CN1626475A - Anti reductive powder of media ceramics and preparation method, as well as method in use for preparing ceramic capacitor in multiple layers - Google Patents
Anti reductive powder of media ceramics and preparation method, as well as method in use for preparing ceramic capacitor in multiple layers Download PDFInfo
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- CN1626475A CN1626475A CN 02134838 CN02134838A CN1626475A CN 1626475 A CN1626475 A CN 1626475A CN 02134838 CN02134838 CN 02134838 CN 02134838 A CN02134838 A CN 02134838A CN 1626475 A CN1626475 A CN 1626475A
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Abstract
A dielectric ceramic powder resisting against reduction contains Ba1-x-ySrxCayTiO3, where x=0.05-0.4 and y=0.01-0.25. It can also contain alpha Y2O3+beta MgO+(1-alpha-beta) MnO where alpha=0.2-0.8 and beta=0.1-0.6, and SiO2-TiO2-Al2O3. Its preparing process and a process for preparing the multi-layer ceramic capacitor frmo it are also disclosed.
Description
Technical field
The present invention relates to anti-reducing medium ceramic powder, particularly a kind of ceramic powder that can under reducing atmosphere, burn altogether with the electrode layer of Ni or Cu conductive powder or their oxide compound composition.
The invention still further relates to the preparation method of this ceramic powder.
The invention still further relates to this ceramic powder and be used to prepare the method for laminated ceramic capacitor.
Background technology
Laminated ceramic capacitor MLCC (Multi-layer Ceramic Capacitor) has high specific volume, highly reliable, characteristics such as frequency response characteristic is good, is at electronic information, computer, electron device is very widely used in field such as control and communication automatically.Direction develops and the developing rapidly of integrated circuit surface field engineering to miniature, thin layer, mixing be integrated etc. along with electronics and components and parts, and the demand of high-performance MLCC is grown with each passing day.High-performance, miniaturization and low cost are the main flows of electronic devices and components development.
In order to satisfy the requirement of complete electronic set, MLCC constantly develops to microminiaturization, high capacity, high reliability and cost degradation direction.If realize high capacity, its method is the number of plies that adopts the ceramic dielectic of high-k, reduces the thickness and the increase ceramic dielectic of ceramic dielectic.Along with the increase of the medium number of plies, the also corresponding increase of the number of plies of interior electrode.At present, the inner electrode great majority are the Pd-Ag system material.This precious metal material costs an arm and a leg.In the MLCC cost, inner electrode accounts for more than 50% of MLCC cost.In order to take into account the requirement to large vol and low-cost two aspects, selecting for use cheaply, base metal Ni electrode replaces the effective measure that the Pd-Ag electrode is the raising ratio of performance to price.
The status that Ni electrode MLCC will progressively replace present conventional MLCC the coming years becomes the main product of MLCC.X7R type MLCC is very important and is a class chip capacitor of large usage quantity that requirement has lower temperature coefficient of capacitance (≤± 15%) in the scope of-55 ℃ to+125 ℃ temperature broad.Its market capacity accounts for more than 40% of MLCC total amount.
But there is a great problem in the interior electrode that adopts Ni to be MLCC: carry out sintering under neutrality or reducing atmosphere.And general dielectric ceramic material sintering under neutrality or reducing atmosphere will be reduced into semi-conductor significantly and lose its function as capacitor material.
For the development of MLCC and the needs in market, the research of satisfying X7R type ceramic powder that people's handle exploitation can stablizing mass industrialized production Ni electrode MLCC uses has been mentioned on the schedule.
Summary of the invention
The objective of the invention is to provide at the demand a kind of anti-reducing medium ceramic powder of the EIA-X7R of satisfying characteristic standard, its energy and Ni, Cu or their oxide compound carry out sintering under neutrality or reducing atmosphere, and can keep high insulation resistance.
The effective chemistry of anti-reducing medium ceramic powder of the present invention consists of:
Ba
1-x-ySr
xCa
yTiO
3，
0.05≤X≤0.4,0.01≤y≤0.25 wherein;
In order to strengthen incinerating resistance to reduction under reducing atmosphere, improve stability, ceramic powder of the present invention can also comprise:
The α Y of (1) 0.2%～2.0% weight
2O
3+ β MgO+ (1-alpha-beta) MnO, wherein the scope of α, β mol ratio is 0.2≤α≤0.8,0.1≤β≤0.6; Be called for short first component.
Can also comprise on this basis:
The SiO of (2) 0.2%～5.0% weight
2-TiO
2-Al
2O
3Be called for short second component.
Ba
1-x-ySr
xCa
yTiO
3The preparation method be with BaCO
3, CaCO
3, SrCO
3And TiO
2Each component places ball mill to carry out wet-milling, and the temperature with 1000～1200 ℃ was calcined 1～3 hour in air subsequently, the powder after obtaining to calcine.
The preparation method of second component is with SiO
2, TiO
2, Al
2O
3Powder weighing also mixes.Place ball mill to carry out wet-milling in mixture, the temperature with 400～1000 ℃ was calcined 1～3 hour in air subsequently, thereby obtained second component powders after the calcining.
When adding first component, second component in the ceramic powder of the present invention, with Ba
1-x-ySr
xCa
yTiO
3, first component and/or second component mixture place ball mill to carry out wet-milling, and be dry in 100～150 ℃ temperature subsequently, thereby obtain dried ceramic powder.
The method that ceramic powder of the present invention prepares laminated ceramic capacitor comprises:
---in ceramic powder, add PVB based adhesive and ethanol, and in ball mill thorough mixing, obtain ceramic mud;
---with casting method ceramic mud is made the multi-disc diaphragm, diaphragm thickness is the 8-12 micron;
---, printing the Ni electrode slurry on the diaphragm diaphragm is overlapped together with the dislocation silk screen print method, thereby obtain electric capacity crust piece, will cling to the piece cutting, obtain the laminated ceramic capacitor green compact;
---the temperature that the laminated ceramic capacitor green compact is heated to 300-400 ℃ in nitrogen atmosphere is to decompose tackiness agent.Subsequently with it at H
2-N
2-H
2Carry out sintering in the reducing atmosphere that O forms, obtain the agglomerating laminated ceramic capacitor.
Use ceramic powder of the present invention, cost is low, satisfies the anti-reducing medium ceramic powder of EIA-X7R characteristic standard, and its energy and Ni, Cu or their oxide compound carry out sintering under neutrality or reducing atmosphere, and can keep high insulation resistance.Can make with metallic nickel is high reliability, small size, the jumbo laminated ceramic capacitor of interior electrode; The present invention has very high industrial use value.
Embodiment
Preparation Ba
1-x-ySr
xCa
yTiO
3
With BaCO
3, CaCO
3, SrCO
3And TiO
2Powder weighing also mixes, and general formula is:
Ba
1-x-ySr
xCa
yTiO
3
Place ball mill to carry out wet-milling in mixture, the temperature with 1000 ℃ was calcined 3 hours in air subsequently, thereby obtained the active principle powder after the calcining.
With SiO
2, TiO
2, Al
2O
3Powder weighing also mixes.Place ball mill to carry out wet-milling in mixture, subsequently in air with 1000 ℃ temperature calcining hour, thereby obtain second component powders after the calcining.
With the active principle powder after the calcining, the Y in first component
2O
3, Mg (OH)
2, MnCO
3Weighing and mix in second component after powder and the calcining; Wherein, contain first component of m weight part and second component of n weight part with respect to the main ingredient of per 100 weight parts; In first component, with general formula
α Y
2O
3+ β MgO+ (1-alpha-beta) MnO represents.Place ball mill to carry out wet-milling in mixture, dry in 100 temperature subsequently, thus obtain dried powder.
In this dried powder, add PVB based adhesive and ethanol subsequently, and in ball mill thorough mixing, thereby obtain ceramic mud.Then, with casting method ceramic mud is made the multi-disc diaphragm, diaphragm thickness is about 10 microns., afterwards, diaphragm is overlapped together printing the Ni electrode slurry on the diaphragm with the dislocation silk screen print method, thereby obtain electric capacity crust piece.To cling to the piece cutting, obtain the laminated ceramic capacitor green compact.
The temperature that then the laminated ceramic capacitor green compact is heated to 350 ℃ in nitrogen atmosphere is to decompose tackiness agent.Subsequently with it at H
2-N
2-H
2Carry out sintering in the reducing atmosphere that O forms, obtain the agglomerating laminated ceramic capacitor.Two end faces at the agglomerating laminated ceramic capacitor are coated the Cu slurry, follow the N at 800 ℃
2Middle roasting, thus the outer electrode that links to each other with the Ni electrode formed.At the outer electrode plated with nickel film that powers on, power at the nickel film at last and plate tin thin film subsequently.
The length of monolithic multilayer ceramic condenser is 2.0mm, and width is 1.3mm, and thickness is 1.2mm.Dielectric thickness is 8um, and effectively the dielectric ceramic number of plies is 20, and the area of every layer of ceramic plane counter electrode is 2.0mm
2
Use the HP4278A electric bridge to be determined at 1KHz, 1V rms, 25 ℃ electrical capacity (C) and dielectric loss (tan δ).Can obtain specific inductivity (ε) by calculating.At 25 ℃ and 125 ℃, 16VDC voltage was put on sample 2 minutes, use the determination of insulation resistance instrument, the insulation resistance of working sample (R), thereby the product of acquisition C and R, promptly CR is long-pending.Mensuration with 20 ℃ be benchmark at-25 ℃, 85 ℃ rate of change of capacitance (Δ C/C
20 ℃); Mensuration is rate of change of capacitance (the Δ C/C-55 ℃ and 125 ℃ of benchmark with 25 ℃
25 ℃), and the maximum rate of the variation of the electrical capacity in-55 ℃ to 125 ℃ temperature range (| Δ C/C|max).
In addition, by high temperature load test, the estimation life of capacitors.Put on 36 electrical condensers of each sample at 150 ℃ of voltages, measure insulation resistance (R) over time 100VDC.The insulation resistance of each sample reaches 10
6Ω or more time at the end obtains the mean lifetime of each sample as its life-span.
Each sample is carried out the high humidity load test, wherein under the relative humidity of 125 ℃, 2 normal atmosphere and 100%, the voltage of 16VDC is put on 72 electrical condensers of each sample, measure insulation resistance (R) over time, calculating beginning to test back 250 hours is 10 with interior demonstration insulation resistance (R)
6The Ω or the substandard product number at the end more.
Above-mentioned measurement result is listed among the table B.All capacitor samples within the scope of the invention have and are not less than 3000 high-k, and have and be not more than 250 * 10
-4Dielectric loss.The volume change rate satisfies the X7R level standard of performance of stipulating in the EIA standard in-55 ℃ to 125 ℃ temperature ranges simultaneously.And these samples of the present invention have high insulating resistance value when measuring for 25 ℃ and 125 ℃, and are long-pending in CR, are not less than 6000M Ω uF and 2000M Ω uF respectively.In addition, capacitor sample has and is not shorter than 300 hours mean lifetime, does not find underproof in the moisture-proof load test.
The reason that used composition among the present invention is limited is described below below:
Ceramic powder main ingredient Ba at first is described
1-x-ySr
xCa
yTiO
3In to the qualification reason of x, y.
Seen at sample 1, when y＜0.01, sample forms semi-conductor; On the other hand, as in sample 5 as seen, when y＞0.25, sample is densified sintering product fully.So limit 0.01≤y≤0.25.
Seen at sample 6, when x＜0.05, the mean lifetime of sample is short; On the other hand, seen at sample 11, when x＞0.4, at the bottom of the insulation resistance of sample.So limit 0.05≤x≤0.4.
The first component α Y
2O
3The qualification of α, β and relative weight part m be the reasons are as follows among+β MgO+ (1-alpha-beta) MnO.
Seen at sample 12, when m＜0.2, sample is sintering fully; On the other hand, seen at sample 18, when m＞2.0, the volume change rate of sample exceeds the EIA-X7R standard.So limit 0.2≤m≤2.0.
Seen at sample 19,20,21,25, when α, β exceed 0.2≤α≤0.8,0.1≤β≤0.6 scope, the volume change rate of sample exceeds the EIA-X7R standard.
The second component S i0
2-TiO
2-Al
2O
3The qualification of relative weight part n be the reasons are as follows.
Seen at sample 26, when n＜0.2, sample is sintering fully; On the other hand, seen at sample 34, when n＞5.0, the volume change rate of sample exceeds the EIA-X7R standard.So limit 0.2≤n≤5.0.
| Sample number into spectrum | Firing temperature (℃) | Specific inductivity 8 | ???tanδ ??(×10 -4) | ???????ΔC/C 20℃(％) | ???????????????ΔC/C 25℃(％) | 25 ℃ of CR long-pending (M Ω uF) | 125 ℃ of CR long-pending (M Ω uF) | Mean lifetime (hr) | Number of non-compliances in the high humidity load test | |||
| ????-25℃ | ????85℃ | ????-55 | ????125 | ????max | ?????16V | ????16V | ||||||
| ??1 * | ??1300 | Form semi-conductor, can not measure | ||||||||||
| ??2 | ??1300 | ??3240 | ????210 | ????-3.4 | ????-6.2 | ????-2.5 | ????-6.7 | ????7.2 | ????6860 | ????2870 | ????526 | ????0 |
| ??3 | ??1300 | ??3520 | ????200 | ????-4.8 | ????-7.0 | ????-3.2 | ????-6.5 | ????8.5 | ????7100 | ????3500 | ????603 | ????0 |
| ??4 | ??1320 | ??3160 | ????240 | ????-5.2 | ????-6.3 | ????-4.3 | ????-5.8 | ????7.5 | ????6840 | ????2850 | ????591 | ????0 |
| ??5 * | ??1360 | Sintering is insufficient, can not measure | ||||||||||
| ??6 * | ??1300 | ??3340 | ????210 | ????-4.8 | ????-5.8 | ????-6.8 | ????-6.6 | ????10.8 | ????6480 | ????2960 | ????195 | ????0 |
| ??7 | ??1300 | ??3340 | ????220 | ????-4.4 | ????-5.2 | ????-4.5 | ????-6.9 | ????7.0 | ????6840 | ????2970 | ????526 | ????0 |
| ??8 | ??1300 | ??3520 | ????220 | ????-4.9 | ????-5.0 | ????-5.2 | ????-6.5 | ????7.5 | ????6500 | ????3200 | ????603 | ????0 |
| ??9 | ??1320 | ??3620 | ????210 | ????-4.2 | ????-5.3 | ????-3.3 | ????-5.5 | ????7.3 | ????7010 | ????3000 | ????581 | ????0 |
| ??10 | ??1300 | ??3230 | ????230 | ????-4.8 | ????-4.3 | ????-5.3 | ????-6.5 | ????8.3 | ????6710 | ????2800 | ????531 | ????0 |
| ??11 * | ??1300 | ??3420 | ????230 | ????-3.3 | ????-6.6 | ????-3.4 | ????-6.5 | ????6.8 | ????2360 | ????620 | ????150 | ????0 |
| ??12 * | ??1360 | Sintering is insufficient, can not measure | ||||||||||
| ??13 | ??1280 | ??3490 | ????220 | ????-1.5 | ????-7.2 | ????-0.3 | ????-9.8 | ????10.5 | ????5780 | ????3260 | ????575 | ????0 |
| ??14 | ??1300 | ??3570 | ????180 | ????-3.4 | ????-4.3 | ????-3.1 | ????-6.8 | ????11.5 | ????5890 | ????2870 | ????544 | ????0 |
| ??15 | ??1300 | ??3050 | ????190 | ????-2.8 | ????-5.6 | ????-2.5 | ????-6.9 | ????9.8 | ????6700 | ????3200 | ????603 | ????0 |
| ??16 | ??1320 | ??3430 | ????200 | ????-1.9 | ????-6.9 | ????-1.8 | ????-8.9 | ????13.5 | ????6010 | ????3300 | ????530 | ????0 |
| ??17 | ??1320 | ??3330 | ????150 | ????-2.6 | ????-7.8 | ????-3.0 | ????-9.1 | ????10.2 | ????6210 | ????3400 | ????501 | ????0 |
| ??18 * | ??1320 | ??3560 | ????180 | ????-0.6 | ????-10.8 | ????-0.2 | ????-16.1 | ????16.1 | ????5710 | ????3200 | ????481 | ????0 |
Table B
| Sample number into spectrum | Firing temperature (℃) | Specific inductivity 8 | ???tanδ ??(×10 -4) | ??????ΔC/C 20℃(％) | ???????????ΔC/C 25℃(％) | 25 ℃ of CR long-pending (M Ω uF) | 125 ℃ of CR long-pending (M Ω uF) | Mean lifetime (hr) | Number of non-compliances in the high humidity load test | |||
| ????-25℃ | ???85℃ | ??-55 | ???125 | ??max | ????16V | ????16V | ||||||
| ?19 * | ??1300 | ??3620 | ????190 | ????-3.9 | ???-15.2 | ??-3.2 | ??-16.5 | ??16.5 | ????6400 | ????2700 | ????453 | ????0 |
| ?20 * | ??1320 | ??3320 | ????210 | ????-3.2 | ???-15.5 | ??-3.3 | ??-15.5 | ??15.5 | ????7030 | ????3240 | ????541 | ????0 |
| ?21 * | ??1300 | ??3730 | ????200 | ????-4.0 | ???-14.9 | ??-4.3 | ??-16.5 | ??16.5 | ????5610 | ????2970 | ????438 | ????0 |
| ?22 | ??1300 | ??3680 | ????170 | ????-3.6 | ???-5.3 | ??-4.1 | ??-6.9 | ??11.4 | ????5450 | ????2980 | ????594 | ????0 |
| ?23 | ??1300 | ??3250 | ????210 | ????-2.7 | ???-5.6 | ??-3.5 | ??-6.7 | ??9.9 | ????6540 | ????3100 | ????600 | ????0 |
| ?24 | ??1320 | ??3630 | ????200 | ????-1.6 | ???-5.9 | ??-2.8 | ??-8.0 | ??10.5 | ????5810 | ????3120 | ????550 | ????0 |
| ?25 * | ??1320 | ??3950 | ????230 | ????-4.0 | ???-16.0 | ??-4.5 | ??-18.5 | ??18.5 | ????6010 | ????2980 | ????450 | ????0 |
| ?26 * | ??1360 | Sintering is insufficient, can not measure | ||||||||||
| ?27 | ??1300 | ??3330 | ????170 | ????-3.5 | ???-5.2 | ??-4.1 | ??-6.9 | ??11.8 | ????4690 | ????3180 | ????594 | ????0 |
| ?28 | ??1300 | ??3240 | ????210 | ????-3.7 | ???-5.0 | ??-2.5 | ??-5.7 | ??9.9 | ????5780 | ????3060 | ????620 | ????0 |
| ?29 | ??1320 | ??3530 | ????220 | ????-3.5 | ???-5.0 | ??-3.8 | ??-8.3 | ??9.5 | ????6790 | ????3020 | ????500 | ????0 |
| ?30 | ??1300 | ??3660 | ????180 | ????-3.0 | ???-4.2 | ??-4.1 | ??-6.9 | ??10.4 | ????5800 | ????2880 | ????494 | ????0 |
| ?31 | ??1320 | ??3100 | ????220 | ????-2.9 | ???-6.6 | ??-3.5 | ??-6.7 | ??9.9 | ????6780 | ????3130 | ????490 | ????0 |
| ?32 | ??1320 | ??3230 | ????200 | ????-2.6 | ???-4.9 | ??-2.8 | ??-8.0 | ??8.5 | ????5900 | ????3420 | ????500 | ????0 |
| ?33 | ??1320 | ??3050 | ????190 | ????-2.8 | ???-5.4 | ??-3.5 | ??-6.8 | ??10.8 | ????4900 | ????3000 | ????493 | ????0 |
| ?34 * | ??1300 | ??3830 | ????220 | ????-4.0 | ???-17.2 | ??-3.5 | ??-19.2 | ??19.2 | ????5010 | ????2900 | ????430 | ????0 |
Continuous table B
Claims (7)
1, a kind of anti-reducing medium ceramic powder is characterized in that effective chemistry consists of:
Ba
1-x-ySr
xCa
yTiO
3，
0.05≤x≤0.4,0.01≤y≤0.25 wherein.
2, anti-reducing medium ceramic powder according to claim 1 is characterized in that also comprising the α Y of 0.2%～2.0% weight
2O
3+ β MgO+ (1-alpha-beta) MnO, wherein the scope of α, β mol ratio is 0.2≤α≤0.8,0.1≤β≤0.6; Be called for short first component.
3, anti-reducing medium ceramic powder according to claim 1 and 2 is characterized in that also comprising the SiO of 0.2%～5.0% weight
2-TiO
2-Al
2O
3Be called for short second component.
4, the preparation method of the described ceramic powder of claim 1 is characterized in that BaCO
3, CaCO
3, SrCO
3And TiO
2Each component places ball mill to carry out wet-milling, and the temperature with 1000～1200 ℃ was calcined 1～3 hour in air subsequently, the powder after obtaining to calcine.
5, the preparation method of described second component of claim 2 is characterized in that SiO
2, TiO
2, Al
2O
3Powder weighing also mixes; Place ball mill to carry out wet-milling in mixture, the temperature with 400～1000 ℃ in air was calcined 1～3 hour, thereby obtained second component powders after the calcining.
6, the preparation method of the described ceramic powder of claim 3 is characterized in that Ba
1-x-ySr
xCa
yTiO
3, first component and/or second component mixture place ball mill to carry out wet-milling, and be dry in 100～150 ℃ temperature subsequently, thereby obtain dried ceramic powder.
7, claim or 2 or 3 described ceramic powders prepare the method for laminated ceramic capacitor, it is characterized in that comprising:
---in ceramic powder, add PVB based adhesive and ethanol, and in ball mill thorough mixing, obtain ceramic mud;
---with casting method ceramic mud is made the multi-disc diaphragm, diaphragm thickness is the 8-12 micron;
---, printing the Ni electrode slurry on the diaphragm diaphragm is overlapped together with the dislocation silk screen print method, thereby obtain electric capacity crust piece, will cling to the piece cutting, obtain the laminated ceramic capacitor green compact;
---the temperature that the laminated ceramic capacitor green compact is heated to 300-400 ℃ in nitrogen atmosphere to be to decompose tackiness agent, with it at H
2-N
2-H
2Carry out sintering in the reducing atmosphere that O forms, obtain the agglomerating laminated ceramic capacitor.
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|---|---|---|---|
| CN 02134838 CN1626475A (en) | 2002-09-27 | 2002-09-27 | Anti reductive powder of media ceramics and preparation method, as well as method in use for preparing ceramic capacitor in multiple layers |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02134838 CN1626475A (en) | 2002-09-27 | 2002-09-27 | Anti reductive powder of media ceramics and preparation method, as well as method in use for preparing ceramic capacitor in multiple layers |
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| Publication Number | Publication Date |
|---|---|
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Family
ID=34754225
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|---|---|---|---|
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1331803C (en) * | 2005-12-28 | 2007-08-15 | 天津大学 | (Balx-ySrxYy) TiO3 based dielectrical ceramic material and preparation process thereof |
| CN102531581A (en) * | 2011-12-31 | 2012-07-04 | 嘉兴佳利电子股份有限公司 | Microwave dielectric ceramic with intermediate dielectric constant and high Q value and preparation method thereof |
| CN105218089A (en) * | 2015-10-13 | 2016-01-06 | 广州创天电子科技有限公司 | The electrical condenser of a kind of barium titanate ceramic dielectric material and gained |
-
2002
- 2002-09-27 CN CN 02134838 patent/CN1626475A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1331803C (en) * | 2005-12-28 | 2007-08-15 | 天津大学 | (Balx-ySrxYy) TiO3 based dielectrical ceramic material and preparation process thereof |
| CN102531581A (en) * | 2011-12-31 | 2012-07-04 | 嘉兴佳利电子股份有限公司 | Microwave dielectric ceramic with intermediate dielectric constant and high Q value and preparation method thereof |
| CN105218089A (en) * | 2015-10-13 | 2016-01-06 | 广州创天电子科技有限公司 | The electrical condenser of a kind of barium titanate ceramic dielectric material and gained |
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