CN106892656A - A kind of low temperature sintering high-dielectric constant capacitor dielectric material - Google Patents
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Abstract
The invention discloses a kind of low temperature sintering high-dielectric constant capacitor dielectric material, chemical formula is Bi2(Mg1‑xCux)2/3Nb4/3O7, wherein x=0.05~0.2；First press chemical formula and weigh dispensing, by ball milling, drying, sieving is calcined at 750 DEG C, synthesizes principal crystalline phase；Base substrate is made required ceramic capacitor dielectric material in 850~950 DEG C of sintering after shaping.Dielectric constant of the present invention between 180~210, low dielectric loss 24.6~55.3 × 10‑4, temperature coefficient of capacitance TCC is 200 × 10‑6/ DEG C~460 × 10‑6/ DEG C between, can be used for the preparation of multiple-layer sheet ceramic capacitor, while having relatively low sintering temperature, it is possible to decrease the cost of multilayer device.
Description
Technical field
The invention belongs to a kind of ceramic composition being characterized with composition, more particularly to a kind of low temperature sintering high-dielectric constant
Temperature-stable ceramic capacitor dielectric material and preparation method.
Background technology
In recent years, the fast development of ICT promotes microwave electron system to broadband, miniaturization, integrated side
To development, it is higher that this just proposes service band wide, capacity big, small volume, easy of integration, frequency self adaptation etc. to electronic component
It is required that.Microwave dielectric material refers to be applied in microwave frequency (mainly 300MHz~300GHz frequency ranges) circuit as medium material
Expect and complete one or more dielectric material of function.This requires that microwave dielectric material has permittivity ε highr, it is low
Dielectric loss tan δ, temperature coefficient of capacitance τεClose to zero or adjustable.
Numerous studies show that Bi-based pyrochlor ceramics are the material systems with lower sintering temperature, can be assisted by doping
Optimization relation between regulation and control each microwave dielectric property of potting porcelain, is capable of achieving low temperature co-fired with silver electrode.And with dielectric
Constant is high, loss is low, temperature coefficient of capacitance is adjustable and the characteristics of low sintering temperature, is applied to multiple-layer sheet ceramic capacitor
(MLCC) preparation, and the cost of multilayer device can be substantially reduced.However, the very low (TCC of the temperature coefficient of capacitance of the material
≈-400×10-6/ DEG C), it is unfavorable for practical application.Therefore, under conditions of high-k is kept, reduce dielectric loss, obtain
Obtain nearly zero temperature coefficient of capacitance and reduce the key issue that sintering temperature etc. is badly in need of solving as researcher.
The content of the invention
The purpose of the present invention, is very low (TCC ≈ -400 × 10 of temperature coefficient of capacitance for overcoming current material-6/℃)、
It is unfavorable for the shortcoming of practical application, there is provided a kind of temperature-stable ceramic capacitor dielectric material and system with high-k
Preparation Method.
The present invention is achieved by following technical solution.
A kind of low temperature sintering high-dielectric constant capacitor dielectric material, chemical formula is Bi2(Mg1-xCux)2/3Nb4/3O7, wherein
X=0.05~0.2；
The preparation method of the capacitor dielectric material, with following steps：
(1) by raw material Bi2O3、Nb2O5, CuO, MgO press Bi2(Mg1-xCux)2/3Nb4/3O7, the wherein change of x=0.05~0.2
Formula weighs dispensing；
(2) powder that step (1) is prepared is put into ball grinder, adds zirconia ball and deionized water, ball milling 4 hours；
The raw material after ball milling is placed in infrared drying oven is again dried, 40 mesh sieves are crossed after drying, obtain evengranular powder；
(3) step (2) evengranular powder is synthesized into principal crystalline phase in being calcined 4 hours at 750 DEG C；
(4) additional mass percent is 0.75% polyvinyl alcohol in the powder after step (3) synthesis principal crystalline phase, is put into
In ball grinder, add zirconia ball and deionized water, ball milling 12 hours, after drying cross 80 mesh sieves, then with powder compressing machine with
The pressure forming of 4MPa is base substrate；
(5) base substrate after step (4) is molded is incubated 4 hours in 850~950 DEG C of sintering, is made high-k temperature
Stabilization type ceramic capacitor dielectric material.
The drying temperature of the step (2) or step (4) is 100 DEG C.
The ceramic powder of the step (2) or step (4) is 1: 1: 2 with the mass ratio of zirconia ball, deionized water.
The base substrate of the step (4) is the disk of Φ 10mm × 1mm.
The sintering temperature of the step (5) is 925 DEG C, and soaking time is 4h.
The present invention has supplied a kind of low temperature sintering high-dielectric constant capacitor dielectric material and preparation method thereof, obtained Bi2
(Mg1-xCux)2/3Nb4/3O7(x=0.05~0.2) material, is 850~950 DEG C with relatively low sintering temperature, and dielectric high is normal
Count between 180~210, low dielectric loss 24.6~55.3 × 10-4, temperature coefficient of capacitance TCC is -200 × 10-6/℃
~460 × 10-6/ DEG C in the range of, can be used for the preparation of multiple-layer sheet ceramic capacitor (MLCC), while material has relatively low burning
Junction temperature, can substantially reduce the cost of multilayer device.
Specific embodiment
Below by specific embodiment, the invention will be further described, raw materials used in example to be the commercially available pure examination of analysis
Agent, specific embodiment is as follows.
Embodiment 1
(1) by raw material Bi2O3、Nb2O5, CuO, MgO press Bi2Mg3/5Cu1/15Nb4/3O7Chemical formula weighs dispensing；
(2) powder by above-mentioned preparation is put into ball grinder, adds zirconia ball and deionized water, ball milling 4 hours, powder
It is 1: 1: 2 with the mass ratio of zirconia ball, deionized water；Raw material after ball milling is placed in infrared drying oven in baking at 100 DEG C
It is dry, 40 mesh sieves are crossed after drying, obtain evengranular powder；
(3) above-mentioned well mixed powder is synthesized into principal crystalline phase in being calcined 4 hours at 750 DEG C；
(4) additional mass percent is 0.75% polyvinyl alcohol in the powder of synthesis principal crystalline phase after firing, is put into ball
In grinding jar, zirconia ball and deionized water are added, powder is 1: 1: 2 with the mass ratio of zirconia ball, deionized water, and ball milling 12 is small
When, 80 mesh sieves are crossed after drying, then with powder compressing machine with base substrate that the pressure forming of 4MPa is Φ 10mm × 1mm；
(5) base substrate after above-mentioned shaping is sintered 4 hours in 925 DEG C, is made low temperature sintering high-dielectric constant capacitor Jie
Material；
(6) its dielectric properties, under 1MHz, ε are tested using Agilent 4278A electric impedance analyzersr=181, tan δ=
24.9×10-4, TCC=-49 × 10-6/℃。
Embodiment 2~6
Embodiment 2~6 is essentially identical with the preparation method of embodiment 1, is only that X values are different with sintering temperature.
The related process parameters and dielectric properties of the specific embodiment of the invention refer to table 1.
Table 1
The present invention is not limited to above-described embodiment, and the change of some details is possible, but therefore this do not run counter to this hair
Bright scope and spirit.
Claims (5)
1. a kind of low temperature sintering high-dielectric constant capacitor dielectric material, chemical formula is Bi2(Mg1-xCux)2/3Nb4/3O7, wherein x
=0.05~0.2.
The preparation method of the capacitor dielectric material, with following steps：
(1) by raw material Bi2O3、Nb2O5, CuO, MgO press Bi2(Mg1-xCux)2/3Nb4/3O7, the wherein chemical formula of x=0.05~0.2
Weigh dispensing；
(2) powder that step (1) is prepared is put into ball grinder, adds zirconia ball and deionized water, ball milling 4 hours；Again will
Raw material after ball milling is placed in infrared drying oven and dries, and 40 mesh sieves are crossed after drying, obtains evengranular powder；
(3) step (2) evengranular powder is synthesized into principal crystalline phase in being calcined 4 hours at 750 DEG C；
(4) additional mass percent is 0.75% polyvinyl alcohol in the powder after step (3) synthesis principal crystalline phase, is put into ball milling
In tank, zirconia ball and deionized water are added, ball milling 12 hours crosses 80 mesh sieves after drying, then with powder compressing machine with 4MPa's
Pressure forming is base substrate；
(5) base substrate after step (4) is molded is incubated 4 hours in 850~950 DEG C of sintering, is made high-k temperature stabilization
Type ceramic capacitor dielectric material.
2. a kind of low temperature sintering high-dielectric constant capacitor dielectric material according to claim 1, it is characterised in that described
The drying temperature of step (2) or step (4) is 100 DEG C.
3. a kind of low temperature sintering high-dielectric constant capacitor dielectric material according to claim 1, it is characterised in that described
The ceramic powder of step (2) or step (4) is 1: 1: 2 with the mass ratio of zirconia ball, deionized water.
4. a kind of low temperature sintering high-dielectric constant capacitor dielectric material according to claim 1, it is characterised in that described
The base substrate of step (4) is the disk of Φ 10mm × 1mm.
5. a kind of low temperature sintering high-dielectric constant capacitor dielectric material according to claim 1, it is characterised in that described
The sintering temperature of step (5) is 925 DEG C, and soaking time is 4h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107459351A (en) * | 2017-08-31 | 2017-12-12 | 天津大学 | A kind of temperature-stable Dielectric Materials at Radio Frequencies |
| CN112851346A (en) * | 2021-02-25 | 2021-05-28 | 电子科技大学 | Ultra-low-loss zirconium magnesium niobate system microwave dielectric ceramic material and preparation method thereof |
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| CN101172849A (en) * | 2007-10-26 | 2008-05-07 | 华南理工大学 | Low-temperature sintering high dielectric constant dielectric ceramic and method for producing the same |
| CN102718477A (en) * | 2012-05-14 | 2012-10-10 | 福建火炬电子科技股份有限公司 | High dielectric constant X8R type MLCC medium material and preparation method |
| CN103467083A (en) * | 2013-08-29 | 2013-12-25 | 中国人民解放军国防科学技术大学 | Low-temperature-sintering microwave dielectric ceramic with high dielectric constant and preparation method of microwave dielectric ceramic |
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2017
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| FR2845685B1 (en) * | 2002-10-15 | 2005-06-17 | CERAMIC MATERIAL WITH HIGH PERMITTIVITY, PROCESS FOR PRODUCING THE MATERIAL AND APPLICATION TO CERAMIC MULTILAYER STRUCTURES | |
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Non-Patent Citations (1)
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| LINGXIA LI ET AL.: ""Structures, phase transformations, and dielectric properties of Bi2(Zn1-xMgx)2/3Nb4/3O7 pyrochlore ceramics as temperature stable LTCC material"", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107459351A (en) * | 2017-08-31 | 2017-12-12 | 天津大学 | A kind of temperature-stable Dielectric Materials at Radio Frequencies |
| CN112851346A (en) * | 2021-02-25 | 2021-05-28 | 电子科技大学 | Ultra-low-loss zirconium magnesium niobate system microwave dielectric ceramic material and preparation method thereof |
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