CN100591642C - Porcelain material for temperature stabilization X9R type multilayer ceramic capacitor and method for producing the same - Google Patents
Porcelain material for temperature stabilization X9R type multilayer ceramic capacitor and method for producing the same Download PDFInfo
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- CN100591642C CN100591642C CN200710053554A CN200710053554A CN100591642C CN 100591642 C CN100591642 C CN 100591642C CN 200710053554 A CN200710053554 A CN 200710053554A CN 200710053554 A CN200710053554 A CN 200710053554A CN 100591642 C CN100591642 C CN 100591642C
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Abstract
The invention relates to stable temperature X9R type multilayer porcelain capacitor porcelain and the preparative method thereof. The porcelain includes the main components of BaTiO3 and BiScO3, as well as the assistant components of Y2O3, MgO, CdO, Bi2O3, Nb2O5 and low temperature additive, the formulation mol ratio is(100-a-b-c-d)[(1-x)BaTiO3-xBiScO3]+aY2O 3+bMgO+c(CdO+Bi2O3+Nb2O5)+d(0.5BaCO3+0.5CaCO3)+low temperature additive, wherein, x is 0.10 to 0.25; a is 0.1 to 1.0; b is 0.15 to 0.8; c is 0.1 to 0.6; and d is 0.1 to 1.0; the low temperature additive occupies 2 to 13 percent of total porcelain; the main components of the low temperature additive include PbO, BaCO3, SiO2, TiO2, Bi2O3, KCO3, and NaCO3. The preparative method comprises the steps as follows: adopting the market selling BaTiO3 powder with the tetragonal structure, mixing equally according to the ratio that Bi2O3: Sc2O3 is 1:1, presintering and keeping temperature for two hours under 850 DEG C to synthesize BiScO3,and then acquire the low temperature additive; The above components are proportioned according to the ratio, mixed with ball milling, dried, presintered, pressed piece to mold and sintered to porcelain. The porcelain which can be sintered with non-noble metal under middle temperature has the temperature character of X9R and cheap price.
Description
Technical field
The invention belongs to the multi-layer ceramic capacitor material technical field, particularly a kind ofly be used for the dielectric materials and preparation method thereof that high temperature has the laminated ceramic capacitor of high stability.
Background technology
Along with the fast development of information technology and electronic technology, also more and more higher to the requirement of electronics.The miniaturization of electronics, chip type and lightness are the inexorable trends of development.The components and parts of electronics will have smaller size smaller and weight accordingly, and laminated ceramic capacitor (being called for short MLCC) needs to arise at the historic moment because of these.According to the international EIA of Electronic Industries Association USA standard, MLCC is a benchmark with 25 ℃ capacitance, in the scope of temperature-55～200 ℃, and rate of change of capacitance≤± 15%, dielectric loss≤2.5%.
The temperature-stable multilayer ceramic capacitor raw material that uses mainly contains two kinds now, and a kind of is plumbiferous ferroelectric material, and a kind of is the barium phthalate base material.Because the needs of environmental protection, scientific effort mainly is non-lead base material now, and the barium phthalate base material is pollution-free, controls its composition during sintering easily, thereby is extensive use of in present multi-layer ceramic capacitor material.
The top temperature that present most of laminated ceramic capacitor uses is about 150 ℃, when using under higher temperature, its rate of change of capacitance will be far longer than ± and 15% requirement.Therefore the use of laminated ceramic capacitor is very restricted.Exploitation has higher use temperature and the higher multi-layer ceramic capacitor material of job stability is necessary.
Because the sintering characteristic of barium titanate ceramics itself, when using barium titanate ceramics as main raw, its sintering temperature is higher, generally greater than 1300 ℃.And laminated ceramic capacitor requires material and interior electrode to burn altogether, and is burning altogether under the temperature, requires not and interior electrode generation chemical reaction, and interior electrode does not melt, and assurance has good electrical conductivity.This makes the selection of laminated ceramic capacitor inner electrode be restricted.During former laminated ceramic capacitor was produced, the precious metal (as Pt, Au, Pd metal or its alloy etc.) that generally uses higher melt was as interior electrode.But, use these precious metals, improved the manufacturing cost of electrical condenser greatly.A lot of document announcements, the precious metal cost is 30～70% of a laminated ceramic capacitor production cost.U.S. Pat 007061748 report uses barium titanate based ceramic as main raw material, and sintering range is at 1200～1320 ℃.The interior electrode that uses is Pt, Au, Pd, Ag, Rh, Ru, a kind of or alloy among the Ir.Consider that from production cost this is worthless.Use cheap metal (as Ni, Fe, Co, Cu etc.) to reduce production costs greatly, enhance competitiveness.But, since Ni, Fe, Co, the fusing point of cheap metals such as Cu is lower, when burning altogether with stupalith, need carry out sintering under middle cold condition.So, want to use cheap metal as inner electrode, best way is to reduce the sintering temperature of pottery.But, add too much low-melting additive, certainly will reduce the dielectric properties of barium titanate based ceramic.
At present, most laminated ceramic capacitor adopts the prescription of X7R and X8R to produce, but because its working temperature stable range maximum at 150 ℃, surpasses this temperature, can not provide stable dielectric properties.
Summary of the invention
The purpose of this invention is to provide a kind of intermediate sintering temperature performance that has, high stability multilayer ceramic capacitor ceramics (dielectric materials) of wide temperature range and preparation method thereof.This porcelain has high-k, and low-loss has the advantages of excellent stability energy simultaneously; Preparation technology is simple, and material cost is lower.
Realize the technical scheme of the object of the invention: a kind of temperature stabilization X 9 R type multilayer ceramic capacitor porcelain that is used for, it is characterized in that: this porcelain comprises main component BaTiO
3And BiScO
3, ancillary component Y
2O
3, MgO, CdO, Bi
2O
3And Nb
2O
5, and the low temperature additive, its prescription is counted with mole:
(100-a-b-c-d) [(1-x) BaTiO
3-xBiScO
3]+aY
2O
3+ bMgO+c (CdO+Bi
2O
3+ Nb
2O
5)+d (0.5BaCO
3+ 0.5CaCO
3)+low temperature additive,
Wherein, x=0.10～0.25; A=0.1～1.0; B=0.15～0.8; C=0.1～0.6; D=0.1～1.0; The low temperature additive is 2～13wt% of porcelain total mass per-cent;
The composition mass percent of its low temperature additive is:
FPbO+gBaCO
3+ hSiO
2+ iTiO
2+ jBi
2O
3+ kK
2CO
3+ lNa
2CO
3Wherein, f=6～25%, g=4～25%, h=7～10%, i=5～15%, j=6～20%, k=9～15%, l=11～20%.
In above-mentioned porcelain, the grain-size of described main component raw material is less than 1 μ m.
In the above-mentioned porcelain ancillary component with purity greater than 99% Y
2O
3, Bi
2O
3, MgO, CdO, Nb
2O
5Be reactant feed.Wherein said CdO+Bi
2O
3+ Nb
2O
5Compound is according to CdO: Bi
2O
3: Nb
2O
5=1: 1: 1 mol ratio is prepared burden.
Described low temperature additive is with PbO, BaCO
3, SiO
2, TiO
2, Bi
2O
3, K
2CO
3, Na
2CO
3Be raw material, according to fPbO+gBaCO
3+ hSiO
2+ iTiO
2+ jBi
2O
3+ kK
2CO
3+ lNa
2CO
3Wherein, f=6～25%, g=4～25%, h=7～10%, i=5～15%, j=6～20%, k=9～15%, l=11～20% mass percent is prepared burden, after mixing, under 900～1000 ℃ temperature, carry out fusion, crystallization, promptly levigate then.
Ancillary component and low temperature additive all join in the main component with form of powder in the described porcelain, and after levigate in ball mill again, mixing, the drying, pre-burning is handled, and be after the pre-burning, once more that compound is levigate, mix;
The preparation process that is used for the temperature stabilization X 9 R type multilayer ceramic capacitor porcelain of the present invention is:
1), according to Bi
2O
3: Sc
2O
3Mix at=1: 1, at 2 hours synthetic BiScO of 850 ℃ of following presintering insulations
3, according to CdO: Bi
2O
3: Nb
2O
5=1: 1: 1 mol ratio is at 900 ℃ of down synthetic Bi
2Nb
2CdO
9, synthetic according to the method described above described low temperature additive is got and is had tetragonal phase structure and get BaTiO
3Powder (commercial, Guangdong Fenghua High Technology Co., Ltd);
2), according to (1-x) BaTiO
3-xBiScO
3Its x=0.10～0.25 stoichiometric ratio is prepared burden, and it is added in the anhydrous ethanol solvent mixing and ball milling 48 hours, oven dry;
3), according to above-mentioned porcelain proportioning, in step 2) the oven dry sample in add ancillary component, in anhydrous ethanol solvent, mixing and ball milling 48 hours is less than 1 μ m until powder fineness again; Presintering is 2 hours under 750～800 ℃ temperature, and ball milling mixes again, oven dry;
4), add the low temperature additive according to above-mentioned porcelain proportioning at the oven dry sample of step 3), in anhydrous ethanol solvent, mixing and ball milling is 48 hours once more, and 40 mesh sieves are crossed in oven dry, and powder carries out pre-burning under 800～900 ℃, powder once more, mixing, oven dry.The sample compression molding that oven dry is made sinters porcelain under 1050～1160 ℃ of temperature, promptly obtain being used for the temperature stabilization X 9 R type multilayer ceramic capacitor porcelain.
The present invention preparation be used for the temperature stabilization X 9 R type multilayer ceramic capacitor porcelain, has high-k, low dielectric loss, excellent temperature stability, material price is cheap, and has two big advantages: the one, have temperature stability scope wide (55～200 ℃); The 2nd, can sintering under middle temperature, be suitable for carrying out co-sintered with cheap metal, be used to prepare the multi-layer ceramic capacitor material of high-temperature stability.
Description of drawings
Fig. 1 is the rational curve that the dielectric constant with temperature of embodiment 1 sample changes
Fig. 2 is the temperature variant curve of temperature coefficient of capacitance of embodiment 1 sample
Fig. 3 is the rational curve that the dielectric constant with temperature of embodiment 2 samples changes
Fig. 4 is the temperature variant curve of temperature coefficient of capacitance of embodiment 2 samples
Fig. 5 is the rational curve that the dielectric constant with temperature of embodiment 3 samples changes
Fig. 6 is the temperature variant curve of temperature coefficient of capacitance of embodiment 3 samples
Fig. 7 is the rational curve that the dielectric constant with temperature of embodiment 4 samples changes
Fig. 8 is the temperature variant curve of temperature coefficient of capacitance of embodiment 4 samples
Embodiment
Following embodiment preparation has the composition and the condition of the multilayer ceramic capacitor ceramics (dielectric material) of higher dielectric constant and high temperature stability:
Porcelain is formed and is comprised main chemical compositions BaTiO
3With BiScO
3, ancillary component Y
2O
3, MgO, CdO, Bi
2O
3, Nb
2O
5With the low temperature additive, wherein, the main component of low temperature additive is PbO, BaCO
3, SiO
2, TiO
2, Bi
2O
3, K
2CO
3, Na
2CO
3
Its prescription is counted with mole:
(100-a-b-c-d) [(1-x) BaTiO
3-xBiScO
3]+aY
2O
3+ bMgO+c (CdO+Bi
2O
3+ Nb
2O
5)+d (0.5BaCO
3+ 0.5CaCO
3)+low temperature additive,
Wherein, x=0.10～0.25, a=0.1～1.0, b=0.15～0.8, c=0.1～0.6, d=0.1～1.0, the amount of low temperature additive accounts for 2～13% of dielectric material total mass,
The quality per distribution ratio of low temperature additive is: fPbO+gBaCO
3+ hSiO
2+ iTiO
2+ jBi
2O
3+ kK
2CO
3+ lNa
2CO
3Wherein, f=6～25%, g=4～25%, h=7～10%, i=5～15%, j=6～20%, k=9～15%, l=11～20%.The low temperature additive is pressed the preceding method preparation.
Preparation process is: with purity greater than 99% Bi
2O
3, Sc
2O
3, TiO
2, CdO, Nb
2O
5And BaCO
3Be initial reactant, according to Bi
2O
3: Sc
2O
3Mix at=1: 1, at 2 hours synthetic BiScO of 850 ℃ of following presintering insulations
3, press CdO: Bi
2O
3: Nb
2O
5=1: 1: 1 mol ratio is synthesized Bi
2Nb
2CdO
9, synthetic low temperature additive adopts the BaTiO with tetragonal phase structure
3Powder (commercial, Guangdong Fenghua High Technology Co., Ltd).With main chemical constitution according to (1-x) BaTiO
3-xBiScO
3, the stoichiometric ratio of x=0.10～0.25 is prepared burden, adds in the anhydrous ethanol solvent, and mixing and ball milling 48 hours, levigate, mix.Afterwards, add ancillary component and self-control low temperature additive according to proportioning, mixing and ball milling is 48 hours once more, and oven dry is sieved, powder carries out pre-burning under 850 ± 50 ℃, grinding once more, mixing, oven dry, the sample compression molding that oven dry is made sinters porcelain under 1050～1160 ℃ of temperature, promptly obtain being used for the temperature stabilization X 9 R type multilayer ceramic capacitor porcelain.
Be used for the pottery preparation.
Embodiment 1
According to batching mode (100-a-b-c-d) [(1-x) BaTiO
3-xBiScO
3]+aY
2O
3+ bMgO+c (CdO+Bi
2O
3+ Nb
2O
5)+d (0.5BaCO
3+ 0.5CaCO
3)+low temperature additive; Earlier according to BaTiO
3: BiScO
3=0.80: 0.20 molar ratio ingredient is got a=1; B=1; C=3; D=2.5; The amount of low temperature additive accounts for the 5wt% of material total mass, and the quality per distribution ratio of low temperature additive is: 6%PbO, 20%BaCO
3, 9%SiO
2, 15%TiO
2, 18%Bi
2O
3, 12%K
2CO
3, 20%Na
2CO
3. above-mentioned materials mixes, ball milling, dry then, after sieving, add binding agent, binding agent employing mass concentration is 5% polyvinyl alcohol (PVA) solution, and dosage is 0.25% of powder total mass, be a granulated into single-size, compression moulding under 200MPa pressure, making the disk diameter is 12mm, thickness is 1mm.Disk calcines the PVA binding agent down at 650 ℃, then Bi is being arranged
2O
3With sintering in the sealing corundum crucible of PbO, 1120 ± 20 ℃ of sintering temperatures, sintering time is 2 hours, and heat-up rate is 3 ℃/minute.The ceramic disks of burning till is through surface finish, and silver ink firing is measured its dielectric properties.The ceramics sample dielectric properties parameter that is obtained sees Table 1.Fig. 1 and Fig. 2
Fig. 1 is the rational curve that the dielectric constant with temperature of embodiment 1 sample changes; Fig. 2 is the temperature variant curve of temperature coefficient of capacitance of embodiment 1 sample;
The dielectric properties parameter of the ceramics sample of table 1 embodiment 1 preparation
Embodiment 2
According to batching mode (100-a-b-c-d) [(1-x) BaTiO
3-xBiScO
3]+aY
2O
3+ bMgO+c (CdO+Bi
2O
3+ Nb
2O
5)+d (0.5BaCO
3+ 0.5CaCO
3)+low temperature additive; Earlier according to BaTiO
3: BiScO
3=0.80: 0.20 molar ratio ingredient is got a=1; B=1; C=3; D=2.5; The amount of low temperature additive accounts for the 8wt% of material total mass, and the quality per distribution ratio of low temperature additive is: 25%PbO, 4%BaCO
3, 10%SiO
2, 13%TiO
2, 15%Bi
2O
3, 13%K
2CO
3, 20%Na
2CO
3. above-mentioned materials mixes, ball milling, dry then, after sieving, add binding agent, binding agent employing mass concentration is 5% polyvinyl alcohol solution, and dosage is 0.25% of powder total mass, be a granulated into single-size, compression moulding under 200MPa pressure, making the disk diameter is 12mm, thickness is 1mm.Disk calcines polyvinyl alcohol adhesive down at 650 ℃, then Bi is being arranged
2O
3In the sealing corundum crucible of PbO, 1100 ± 20 ℃ of sintering temperatures, sintering time is 2 hours, heat-up rate is 3 ℃/minute.The ceramic disks of burning till is through surface finish, and silver ink firing is measured its dielectric properties.The ceramics sample dielectric properties parameter that is obtained sees Table 2.Fig. 3, Fig. 4
Fig. 3 is the rational curve that the dielectric constant with temperature of embodiment 2 samples changes; Fig. 4 is the temperature variant curve of temperature coefficient of capacitance of embodiment 2 samples;
The dielectric properties parameter of the ceramics sample of table 2 embodiment 2 preparations
Embodiment 3
According to batching mode (100-a-b-c-d) [(1-x) BaTiO
3-xBiScO
3]+aY
2O
3+ bMgO+c (CdO+Bi
2O
3+ Nb
2O
5)+d (0.5BaCO
3+ 0.5CaCO
3)+low temperature additive; Earlier according to BaTiO
3: BiScO
3=0.90: 0.10 molar ratio ingredient is got a=1; B=1; C=3; D=2.5; The amount of low temperature additive accounts for the 8wt% of material total mass, and the quality per distribution ratio of low temperature additive is: 18%PbO, 25%BaCO
3, 7%SiO
2, 9%TiO
2, 15%Bi
2O
3, 15%K
2CO
3, 11%Na
2CO
3. above-mentioned materials mixes, ball milling, dry then, after sieving, add binding agent, binding agent employing mass concentration is 5% polyvinyl alcohol solution, and dosage is 0.25% of powder total mass, be a granulated into single-size, compression moulding under 200MPa pressure, making the disk diameter is 12mm, thickness is 1mm.Disk calcines polyvinyl alcohol adhesive down at 650 ℃, then Bi is being arranged
2O
3In the sealing corundum crucible of PbO, 1140 ± 20 ℃ of sintering temperatures, sintering time is 2 hours, heat-up rate is 3 ℃/minute.The ceramic disks of burning till is through surface finish, and silver ink firing is measured its dielectric properties.The ceramics sample dielectric properties parameter that is obtained sees Table 3.Fig. 5 and Fig. 6
Fig. 5 is the rational curve that the dielectric constant with temperature of embodiment 3 samples changes; Fig. 6 is the temperature variant curve of temperature coefficient of capacitance of embodiment 3 samples;
The dielectric properties parameter of the ceramics sample of table 3 embodiment 3 preparations
Embodiment 4
According to batching mode (100-a-b-c-d) [(1-x) BaTiO
3-xBiScO
3]+aY
2O
3+ bMgO+c (CdO+Bi
2O
3+ Nb
2O
5)+d (0.5BaCO
3+ 0.5CaCO
3)+low temperature additive; Earlier according to BaTiO
3: BiScO
3=0.80: 0.20 molar ratio ingredient is got a=1; B=1; C=3; D=2.5; The amount of low temperature additive accounts for the 10wt% of material total mass, and the quality per distribution ratio of low temperature additive is: 22%PbO, 22%BaCO
3, 10%SiO
2, 8%TiO
2, 6%Bi
2O
3, 12%K
2CO
3, 20%Na
2CO
3. above-mentioned materials mixes, ball milling, dry then, after sieving, add binding agent, binding agent employing mass concentration is 5% polyvinyl alcohol solution, and dosage is 0.25% of powder total mass, be a granulated into single-size, compression moulding under 200MPa pressure, making the disk diameter is 12mm, thickness is 1mm.Disk calcines polyvinyl alcohol adhesive down at 650 ℃, then Bi is being arranged
2O
3Just pressed in the crucible with the sealing of PbO, 1070 ± 20 ℃ of sintering temperatures, sintering time is 2 hours, heat-up rate is 3 ℃/minute.The ceramics sample dielectric properties parameter that is obtained sees Table 4.Fig. 7 and Fig. 8, the ceramic disks of burning till is through surface finish, and silver ink firing is measured its dielectric properties.
The dielectric properties parameter of the ceramics sample of table 4 embodiment 4 preparations
Claims (4)
1, a kind of temperature stabilization X 9 R type multilayer ceramic capacitor porcelain that is used for, it is characterized in that: this porcelain comprises main component BaTiO3 and BiScO3, ancillary component Y2O3, MgO, CdO, Bi2O3 and Nb2O5, and low temperature additive, its prescription is counted with mole:
(100-a-b-c-d) [(1-x) BaTiO3-xBiScO3]+aY2O3+bMgO+c (CdO+Bi2O3+Nb2O5)+d (0.5BaCO3+0.5CaCO3)+low temperature additive,
Wherein, x=0.10～0.25; A=0.1～1.0; B=0.15～0.8; C=0.1～0.6; D=0.1～1.0; The low temperature additive is 2～13wt% of porcelain total mass per-cent;
Described low temperature additive is a raw material with PbO, BaCO3, SiO2, TiO2, Bi2O3, K2CO3, Na2CO3, according to fPbO+gBaCO3+hSiO2+iTiO2+jBi2O3+kK2CO3+lNa2CO3; Wherein, f=6～25%, g=4～25%, h=7～10%, i=5～15%, j=6～20%, k=9～15%, l=11～20% mass percent is prepared burden, after mixing, under 900～1000 ℃ temperature, carry out fusion, crystallization, promptly levigate then.
2. the temperature stabilization X 9 R type multilayer ceramic capacitor porcelain that is used for as claimed in claim 1 is characterized in that: described main component grain-size is less than 1 μ m.
3. the temperature stabilization X 9 R type multilayer ceramic capacitor porcelain that is used for as claimed in claim 1 is characterized in that: wherein said CdO+Bi2O3+Nb2O5 compound, according to CdO: Bi2O3: Nb2O5=1: 1: 1 mol ratio is prepared burden.
4. preparation method who is used for the temperature stabilization X 9 R type multilayer ceramic capacitor porcelain: it is characterized in that: preparation process is:
1), according to Bi2O3: Sc2O3=1: 1 mixes, at 2 hours synthetic BiScO3 of 850 ℃ of following presintering insulations, according to CdO: Bi2O3: Nb2O5=1: 1: 1 mol ratio is at 900 ℃ of down synthetic Bi2Nb2CdO9, the synthetic described low temperature additive of claim 4 is got the BaTiO3 powder with tetragonal phase structure;
2), prepare burden, it is added in anhydrous ethanol solvent mixing and ball milling 48 hours, oven dry according to its x=0.10 of (1-x) BaTiO3-xBiScO3～0.25 stoichiometric ratio;
3), according to the proportioning of claim 1, in step 2) the oven dry sample in add ancillary component respectively, in anhydrous ethanol solvent, mixing and ball milling 48 hours is less than 1 μ m until powder fineness again; Presintering is 2 hours under 750～800 ℃ temperature, and ball milling mixes again, oven dry;
4), according to claim 1 proportioning, in the oven dry sample of step 3), add the low temperature additive, in anhydrous ethanol solvent, mixing and ball milling is 48 hours once more, 40 mesh sieves are crossed in oven dry, and powder carries out pre-burning under 800～900 ℃, powder once more, mixing, oven dry, the sample compression molding that oven dry is made, under 1050 ~ 1160 ℃ of temperature, sinter porcelain into, promptly obtain being used for the temperature stabilization X 9 R type multilayer ceramic capacitor porcelain.
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| CN102976753B (en) * | 2012-12-05 | 2014-01-22 | 中国科学院上海硅酸盐研究所 | Low-frequency-constant modified lead metaniobate piezoelectric ceramic material as well as preparation method and application thereof |
| CN103342556B (en) * | 2013-06-24 | 2014-12-03 | 湖北大学 | Preparation method of two-phase low-temperature co-sintered temperature stable dielectric ceramic material |
| CN103864435B (en) * | 2014-03-07 | 2015-07-22 | 武汉理工大学 | Preparation method of wide-temperature, high-pressure-resistant and high-energy-density ceramic dielectric material |
| CN105367052B (en) * | 2015-06-29 | 2018-07-20 | 福建火炬电子科技股份有限公司 | A kind of high-temperature ceramic capacitor dielectric material and preparation method thereof |
| CN105367053B (en) * | 2015-06-29 | 2018-12-11 | 福建火炬电子科技股份有限公司 | A kind of low-loss X9R type multilayer ceramic capacitor dielectric material and preparation method thereof |
| CN106952742A (en) * | 2017-03-14 | 2017-07-14 | 苏州海凌达电子科技有限公司 | A kind of preparation method of high-performance barium titanate based coextruded film super capacitor material |
| CN108281283A (en) * | 2017-12-28 | 2018-07-13 | 山东迪电子科技有限公司 | The manufacturing process and its capacitor packages of vertical type ceramic patch capacitor |
| CN110304916B (en) * | 2019-04-25 | 2022-01-04 | 武汉理工大学 | Anti-reduction BaTiO3Base medium ceramic and preparation method thereof |
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