CN106548840A - A kind of lamination sheet type zno varistor and preparation method thereof - Google Patents
A kind of lamination sheet type zno varistor and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of lamination sheet type zno varistor and preparation method thereof.Piezoresistor is generated by ceramics and Ni electrodes alternatively laminated, and two ends scribble termination electrode；The ceramics is by ZnO, Bi2O3, the oxide of Mn and Co, and BN compositions, wherein, the molar fraction of ZnO is 93%～98.7%, Bi2O3Molar fraction for 0.2%～5%, Mn and Co oxide molar fraction be 0.01%～5%, BN molar fraction be 0.1%～6%.The present invention while Ni anodizings can be prevented, and effectively suppresses ZnO and other additives to be reduced in reducing atmosphere using base metal Ni as interior electrode, promote ZnO in sintering process into porcelain, piezoresistor possesses good non-linear, low manufacture cost, is suitable to large-scale production.
Description
Technical field
The invention belongs to electrode component technical field, more particularly, to a kind of lamination sheet type
Zno varistor and preparation method thereof.
Background technology
Zno varistor has superior nonlinear characteristic (non-linear I-V characteristic), extensive
For voltage stabilizing and overvoltage protection.Multilayer chip ZnO varistor is developed first by Schohara et al.
Come, just obtained extensive concern.The generation of multilayer chip ZnO varistor, primarily to energy
Enough suitable for the small-sized electronic product of low pressure range.As multilayer chip ZnO varistor is typically in sky
Higher temperature sintering (being higher than 1000 DEG C) in gas, within institute, electrode uses high-melting-point and resistance to oxidation
Platinum (Pt) or silver-colored (Ag)/palladium (Pd) alloy.With the reduction of thickness, the increase of the number of plies is interior
The shared proportion in lamination sheet type low voltage varistor of electrode material is increasing, account for totle drilling cost
More than 50%.Additionally, ZnO-Bi2O3Bi in based material2O3Component highly volatile in sintering process,
And the Pd easily and in electrode material reacts, device performance is reduced.Many researcheres and manufacturer
The co-fired temperature of ceramic body and interior electrode is reduced in research all, so that oxidation resistance temperature is relatively low and price
Relatively low fine silver (Ag), copper (Cu) are replacing electrode in current Ag/Pd.
It is compatible with the common burning of ZnO voltage-sensitive ceramics that Lavrov etc. realizes Cu using electrodeposition process, but makes
Preparation Method is extremely complex；Changzhou Hylink Technology Co., Ltd. was disclosed with regard to using pure Ag in 2011
Electrode substitutes the patent that Ag/Pd prepares zinc oxide varistor, but Ag electrode costs are still higher.Japan
The companies such as TDK, Panasonic propose to adopt SrTiO3Material system, with base metal as interior electrode, adopts
The preparation method that reduction is reoxidized realizes the lamination type piezoresistor of base-metal inner-electrode, but which is difficult
It is SrTiO with the defect for overcoming3The nonlinear factor very low (less than 10) of material system varistor,
Limit the application of varistor.
The content of the invention
For the disadvantages described above or Improvement requirement of prior art, the invention provides a kind of lamination sheet type
Zno varistor and preparation method thereof, using base metal Ni as interior electrode, while can prevent
Ni anodizings, and effectively suppress ZnO and other additives to be reduced in reducing atmosphere, promote
Into porcelain in sintering process, piezoresistor possesses good non-linear, low manufacture cost to ZnO, fits
In large-scale production.
For achieving the above object, according to one aspect of the present invention, there is provided a kind of lamination sheet type ZnO
Piezoresistor, it is characterised in that generated by ceramics and Ni electrodes alternatively laminated, two ends scribble end electricity
Pole；The ceramics is by ZnO, Bi2O3, the oxide of Mn and Co, and BN compositions, wherein,
The molar fraction of ZnO is 93%～98.7%, Bi2O3Molar fraction be 0.2%～5%, Mn and Co
Oxide molar fraction be 0.01%～5%, BN molar fraction be 0.1%～6%.
Preferably, by by the structure of ceramics and Ni electrode alternatively laminateds in noble gases or noble gases
With 850 DEG C in the mixed gas of hydrogen～1150 DEG C at sinter after, coat termination electrode, then in oxygen or sky
It is thermally treated resulting at 500 DEG C～800 DEG C in gas.
Preferably, the oxide of Al and/or Nb is mixed in the ceramics, adds total amount to be less than institute
State the 4mol% of ceramics.
Preferably, incorporation Cr, Sb, Si and V a kind of at least within oxide in the ceramics,
Add 8mol% of the total amount less than the ceramics.
It is another aspect of this invention to provide that there is provided a kind of preparation of lamination sheet type zno varistor
Method, it is characterised in that comprise the steps：(1) to by ZnO, Bi2O3, Mn's and Co
Deionized water is added to carry out ball milling in the mixture of oxide and BN compositions, by the drying of gained slurry, mistake
Sieve obtains powder body；In mixture, the molar fraction of ZnO is 93%～98.7%, Bi2O3Molar fraction
Oxide molar fraction for 0.2%～5%, Mn and Co is the molar fraction of 0.01%～5%, BN
For 0.1%～6%；(2) addition dispersant, defoamer, solvent and binding agent, Ran Houqiu in powder body
Mill mixing, obtains casting slurry；(3) casting slurry flow casting molding is obtained into base substrate, and with base metal
Ni obtains molded samples as interior electrode, lamination, tabletting and section；(4) by molded samples lazy
Property gas or noble gases and hydrogen mixed gas in sinter at 850 DEG C～1150 DEG C, obtain chip pottery
Porcelain resistance；(5) after two terminations of chip ceramic resistor are electrode coated, in oxygen or air
Heat treatment at 500 DEG C～800 DEG C, obtains lamination sheet type zno varistor.
Preferably, the oxygen of Al and/or Nb in the step (1), is added also in the mixture
Compound, adds 4mol% of the total amount less than the mixture.
Preferably, in the step (1), Cr, Sb, Si and V are added also in the mixture
Oxide a kind of at least within, adds 8mol% of the total amount less than the mixture.
In general, by the contemplated above technical scheme of the present invention compared with prior art, have
Following beneficial effect：
1st, sintering atmosphere adds hydrogen on the basis of noble gases, is conducive to protecting Ni electrodes, prevents
Stop its oxidation, while BN is added in composition of raw materials, can effectively suppress ZnO and other additives to exist
It is reduced in reducing atmosphere.
2nd, sintering is completed in noble gases, while adding BN in zno-based bottom, can effectively facilitate
ZnO is in sintering process into porcelain.
3rd, sintering is completed in the mixed gas of noble gases or noble gases and hydrogen first, then in sky
Carry out heat treatment in gas at a lower temperature, possess piezoresistor good non-linear：In protection
The piezoresistor nonlinear factor reoxidized after sintering in atmosphere reaches as high as more than 40, pressure sensitive voltage
Minimum to be smaller than 15V, leakage current is in μ A ranks；The varistor reoxidized after sintering in reducing atmosphere
The nonlinear factor of device can reach more than 20, and pressure sensitive voltage is minimum to be smaller than 20V, and leakage current is in μ A
Rank.
4th, using base metal Ni as interior electrode, replace the precious metal materials such as Ag, Pd, significantly can drop
The preparation cost of low stacking slice type piezoresistor, using solid-phase sintering method, holds burning infiltration and the porcelain of silver
Body oxidation is disposably completed, and is suitable to large-scale production.
Description of the drawings
Fig. 1 is the structural representation of the lamination sheet type zno varistor of the embodiment of the present invention；
Fig. 2 is the preparation method flow chart of the lamination sheet type zno varistor of the embodiment of the present invention.
In all of the figs, identical reference be used for represent identical element or structure, wherein：
1-Ni electrodes, 2- ceramics, 3- termination electrodes.
Specific embodiment
In order that the objects, technical solutions and advantages of the present invention become more apparent, below in conjunction with accompanying drawing
And embodiment, the present invention will be described in further detail.It should be appreciated that described herein concrete
Embodiment only to explain the present invention, is not intended to limit the present invention.Additionally, disclosed below
Can as long as the technical characteristic involved by each embodiment of the invention does not constitute conflict each other
To be mutually combined.
As shown in figure 1, the lamination sheet type zno varistor of the embodiment of the present invention is by ceramics 2 and Ni
Electrode alternatively laminated is generated, and two ends scribble termination electrode 3.Ceramics 2 is by ZnO, Bi2O3, Mn and Co
Oxide, and BN constitutes, wherein, the molar fraction of ZnO is 93%～98.7%, Bi2O3
Molar fraction be 0.01%～5% for the molar fraction of oxide of 0.2%～5%, Mn and Co,
The molar fraction of BN is 0.1%～6%.
Above-mentioned zno varistor by by the structure of ceramics 2 and Ni electrode alternatively laminateds in indifferent gas
After sintering at 850 DEG C～1150 DEG C in the mixed gas of body or noble gases and hydrogen, termination electrode 3 is coated,
It is thermally treated resulting at 500 DEG C～800 DEG C in oxygen or air again.
As shown in Fig. 2 the preparation method bag of the lamination sheet type zno varistor of the embodiment of the present invention
Include following steps：
(1) to by Zinc Oxide (ZnO), bismuth oxide (Bi2O3), manganese (Mn) and cobalt (Co)
Oxide and the mixture that constitutes of boron nitride (BN) in plus deionized water carry out ball milling, by gained
Slurry is dried, sieving obtains powder body；In mixture, the molar fraction of ZnO is 93%～98.7%, Bi2O3
Molar fraction be 0.01%～5%, BN for the oxide molar fraction of 0.2%～5%, Mn and Co
Molar fraction be 0.1%～6%.
(2) dispersant, defoamer, solvent and binding agent are added in powder body, then ball milling mixing,
Obtain casting slurry；
(3) casting slurry flow casting molding is obtained into base substrate, and using base metal nickel (Ni) as interior electrode,
Lamination, tabletting and section, obtain molded samples；
(4) by molded samples in the mixed gas of noble gases or noble gases and hydrogen
Sinter at 850 DEG C～1150 DEG C, obtain chip ceramic resistor；
(5) after silver-colored (Ag) electrode of two termination coatings of chip ceramic resistor, in oxygen or air
In heat treatment at 500 DEG C～800 DEG C, obtain lamination sheet type zno varistor.
In another embodiment of the present invention, also in the mixture of step (1) add Al and/or
The oxide of Nb, adds 4mol% of the total amount less than mixture.
In another embodiment of the present invention, also in the mixture of step (1) add Cr, Sb,
Si and V a kind of at least within oxide, adds 8mol% of the total amount less than mixture.
ZnO is the bulk composition in this formula, Bi2O3It is the forming agent of voltage-dependent characteristic, the addition of BN
It is reduced when can be sintered with suppression formulation component under reducing atmosphere, and promotes ZnO in sintering process
Into porcelain.The oxide for adding Al, Nb, Cr, Sb, Si and V a kind of at least within, can improve pressure-sensitive
Non-linear, the reduction leakage current of resistor, improves stability, improves aging characteristics.
Embodiment 1
(1) to by Zinc Oxide (ZnO), bismuth oxide (Bi2O3), manganese (Mn) and cobalt (Co)
Oxide and the mixture that constitutes of boron nitride (BN) in plus deionized water carry out ball milling, by gained
Slurry carries out drying, sieving obtains powder body；In mixture, the molar fraction of ZnO is 98.7%, Bi2O3
Molar fraction for 0.2%, Mn and Co oxide molar fraction be 0.5%, BN mole
Fraction is 0.1%.
(2) dispersant, defoamer, solvent and binding agent are added in powder body, then ball milling mixing,
Obtain casting slurry；
(3) casting slurry flow casting molding is obtained into base substrate, and using base metal nickel (Ni) as interior electrode,
Lamination, tabletting and section, obtain molded samples；
(4) by molded samples 1100 DEG C in the mixed gas of nitrogen or nitrogen and hydrogen at sinter, obtain
To chip ceramic resistor；
(5) after silver-colored (Ag) electrode of two termination coatings of chip ceramic resistor, 700 DEG C in atmosphere
Lower heat treatment, obtains lamination sheet type zno varistor.
Embodiment 2
(1) to by Zinc Oxide (ZnO), bismuth oxide (Bi2O3), manganese (Mn) and cobalt (Co)
Oxide and the mixture that constitutes of boron nitride (BN) in plus deionized water carry out ball milling, by gained
Slurry carries out drying, sieving obtains powder body；In mixture, the molar fraction of ZnO is 95.78%, Bi2O3
Molar fraction for 0.2%, Mn and Co oxide molar fraction be 0.01%, BN mole
Fraction is 4%.
(2) dispersant, defoamer, solvent and binding agent are added in powder body, then ball milling mixing,
Obtain casting slurry；
(3) casting slurry flow casting molding is obtained into base substrate, and using base metal nickel (Ni) as interior electrode,
Lamination, tabletting and section, obtain molded samples；
(4) by molded samples 1100 DEG C in the mixed gas of nitrogen or nitrogen and hydrogen at sinter, obtain
To chip ceramic resistor；
(5) after silver-colored (Ag) electrode of two termination coatings of chip ceramic resistor, 700 DEG C in atmosphere
Lower heat treatment, obtains lamination sheet type zno varistor.
Embodiment 3
(1) to by Zinc Oxide (ZnO), bismuth oxide (Bi2O3), manganese (Mn) and cobalt (Co)
Oxide and the mixture that constitutes of boron nitride (BN) in plus deionized water carry out ball milling, by gained
Slurry carries out drying, sieving obtains powder body；In mixture, the molar fraction of ZnO is 93%, Bi2O3
Molar fraction for 0.5%, Mn and Co oxide molar fraction be 0.25%, BN mole
Fraction is 6%.
(2) dispersant, defoamer, solvent and binding agent are added in powder body, then ball milling mixing,
Obtain casting slurry；
(3) casting slurry flow casting molding is obtained into base substrate, and using base metal nickel (Ni) as interior electrode,
Lamination, tabletting and section, obtain molded samples；
(4) by molded samples 1100 DEG C in the mixed gas of nitrogen or nitrogen and hydrogen at sinter, obtain
To chip ceramic resistor；
(5) after silver-colored (Ag) electrode of two termination coatings of chip ceramic resistor, 700 DEG C in atmosphere
Lower heat treatment, obtains lamination sheet type zno varistor.
Embodiment 4
(1) to by Zinc Oxide (ZnO), bismuth oxide (Bi2O3), manganese (Mn) and cobalt (Co)
Oxide and the mixture that constitutes of boron nitride (BN) in plus deionized water carry out ball milling, by gained
Slurry carries out drying, sieving obtains powder body；In mixture, the molar fraction of ZnO is 93%, Bi2O3
Molar fraction for 5%, Mn and Co oxide molar fraction be 0.5%, BN mole point
Number is 1%.
(2) dispersant, defoamer, solvent and binding agent are added in powder body, then ball milling mixing,
Obtain casting slurry；
(3) casting slurry flow casting molding is obtained into base substrate, and using base metal nickel (Ni) as interior electrode,
Lamination, tabletting and section, obtain molded samples；
(4) by molded samples 1150 DEG C in the mixed gas of nitrogen or nitrogen and hydrogen at sinter, obtain
To chip ceramic resistor；
(5) after silver-colored (Ag) electrode of two termination coatings of chip ceramic resistor, 800 DEG C in oxygen
Lower heat treatment, obtains lamination sheet type zno varistor.
Embodiment 5
(1) to by Zinc Oxide (ZnO), bismuth oxide (Bi2O3), manganese (Mn) and cobalt (Co)
Oxide and the mixture that constitutes of boron nitride (BN) in plus deionized water carry out ball milling, by gained
Slurry carries out drying, sieving obtains powder body；In mixture, the molar fraction of ZnO is 93%, Bi2O3
Molar fraction for 5%, Mn and Co oxide molar fraction be 0.5%, BN mole point
Number is 1%.
(2) dispersant, defoamer, solvent and binding agent are added in powder body, then ball milling mixing,
Obtain casting slurry；
(3) casting slurry flow casting molding is obtained into base substrate, and using base metal nickel (Ni) as interior electrode,
Lamination, tabletting and section, obtain molded samples；
(4) by molded samples 850 DEG C in the mixed gas of nitrogen or nitrogen and hydrogen at sinter, obtain
To chip ceramic resistor；
(5) after silver-colored (Ag) electrode of two termination coatings of chip ceramic resistor, 500 DEG C in oxygen
Lower heat treatment, obtains lamination sheet type zno varistor.
Electric performance test is carried out to lamination sheet type zno varistor obtained in embodiment 1～3, as a result
It is as shown in the table.
Data display in table, when addition BN amounts are 4mol%, the properties of varistor reach most
It is good, in N2The non-linear resistance reoxidized after middle sintering reaches 41, pressure sensitive voltage as little as 12V, and leaks
Electric current as little as 12 μ A；In N2-H2The resistor non-linear up to 27 reoxidized after sintering in gaseous mixture,
Pressure sensitive voltage as little as 18V, leakage current are 18 μ A.When BN additions very few (0.1mol%) or mistake
When many (6mol%), there is certain infringement to voltage-dependent characteristic, but still possess preferable pressure-sensitive character.
It can be seen that, the stacking slice type piezoresistor prepared using the formula and technique of the present invention possesses good
Pressure-sensitive character.
As it will be easily appreciated by one skilled in the art that presently preferred embodiments of the present invention is the foregoing is only,
Not to limit the present invention, all any modifications made within the spirit and principles in the present invention, etc.
With replacement and improvement etc., should be included within the scope of the present invention.
Claims (7)
1. a kind of lamination sheet type zno varistor, it is characterised in that handed over by ceramics and Ni electrodes
Generate for lamination, two ends scribble termination electrode；The ceramics is by ZnO, Bi2O3, the oxidation of Mn and Co
Thing, and BN compositions, wherein, the molar fraction of ZnO is 93%～98.7%, Bi2O3Mole point
Number for 0.2%～5%, Mn and Co oxides molar fraction be 0.01%～5%, BN mole
Fraction is 0.1%～6%.
2. lamination sheet type zno varistor as claimed in claim 1, it is characterised in that pass through
By the structure of ceramics and Ni electrode alternatively laminateds in noble gases or the mixed gas of noble gases and hydrogen
In sinter at 850 DEG C～1150 DEG C after, coat termination electrode, then 500 DEG C～800 DEG C in oxygen or air
Under be thermally treated resulting in.
3. lamination sheet type zno varistor as claimed in claim 1 or 2, it is characterised in that
The oxide of Al and/or Nb is mixed in the ceramics, total amount is added less than the ceramics
4mol%.
4. lamination sheet type zno varistor as claimed in claim 1 or 2, it is characterised in that
Cr, Sb, Si and V oxide a kind of at least within is mixed in the ceramics, adds total amount not surpass
Cross the 8mol% of the ceramics.
5. a kind of preparation method of lamination sheet type zno varistor, it is characterised in that including as follows
Step：
(1) to by ZnO, Bi2O3, in the mixture that the oxide of Mn and Co and BN are constituted
Plus deionized water carries out ball milling, by the drying of gained slurry, sieving obtains powder body；In mixture, ZnO
Molar fraction be 93%～98.7%, Bi2O3Molar fraction for 0.2%～5%, Mn and Co oxygen
It is 0.1%～6% that compound molar fraction is the molar fraction of 0.01%～5%, BN；
(2) dispersant, defoamer, solvent and binding agent are added in powder body, then ball milling mixing,
Obtain casting slurry；
(3) casting slurry flow casting molding is obtained into base substrate, and using base metal Ni as interior electrode, is folded
Layer, tabletting and section, obtain molded samples；
(4) by molded samples in the mixed gas of noble gases or noble gases and hydrogen
Sinter at 850 DEG C～1150 DEG C, obtain chip ceramic resistor；
(5) after two terminations of chip ceramic resistor are electrode coated, in oxygen or air
Heat treatment at 500 DEG C～800 DEG C, obtains lamination sheet type zno varistor.
6. the preparation method of lamination sheet type zno varistor as claimed in claim 5, its feature
It is that the oxide of Al and/or Nb in the step (1), is added also in the mixture,
Add 4mol% of the total amount less than the mixture.
7. the preparation method of the lamination sheet type zno varistor as described in claim 5 or 6, its
Be characterised by, in the step (1), Cr, Sb, Si and V are added extremely also in the mixture
The oxide of few one of which, adds 8mol% of the total amount less than the mixture.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109867519A (en) * | 2019-04-25 | 2019-06-11 | 重庆大学 | A kind of high-potential gradient ZnO voltage-sensitive ceramic and preparation method thereof |
| CN116354732A (en) * | 2023-04-19 | 2023-06-30 | 贵州大学 | Sintering method of ZnO pressure-sensitive ceramic with high density and high electrical property |
| CN117198769A (en) * | 2023-08-30 | 2023-12-08 | 深圳市嘉容微电子有限公司 | Laminated electronic component, manufacturing method thereof and driving circuit |
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| CN103632784A (en) * | 2013-11-23 | 2014-03-12 | 华中科技大学 | Lamination sheet-type heat and pressure sensitive composite resistor and preparation method thereof |
| CN104658727A (en) * | 2013-11-22 | 2015-05-27 | 华中科技大学 | Base metal inner-electrode multilayer chip ZnO varistor and preparation method thereof |
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| CN109867519A (en) * | 2019-04-25 | 2019-06-11 | 重庆大学 | A kind of high-potential gradient ZnO voltage-sensitive ceramic and preparation method thereof |
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| CN116354732A (en) * | 2023-04-19 | 2023-06-30 | 贵州大学 | Sintering method of ZnO pressure-sensitive ceramic with high density and high electrical property |
| CN117198769A (en) * | 2023-08-30 | 2023-12-08 | 深圳市嘉容微电子有限公司 | Laminated electronic component, manufacturing method thereof and driving circuit |
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