CN104310999A - Preparation method of low-temperature sintered X8R type ceramic capacitor medium - Google Patents
Preparation method of low-temperature sintered X8R type ceramic capacitor medium Download PDFInfo
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Abstract
The invention discloses a preparation method of a low-temperature sintered X8R type ceramic capacitor medium. The preparation method comprises the following steps: firstly, weighing CoO and Nb2O5 in a weight ratio of 74.7: 265.8 to prepare CoNb2O6; further weighing MnCO3 and Nb2O5 in a weight ratio of 114.9: 265.8 to prepare MnNb2O6; then, burdening Na2CO3, Bi2O3 and TiO2 in a weight ratio of 3:15:10 to prepare Na0.5Bi0.5TiO3 powder; then burdening BaCO3, CuO and B2O3 to prepare BaCuB2O5; based on 100g of BaTiO3, further adding 0.8-2.5g of CoNb2O6, 0.15-0.6g of MnNb2O6, 0.3-0.5g of Na0.5Bi0.5TiO3 and 1-10g of BaCuB2O5 to prepare the powdery material of the ceramic capacitor medium; granulating, compressing into blanks, dewaxing the blanks, sintering at 850-950 DEG C to prepare the X8R type ceramic capacitor medium. The sintering temperature of the ceramic capacitor medium is reduced from 1280 to 900-950 DEG C, the medium is co-fired with a pure silver inner electrode, the dielectric constant epsilon is greater than or equal to 1500, the dielectric loss tg theta is less than or equal to 0.013, and the working temperature ranges from -55 DEG C to 150 DEG C. The ceramic capacitor medium is relatively low in cost and free of harmful substances and has a good application prospect.
Description
Technical field
The invention belongs to a kind of take composition as the ceramic composition of feature, particularly a kind of preparation method of sintering temperature and low barium phthalate base ceramic capacity medium.
Background technology
Chip multilayer ceramic capacitor (Multilayer Ceramic Capacitor, be called for short MLCC) based on electronic devices and components, generally use in the products for civilian use such as smart mobile phone, panel computer, broadcast television, mobile communication, home computer, household electrical appliance, surveying instrument, medical facilities and consumer electronics, the rate of growth with annual 30% becomes the main flow in electrical condenser market.
While the demand of MLCC is continuous ascendant trend, the renewal of electronic product proposes requirements at the higher level to the technology of MLCC and performance.MLCC is to miniaturization, high capacity, cost degradation, the direction development such as highly integrated, and the lamination number of MLCC constantly increases, and the number of plies of interior electrode and ratio also increase thereupon gradually, and the cost of interior electrode directly decides the cost of MLCC.BaTiO
3based material is the dielectric material preparing MLCC widespread use at present, but its sintering temperature is high, usually 1300 DEG C are greater than, only have precious metals pt, Au, Pd or the alloy between them could meet the demand of interior electrode, but the cost of this kind of interior electrode is very high, and the price of precious metals pd goes up always, it is more and more outstanding that this just makes to reduce this technical barrier of MLCC production cost; The key reduced costs does not re-use expensive noble metal electrode, and reach above-mentioned target has two schemes optional.One is use base-metal inner-electrode, and as Ni, Cu etc. do interior electrode, but whole material all must sinter in reducing atmosphere, and this also will increase production cost and difficulty.Second method is exactly the fine silver electrode using price more cheap, and this just requires the sintering temperature significantly reducing BaTiO3.Like this reduce laminated ceramic capacitor material cost while, the energy consumption of sintering process can also be reduced, thus reduce the cost of whole multi-layer ceramic capacitor material and manufacture.
BaCu (B
2o
5) there is lower fusing point (850 DEG C), in sintering process, the microstructure of ceramic structure can be improved by the mode of mass transfer in liquid phase, meanwhile, significantly can reduce BaTiO
3the sintering temperature of base ceramic capacity medium material.At present, there is not yet with BaCu (B
2o
5) reduce BaTiO
3the report of base ceramic capacity medium material sintering temperature.
Summary of the invention
Object of the present invention, it is the shortcoming that cost is high, sintering temperature is high overcoming prior art, provide a kind of sintering temperature and low, cost is low, and there is preparation method's (operating temperature range that X8R Xing Shi International Electro TIA EIA specifies is the chip multilayer ceramic capacitor of-55 ~ 150 DEG C) of the X8R type medium material for multilayer ceramic capacitors of high dielectric constant.
A preparation method for low-temperature sintering X8R type ceramic capacitor dielectric, has following steps:
The present invention is achieved by following technical solution.
(1) CoO and Nb is taken by weight for 74.7:265.8
2o
5, mixing, ball milling, dry, sieve after in 800 ~ 1000 DEG C of calcinings, then through ball milling, dry obtained CoNb
2o
6;
(2) MnCO is taken by weight for 114.9:265.8
3and Nb
2o
5, mixing, ball milling, dry, sieve after in 800 ~ 1000 DEG C of calcinings, then through ball milling, dry obtained MnNb
2o
6;
(3) by Na
2cO
3, Bi
2o
3, TiO
23:15:10 batching in mass ratio, with deionized water mixing and ball milling 6h post-drying, then in 800 DEG C of calcinings, obtained Na
0.5bi
0.5tiO
3powder;
(4) stoichiometrically formula BaCuB
2o
5, by raw material BaCO
3, CuO and B
2o
3weigh batching, mixing, ball milling, dry, sieve after in 700 ~ 850 DEG C of calcinings, then through ball milling, dry obtained BaCuB
2o
5;
(5) BaTiO is taken by quality
3100g, CoNb prepared by add-on step (1)
2o
6mnNb prepared by 0.8 ~ 2.5g, step (2)
2o
6na prepared by 0.15 ~ 0.6g, step (3)
0.5bi
0.5tiO
3baCuB prepared by 0.3 ~ 0.5g and step (4)
2o
51 ~ 10g, after mixing with deionized water, ball milling 2 ~ 10 hours, dries 5 ~ 8 hours, the powder of obtained ceramic capacitor dielectric;
(6) by the additional mass percent of raw material that step (5) is dried be 7% paraffin granulation, then cross 1000 holes/cm
2sub-sieve, is pressed into green compact;
(7) green compact that step (6) is suppressed are warming up to 550 DEG C of de-waxings through 3.5h, are being warming up to 850 ~ 950 DEG C of sintering through 1 ~ 5h, insulation 1 ~ 4h, obtained BaTiO
3base low-temperature sintered X8R type ceramic capacitor dielectric.
Described step (6) is pressed into green compact under 4 ~ 10Mpa pressure.
The bake out temperature of described step (1), step (2), step (3) step (4) and step (5) is 120 DEG C.
The sintering temperature of X8R type medium material for multilayer ceramic capacitors disclosed by the invention is down to 900 ~ 950 DEG C from 1280 DEG C of prior art, achieve and burn altogether with pure Ag inner electrode, and obtain higher specific inductivity (ε >=1500), very low dielectric loss (tg δ≤0.013), operating temperature range be-55 ~ 150 DEG C, and cost is lower, sintering condition is simple, system component is controlled, not containing to environmentally hazardous substance, have a good application prospect.
Embodiment
The present invention is raw materials used is analytical pure raw material, and below by specific embodiment, the invention will be further described.
First take CoO and Nb by weight for 74.7:265.8 precision
2o
5, mixing, ball milling, dry, sieve, in 1000 DEG C of sintering, then through ball milling, dry obtained CoNb
2o
6;
Another by weight for 114.9:265.8 precision takes MnCO
3and Nb
2o
5, mixing, ball milling, dry, sieve, in 1000 DEG C of sintering, then through ball milling, dry obtained MnNb
2o
6;
By Na
2cO
3, Bi
2o
3, TiO
23:15:10 batching, calcine in 800 DEG C with deionized water mixing and ball milling 6h post-drying by mass percentage, obtains Na
0.5bi
0.5tiO
3powder;
Stoichiometrically formula BaCuB again
2o
5, by raw material BaCO
3, CuO and B
2o
3weigh batching, mixing, ball milling, dries, sieves, in 700 ~ 850 DEG C of sintering, then through ball milling, oven dry, and obtained BaCuB
2o
5powder;
BaTiO3 100g is taken, with above-mentioned CoNb by quality
2o
60.8 ~ 2.5g, MnNb
2o
60.15 ~ 0.6g, Na
0.5bi
0.5tiO
30.3 ~ 0.5g and BaCuB
2o
51 ~ 10g prepares burden, and ball milling 2 ~ 10 hours after mixing with deionized water, dries 5 ~ 8 hours in 120 DEG C, the powder of obtained ceramic capacitor dielectric; On this powder basis, added weight per-cent is the paraffin binder of 7%, homogeneous heating, crosses 1000 holes/cm
2sub-sieve, makes green compact under the pressure of 4 ~ 10Mpa; Again green compact were warming up to 550 DEG C through 3.5 hours, then were heated to 850 ~ 950 DEG C through 1 ~ 5 hour, be incubated 1 ~ 4 hour, obtained BaTiO3 base low-temperature sintered X8R type multilayer ceramic capacitor medium.
The main technologic parameters of the specific embodiment of the invention refers to table 1.
Table 1
The dielectric properties of the specific embodiment of the invention refer to table 2.
Table 2
The present invention is not limited to above-described embodiment, possible during the change of a lot of details, but therefore this do not run counter to scope and spirit of the present invention.
Claims (3)
1. a preparation method for low-temperature sintering X8R type ceramic capacitor dielectric, has following steps:
(1) CoO and Nb is taken by weight for 74.7:265.8
2o
5, mixing, ball milling, dry, sieve after in 800 ~ 1000 DEG C of calcinings, then through ball milling, dry obtained CoNb
2o
6;
(2) MnCO is taken by weight for 114.9:265.8
3and Nb
2o
5, mixing, ball milling, dry, sieve after in 800 ~ 1000 DEG C of calcinings, then through ball milling, dry obtained MnNb
2o
6;
(3) by Na
2cO
3, Bi
2o
3, TiO
23:15:10 batching in mass ratio, with deionized water mixing and ball milling 6h post-drying, then in 800 DEG C of calcinings, obtained Na
0.5bi
0.5tiO
3powder;
(4) stoichiometrically formula BaCuB
2o
5, by raw material BaCO
3, CuO and B
2o
3weigh batching, mixing, ball milling, dry, sieve after in 700 ~ 850 DEG C of calcinings, then through ball milling, dry obtained BaCuB
2o
5;
(5) BaTiO is taken by quality
3100g, CoNb prepared by add-on step (1)
2o
6mnNb prepared by 0.8 ~ 2.5g, step (2)
2o
6na prepared by 0.15 ~ 0.6g, step (3)
0.5bi
0.5tiO
3baCuB prepared by 0.3 ~ 0.5g and step (4)
2o
51 ~ 10g, after mixing with deionized water, ball milling 2 ~ 10 hours, dries 5 ~ 8 hours, the powder of obtained ceramic capacitor dielectric;
(6) by the additional mass percent of raw material that step (5) is dried be 7% paraffin granulation, then cross 1000 holes/cm
2sub-sieve, is pressed into green compact;
(7) green compact that step (6) is suppressed are warming up to 550 DEG C of de-waxings through 3.5h, are being warming up to 850 ~ 950 DEG C of sintering through 1 ~ 5h, insulation 1 ~ 4h, obtained BaTiO
3base low-temperature sintered X8R type ceramic capacitor dielectric.
2. the preparation method of low-temperature sintering X8R type ceramic capacitor dielectric according to claim 1, is characterized in that, described step (6) is pressed into green compact under 4 ~ 10Mpa pressure.
3. the preparation method of low-temperature sintering X8R type ceramic capacitor dielectric according to claim 1, it is characterized in that, the bake out temperature of described step (1), step (2), step (3) step (4) and step (5) is 120 DEG C.
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|---|---|---|---|
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ID=52366350
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106938928A (en) * | 2017-03-31 | 2017-07-11 | 天津大学 | A kind of anti-reduction huge dielectric constant low loss, high value ceramic capacitor dielectric material |
| CN107285762A (en) * | 2017-06-23 | 2017-10-24 | 汕头市瑞升电子有限公司 | A kind of high pressure low-loss ceramic capacitor dielectric and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101781115A (en) * | 2009-01-19 | 2010-07-21 | 清华大学 | X8R type multilayer ceramic capacitor dielectric material and preparation method thereof |
| CN103864416A (en) * | 2014-02-27 | 2014-06-18 | 天津大学 | Method for preparing barium titanate ceramic capacitor medium at low sintering temperature |
| CN103896581A (en) * | 2014-02-27 | 2014-07-02 | 天津大学 | Preparation method of multilayer ceramic capacitor medium with wide operating temperature range |
-
2014
- 2014-09-26 CN CN201410504643.XA patent/CN104310999A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101781115A (en) * | 2009-01-19 | 2010-07-21 | 清华大学 | X8R type multilayer ceramic capacitor dielectric material and preparation method thereof |
| CN103864416A (en) * | 2014-02-27 | 2014-06-18 | 天津大学 | Method for preparing barium titanate ceramic capacitor medium at low sintering temperature |
| CN103896581A (en) * | 2014-02-27 | 2014-07-02 | 天津大学 | Preparation method of multilayer ceramic capacitor medium with wide operating temperature range |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106938928A (en) * | 2017-03-31 | 2017-07-11 | 天津大学 | A kind of anti-reduction huge dielectric constant low loss, high value ceramic capacitor dielectric material |
| CN107285762A (en) * | 2017-06-23 | 2017-10-24 | 汕头市瑞升电子有限公司 | A kind of high pressure low-loss ceramic capacitor dielectric and preparation method thereof |
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Application publication date: 20150128 |