CN108610042A - Dielectric material and preparation method thereof with the high insulation characterisitic of huge dielectric constant - Google Patents

Dielectric material and preparation method thereof with the high insulation characterisitic of huge dielectric constant Download PDF

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CN108610042A
CN108610042A CN201810395427.4A CN201810395427A CN108610042A CN 108610042 A CN108610042 A CN 108610042A CN 201810395427 A CN201810395427 A CN 201810395427A CN 108610042 A CN108610042 A CN 108610042A
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dielectric constant
high insulation
insulation characterisitic
medium material
ceramic medium
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李玲霞
王瑞杰
王文波
张宁
卢特
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Tianjin University
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Abstract

A kind of ceramic medium material with the high insulation characterisitic of huge dielectric constant, raw material composition and its molar ratio are BaCO3︰ TiO2︰ Nb2O51 ︰ of ︰ MgO=1 ︰, 0.001~0.02 ︰ 0.001~0.02；After weighing dispensing by chemical formula, through ball milling, drying, sieving, then additional mass percent are 7% binder, it is granulated, is pressed into green compact, then after dumping, under reducing atmosphere, in 1300~1450 DEG C of sintering, the ceramic medium material of the high insulation characterisitic of huge dielectric constant is made.For dielectric constant of the present invention 40000, insulation resistivity can reach 1011The order of magnitude can be used for the preparation of multiple-layer sheet ceramic capacitor under reducing atmosphere (MLCC), substantially increase the performance of multilayer ceramic capacitor device.

Description

Dielectric material and preparation method thereof with the high insulation characterisitic of huge dielectric constant
Technical field
The ceramic composition that the invention belongs to a kind of characterized by ingredient, more particularly to a kind of huge dielectric constant height insulation are special The ceramic medium material and preparation method thereof of property.
Background technology
World today's electronic technology is developed by leaps and bounds, and people are to lightening, miniaturization laptop and smart mobile phone etc. The demand of electronic equipment steeply rises, and promotes electronic component to develop towards micromation direction, lot of domestic and foreign scholar also phase After having carried out relevant research work.The component one of most as usage amount in electronic product --- capacitor micromation It realizes and largely affects the micromation of electronic product and the realization of each performance.The ability that capacitor stores charge is main Depending on its size and used dielectric constant of the dielectric material, the big dielectric material of dielectric constant can ensure same stored Capacitor sizes are substantially reduced under the premise of ability.Have excellent performance huge dielectric constant material (ε ＞ 10 so developing4), Various fields in electronics technology can be made to realize breakthrough.In addition to this, dielectric loss and insulation characterisitic are also to weigh material One of important indicator parameter of system, closely and reliability is related, low-dielectric loss and high spy of insulating to the low-loss of component Property realization be the key that realize material electronic component industry production apply.
Barium titanate is a kind of excellent strong dielectric material, but pure phase barium titanate room temperature dielectric constant is relatively low and dielectric constant with Temperature change is larger, to meet the requirement of practical application, usually need to be doped modification to it.Existing experimental data is found Nb2O5Barium titanate doping is in N2Lower annealing will appear huge dielectric constant phenomenon；In addition, when being sintered under air, the incorporation meeting of MgO So that the dielectric loss and insulation characterisitic of the system are promoted.This invention is expected that by both the above dopant and mixes jointly It is miscellaneous, sintering condition is adjusted to prepare each performance preferably barium titanate based ceramic.
In reducing atmosphere (N2/H2) under be sintered, be conducive to the generation of barium titanate based ceramic material Lacking oxygen, in this process In, to ensure that charge balance will produce electronics.The electronics of generation jumps between each lattice point of intra-die can cause grain semiconducting The dielectric constant and conductivity difference of effect, crystal grain and grain boundaries can cause crystal particle crystal boundary interface to assemble a large amount of space electricity Lotus forms interfacial polarization so as to cause huge dielectric constant.By changing sintering atmosphere, ventilation content etc. to obtain best performance Barium phthalate base huge dielectric constant ceramics.
Invention content
The purpose of the present invention, be the prior art on the basis of, adapt to electronic component towards micromation direction develop, A kind of ceramic medium material and preparation method thereof with the high insulation characterisitic of huge dielectric constant is provided.
The present invention is achieved by following technical solution.
A kind of ceramic medium material with the high insulation characterisitic of huge dielectric constant, raw material composition and its molar ratio are BaCO3︰ TiO2︰ Nb2O51 ︰ of ︰ MgO=1 ︰, 0.001~0.02 ︰ 0.001~0.02, are abbreviated as BTN0.001~0.02M0.001~0.02；
The preparation method of the above-mentioned ceramic medium material with the high insulation characterisitic of huge dielectric constant, is as follows：
(1) by BaTiO3、TiO2、Nb2O5, MgO in molar ratio 1 ︰, 1 ︰, 0.01 ︰ 0.01 weigh dispensing；
(2) powder that step (1) is prepared is put into ball grinder, zirconia ball and deionized water, ball milling 4 hours is added； The raw material after ball milling is placed in infrared drying oven again and is dried, 40 mesh sieve is crossed after drying, obtains evengranular powder；
(3) binder for being 7% in step (2) treated powder additional mass percent is crossed 80 mesh sub-sieves, is made Grain；
(4) the granulation powder of step (3) is pressed into green compact, after dumping, under reducing atmosphere, in 1320~1400 DEG C Sintering keeps the temperature 2~4 hours, and the ceramic medium material of the high insulation characterisitic of huge dielectric constant is made.
2. the ceramic medium material according to claim 1 with the high insulation characterisitic of huge dielectric constant, feature exist In the drying temperature of the step (2) is 100 DEG C.
The mass ratio of the powder of the step (2) and zirconia ball, deionized water is 1: 1: 2.
The green body of the step (5) is the disk shape of Φ 10mm × 1mm.
The green compact of the step (4) were warming up to 600 DEG C of progress dumpings by room temperature through 5 hours, and kept the temperature 5h.
The sintering process of the step (4) is：Green compact by room temperature through 5 DEG C/min heating rates to 1000 DEG C, then with 2 DEG C/ Min heating rates keep the temperature 3~3.5h to 1300~1450 DEG C.
The reducing atmosphere of the step (4) is to be passed through N always in sintering process2Or N2/H2Mixed gas；N2Gas Flow velocity is 50ml/min, N2/H2The gas flow rate of mixed gas is 50: 1~5ml/min.
The present invention provides a kind of ceramic medium material and preparation method thereof of the high insulation characterisitic of huge dielectric constant, the ceramics The sintering temperature of dielectric material is 1320~1400 DEG C, and for dielectric constant 40000, insulation resistivity can reach 1011The order of magnitude, can For the preparation of multiple-layer sheet ceramic capacitor under reducing atmosphere (MLCC), the property of multilayer ceramic capacitor device is substantially increased Energy.
Specific implementation mode
Below with reference to specific embodiment, the present invention is described in further detail, and the present invention is not limited to following implementations Example：
Embodiment 1
(1) by BaTiO3、TiO2、Nb2O, 1 ︰, 1 ︰, 0.005~0.015 ︰ 0.005~0.015 are weighed MgO in molar ratio Dispensing；
(2) powder that step (1) is prepared is put into ball grinder, zirconia ball and deionized water, ball milling 4 hours is added； Raw material after ball milling is placed in infrared drying oven and is dried, 40 mesh sieve is crossed after drying, obtains evengranular powder；
(3) binder that mass percent is 7% is added in step (2) treated powder, crosses 80 mesh sub-sieves, makes Grain；
(4) powder after being granulated step (3) is pressed into the disk green compact of 10 × 1.0mm of Ф at 3MPa, through 3.5h skies 600 DEG C of dumpings are warming up in gas.After dumping flow velocity be 50ml/min N2With 3.5ml/min H2In mixed airflow, then through 2 DEG C/ Min rises to 1350 DEG C of sintering, keeps the temperature 3.5h, and the ceramic medium material of the high insulation characterisitic of huge dielectric constant is made.
(5) dielectric properties and electrical property of the test article under 1KHz frequencies.
Test method is as follows：
Silver paste is uniformly coated in resulting product upper and lower surface, electrode is prepared through 850 DEG C of burning infiltrations, sample to be tested, test is made Dielectric properties.
The capacitance C and loss tan δ for the accurate LCR digital electric bridges test sample that shone together using TH2828S 1MHz, and calculate Go out the dielectric constant of sample, calculation formula is：
Embodiment 2~8
The main technologic parameters of embodiment 2~8 and its related dielectric properties and electrical property are in detail referring to table 1, Qi Tagong Skill step is substantially identical to embodiment 1.
Table 1
The invention is not limited in above-described embodiment, the variation of many details is possible, but therefore this does not violate this The scope and spirit of invention.

Claims (7)

1. a kind of ceramic medium material with the high insulation characterisitic of huge dielectric constant, raw material composition and its molar ratio are BaCO3︰ TiO2︰ Nb2O51 ︰ of ︰ MgO=1 ︰, 0.001~0.02 ︰ 0.001~0.02, are abbreviated as BTN0.001~0.02M0.001~0.02。
The preparation method of the above-mentioned ceramic medium material with the high insulation characterisitic of huge dielectric constant, is as follows：
(1) by BaTiO3、TiO2、Nb2O5, MgO in molar ratio 1 ︰, 1 ︰, 0.01 ︰ 0.01 weigh dispensing；
(2) powder that step (1) is prepared is put into ball grinder, zirconia ball and deionized water, ball milling 4 hours is added；Again will Raw material after ball milling, which is placed in infrared drying oven, dries, and 40 mesh sieve is crossed after drying, obtains evengranular powder；
(3) binder for being 7% in step (2) treated powder additional mass percent crosses 80 mesh sub-sieves, is granulated；
(4) the granulation powder of step (3) is pressed into green compact, after dumping, under reducing atmosphere, in 1320~1400 DEG C of burnings Knot keeps the temperature 2~4 hours, and the ceramic medium material of the high insulation characterisitic of huge dielectric constant is made.
2. the ceramic medium material according to claim 1 with the high insulation characterisitic of huge dielectric constant, which is characterized in that institute The drying temperature for stating step (2) is 100 DEG C.
3. the ceramic medium material according to claim 1 with the high insulation characterisitic of huge dielectric constant, which is characterized in that institute The mass ratio of the powder and zirconia ball, deionized water of stating step (2) is 1: 1: 2.
4. the ceramic medium material according to claim 1 with the high insulation characterisitic of huge dielectric constant, which is characterized in that institute The green body for stating step (5) is the disk shape of Φ 10mm × 1mm.
5. the ceramic medium material according to claim 1 with the high insulation characterisitic of huge dielectric constant, which is characterized in that institute The green compact for stating step (4) were warming up to 600 DEG C of progress dumpings by room temperature through 5 hours, and kept the temperature 5h.
6. the ceramic medium material according to claim 1 with the high insulation characterisitic of huge dielectric constant, which is characterized in that institute The sintering process for stating step (4) is：Green compact by room temperature through 5 DEG C/min heating rates to 1000 DEG C, then with 2 DEG C/min heating rates To 1300~1450 DEG C, and keep the temperature 3~3.5h.
7. the ceramic medium material according to claim 1 with the high insulation characterisitic of huge dielectric constant, which is characterized in that institute The reducing atmosphere for stating step (4) is to be passed through N always in sintering process2Or N2/H2Mixed gas；N2Gas flow rate be 50ml/ Min, N2/H2The gas flow rate of mixed gas is 50: 1~5ml/min.
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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109437888A (en) * 2018-10-24 2019-03-08 天津大学 A kind of preparation method of low-loss huge dielectric constant X8R type dielectric substance
CN110256067A (en) * 2019-06-19 2019-09-20 天津大学 A kind of preparation method of the anti-reduced form dielectric substance of niobium additive Mn
CN113277847A (en) * 2021-06-10 2021-08-20 天津大学 Anti-reduction X8R type BaTiO3Base medium ceramic material and preparation method thereof
CN114230335A (en) * 2021-12-22 2022-03-25 福建贝思科电子材料股份有限公司 BaTiO with giant dielectric constant, low loss and high resistivity3Fine crystal ceramic and its prepn
CN114436645A (en) * 2021-08-18 2022-05-06 桂林理工大学 Rare earth element doped barium titanate giant dielectric ceramic material and preparation method thereof
CN116143513A (en) * 2023-01-06 2023-05-23 陕西科技大学 Low-temperature sintering BaTiO 3 Base X8R temperature stable ceramic material and preparation method and application thereof

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