensure its low-temperature sintering characteristic；Also have through addition frit and drop
Sintering temperature and low, such as " preparation process of the piezoresistive material containing bismuth boron glass ", CN06145925A；Such as " Varistor
Composition and multilayer varistor ", US2018/0099910A1.Although these methods are attained by drop
The purpose of sintering temperature and low, but the electrology characteristic of resistance material is also sacrificed to a certain extent, pressure-sensitive character all need
It further increases.
Summary of the invention
It is bad to solve existing low-temperature sintering lamination type piezoresistor material property for above-mentioned there are problem or deficiency
The problem of, the present invention provides a kind of high-performance low-temperature sintered lamination type piezoresistor materials, in ZnO-Bi2O3The pressure-sensitive electricity of base
Ta is added on resistance material foundation2O5With zinc borosilicate bismuth glass (BBSZ), the boundary barrier potential and densified sintering product of material are improved.
A kind of high-performance low-temperature sintered lamination type piezoresistor material, in ZnO-Bi2O3Base low-temperature sintered varistor material
Ta is added in material2O5With zinc borosilicate bismuth glass (BBSZ), material quantity Ta2O5: BBSZ:ZnO-Bi2O3The molar ratio of base be 0.02~
0.50:0.60~0.88:100.00~100.60.
Wherein ZnO-Bi2O3Base includes Bi2O3、Co3O4、MnCO3、Sb2O3、Cr2O3、MgO、SiO2, material quantity ZnO:Bi2O3:
Co3O4: MnCO3: Sb2O3: Cr2O3: MgO:SiO2Molar ratio be 94.70~95.80:0.58~0.72:0.11~0.19:
0.38~0.58:0.88~2.10:0.24~0.39:0.30~1.10:0.40~0.72.
By above-mentioned raw materials through ball milling mixing, dry, pulverize and sieve that can be prepared by high-performance low-temperature sintered lamination sheet type pressure-sensitive
Resistance material, sintering temperature is low (850 DEG C~925 DEG C), and nonlinear factor height (>=86.26), leakage current is small.
Above-mentioned material is prepared into slice type piezoresistor by lamination sheet type capacitor manufacturing process, i.e., is passed through material
Slurry preparation, be cast, laminate, forming, etc. static pressure, cutting, dumping, sintering, chamfering, spraying, sealing end, plating etc., obtain lamination
Slice type piezoresistor, wherein 50 μm of the diaphragm thickness being cast, hydrostatic pressure 32MPa and pressure maintaining 15min, sintering temperature are
850 DEG C~925 DEG C, heating rate is 1~2 DEG C/min, and soaking time is 4~8h.
Piezoresistive material formula rate of the present invention is rationally, it can be achieved that low-temperature sintering, to ZnO-Bi2O3Base low-temperature sintered pressure
Quick resistance material, passes through Ta2O5Addition, prevent ZnO varistor material grains misgrowth, grain growth more evenly, mentions
High crystal boundary stability, and improve the densified sintering product of material；In addition, Ta ion is adulterated as donor ion, varistor
Boundary barrier potential is improved, and potential barrier thickness narrows, to play the role of improving non-linear, reduction leakage current.BBSZ glass
It is added, mass transport process is accelerated by liquid phase sintering mechanism, the sintered density of material is further improved, reduces material
Sintering temperature.Thus material passes through slice type piezoresistor prepared by lamination sheet type capacitor manufacturing process, has height
Stable pressure-sensitive character, sintering temperature is low (850 DEG C~925 DEG C), and nonlinear factor high (>=86.26), leakage current are small, have
Good application prospect.
In conclusion the present invention is in the ZnO-Bi with low-temperature sintering characteristic2O3Base low-temperature sintered piezoresistive material basis
Upper addition Ta2O5With zinc borosilicate bismuth glass (BBSZ), make piezoresistive material realize low-temperature sintering, and crystallite dimension consistency,
Crystal boundary uniformity, crystal boundary stability and densified sintering product are improved, thus pressure-sensitive to obtain lamination sheet type with high performance
Resistor provides the foundation.
Detailed description of the invention
Fig. 1 is slice type piezoresistor preparation technology flow chart；
Fig. 2 is the slice type piezoresistor cross-sectional scans electromicroscopic photograph of embodiment 1；
Fig. 3 is the slice type piezoresistor cross-sectional scans electromicroscopic photograph of embodiment 2；
Fig. 4 is the slice type piezoresistor cross-sectional scans electromicroscopic photograph of embodiment 3；
Fig. 5 is the slice type piezoresistor cross-sectional scans electromicroscopic photograph of embodiment 4.
Specific embodiment
Embodiment 1:(1) use following raw material constituents and its content preparing materials:
Table 1: 1 formula table of embodiment (unit: mol)
| ZnO | Bi2O3 | Co3O4 | MnCO3 | Sb2O3 | Cr2O3 | MgO | SiO2 | BBSZ | Ta2O5 |
| 95.06 | 0.68 | 0.15 | 0.49 | 1.45 | 0.29 | 1.10 | 0.58 | 0.71 | 0 |
(2) weigh raw material by 1 formula rate of table, by raw material through ball milling mixing, dry, pulverize and sieve obtained high performance low temperature
It is sintered lamination type piezoresistor material, then is prepared into slice type piezoresistor by lamination sheet type capacitor manufacturing process,
I.e. by piezoresistive material through slurry preparation, be cast, laminate, form, etc. static pressure, cutting, dumping, sintering, chamfering, spraying, envelope
End, plating etc., obtain stacking slice type piezoresistor, wherein 50 μm of the diaphragm thickness being cast, hydrostatic pressure 32MPa and pressure maintaining
15min, 915 DEG C of sintering temperature simultaneously keep the temperature natural cooling after 6h.
Embodiment 2:(1) use following raw material constituents and its content preparing materials:
Table 2: 2 formula table of embodiment (unit: mol)
| ZnO | Bi2O3 | Co3O4 | MnCO3 | Sb2O3 | Cr2O3 | MgO | SiO2 | BBSZ | Ta2O5 |
| 95.06 | 0.68 | 0.15 | 0.49 | 1.45 | 0.29 | 1.10 | 0.58 | 0.71 | 0.05 |
(2) weigh raw material by 2 formula rate of table, by raw material through ball milling mixing, dry, pulverize and sieve obtained high performance low temperature
It is sintered lamination type piezoresistor material, then is prepared into slice type piezoresistor by lamination sheet type capacitor manufacturing process,
I.e. by piezoresistive material through slurry preparation, be cast, laminate, form, etc. static pressure, cutting, dumping, sintering, chamfering, spraying, envelope
End, plating etc., obtain stacking slice type piezoresistor, wherein 50 μm of the diaphragm thickness being cast, hydrostatic pressure 32MPa and pressure maintaining
15min, 915 DEG C of sintering temperature simultaneously keep the temperature natural cooling after 6h.
Embodiment 3:(1) use following raw material constituents and its content preparing materials:
Table 3: 3 formula table of embodiment (unit: mol)
| ZnO | Bi2O3 | Co3O4 | MnCO3 | Sb2O3 | Cr2O3 | MgO | SiO2 | BBSZ | Ta2O5 |
| 95.06 | 0.68 | 0.15 | 0.49 | 1.45 | 0.29 | 1.10 | 0.58 | 0.71 | 0.15 |
(2) weigh raw material by 3 formula rate of table, by raw material through ball milling mixing, dry, pulverize and sieve obtained high performance low temperature
It is sintered lamination type piezoresistor material, then is prepared into slice type piezoresistor by lamination sheet type capacitor manufacturing process,
I.e. by piezoresistive material through slurry preparation, be cast, laminate, form, etc. static pressure, cutting, dumping, sintering, chamfering, spraying, envelope
End, plating etc., obtain stacking slice type piezoresistor, wherein 50 μm of the diaphragm thickness being cast, hydrostatic pressure 32MPa and pressure maintaining
15min, 915 DEG C of sintering temperature simultaneously keep the temperature natural cooling after 6h.
Embodiment 4:(1) use following raw material constituents and its content preparing materials:
Table 4: 4 formula table of embodiment (unit: mol)
| ZnO | Bi2O3 | Co3O4 | MnCO3 | Sb2O3 | Cr2O3 | MgO | SiO2 | BBSZ | Ta2O5 |
| 95.06 | 0.68 | 0.15 | 0.49 | 1.45 | 0.29 | 1.10 | 0.58 | 0.71 | 0.25 |
(2) weigh raw material by 4 formula rate of table, by raw material through ball milling mixing, dry, pulverize and sieve obtained high performance low temperature
It is sintered lamination type piezoresistor material, then is prepared into slice type piezoresistor by lamination sheet type capacitor manufacturing process,
I.e. by piezoresistive material through slurry preparation, be cast, laminate, form, etc. static pressure, cutting, dumping, sintering, chamfering, spraying, envelope
End, plating etc., obtain stacking slice type piezoresistor, wherein 50 μm of the diaphragm thickness being cast, hydrostatic pressure 32MPa and pressure maintaining
15min, 915 DEG C of sintering temperature simultaneously keep the temperature natural cooling after 6h.
Product is made to the above various embodiments to test, test result such as table 5:
Table 5: embodiment test result
According to above embodiments data as it can be seen that the present invention is while making piezoresistive material realize low-temperature sintering, and protect
The raising of material various aspects performance is demonstrate,proved, to obtain stacking slice type piezoresistor with high performance.
Claims (3)
1. a kind of high-performance low-temperature sintered lamination type piezoresistor material, it is characterised in that:
In ZnO-Bi2O3Ta is added in base low-temperature sintered piezoresistive material2O5With zinc borosilicate bismuth glass BBSZ, material quantity Ta2O5:
BBSZ:ZnO-Bi2O3The molar ratio of base is 0.02~0.50:0.60~0.88:100.00~100.60；
Wherein ZnO-Bi2O3Base includes Bi2O3、Co3O4、MnCO3、Sb2O3、Cr2O3、MgO、SiO2, material quantity ZnO:Bi2O3:
Co3O4: MnCO3: Sb2O3: Cr2O3: MgO:SiO2Molar ratio be 94.70~95.80:0.58~0.72:0.11~0.19:
0.38~0.58:0.88~2.10:0.24~0.39:0.30~1.10:0.40~0.72；
By above-mentioned raw materials through ball milling mixing, dry, pulverize and sieve and can be prepared by high-performance low-temperature sintered lamination type piezoresistor
Material.
2. a kind of high-performance low-temperature sintered lamination type piezoresistor material, it is characterised in that: sintering temperature is 850 DEG C~925
DEG C, heating rate is 1~2 DEG C/min, and soaking time is 4~8h.
3. a kind of stacking slice type piezoresistor, it is characterised in that:
Prepared using high-performance low-temperature sintered lamination type piezoresistor material as described in claim 1, successively formulated slurry,
Be cast, laminate, forming, etc. static pressure, cutting, dumping, sintering, chamfering, spraying, sealing end, plating, obtain lamination type piezoresistor
Device；50 μm of the diaphragm thickness being wherein cast, hydrostatic pressure 32MPa and pressure maintaining 15min, sintering temperature are 850 DEG C~925 DEG C,
Heating rate is 1~2 DEG C/min, and soaking time is 4~8h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113896523A (en) * | 2021-09-16 | 2022-01-07 | 清华大学深圳国际研究生院 | Pressure-sensitive ceramic material and preparation method and application thereof |
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| CN113896523A (en) * | 2021-09-16 | 2022-01-07 | 清华大学深圳国际研究生院 | Pressure-sensitive ceramic material and preparation method and application thereof |
| CN113896523B (en) * | 2021-09-16 | 2023-01-06 | 清华大学深圳国际研究生院 | Pressure-sensitive ceramic material and preparation method and application thereof |
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