CN101030478A - High-dielectric metal-electric medium composite ceramic capacitance and its production - Google Patents
High-dielectric metal-electric medium composite ceramic capacitance and its production Download PDFInfo
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- CN101030478A CN101030478A CN 200710057006 CN200710057006A CN101030478A CN 101030478 A CN101030478 A CN 101030478A CN 200710057006 CN200710057006 CN 200710057006 CN 200710057006 A CN200710057006 A CN 200710057006A CN 101030478 A CN101030478 A CN 101030478A
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Abstract
The invention is concerned with a kind of high permittivity metal-dielectric complex ceramic capacitor medium and its production. Mix 100 parts of BaTiO3, 0.5 to 4 parts of Nb2O5, 3 to 6 parts of MgO, 0.5 to 3 parts of Gd2O3, 0.02 to 0.2 parts of MnCO3 and 3 to 8 parts of glass powder with deionied water, ball milling, dry and pre-sintering. Mix the sintered powder, Ag2O with deionied water, ball milling and dry. Add olefin, heat and griddle, compress molding with 4 to 8 Mpa pressure and warm to remove wax. Heat and keep warm to get the high permittivity metal-dielectric complex ceramic capacitor medium. This invention improves the capacitance temperature variation of ceramic with high dielectric constant at room temperature and reduces waste.
Description
Technical field
The invention belongs to electronic information material and components and parts field, particularly relate to a kind of metal-dielectric ceramics condenser dielectric and preparation method thereof.
Background technology
Anti-electromagnetic interference (EMI) filter is a kind of novel assembling device that is widely used in recent years.It can suppress electromagnetic noise effectively, improves the antijamming capability of electronic equipment and the reliability of microcircuit system.It is the X7R ceramic formula of base that the dielectric material of present most of EMI capacitive filters adopts with the barium titanate, according to EIA (Electronic IndustriesAssociation) standard, X represents the low temperature limit-55 ℃ of operation temperature area, 7 represent high temperature limit+125 ℃ of operation temperature area, and the rate of change of the capacitance of R representative all temperature spots in operation temperature area during with respect to 25 ℃ of room temperatures be less than or equal to ± and 15%.But performance can rapid deterioration more than+125 ℃ the time for X7R series ceramic material, in order to adapt to the application under the specific hot environment, can use the EMI filtering capacitor ceramic medium material of X8R series (wherein the high temperature limit of 8 expression operation temperature areas is+150 ℃) to replace X7R series.This just requires to improve in the preparation process of material in the room temperature dielectric constant, further the broadening operation temperature area.
Yet existing is the conventional doping modification method of the ceramic capacitor dielectric material of base with the barium titanate, all is to realize by kind and the addition of regulating modifier, though this kind method energy broadening operation temperature area can make dielectric constant decrease.People such as Wang Sheng are at the 21st volume the 2nd interim " BaTiO that delivers in the March, 2006 of " Journal of Inorganic Materials "
3-Nb
2O
5-Ni
2O
3The Dielectric Properties of ternary system " room temperature dielectric constant of mentioning the X8R material that they make in the literary composition reaches 2080, and this is difficult to satisfy ceramic capacitor miniaturization, high performance requirement.
Summary of the invention
The objective of the invention is to overcome deficiency of the prior art, provide a kind of and can satisfy the X8R performance requirement, in the broadening operation temperature area, effectively improve the high-dielectric metal-electric composite ceramic capacitor medium of its dielectric constant.
Second purpose of the present invention provides a kind of preparation method of high-dielectric metal-electric composite ceramic capacitor medium.
Technical scheme of the present invention is summarized as follows:
A kind of high-dielectric metal-electric composite ceramic capacitor medium, make with following method:
(1) takes by weighing raw material: BaTiO by weight
3100 parts, Nb
2O
50.5~4 parts, 3~6 parts of MgO, Gd
2O
30.5~3 parts, MnCO
30.02~0.2 part, 3~8 parts in glass dust, described glass dust are to be made up of following component by weight percentage: Bi
2O
315~40%, Pb
3O
415~25%, TiO
210~40%, H
3BO
310~30%; Described BaTiO
3Be to handle through 1050~1100 ℃ of pre-burnings;
(2) be that 1: 1~5 ratio adds deionized water by weight with raw material, mix that ball milling 3~6 hours was in 120~140 ℃ of bakings 5~8 hours;
(3) 300~400 ℃ of pre-burnings 3~6 hours;
(4) be 100: 2~6: 100~500 ratio powder, the Ag after with pre-burning by weight
2O and deionized water mixed the back ball milling 0.5~2 hour, in 120~140 ℃ of bakings 5~8 hours;
(5) adding percentage by weight in the powder after step (4) baking is 5%~7% binding agent heating paraffin mixing, crosses 1000 holes/cm
2Sub-sieve is pressed into the disc green compact under 4~8Mpa pressure, green compact were warming up to 450~600 ℃ of de-waxings 0.5~2.5 hour through 3~6 hours;
(6) be heated to 1130~1150 ℃ through 1~3 hour, be incubated 1~4 hour, make the high-dielectric metal-electric composite ceramic capacitor medium.
Preferably, described step (1) takes by weighing raw material: BaTiO by weight
3100 parts, Nb
2O
51 part, 4 parts of MgO, Gd
2O
32 parts, MnCO
30.05 part, 6 parts in glass dust, described glass dust are to be made up of following component by weight percentage: Bi
2O
325%, Pb
3O
425%, TiO
230%, H
3BO
320%; Described BaTiO
3Be to handle through 1050~1100 ℃ of pre-burnings.
A kind of preparation method of high-dielectric metal-electric composite ceramic capacitor medium comprises the steps:
(1) takes by weighing raw material: BaTiO by weight
3100 parts, Nb
2O
50.5~4 parts, 3~6 parts of MgO, Gd
2O
30.5~3 parts, MnCO
30.02~0.2 part, 3~8 parts in glass dust, described glass dust are to be made up of following component by weight percentage: Bi
2O
315~40%, Pb
3O
415~25%, TiO
210~40%, H
3BO
310~30%; Described BaTiO
3Be to handle through 1050~1100 ℃ of pre-burnings;
(2) be that 1: 1~5 ratio adds deionized water by weight with raw material, mix that ball milling 3~6 hours was in 120~140 ℃ of bakings 5~8 hours;
(3) 300~400 ℃ of pre-burnings 3~6 hours;
(4) be 100: 2~6: 100~500 ratio powder, the Ag after with pre-burning by weight
2O and deionized water mixed the back ball milling 0.5~2 hour, in 120~140 ℃ of bakings 5~8 hours;
(5) adding percentage by weight in the powder after step (4) baking is 5%~7% binding agent heating paraffin mixing, crosses 1000 holes/cm
2Sub-sieve is pressed into the disc green compact under 4~8Mpa pressure, green compact were warming up to 450~600 ℃ of de-waxings 0.5~2.5 hour through 3~6 hours;
(6) be heated to 1130~1150 ℃ through 1~3 hour, be incubated 1~4 hour, make the high-dielectric metal-electric composite ceramic capacitor medium.
Preferably, described step (1) takes by weighing raw material: BaTiO by weight
3100 parts, Nb
2O
51 part, 4 parts of MgO, Gd
2O
32 parts, MnCO
30.05 part, 6 parts in glass dust, described glass dust are to be made up of following component by weight percentage: Bi
2O
325%, Pb
3O
425%, TiO
230%, H
3BO
320%; Described BaTiO
3Be to handle through 1050~1100 ℃ of pre-burnings.
The present invention is by metal and BaTiO
3The compound dielectric constant that can increase porcelain effectively of base pottery cooperates and adds MnCO
3With Gd
2O
3Can significantly improve the capacity rate of temperature change of porcelain, and make porcelain at room temperature have higher dielectric constant.The interpolation of glass can effectively reduce sintering temperature, and reduces the loss under the room temperature.High-dielectric metal-electric composite ceramic capacitor medium sintering temperature of the present invention low (1130~1150 ℃), and have big capacity (ε 〉=5000), high-temperature stability (Δ C/C
25 ℃≤ ± 15% ,-55~+ 150 ℃), low-loss (tg δ≤1.5%) and good insulation electricalresistivity
v〉=10
11Premium properties such as Ω cm have wide application development prospect.In addition, preparation technology of the present invention is simple, preparation process is pollution-free, and can use the electrode slurry of 30%Pd-70%Ag, interior electrode of chip capacitor and complex media material is burnt till simultaneously, thereby can further reduce production costs.
Embodiment
Below in conjunction with specific embodiment invention is further described.
Embodiment 1
A kind of preparation method of high-dielectric metal-electric composite ceramic capacitor medium comprises the steps:
(1) takes by weighing raw material: BaTiO by weight
3100 parts, Nb
2O
51 part, 4 parts of MgO, Gd
2O
32 parts, MnCO
30.05 part, 6 parts in glass dust, described glass dust are to be made up of following component by weight percentage: Bi
2O
325%, Pb
3O
425%, TiO
230%, H
3BO
320%; Described BaTiO
3Be to handle through 1060 ℃ of pre-burnings;
(2) be that 1: 3 ratio adds deionized water by weight with raw material, mix that ball milling 5 hours was in 130 ℃ of bakings 6 hours;
(3) 300 ℃ of pre-burnings 4 hours;
(4) be 100: 5: 300 ratio powder, the Ag after with pre-burning by weight
2O and deionized water mixed the back ball milling 1.5 hours, in 130 ℃ of bakings 6 hours;
(5) adding percentage by weight in the powder after step (4) baking is 6% binding agent heating paraffin mixing, crosses 1000 holes/cm
2Sub-sieve is pressed into the disc green compact under 6Mpa pressure, green compact were warming up to 550 ℃ of de-waxings 0.5 hour through 4 hours;
(6) be heated to 1130 ℃ through 2 hours, (also can be heated to 1140 ℃ or 1150 ℃) is incubated 3 hours, makes the high-dielectric metal-electric composite ceramic capacitor medium.
Embodiment 2
A kind of preparation method of high-dielectric metal-electric composite ceramic capacitor medium comprises the steps:
(1) takes by weighing raw material: BaTiO by weight
3100 parts, Nb
2O
50.5 part, 3 parts of MgO, Gd
2O
30.5 part, MnCO
30.2 part, 3 parts in glass dust, described glass dust are to be made up of following component by weight percentage: Bi
2O
315%, Pb
3O
415%, TiO
240%, H
3BO
330%; Described BaTiO
3Be to handle through 1050 ℃ of pre-burnings;
(2) be that 1: 1 ratio adds deionized water by weight with raw material, mix that ball milling 3 hours was in 120 ℃ of bakings 8 hours;
(3) 400 ℃ of pre-burnings 3 hours;
(4) be 100: 2: 100 ratio powder, the Ag after with pre-burning by weight
2O and deionized water mixed the back ball milling 0.5 hour, in 120 ℃ of bakings 8 hours;
(5) adding percentage by weight in the powder after step (4) baking is 5% binding agent heating paraffin mixing, crosses 1000 holes/cm
2Sub-sieve is pressed into the disc green compact under 4Mpa pressure, green compact were warming up to 450 ℃ of de-waxings 2.5 hours through 3 hours;
(6) be heated to 1130 ℃ (also can be heated to 1140 ℃ or 1150 ℃) through 1 hour, be incubated 1 hour, make the high-dielectric metal-electric composite ceramic capacitor medium.
Embodiment 3
A kind of preparation method of high-dielectric metal-electric composite ceramic capacitor medium comprises the steps:
(1) takes by weighing raw material: BaTiO by weight
3100 parts, Nb
2O
54 parts, 6 parts of MgO, Gd
2O
33 parts, MnCO
30.02 part, 8 parts in glass dust, described glass dust are to be made up of following component by weight percentage: Bi
2O
340%, Pb
3O
425%, TiO
225%, H
3BO
310%; Described BaTiO
3Be to handle through 1100 ℃ of pre-burnings;
(2) be that 1: 5 ratio adds deionized water by weight with raw material, mix that ball milling 6 hours was in 140 ℃ of bakings 5 hours;
(3) 300 ℃ of pre-burnings 6 hours;
(4) be 100: 6: 500 ratio powder, the Ag after with pre-burning by weight
2O and deionized water mixed the back ball milling 2 hours, in 140 ℃ of bakings 5 hours;
(5) adding percentage by weight in the powder after step (4) baking is 7% binding agent heating paraffin mixing, crosses 1000 holes/cm
2Sub-sieve is pressed into the disc green compact under 8Mpa pressure, green compact were warming up to 600 ℃ of de-waxings 1 hour through 6 hours;
(6) be heated to 1130 ℃ (also can be heated to 1140 ℃ or 1150 ℃) through 3 hours, be incubated 4 hours, make the high-dielectric metal-electric composite ceramic capacitor medium.
Embodiment 4
A kind of preparation method of high-dielectric metal-electric composite ceramic capacitor medium comprises the steps:
(1) takes by weighing raw material: BaTiO by weight
3100 parts, Nb
2O
53 parts, 5 parts of MgO, Gd
2O
31.5 part, MnCO
30.1 part, 5 parts in glass dust, described glass dust are to be made up of following component by weight percentage: Bi
2O
335%, Pb
3O
425%, TiO
210%, H
3BO
330%; Described BaTiO
3Be to handle through 1070 ℃ of pre-burnings;
(2) be that 1: 4 ratio adds deionized water by weight with raw material, mix that ball milling 4 hours was in 130 ℃ of bakings 7 hours;
(3) 350 ℃ of pre-burnings 4 hours;
(4) be 100: 4: 300 ratio powder, the Ag after with pre-burning by weight
2O and deionized water mixed the back ball milling 1 hour, in 130 ℃ of bakings 8 hours;
(5) adding percentage by weight in the powder after step (4) baking is 6% binding agent heating paraffin mixing, crosses 1000 holes/cm
2Sub-sieve is pressed into the disc green compact under 5Mpa pressure, green compact were warming up to 550 ℃ of de-waxings 1 hour through 4 hours;
(6) be heated to 1130 ℃ (also can be heated to 1140 ℃ or 1150 ℃) through 2 hours, be incubated 2 hours, make the high-dielectric metal-electric composite ceramic capacitor medium.
Embodiment 5
Method of testing of the present invention is as follows:
One, the detection of the dielectric constant of disc medium
Utilize the capacitance C of HP427gA electric capacity instrument measuring samples, according to the dielectric constant of formula 1 calculation sample.
Wherein: C is the capacitance of sample, and unit is pF.
D is the diameter of sample, and unit is cm.
D is the thickness of sample, and unit is cm.
Two, the measurement of sample insulation resistivity
Utilize ZC36 type ultra-high resistance instrument to measure the Yang Pinde insulation resistance, utilize following formula to calculate the volume resistivity ρ of material
v(unit is Ω cm):
Wherein: R
iBe the insulation resistance of sample, unit is Ω.
D is the diameter of sample, and unit is cm.
D is the thickness of sample, and unit is cm.
Three, the measurement of sample dielectric loss
Utilize the dielectric loss tg δ (1kHz) of HP4278A electric capacity instrument measuring samples.
The test result of the embodiment of the invention is listed in the table 1, Max| Δ C/C
25 ℃| (%) Zhi warm area scope is-55 ℃~+ 150 ℃.
The test result of table 1 ceramic capacitor dielectric sample of the present invention
Embodiment | Firing temperature ℃ | Temperature retention time (hour) | The sample dielectric property | |||
ε | tanδ | ρ v(Ω·cm) | Max|ΔC/C 25℃|(%) | |||
1 | 1130 | 3 | 5460 | 0.0125 | 9.76×10 11 | 13.7 |
1140 | 3 | 5589 | 0.0134 | 8.94×10 11 | 13.5 | |
1150 | 3 | 5294 | 0.0119 | 9.02×10 11 | 12.7 | |
2 | 1130 | 1 | 5241 | 0.0142 | 6.79×10 11 | 11.6 |
1140 | 1 | 5344 | 0.0137 | 7.36×10 11 | 10.8 | |
1150 | 1 | 5407 | 0.0148 | 7.89×10 11 | 10.4 | |
3 | 1130 | 4 | 5298 | 0.0158 | 9.86×10 11 | 14.1 |
1140 | 4 | 5167 | 0.0146 | 1.02×10 12 | 13.7 | |
1150 | 4 | 4934 | 0.0147 | 1.78×10 12 | 13.6 | |
4 | 1130 | 2 | 5069 | 0.0124 | 9.77×10 11 | 12.9 |
1140 | 2 | 5287 | 0.0126 | 9.32×10 11 | 11.6 | |
1150 | 2 | 5146 | 0.013 | 8.49×10 11 | 12.5 |
By the test result of table 1 as can be seen, whole high-temperature stabilities of embodiment, Δ C/C in-55~+ 150 ℃ scope
25 ℃Less than ± 15%, loss tg δ less than 1.5%, the electricalresistivity
vGreater than 10
11Ω cm, except that 1150 ℃ of firing temperatures of embodiment 3, all the other embodiment all have larger capacity, ε reaches intermediate sintering temperature provided by the invention, has than the goal of the invention of the X8R composite ceramic capacitor medium of current more high-k greater than 5000.
Claims (4)
1. high-dielectric metal-electric composite ceramic capacitor medium is characterized in that making with following method:
(1) takes by weighing raw material: BaTiO by weight
3100 parts, Nb
2O
50.5~4 parts, 3~6 parts of MgO, Gd
2O
30.5~3 parts, MnCO
30.02~0.2 part, 3~8 parts in glass dust, described glass dust are to be made up of following component by weight percentage: Bi
2O
315~40%, Pb
3O
415~25%, TiO
210~40%, H
3BO
310~30%; Described BaTiO
3Be to handle through 1050~1100 ℃ of pre-burnings;
(2) be that 1: 1~5 ratio adds deionized water by weight with raw material, mix that ball milling 3~6 hours was in 120~140 ℃ of bakings 5~8 hours;
(3) 300~400 ℃ of pre-burnings 3~6 hours;
(4) be 100: 2~6: 100~500 ratio powder, the Ag after with pre-burning by weight
2O and deionized water mixed the back ball milling 0.5~2 hour, in 120~140 ℃ of bakings 5~8 hours;
(5) adding percentage by weight in the powder after step (4) baking is 5%~7% binding agent heating paraffin mixing, crosses 1000 holes/cm
2Sub-sieve is pressed into the disc green compact under 4~8Mpa pressure, green compact were warming up to 450~600 ℃ of de-waxings 0.5~2.5 hour through 3~6 hours;
(6) be heated to 1130~1150 ℃ through 1~3 hour, be incubated 1~4 hour, make the high-dielectric metal-electric composite ceramic capacitor medium.
2. a kind of high-dielectric metal-electric composite ceramic capacitor medium according to claim 1 is characterized in that described step (1) is for taking by weighing raw material: BaTiO by weight
3100 parts, Nb
2O
51 part, 4 parts of MgO, Gd
2O
32 parts, MnCO
30.05 part, 6 parts in glass dust, described glass dust are to be made up of following component by weight percentage: Bi
2O
325%, Pb
3O
425%, TiO
230%, H
3BO
320%; Described BaTiO
3Be to handle through 1050~1100 ℃ of pre-burnings.
3. the preparation method of a high-dielectric metal-electric composite ceramic capacitor medium is characterized in that comprising the steps:
(1) takes by weighing raw material: BaTiO by weight
3100 parts, Nb
2O
50.5~4 parts, 3~6 parts of MgO, Gd
2O
30.5~3 parts, MnCO
30.02~0.2 part, 3~8 parts in glass dust, described glass dust are to be made up of following component by weight percentage: Bi
2O
315~40%, Pb
3O
415~25%, TiO
210~40%, H
3BO
310~30%; Described BaTiO
3Be to handle through 1050~1100 ℃ of pre-burnings;
(2) be that 1: 1~5 ratio adds deionized water by weight with raw material, mix that ball milling 3~6 hours was in 120~140 ℃ of bakings 5~8 hours;
(3) 300~400 ℃ of pre-burnings 3~6 hours;
(4) be 100: 2~6: 100~500 ratio powder, the Ag after with pre-burning by weight
2O and deionized water mixed the back ball milling 0.5~2 hour, in 120~140 ℃ of bakings 5~8 hours;
(5) adding percentage by weight in the powder after step (4) baking is 5%~7% binding agent heating paraffin mixing, crosses 1000 holes/cm
2Sub-sieve is pressed into the disc green compact under 4~8Mpa pressure, green compact were warming up to 450~600 ℃ of de-waxings 0.5~2.5 hour through 3~6 hours;
(6) be heated to 1130~1150 ℃ through 1~3 hour, be incubated 1~4 hour, make the high-dielectric metal-electric composite ceramic capacitor medium.
4. the preparation method of a kind of high-dielectric metal-electric composite ceramic capacitor medium according to claim 3 is characterized in that described step (1) is for taking by weighing raw material: BaTiO by weight
3100 parts, Nb
2O
51 part, 4 parts of MgO, Gd
2O
32 parts, MnCO
30.05 part, 6 parts in glass dust, described glass dust are to be made up of following component by weight percentage: Bi
2O
325%, Pb
3O
425%, TiO
230%, H
3BO
320%; Described BaTiO
3Be to handle through 1050~1100 ℃ of pre-burnings.
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CN2007100570062A CN101030478B (en) | 2007-03-27 | 2007-03-27 | High-dielectric metal-electric medium composite ceramic capacitance and its production |
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CN2007100570062A CN101030478B (en) | 2007-03-27 | 2007-03-27 | High-dielectric metal-electric medium composite ceramic capacitance and its production |
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CN101030478A true CN101030478A (en) | 2007-09-05 |
CN101030478B CN101030478B (en) | 2010-11-17 |
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ID=38715730
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Cited By (5)
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CN101226827B (en) * | 2007-12-28 | 2010-05-19 | 天津大学 | Ultra-high dielectric constant multilayer ceramic capacitor medium and preparation method thereof |
CN101868432A (en) * | 2007-10-29 | 2010-10-20 | 京瓷株式会社 | Dielectric ceramic and laminated ceramic capacitor |
CN103992107A (en) * | 2014-04-28 | 2014-08-20 | 天津大学 | Low-loss multilayer ceramic capacitor dielectric material |
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Family Cites Families (4)
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CN1065349A (en) * | 1991-03-27 | 1992-10-14 | 天津大学 | The manufacture method of high-voltage ceramic condenser medium |
CN100452257C (en) * | 2005-07-15 | 2009-01-14 | 天津大学 | Barium titanate ceramic capacitor medium and preparing method thereof |
CN100378032C (en) * | 2005-11-21 | 2008-04-02 | 天津大学 | Barium phthalate base ceramic capacity medium and preparation process thereof |
CN100456397C (en) * | 2005-11-21 | 2009-01-28 | 天津大学 | Titanium-position precursor doping modification method for Barium titanate ceramic capasitor |
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101868432A (en) * | 2007-10-29 | 2010-10-20 | 京瓷株式会社 | Dielectric ceramic and laminated ceramic capacitor |
CN101868432B (en) * | 2007-10-29 | 2013-05-29 | 京瓷株式会社 | Dielectric ceramic and laminated ceramic capacitor |
CN101226827B (en) * | 2007-12-28 | 2010-05-19 | 天津大学 | Ultra-high dielectric constant multilayer ceramic capacitor medium and preparation method thereof |
CN103992107A (en) * | 2014-04-28 | 2014-08-20 | 天津大学 | Low-loss multilayer ceramic capacitor dielectric material |
CN103992107B (en) * | 2014-04-28 | 2015-12-02 | 天津大学 | A kind of low-loss medium material for multilayer ceramic capacitors |
CN104030677A (en) * | 2014-06-24 | 2014-09-10 | 天津大学 | Low-loss multilayer ceramic capacitor dielectric material and preparation method thereof |
CN108610042A (en) * | 2018-04-27 | 2018-10-02 | 天津大学 | Dielectric material and preparation method thereof with the high insulation characterisitic of huge dielectric constant |
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