CN105294097B - A kind of low-loss high-temp leadless capacitor material and preparation method thereof - Google Patents
A kind of low-loss high-temp leadless capacitor material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of low-loss high-temp leadless capacitor material and preparation method thereof, the material is Bi (Mg0.5Ti0.5)O3With (Ba0.8Sr0.2)(1‑x)Ce2x/3TiO3The two-phase complex of formation, 0<x<0.40, x is molar fraction；It is by by Bi (Mg0.5Ti0.5)O3Powder is coated on (Ba using gel process0.8Sr0.2)(1‑x)Ce2x/3TiO3Particle outside, and Bi (Mg0.5Ti0.5)O3With (Ba0.8Sr0.2)(1‑x)Ce2x/3TiO3Mol ratio be 0.5~1.5.Low-loss high-temp leadless capacitor material temperature stability disclosed by the invention is good, low-loss with warm area wide and high dielectric constant.
Description
Technical field
The present invention relates to a kind of low-loss high temperature barium titanate-based lead-free capacitor material and preparation method thereof, belong to electric Jie
Matter technical field.
Background technology
The use temperature upper limit of commercial X7R, X8R and X9R capacitor is respectively in 125 DEG C, 150 DEG C and 175 DEG C, these classes
The capacitor of type can be widely applied to different occasions.But with the development of technology the temperature in use of capacitor is proposed it is higher
Requirement.The ceramic capacitor for being such as applied to hybrid power or electric driver needs to use temperature upper limit more than 200 DEG C, and
With good dielectric properties.
Such as Pb (ZrTi) O3Deng Pb based perovskites have dielectric constant very high the characteristics of, but in raw material add lead pair
The pollution of operator and environment is very big, not enough environmental protection.Lead-free ceramicses material 0.4Ba0.8Ca0.2TiO3-0.6Bi(Mg0.5Ti0.5)O3
Temperature range of the change in dielectric constant scope within ± 10% be 140 DEG C -420 DEG C, temperature of the dielectric loss less than 0.025
It is interval narrower, be~170 DEG C -300 DEG C, more than 200 DEG C within the temperature range of dielectric-temperature stability it is poor [A.Zeb,
S.J.Milne,Stability of High-Temperature Dielectric Properties for(1-x)
Ba0.8Ca0.2TiO3–xBi(Mg0.5Ti0.5)O3Ceramics,Journal oftheAmerican Ceramic Society 96
(9)(2013)2887-2892.].The main source of high-temperature dielectric loss is the migration of Lacking oxygen and the increase of crystal boundary conductance.For
Obtain the good lead-free capacitor material of comprehensive comparison, the point that intra-die is typically adjusted using rare earth doped is lacked
Concentration is fallen into, core shell structure is combined or built using multiphase to improve crystal boundary electric property, wherein core shell structure is in control crystal boundary
Behavior aspect is advantageously.
The content of the invention
The pressure caused to operator and environment with application process is prepared the invention aims to reduce, there is provided a kind of
High-dielectric-constant ceramics, are the core shell structure barium titanate-based lead-free capacitor materials with crystal grain doping, and dielectric loss is low, temperature
Good stability, for the excellent electronic device of processability provides technical foundation.
A kind of barium titanate-based lead-free capacitor material, is by Bi (Mg0.5Ti0.5)O3With (Ba0.8Sr0.2)(1-x)Ce2x/3TiO3
The two-phase complex of formation, 0<x<0.4, x is molar fraction；Wherein Bi (Mg0.5Ti0.5)O3It is to be coated on using gel process
(Ba0.8Sr0.2)(1-x)Ce2x/3TiO3Particle outside, and Bi (Mg0.5Ti0.5)O3With (Ba0.8Sr0.2)(1-x)Ce2x/3TiO3Mole
Than being 4：6~6：4；；
The preparation method of barium titanate-based lead-free capacitor material, step is as follows：
(1) traditional process for solid phase synthesis [Z.Chen, G.Li, X.Sun, L.Liu, L.Fang, La are used2O3modified
0.4(Ba0.8Ca0.2)TiO3-0.6Bi(Mg0.5Ti0.5)O3Ceramics for High-temperature capacitor
applications,Ceramics International,2015(41):11057-11061] prepare (Ba0.8Sr0.2)(1-x)
Ce2x/3TiO3Powder, 0<x<0.4, x is molar fraction；Preferable 0.15<x<0.3, more preferably x=0.15, or x=0.3；
(2) it is 1 by mol ratio：The 2 pure magnesium nitrate of analysis and the pure bismuth nitrate of analysis, is dissolved in glycol monoethyl ether, second two
Alcohol monomethyl ether quality is 5~10 times of the pure magnesium nitrate of analysis and the pure bismuth nitrate gross mass of analysis, and uniform solution is obtained；
(3) on the basis of the amount of the pure magnesium nitrate of analysis is added in step (2), by Mg：Ti mol ratios are 1：1, will analyze pure
Butyl titanate, be dissolved in methyl alcohol, methyl alcohol volume is 5~10 times of butyl titanate volume, and homogeneous solution is obtained；
(4) solution obtained in step (3) is added in the solution of step (2), it is 3~15 milliliters per second to add speed,
While being poured into edge the stirring of direction, mixing speed is 40~200 revs/min, is poured into after finishing that to be stirred for 0.5~2 small
When, obtain uniform colloidal sol；
(5) by (Ba obtained in step (1)0.8Sr0.2)(1-x)Ce2x/3TiO3Powder is added to colloidal sol obtained in step (4)
In, and a direction stirring is continued along, powder is uniformly suspended in colloidal sol, on the basis of the amount of the material of titanium, in colloidal sol
Titanium and powder in the ratio between the amount of material of titanium be 4：6~6：4；
(6) toward ethanol water is added dropwise in the colloidal sol obtained by step (5), the ratio between the volume of its reclaimed water and the volume of ethanol
VH2O：VEthanol=0.5~2.0, the volume of the ethanol water of dropwise addition is the 5~20% of sol volume, and side is added dropwise edge and one
Direction is stirred, and mixing speed is 20~120 revs/min, and mixing time is 0.2~1 hour, obtains gel；
(7) step (6) gained gel is stood 0.5~10 hour, 1~3 is heat-treated at a temperature of 700~1100 DEG C small
When, then grind, obtain Bi (Mg0.5Ti0.5)O3Cladding (Ba0.8Sr0.2)(1-x)Ce2x/3TiO3Complex outside particle；
(8) complex for obtaining step (7) is obtained barium titanate-based lead-free condenser ceramics by electronic ceramic process.
The present invention makes Bi (Mg using sol gel process0.5Ti0.5)O3It is coated on (Ba0.8Sr0.2)(1-x)Ce2x/3TiO3Particle
Outside, forms Two-phase composite structure and has obtained good interface feature.Due to SrTiO3Dielectric constant be far above CaTiO3,
Therefore the component announced shows dielectric constant higher；Rare earth La only has+trivalent state, and usually as donor ion, and Ce is deposited
+ 3 and+4 valencys, while donor and acceptor role can be played the part of, therefore dielectric loss containing Ce ceramics is smaller and temperature stability
Preferably.
Beneficial effects of the present invention：(1) compound is not leaded, production, using and waste procedures in will not be to environment
Produce harm；(2) by controlling Bi (Mg0.5Ti0.5)O3(Ba0.8Sr0.2)(1-x)Ce2x/3TiO3Ratio can obtain not equality of temperature
Spend the high-temperature dielectric material of scope；(3) Bi (Mg are built using sol gel process0.5Ti0.5)O3With (Ba0.8Sr0.2)(1-x)Ce2x/ 3TiO3Interface, formed complex, effectively expand dielectric peak width, reduce the dielectric temperature sensitiveness of material；(4) colloidal sol coagulates
Adhesive process and its cladding to powder improve interface carrier and transport and dipole polarization state, reduce dielectric loss.This
The barium titanate-based lead-free capacitor material of disclosure of the invention is expected to that business application can be obtained.
Brief description of the drawings
Fig. 1 is 0.4 (Ba of the gained of the embodiment of the present invention 10.8Sr0.2)0.85Ce0.1TiO3-0.6Bi(Mg0.5Ti0.5)O3Ceramic material
The relative dielectric constant and dielectric loss of material with frequency variation relation collection of illustrative plates.
Fig. 2 is 0.5 (Ba of the gained of the embodiment of the present invention 20.8Sr0.2)0.85Ce0.1TiO3–0.5Bi(Mg0.5Ti0.5)O3Ceramic material
The dielectric constant and dielectric loss of material with frequency variation relation collection of illustrative plates.
Fig. 3 is 0.6 (Ba of the gained of the embodiment of the present invention 30.8Sr0.2)0.7Ce0.2TiO3–0.4Bi(Mg0.5Ti0.5)O3Ceramic material
The dielectric constant and dielectric loss of material with frequency variation relation collection of illustrative plates.
Fig. 4 is 0.4 (Ba of the gained of the embodiment of the present invention 40.8Sr0.2)0.7Ce0.2TiO3–0.6Bi(Mg0.5Ti0.5)O3Ceramic material
The dielectric constant and dielectric loss of material with frequency variation relation collection of illustrative plates.
Specific embodiment
The technical scheme of the application is illustrated below with reference to embodiment：
Embodiment 1：
(1) with analytically pure cerium oxide, barium carbonate, strontium carbonate, titanium dioxide, bismuth nitrate, butyl titanate and magnesium nitrate
It is raw material, 2.5 hours prepare compound (Ba is incubated at 1250 DEG C using traditional process for solid phase synthesis0.8Sr0.2)0.85Ce0.1TiO3Powder；
(2) it is in molar ratio 1 to analyze pure magnesium nitrate, bismuth nitrate：2 carry out weighing dispensing, are dissolved in glycol monoethyl ether, second
Glycol monomethyl ether quality is 5 times of magnesium nitrate and bismuth nitrate quality, and uniform solution is obtained；
(3) on the basis of the magnesium nitrate of step (2), by Mg：Ti mol ratios are 1：1 metatitanic acid four that respective amount is measured with graduated cylinder
Butyl ester is dissolved in methyl alcohol, and methyl alcohol volume is 10 times of butyl titanate volume, is sufficiently stirred for, and solves homogeneously in butyl titanate
In methyl alcohol, uniform solution is obtained；
(4) step (3) is obtained during solution instills step (2) solution for obtaining, it is 3 milliliters per second to add speed, side drop
Enter side stirring, mixing speed is 40 revs/min, after completion of dropping, is stirred for 0.8 hour, obtains Bi (Mg0.5Ti0.5)O3It is molten
Glue；
(5) powder obtained in step (1) is added in colloidal sol obtained in step (4), and continues along a direction and stirred
Mix, powder is uniformly suspended in colloidal sol.On the basis of the amount of the material of titanium, the material of the titanium in titanium and colloidal sol in powder
The ratio between amount is 4：6；
(6) toward the dropwise addition water-reducible ethanol of deionization in the colloidal sol obtained by step (5), wherein deionized water volume is ethanol
0.5 times of volume, the volume of dropwise addition is the 20% of sol volume, is stirred when being added dropwise, and mixing speed is 20 revs/min, stirring
Time is 0.1 hour, obtains gel；
(7) it is heat-treated 1 hour at a temperature of 700 DEG C after step (6) gel being stood into 0.5 hour, is then ground in agate
It is finely ground in alms bowl to obtain 0.4 (Ba0.8Sr0.2)0.85Ce0.1TiO3-0.6Bi(Mg0.5Ti0.5)O3Powder；
(8) step (7) is obtained into 0.4 (Ba0.8Sr0.2)0.85Ce0.1TiO3-0.6Bi(Mg0.5Ti0.5)O3Powder is by electronics
Ceramic process is obtained barium titanate-based lead-free condenser ceramics.
Barium titanate-based lead-free capacitor material obtained in the present embodiment by surface polish and by silver-colored operation after carry out dielectric
Temperature spectrum test, dielectric properties are shown in Fig. 1, and dielectric constant is 4000 or so in 100-300 degree Celsius ranges, and dielectric loss keeps
It is relatively low.
Embodiment 2：
(1) with analytically pure cerium oxide, barium carbonate, strontium carbonate, titanium dioxide, bismuth nitrate, butyl titanate and magnesium nitrate
It is raw material, 2 hours prepare compound (Ba is incubated at 1200 DEG C using traditional process for solid phase synthesis0.8Sr0.2)0.85Ce0.1TiO3；
(2) it is in molar ratio 1 to analyze pure magnesium nitrate, bismuth nitrate：2 carry out weighing dispensing, are dissolved in glycol monoethyl ether, second
Glycol monomethyl ether quality is 7 times of material quality, and uniform solution is obtained；
(3) on the basis of the magnesium nitrate of step (2), by Mg：Ti mol ratios are 1：1 metatitanic acid four that respective amount is measured with graduated cylinder
Butyl ester is dissolved in methyl alcohol, and methyl alcohol volume is 8 times of butyl titanate volume, is sufficiently stirred for, and solves homogeneously in butyl titanate
In methyl alcohol, uniform solution is obtained；
(4) step (3) is obtained during solution instills step (2) solution for obtaining, it is 5 milliliters per second to add speed, side drop
Enter side stirring, mixing speed is 90 revs/min, after completion of dropping, is stirred for 1 hour, obtains Bi (Mg0.5Ti0.5)O3Colloidal sol；
(5) powder obtained in step (1) is added in colloidal sol obtained in step (4), and continues along a direction and stirred
Mix, powder is uniformly suspended in colloidal sol.On the basis of the amount of the material of titanium, the material of the titanium in titanium and colloidal sol in powder
The ratio between amount is 5：5；
(6) toward the dropwise addition water-reducible ethanol of deionization in the colloidal sol obtained by step (5), wherein deionized water volume is ethanol
0.9 times of volume, the volume of dropwise addition is the 11% of sol volume, is stirred when being added dropwise, and mixing speed is 80 revs/min, stirring
Time is 0.6 hour, obtains gel；
(7) it is heat-treated 1.5 hours at a temperature of 900 DEG C after step (6) gel being stood into 3 hours, is then ground in agate
It is finely ground in alms bowl to obtain 0.5 (Ba0.8Sr0.2)0.85Ce0.1TiO3–0.5Bi(Mg0.5Ti0.5)O3Powder；
(8) step (7) is obtained into 0.5 (Ba0.8Sr0.2)0.85Ce0.1TiO3–0.5Bi(Mg0.5Ti0.5)O3Powder is by electronics
Ceramic process is obtained barium titanate-based lead-free condenser ceramics.
Barium titanate-based lead-free capacitor material obtained in the present embodiment by surface polish and by silver-colored operation after carry out dielectric
Temperature spectrum test, dielectric properties are shown in Fig. 2, and dielectric constant is 3000 or so in 200-400 degree Celsius ranges, and dielectric loss keeps
It is relatively low.
Embodiment 3：
(1) with analytically pure cerium oxide, barium carbonate, strontium carbonate, titanium dioxide, bismuth nitrate, butyl titanate and magnesium nitrate
It is raw material, 2 hours prepare compound (Ba is incubated at 1300 DEG C using traditional process for solid phase synthesis0.8Sr0.2)0.7Ce0.2TiO3；
(2) it is in molar ratio 1 with magnesium nitrate, the bismuth nitrate of the pure level of analysis：2 carry out weighing dispensing, are dissolved in ethylene glycol list first
In ether, glycol monoethyl ether quality is 8 times of material quality, and uniform solution is obtained；
(3) on the basis of the magnesium nitrate of step (2), by Mg：Ti mol ratios are 1：1 metatitanic acid four that respective amount is measured with graduated cylinder
Butyl ester is dissolved in methyl alcohol, and methyl alcohol volume is 7 times of butyl titanate volume, is sufficiently stirred for, and solves homogeneously in butyl titanate
In methyl alcohol, uniform solution is obtained；
(4) step (2) is obtained during solution instills step (3) solution for obtaining, it is 9 milliliters per second to add speed, side drop
Enter side stirring, mixing speed is 150 revs/min, after dripping off, is stirred for 1.5 hours, obtains Bi (Mg0.5Ti0.5)O3Colloidal sol；
(5) powder obtained in step (1) is added in colloidal sol obtained in step (4), and continues along a direction and stirred
Mix, powder is uniformly suspended in colloidal sol.On the basis of the amount of the material of titanium, the material of the titanium in titanium and colloidal sol in powder
The ratio between amount is 6：4；
(6) toward the dropwise addition water-reducible ethanol of deionization in the colloidal sol obtained by step (5), wherein deionized water volume is ethanol
1.6 times of volume, the volume of dropwise addition is the 9% of sol volume, is stirred when being added dropwise, and mixing speed is 90 revs/min, during stirring
Between be 0.9 hour, obtain gel；
(7) it is heat-treated 2 hours at a temperature of 1000 DEG C after step (6) gel being stood into 8 hours, then in agate mortar
In finely ground obtain 0.6 (Ba0.8Sr0.2)0.7Ce0.2TiO3–0.4Bi(Mg0.5Ti0.5)O3Powder；
(8) step (7) is obtained into 0.6 (Ba0.8Sr0.2)0.7Ce0.2TiO3–0.4Bi(Mg0.5Ti0.5)O3Powder is by electronics
Ceramic process is obtained barium titanate-based lead-free condenser ceramics.
Barium titanate-based lead-free capacitor material obtained in the present embodiment by surface polish and by silver-colored operation after carry out dielectric
Temperature spectrum test, dielectric properties are shown in Fig. 3, and dielectric constant is in 2000-3000 in 300 degrees Celsius of range above, and dielectric loss does not have
There is obvious increase.
Embodiment 4：
(1) with analytically pure cerium oxide, barium carbonate, strontium carbonate, titanium dioxide, bismuth nitrate, butyl titanate and magnesium nitrate
It is raw material, is incubated 3 hours (Ba of prepare compound 0.4 at 1200 DEG C using traditional process for solid phase synthesis0.8Sr0.2)0.7Ce0.2TiO3。
(2) it is in molar ratio 1 with magnesium nitrate, the bismuth nitrate of the pure level of analysis：2 carry out weighing dispensing, are dissolved in ethylene glycol list first
In ether, glycol monoethyl ether quality is 10 times of material quality, and uniform solution is obtained；
(3) on the basis of the magnesium nitrate of step (2), by Mg：Ti mol ratios are 1：1 metatitanic acid four that respective amount is measured with graduated cylinder
Butyl ester is dissolved in methyl alcohol, and methyl alcohol volume is 5 times of butyl titanate volume, is sufficiently stirred for, and solves homogeneously in butyl titanate
In methyl alcohol, uniform solution is obtained；
(4) solution for obtaining step (2) is instilled in the solution that step (3) is obtained, and it is 15 milliliters per second, side to add speed
Side stirring is instilled, mixing speed is 200 revs/min, after dripping off, is stirred for 2 hours, obtains Bi (Mg0.5Ti0.5)O3Colloidal sol；
(5) powder obtained in step (1) is added in colloidal sol obtained in step (4), and continues along a direction and stirred
Mix, powder is uniformly suspended in colloidal sol.On the basis of the amount of the material of titanium, the material of the titanium in titanium and colloidal sol in powder
The ratio between amount is 4：6；
(6) toward the dropwise addition water-reducible ethanol of deionization in the colloidal sol obtained by step (5), wherein deionized water volume is ethanol
2.0 times of volume, the volume of dropwise addition is the 5% of sol volume, is stirred when being added dropwise, and mixing speed is 120 revs/min, stirring
Time is 1 hour, obtains gel；
(7) it is heat-treated 3 hours at a temperature of 1100 DEG C after step (6) gel being stood into 10 hours, is then ground in agate
It is finely ground in alms bowl to obtain 0.4 (Ba0.8Sr0.2)0.7Ce0.2TiO3–0.6Bi(Mg0.5Ti0.5)O3Powder；
(8) step (7) is obtained into 0.4 (Ba0.8Sr0.2)0.7Ce0.2TiO3–0.6Bi(Mg0.5Ti0.5)O3Powder is by electronics
Ceramic process is obtained barium titanate-based lead-free condenser ceramics.
Barium titanate-based lead-free capacitor material obtained in the present embodiment by surface polish and by silver-colored operation after carry out dielectric
Temperature spectrum test, dielectric properties are shown in Fig. 4, and dielectric constant is 2000 or so in 100-250 degree Celsius ranges, and dielectric loss keeps
It is relatively low.
The above-mentioned specific embodiment technical scheme that the invention is not limited in any way, every use equivalent or waits
The technical scheme that the mode of effect conversion is obtained all falls within protection scope of the present invention.
Claims (3)
1. the preparation method of barium titanate-based lead-free capacitor material, described barium titanate-based lead-free capacitor material, is by Bi
(Mg0.5Ti0.5)O3With (Ba0.8Sr0.2)(1-x)Ce2x/3TiO3The two-phase complex of formation, 0<x<0.4, x is molar fraction；Wherein
Bi(Mg0.5Ti0.5)O3It is that (Ba is coated on using gel process0.8Sr0.2)(1-x)Ce2x/3TiO3Particle outside, and Bi
(Mg0.5Ti0.5)O3With (Ba0.8Sr0.2)(1-x)Ce2x/3TiO3Mol ratio be 4：6~6：4, it is characterised in that step is as follows：
(1) (Ba is prepared using process for solid phase synthesis0.8Sr0.2)(1-x)Ce2x/3TiO3Powder；
(2) it is 1 by mol ratio：2 magnesium nitrate and bismuth nitrate, is dissolved in glycol monoethyl ether, and glycol monoethyl ether quality is to divide
Analyse pure magnesium nitrate and the pure bismuth nitrate gross mass of analysis 5~10 times, are obtained uniform solution；
(3) on the basis of the amount of the pure magnesium nitrate of analysis is added in step (2), by Mg：Ti mol ratios are 1：1, by analytically pure titanium
Acid butyl ester, is dissolved in methyl alcohol, and methyl alcohol volume is 5~10 times of butyl titanate volume, and homogeneous solution is obtained；
(4) solution obtained in step (3) is added in the solution of step (2), it is 3~15 milliliters per second to add speed, while inclining
Enter edge and a direction stirring, mixing speed is 40~200 revs/min, is poured into after finishing and is stirred for 0.5~2 hour, is obtained
To uniform colloidal sol；
(5) by (Ba obtained in step (1)0.8Sr0.2)(1-x)Ce2x/3TiO3Powder is added in colloidal sol obtained in step (4), and is held
It is continuous to be stirred along a direction, powder is uniformly suspended in colloidal sol；
(6) toward ethanol water is added dropwise in the colloidal sol obtained by step (5), side is added dropwise edge and a direction stirring, mixing speed
It it is 20~120 revs/min, mixing time is 0.2~1 hour, obtains gel；
(7) step (6) gained gel is stood 0.5~10 hour, heat treatment 1~3 hour at a temperature of 700~1100 DEG C, so
After grind, obtain Bi (Mg0.5Ti0.5)O3Cladding (Ba0.8Sr0.2)(1-x)Ce2x/3TiO3Complex outside particle；
(8) complex for obtaining step (7) is obtained barium titanate-based lead-free condenser ceramics by electronic ceramic process.
2. the preparation method of barium titanate-based lead-free capacitor material according to claim 1, it is characterised in that 0.15<x<
0.3。
3. the preparation method of barium titanate-based lead-free capacitor material according to claim 1, it is characterised in that in step (6)
The ratio between the volume of ethanol water reclaimed water and the volume of ethanol VH2O：VEthanol=0.5~2.0, the volume of ethanol water is colloidal sol
The 5~20% of volume.
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