CN116102347A - High-dielectric-constant microwave dielectric ceramic for MLCC (multi-layer ceramic) and preparation method thereof - Google Patents
High-dielectric-constant microwave dielectric ceramic for MLCC (multi-layer ceramic) and preparation method thereof Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 238000005245 sintering Methods 0.000 claims abstract description 7
- 239000000126 substance Substances 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims description 7
- 238000000498 ball milling Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 claims description 3
- 229910021193 La 2 O 3 Inorganic materials 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 3
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 2
- 238000000034 method Methods 0.000 claims 3
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 6
- 238000013461 design Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 3
- 238000010295 mobile communication Methods 0.000 description 3
- 238000004891 communication Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000003989 dielectric material Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000009740 moulding (composite fabrication) Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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Abstract
The invention relates to a high dielectric constant low-loss microwave dielectric ceramic for MLCC and a preparation method thereof, wherein the chemical composition formula is aBaO-bTiO 2 ‑cSm 2 O 3 ‑dBi 2 O 3 ‑eLa 2 O 3 ‑fMnO 2 . Wherein a, b, c, d, e, f is molar proportion content, and sintering temperature is 1300-1350 ℃. The molar ratio of the alpha to the beta is 12 percent or more and 16 percent or less; b is more than or equal to 65% and less than or equal to 70%; c is more than or equal to 10% and less than or equal to 13%; d is more than or equal to 1% and less than or equal to 3%; e is more than or equal to 2% and less than or equal to 5%; e is more than or equal to 0.1% and less than or equal to 1%. The invention has the advantages that: the composition and the preparation method are reasonable in design, the obtained microwave dielectric ceramic material is good in microwave performance, the dielectric constant is 100+/-5, the dielectric loss is less than or equal to 0.03%, and the capacitance temperature coefficient TCC is less than or equal to +/-30 ppm/DEG C. The preparation method is simple to operate, good in repeatability, low in equipment requirement and very suitable for popularization and use.
Description
Technical Field
The invention relates to a high-dielectric-constant microwave dielectric ceramic for an MLCC and a preparation method thereof, belonging to the technical field of electronic ceramics and preparation thereof.
Background
The microwave dielectric ceramic is a ceramic material which is used as a dielectric material in a microwave frequency band (mainly 300MHz-300GHz frequency band) circuit and performs one or more functions, and is a key material for manufacturing a microwave dielectric filter and a resonator. With the rapid development of mobile communication industry, novel functional ceramic materials are made into microwave elements such as dielectric resonators, dielectric antennas, diplexers, dielectric wave guide loops, dielectric frequency stabilization oscillators and the like, and are widely applied to a plurality of fields such as mobile communication, satellite television broadcast communication, scattering communication military radars, satellite navigation positioning systems and the like. In recent years, due to the rapid development of fields of mobile communication, aerospace, military, modern medicine and the like, higher requirements are also put forward on microwave dielectric ceramic materials, so that searching, preparing and researching novel microwave dielectric ceramic with proper dielectric constant, low loss, near zero resonance frequency temperature coefficient and low cost and environmental protection has become a hotspot and focus of current research.
In view of the current trend of SLCC (single layer thin film capacitor) used in the microwave frequency band, it is highly demanded to reduce the size of SLCC with as high a dielectric constant as possible, to realize light, thin, short, small demands, and in some application fields, it is demanded that its dielectric loss must be 0.03% or less and its dielectric constant temperature coefficient TCC be 30ppm/°c or less.
It is well known that microwave ceramic dielectric materials have a see-saw effect between dielectric loss and temperature coefficient, and between dielectric constant and dielectric loss. And dielectric loss increases as the temperature coefficient fluctuation range increases and dielectric constant increases (equivalent to a decrease in quality factor). Therefore, it is very difficult to achieve both the reduction of the dielectric loss of high dielectric constant and the reduction of the fluctuation range value of the temperature coefficient.
For example, CN115093220A is a Mg0.5Ti0.5TaO4-based microwave dielectric ceramic material sintered at low temperature, and the dielectric loss is 0.0274 percent, but the TCC is 123.19 ppm/DEG C.
Disclosure of Invention
The invention provides a high-dielectric-constant microwave dielectric ceramic for an MLCC and a preparation method thereof, and aims to overcome the defects in the prior art, and effectively reduce the high-dielectric-constant dielectric loss and the fluctuation range value of a temperature coefficient on the premise of ensuring simple operation, good repeatability and low equipment requirement of the preparation method.
The technical solution of the invention is as follows: MLCC usesHigh-dielectric constant low-loss microwave dielectric ceramic with chemical composition formula of aBaO-bTiO 2 -cSm 2 O 3 -dBi 2 O 3 -eLa 2 O 3 -fMnO 2 . Wherein a, b, c, d, e, f is the molar ratio content. The molar ratio of the alpha to the beta is 12 percent or more and 16 percent or less; b is more than or equal to 65% and less than or equal to 70%; c is more than or equal to 10% and less than or equal to 13%; d is more than or equal to 1% and less than or equal to 3%; e is more than or equal to 2% and less than or equal to 5%; e is more than or equal to 0.1% and less than or equal to 1%. The dielectric constant of the obtained finished microwave dielectric ceramic is 100+/-5, the dielectric loss is less than or equal to 0.03%, and the capacitance temperature coefficient TCC is less than or equal to +/-30 ppm/DEG C. The fluctuation range value of the high dielectric constant dielectric loss and the temperature coefficient is reduced.
The preparation method comprises the following steps:
(1) According to aBaO-bTiO 2 -cSm 2 O 3 -dBi 2 O 3 -eLa 2 O 3 -fMnO 2 The molar ratio of (1) is taken according to aBaO-bTiO 2 -cSm 2 O 3 -dBi 2 O 3 -eLa 2 O 3 -fMnO 2 Molar ratio of BaCO 3 、TiO 2 、Sm 2 O 3 、Bi 2 O 3 、La 2 O 3 、MnO 2 Ball milling, drying and presintering after mixing to obtain a main phase material;
(2) And (3) ball milling, drying and granulating the main phase material obtained in the step (1) again, and forming, sintering and sintering at 1300-1350 ℃ to obtain the finished microwave dielectric ceramic.
The invention has the advantages that: the composition and the preparation method are reasonable in design, the obtained microwave dielectric ceramic material is good in microwave performance, the dielectric constant is 100+/-5, the dielectric loss is less than or equal to 0.03%, and the capacitance temperature coefficient TCC is less than or equal to +/-30 ppm/DEG C. The preparation method is simple to operate, good in repeatability, low in equipment requirement and very suitable for popularization and use.
Detailed Description
The present invention will be described in further detail with reference to examples and embodiments.
Examples 1 to 3 and comparative examples 1 to 3
A high-dielectric constant low-loss microwave dielectric ceramic for MLCC has a chemical composition formula of aBaO-bTiO 2 -cSm 2 O 3 -dBi 2 O 3 -eLa 2 O 3 -fMnO 2 . Wherein a, b, c, d, e, f is the molar ratio content. The molar ratios of the examples and comparative examples are set forth in the following table.
A preparation method of a high-dielectric constant low-loss microwave dielectric ceramic for MLCC comprises the following steps:
(1) According to aBaO-bT iO 2 -cSm 2 O 3 -dBi 2 O 3 -eLa 2 O 3 -fMnO 2 Molar ratio of BaCO 3 、T iO 2 、Sm 2 O 3 、Bi 2 O 3 、La 2 O 3 、MnO 2 Ball milling, drying and presintering after mixing to obtain a main phase material;
(2) And (3) ball milling, drying and granulating the main phase material obtained in the step (1) again, and finally obtaining the required microwave dielectric ceramic by molding, sintering and sintering at the temperature shown in the following table.
As can be seen from the above table, the dielectric constant (Er/Dk) of each example of the present invention is 100.+ -. 5, the dielectric loss (Df) is less than or equal to 0.03%, and the capacitance temperature coefficient TCC is less than or equal to.+ -. 30 ppm/DEG C, which is significantly better than that of each comparative example.
The foregoing is merely a preferred embodiment of the present invention, and it should be noted that modifications and improvements could be made by those skilled in the art without departing from the inventive concept, which falls within the scope of the present invention.
Claims (3)
1. A high dielectric constant low-loss microwave dielectric ceramic for MLCC is characterized in that the chemical composition formula of the microwave dielectric ceramic is aBaO-bTiO 2 -cSm 2 O 3 -dBi 2 O 3 -eLa 2 O 3 -fMnO 2 The molar ratio of a is more than or equal to 12 percent and less than or equal to 16 percent; b is more than or equal to 65% and less than or equal to 70%; c is more than or equal to 10% and less than or equal to 13%; d is more than or equal to 1 percent and less than or equal to 3 percentThe method comprises the steps of carrying out a first treatment on the surface of the E is more than or equal to 2% and less than or equal to 5%; e is more than or equal to 0.1% and less than or equal to 1%, the dielectric constant of the microwave dielectric ceramic is 100+/-5, the dielectric loss is less than or equal to 0.03%, and the capacitance temperature coefficient TCC is less than or equal to +/-30 ppm/DEG C.
2. The method for preparing the high-dielectric constant low-loss microwave dielectric ceramic for the MLCC according to claim 1, comprising the following steps:
(1) According to aBaO-bTiO 2 -cSm 2 O 3 -dBi 2 O 3 -eLa 2 O 3 -fMnO 2 Molar ratio of BaCO 3 、TiO 2 、Sm 2 O 3 、Bi 2 O 3 、La 2 O 3 、MnO 2 Ball milling, drying and presintering after mixing to obtain a main phase material;
(2) And (3) ball milling, drying, granulating, molding and sintering the main phase material obtained in the step (1) again to obtain the finished microwave dielectric ceramic.
3. The method of producing a high dielectric constant low loss microwave dielectric ceramic for MLCC according to claim 2, wherein the molding sintering temperature in said step (2) is 1300-1350 ℃.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10017422B1 (en) * | 2017-03-15 | 2018-07-10 | Huazhong University Of Science And Technology | Regulator for regulating frequency-temperature characteristics of microwave dielectric ceramics and low temperature co-fired ceramic material comprising the same |
| CN112552034A (en) * | 2020-12-25 | 2021-03-26 | 无锡鑫圣慧龙纳米陶瓷技术有限公司 | Low-loss low-dielectric-constant temperature-stable microwave dielectric ceramic and preparation method thereof |
| CN114180956A (en) * | 2021-12-20 | 2022-03-15 | 无锡鑫圣慧龙纳米陶瓷技术有限公司 | Microwave dielectric ceramic for high-dielectric-constant 5G waveguide and preparation method and application thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10017422B1 (en) * | 2017-03-15 | 2018-07-10 | Huazhong University Of Science And Technology | Regulator for regulating frequency-temperature characteristics of microwave dielectric ceramics and low temperature co-fired ceramic material comprising the same |
| CN112552034A (en) * | 2020-12-25 | 2021-03-26 | 无锡鑫圣慧龙纳米陶瓷技术有限公司 | Low-loss low-dielectric-constant temperature-stable microwave dielectric ceramic and preparation method thereof |
| CN114180956A (en) * | 2021-12-20 | 2022-03-15 | 无锡鑫圣慧龙纳米陶瓷技术有限公司 | Microwave dielectric ceramic for high-dielectric-constant 5G waveguide and preparation method and application thereof |
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Inventor after: Ji An Inventor after: Jin Zhenlong Inventor after: Zhang Bin Inventor before: Ji An Inventor before: Wang Xiaohui Inventor before: Jin Zhenlong Inventor before: Zhang Bin |