CN103992107B - A kind of low-loss medium material for multilayer ceramic capacitors - Google Patents
A kind of low-loss medium material for multilayer ceramic capacitors Download PDFInfo
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- CN103992107B CN103992107B CN201410174177.3A CN201410174177A CN103992107B CN 103992107 B CN103992107 B CN 103992107B CN 201410174177 A CN201410174177 A CN 201410174177A CN 103992107 B CN103992107 B CN 103992107B
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Abstract
The invention discloses a kind of low-loss medium material for multilayer ceramic capacitors, with BaTiO
3powder is base-material, and on this basis, additional mass percent is the MnCO of 0.4 ~ 0.6%
3; (NiO) of 0.6 ~ 1.8%
1-x(NbO
2.5)
x, wherein x=0.6 ~ 0.8; The CaZrO of 0.5 ~ 3.0%
3and the glass flux of 4 ~ 7%; Described (NiO)
1-x(NbO
2.5)
xcompound is by NiO and Nb
2o
51-x:x/2 in molar ratio, wherein x=0.6 ~ 0.8 is synthesized.The present invention, by the interpolation of manganese carbonate, can effectively improve ceramic micro-structure, and improve the dielectric property of pottery, reduce dielectric loss, room temperature loss value reaches less than 0.5% (tan δ & lt; 0.5%); The present invention has excellent dielectric property: in-55 DEG C ~ 150 DEG C warm areas, and rate of change of capacitance within ± 15%, and has higher room temperature dielectric constant (~ 2700).
Description
Technical field
The invention belongs to a kind of take composition as the ceramic composition of feature, is specifically related to a kind of low-loss and X8R type medium material for multilayer ceramic capacitors with temperature stability and preparation method thereof
Background technology
Chip multilayer ceramic capacitor (MultilayerCeramicCapacitor, be called for short MLCC) based on electronic devices and components, except generally using in the products for civilian use such as smart mobile phone, panel computer, radio and television, mobile communication, home computer, household electrical appliance, measuring instrument, Medical Devices and consumer electronics, all have in industries such as Military Electronic Equipment and oil exploration such as Aero-Space, tank electronics, military mobile communication, the control of weapon bullet and military signal monitorings and apply quite widely.Barium titanate (BaTiO
3) base temperature-stable MLCC dielectric material because of its environmental sound, be the focus of research always, use at present maximum be EIAX7R (-55 DEG C ~ 125 DEG C, Δ C/C
25 DEG C≤ ± 15%) dielectric material.Along with the develop rapidly of MLCC, higher requirement has been researched and proposed to MLCC dielectric material, namely in higher temperature environment, stable dielectric property are still kept, as in summer, temperature in automobile engine nacelle can reach more than 130 DEG C, now, X7R type dielectric material is just difficult to meet actual needs.Therefore, and X8R (-55 DEG C ~ 150 DEG C, Δ C/C
25 DEG C≤ ± 15%) development of type MLCC dielectric material, has very important practical significance.
But within the scope of this operation temperature area, though this series ceramic condenser dielectric Capacitance Shift Rate can reach the requirement of X8R, but its room temperature dielectric loss is still more than 1%, affect useful life and the stability of components and parts, restrict its application in some aspects, as low-loss EMI filtering multilayer ceramic capacitor, therefore reduce the loss of ceramic capacitor, become the key promoting capacitor performance.
Summary of the invention
Object of the present invention, though be that the Capacitance Shift Rate of the ceramic capacitor dielectric overcoming prior art can reach the requirement of X8R, but its dielectric loss is still more than 1%, the defect of some special occasions needs can not be adapted to completely, provide a kind of low-loss (tan δ≤0.5%) and intermediate sintering temperature X8R type medium material for multilayer ceramic capacitors with high dielectric constant and preparation method thereof.This
The present invention is achieved by following technical solution.
A kind of low-loss medium material for multilayer ceramic capacitors, with BaTiO
3powder is base-material, and on this basis, additional mass percent is the MnCO of 0.4 ~ 0.6%
3; (NiO) of 0.6 ~ 1.8%
1-x(NbO
2.5)
x, wherein x=0.6 ~ 0.8; The CaZrO of 0.5 ~ 3.0%
3and the glass flux of 4 ~ 7%;
Described (NiO)
1-x(NbO
2.5)
xcompound is by NiO and Nb
2o
51-x:x/2 in molar ratio, wherein x=0.6 ~ 0.8 is synthesized;
Described CaZrO
3by CaCO
3and ZrO
21: 1 synthesis in molar ratio;
Raw material components and the mass percentage content thereof of described glass flux are: the TiO of 17%
2, 34% H
3bO
3, 26% ZnO and 23%Bi
2o
3;
The preparation method of this low-loss medium material for multilayer ceramic capacitors, has following steps:
(1) (NiO) is synthesized
1-x(NbO
2.5)
xcompound, wherein x=0.6 ~ 0.8
By NiO, Nb
2o
51-x:x/2 in molar ratio, wherein prepare burden in x=0.6 ~ 0.8, ball milling 4 hours after raw material mix with deionized water, in 120 DEG C of oven dry, crosses 40 order sub-sieves, in 1000 DEG C of calcinings, then secondary ball milling 6 hours, oven dry, 80 order sub-sieves, obtain (NiO)
1-x(NbO
2.5)
x, wherein x=0.6 ~ 0.8;
(2) CaZrO is synthesized
3
By CaCO
3, ZrO
21:1 batching in molar ratio, ball milling 4 hours after raw material mixes with deionized water, in 120 DEG C of oven dry, crosses 40 order sub-sieves, in 1000 DEG C of calcinings, obtained CaZrO
3;
(3) synthetic glass flux
By mass percentage, by the TiO of 17%
2, 34% H
3bO
3, the ZnO of the 26% and Bi of 23%
2o
3abundant mixing, melting, quenching, levigate, mistake 200 order sub-sieves, obtained glass flux;
(4) with BaTiO
3as base-material, add the composition of following mass percent wherein: the MnCO of 0.4 ~ 0.6%
3, (NiO) of 0.6 ~ 1.8%
1-x(NbO
2.5)
x, wherein x=0.6 ~ 0.8; The CaZrO of 0.5 ~ 3.0%
3with the glass flux of 4 ~ 7%, after being mixed with deionized water by joined raw material, ball milling 4 ~ 8 hours, adds the binding agent that mass percent is 7% after oven dry, crosses 80 order sub-sieve granulations;
(5) the granulation powder of step (4) is pressed into green compact, after binder removal, in 1150 DEG C of sintering, is incubated 3 hours, obtained low-loss medium material for multilayer ceramic capacitors.
Described MnCO
3preferred addition be 0.5wt%.
The green compact of described step (5) are the disk green compact of Ф 15 × 1 ~ 1.3mm.
The green compact of described step (5) were warming up to 550 DEG C of binder removals through 3.5 hours, then rose to 1150 DEG C of sintering through 1 hour, were incubated 3 hours.
Beneficial effect of the present invention is as follows:
1. medium material for multilayer ceramic capacitors of the present invention is by the interpolation of manganese carbonate, effectively can improve ceramic micro-structure, promote the dielectric property of pottery, reduce dielectric loss, room temperature loss value reaches less than 0.5% (tan δ <0.5%);
2. medium material for multilayer ceramic capacitors of the present invention has excellent dielectric property: in-55 DEG C ~ 150 DEG C warm areas, and rate of change of capacitance within ± 15%, and has higher room temperature dielectric constant (~ 2700).
Embodiment
Below with reference to specific embodiment, the present invention is described in further detail.
Embodiment 1
First, 2.2410gNiO and 9.3033gNb of pure level (>=99%) is analyzed with electronic balance weighing
2o
5, mixing, using deionized water as ball-milling medium, ball milling in 120 DEG C of oven dry, was crossed 40 order sub-sieves, is obtained (NiO) in 1000 DEG C of calcinings after 4 hours
0.3(NbO
2.5)
0.7compound, then secondary ball milling 6 hours, in 120 DEG C of oven dry, cross 80 order sub-sieves for subsequent use;
Again by 22.3291gCaCO
3and 27.5114gZrO
2mixing, using deionized water as ball-milling medium, ball milling in 120 DEG C of oven dry, excessively 40 order sub-sieves, in 1000 DEG C of calcinings, obtained CaZrO after 4 hours
3;
Again by 17gTiO
2, 34gH
3bO
3, 26gZnO and 23gBi
2o
3abundant mixing, melting, quenching, levigate, mistake 200 order sub-sieves, obtained glass flux.
By 50gBaTiO
3, 0.25gMnCO
3, 0.45g (NiO)
0.3(NbO
2.5)
0.7, 0.5gCaZrO
3ball milling 4 hours after mixing with deionized water with 2.5g glass flux, after drying, additional mass percent is the paraffin of 7%, crosses 80 order sub-sieve granulations.
Shaping with sintering:
(1) powder after granulation is pressed under 3MPa the disk green compact of Ф 15 × 1.2mm, was warming up to 550 DEG C of binder removals through 3.5 hours, then rose to 1150 DEG C of sintering through 1 hour, be incubated 3 hours, obtained low-loss medium material for multilayer ceramic capacitors.
Evenly apply silver slurry in resulting product upper and lower surface, prepare electrode through 850 DEG C of burning infiltrations, obtained testing sample, test dielectric property and TC characteristic.
The concrete pulp furnish of embodiment 1-5 refers to table 1, and other manufacture craft of embodiment 2-5 is same as embodiment 1.
Table 1
Method of testing of the present invention and checkout equipment as follows:
(1) dielectric property test (AC test signals: frequency is 1kHz, voltage is 1V)
Use capacitance C and the loss tan δ of HEWLETTPACKARD4278A type capacitance tester test sample, and calculate the dielectric constant of sample, computing formula is:
(2) TC characteristic test
GZ-ESPECMPC-710P type high/low temperature circulation incubator, HM27002 type capacitor C-T/V characteristic dedicated tester and HEWLETTPACKARD4278A is utilized to test.Measure the capacitance of sample in warm area-55 DEG C ~ 150 DEG C, adopt following formulae discovery rate of change of capacitance:
The dielectric property of embodiment 1-5 disc-shaped medium material for multilayer ceramic capacitors are in table 2.
Table 2
The present invention is not limited to above-described embodiment, and the change of a lot of details is possible, but therefore this do not run counter to scope and spirit of the present invention.
Claims (4)
1. a low-loss medium material for multilayer ceramic capacitors, with BaTiO
3powder is base-material, and on this basis, additional mass percent is the MnCO of 0.4 ~ 0.6%
3; (NiO) of 0.6 ~ 1.8%
1-x(NbO
2.5)
x, wherein x=0.6 ~ 0.8; The CaZrO of 0.5 ~ 3.0%
3and the glass flux of 4 ~ 7%;
Described (NiO)
1-x(NbO
2.5)
xcompound is by NiO and Nb
2o
51-x:x/2 in molar ratio, wherein x=0.6 ~ 0.8 is synthesized;
Described CaZrO
3by CaCO
3and ZrO
21: 1 synthesis in molar ratio;
Raw material components and the mass percentage content thereof of described glass flux are: the TiO of 17%
2, 34% H
3bO
3, 26% ZnO and 23%Bi
2o
3;
The preparation method of this low-loss medium material for multilayer ceramic capacitors, has following steps:
(1) (NiO) is synthesized
1-x(NbO
2.5)
xcompound, wherein x=0.6 ~ 0.8
By NiO, Nb
2o
51-x:x/2 in molar ratio, wherein prepare burden in x=0.6 ~ 0.8, ball milling 4 hours after raw material mixes with deionized water, in 120 DEG C of oven dry, crosses 40 order sub-sieves, in 1000 DEG C of calcinings, obtained (NiO)
1-x(NbO
2.5)
x, wherein x=0.6 ~ 0.8; Secondary ball milling 6 hours again, dries, crosses 80 order sub-sieves,
(2) CaZrO is synthesized
3
By CaCO
3, ZrO
21:1 batching in molar ratio, ball milling 4 hours after raw material mixes with deionized water, in 120 DEG C of oven dry, crosses 40 order sub-sieves, in 1000 DEG C of calcinings, obtained CaZrO
3;
(3) synthetic glass flux
By mass percentage, by the TiO of 17%
2, 34% H
3bO
3, the ZnO of the 26% and Bi of 23%
2o
3abundant mixing, melting, quenching, levigate, mistake 200 order sub-sieves, obtained glass flux;
(4) with BaTiO
3as base-material, add the composition of following mass percent wherein: the MnCO of 0.4 ~ 0.6%
3, (NiO) of 0.6 ~ 1.8%
1-x(NbO
2.5)
x, wherein x=0.6 ~ 0.8; The CaZrO of 0.5 ~ 3.0%
3with the glass flux of 4 ~ 7%, after being mixed with deionized water by joined raw material, ball milling 4 ~ 8 hours, adds the binding agent that mass percent is 7% after oven dry, crosses 80 order sub-sieve granulations;
(5) the granulation powder of step (4) is pressed into green compact, after binder removal, in 1150 DEG C of sintering, is incubated 3 hours, obtained low-loss medium material for multilayer ceramic capacitors.
2. a kind of low-loss medium material for multilayer ceramic capacitors according to claim 1, is characterized in that, described MnCO
3preferred addition be 0.5wt%.
3. a kind of low-loss medium material for multilayer ceramic capacitors according to claim 1, is characterized in that, the green compact of described step (5) are the disk green compact of Ф 15 × 1 ~ 1.3mm.
4. a kind of low-loss medium material for multilayer ceramic capacitors according to claim 1, is characterized in that, the green compact of described step (5) were warming up to 550 DEG C of binder removals through 3.5 hours, then rose to 1150 DEG C of sintering through 1 hour, was incubated 3 hours.
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|---|---|---|---|
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|---|---|---|---|
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| CN103992107B true CN103992107B (en) | 2015-12-02 |
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| CN105084891A (en) * | 2015-08-05 | 2015-11-25 | 天津大学 | Intermediate-temperature sintering unleaded multilayer ceramic capacitor dielectric material and preparing method thereof |
| CN105016727B (en) * | 2015-08-05 | 2017-08-11 | 天津大学 | The preparation method of high withstand voltage medium material for multilayer ceramic capacitors |
| CN106478092B (en) * | 2015-09-01 | 2019-10-29 | 华北理工大学 | A kind of preparation method of high-intensity high-density calcium zirconate ceramics |
| CN109293353B (en) * | 2018-09-03 | 2021-05-25 | 中国科学院上海硅酸盐研究所 | Lead-free BiFeO with high energy storage density and high energy storage efficiency3Ferroelectric ceramic material and its preparation method |
| CN113248252A (en) * | 2021-06-10 | 2021-08-13 | 天津大学 | Stable dielectric material for MLCC and preparation method thereof |
| CN115141013A (en) * | 2022-07-28 | 2022-10-04 | 电子科技大学 | BaTiO 3 X8R-based ceramic substrate material and preparation method thereof |
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| CN101030478A (en) * | 2007-03-27 | 2007-09-05 | 天津大学 | High-dielectric metal-electric medium composite ceramic capacitance and its production |
| CN101226827A (en) * | 2007-12-28 | 2008-07-23 | 天津大学 | Ultra-high dielectric constant multilayer ceramic capacitor medium and preparation method thereof |
| CN102363579A (en) * | 2011-06-21 | 2012-02-29 | 天津大学 | High performance multilayer ceramic capacitor medium and preparation method thereof |
| CN103553591A (en) * | 2013-10-11 | 2014-02-05 | 山东国瓷功能材料股份有限公司 | Dielectric ceramic material for multilayer ceramic capacitor with high temperature insulation performance |
| CN103601486A (en) * | 2013-11-14 | 2014-02-26 | 天津大学 | Medium-temperature sintered multiplayer ceramic capacitor dielectric material and preparation method thereof |
-
2014
- 2014-04-28 CN CN201410174177.3A patent/CN103992107B/en not_active Expired - Fee Related
Patent Citations (5)
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|---|---|---|---|---|
| CN101030478A (en) * | 2007-03-27 | 2007-09-05 | 天津大学 | High-dielectric metal-electric medium composite ceramic capacitance and its production |
| CN101226827A (en) * | 2007-12-28 | 2008-07-23 | 天津大学 | Ultra-high dielectric constant multilayer ceramic capacitor medium and preparation method thereof |
| CN102363579A (en) * | 2011-06-21 | 2012-02-29 | 天津大学 | High performance multilayer ceramic capacitor medium and preparation method thereof |
| CN103553591A (en) * | 2013-10-11 | 2014-02-05 | 山东国瓷功能材料股份有限公司 | Dielectric ceramic material for multilayer ceramic capacitor with high temperature insulation performance |
| CN103601486A (en) * | 2013-11-14 | 2014-02-26 | 天津大学 | Medium-temperature sintered multiplayer ceramic capacitor dielectric material and preparation method thereof |
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