CN113004028B - Silicon-based low-dielectric microwave dielectric ceramic and preparation method thereof - Google Patents
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Abstract
The invention belongs to the technical field of microwave dielectric ceramics, and particularly relates to a silicon-based low-dielectric microwave dielectric ceramic and a preparation method thereof. The chemical general formula is xBaO-yMO-zSiO 2 (M＝Ca,Sr；0<x is less than or equal to 1.0; y is more than or equal to 1.0 and less than or equal to 2.0; z is more than or equal to 1.0 and less than or equal to 3.0) is used for preparing the microwave dielectric ceramic material. The ceramic has a low dielectric constant (epsilon) r = 7.3-11.0), excellent quality factor (Q multiplied by f = 5370-40500 GHz) and wider sintering temperature (1150-1250 ℃), and the microwave dielectric ceramic has negative temperature coefficient of resonance frequency (-76.6 ppm/DEG C ≦ tau f Less than or equal to-36.3 ppm/DEG C). The low sintering temperature and the excellent quality factor of the microwave dielectric ceramic can enable the silicon-based low-dielectric microwave dielectric material to be applied to the BME-MLCC field.
Description
Technical Field
The invention belongs to the technical field of microwave dielectric ceramics, and particularly relates to a silicon-based low-dielectric microwave dielectric ceramic and a preparation method thereof.
Background
The microwave dielectric ceramic is a ceramic material which is used as a medium in a microwave frequency band (300 MHz-300 GHz) circuit. With the continuous improvement of the operating frequency of the communication equipment, the signal delay phenomenon becomes more obvious, the system loss and the heat productivity are increased, and the system stability is gradually deteriorated. The low dielectric constant can reduce the cross coupling loss between the material and the electrode, and can improve the transmission rate of the electric signal, and the excellent quality factor can reduce the system loss and can improve the frequency selection characteristic of the material. In consideration of environmental friendliness, low cost and other factors, the research on the silicon-based low-dielectric-constant microwave dielectric ceramic is particularly important.
A multilayer ceramic capacitor (MLCC) is a component widely used in surface mount technology, and as a basic element in the electronic industry, the demand of MLCCs has increased by about 10% per year in recent years, but the export of MLCCs is more than 90% from countries such as japan and usa. MLCCs are classified into Precious Metal inner Electrode multilayer ceramic capacitors (PME-MLCCs) and Base Metal inner Electrode multilayer ceramic capacitors (BME-MLCCs) according to the types of inner electrodes. The PME-MLCC adopts an expensive Ag or Ag-Pd electrode and can be sintered in the air. While BME-MLCCs generally employ relatively inexpensive Cu or Ni electrodes, BME-MLCCs are relatively inexpensive but require sintering in a reducing atmosphere. The low production cost and the stable production process are the targets of the need of efforts in the MLCC field in China.
In order to prepare a competitive MLCC product, it is important to research a microwave dielectric ceramic that can resist reduction (does not contain variable-price elements), is low in price (is rich in Si, ba, ca, etc.), and has a sintering temperature below the melting point of a Cu or Ni electrode.
Disclosure of Invention
Aiming at the defects or improvement requirements of the prior art, the invention provides the application of the compound in preparing the microwave dielectric ceramic, and widens the selection range of the BME-MLCC microwave dielectric ceramic material with low dielectric constant.
To achieve the above object, according to one aspect of the present invention, there is provided a use of a compound having a chemical formula of xBaO-yMO-zSiO for preparing a microwave dielectric ceramic 2 Wherein M = Ca, sr;0<x≤1.0；1.0≤y≤2.0；1.0≤z≤3.0。
Preferably, the dielectric constant of the microwave dielectric ceramic prepared by the compound is between 7.3 and 11.0, the quality factor Qxf is 5370 to 40500GHz, and the temperature coefficient tau of the resonant frequency is f The range of (A) is as follows: -76.6 ppm/. Degree.C.ltoreq.tau f ≤-36.3ppm/℃。
Preferably, the microwave dielectric ceramic is prepared according to the following method:
step (1): according to the chemical expression of xBaO-yMO-zSiO 2 Weighing BaCO according to the stoichiometric ratio 3 、CaCO 3 、SrCO 3 And SiO 2 Weighing the powder M to obtain Ca or Sr, performing wet ball milling treatment, drying after ball milling, and then pre-sintering to obtain pre-sintered ceramic powder;
step (2): and (2) performing secondary wet ball milling treatment on the pre-sintered ceramic powder obtained in the step (1), drying, adding a binder for granulation, tabletting and sintering to obtain the microwave dielectric ceramic.
Preferably, in the wet ball milling treatment in the step (1), the wet ball milling dispersing agent is 300wt% of deionized water and the medium is zirconium balls, and the ball milling process is ball milling at a speed of 360r/min for 5 hours.
Preferably, the temperature of the pre-sintering in the step (1) is 1000-1100 ℃, and the pre-sintering time is 5-10 hours.
Preferably, the binder in the step (2) is PVA or paraffin, and the mass fraction of the added binder is 5-10%.
Preferably, the sintering temperature in the step (2) is 1150-1250 ℃, and the sintering time is 5-10 hours.
In general, compared with the prior art, the above technical solution contemplated by the present invention can achieve the following beneficial effects:
(1) The invention adopts the chemical general formula of xBaO-yMO-zSiO 2 (M＝Ca,Sr；0<x is less than or equal to 1.0; y is more than or equal to 1.0 and less than or equal to 2.0; z is more than or equal to 1.0 and less than or equal to 3.0) is used for preparing the microwave dielectric ceramic material, and the novel microwave dielectric ceramic has the advantages of low dielectric constant, excellent quality factor, single phase component and stable performance.
(2) The invention provides a microwave dielectric ceramic for BME-MLCC, which does not contain variable valence elements, has low raw material cost and sintering temperature below the melting point of a Ni electrode.
Drawings
FIG. 1 is a flow chart of the preparation of the silicon-based low dielectric microwave dielectric ceramic of the present invention;
FIG. 2 is an XRD spectrum of the silicon-based low dielectric microwave dielectric ceramic of the present invention;
FIG. 3 is an SEM image of a silicon-based low-dielectric microwave dielectric ceramic according to the present invention;
FIG. 4 is a diagram of the dielectric properties of a silicon-based low dielectric microwave ceramic sample and microwave.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the invention. In addition, the technical features involved in the respective embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The invention provides an application of a compound in preparing microwave dielectric ceramics, wherein the chemical formula of the compound is xBaO-yMO-zSiO 2 Wherein M = Ca, sr;0<x≤1.0；1.0≤y≤2.0；1.0≤z≤3.0。
When the compound is used for preparing microwave dielectric ceramics, the microwave dielectric ceramics has low dielectric constant and excellent quality factor (Q multiplied by f = 5370-40500 GHz), the dielectric constant range is wide and is between 7.3 and 11.0, and the microwave dielectric ceramics has low dielectric constant and negative resonant frequency temperature coefficient (-76.6 ppm/DEG C ≦ tau ≦ T ≦ f ≤-36.3ppm/℃)。
The microwave dielectric ceramic is prepared by the following method:
step (1): according to the chemical expression of xBaO-yMO-zSiO 2 Weighing BaCO according to the stoichiometric ratio 3 、CaCO 3 、SrCO 3 And SiO 2 Wherein M = Ca, sr;0<x is less than or equal to 1.0; y is more than or equal to 1.0 and less than or equal to 2.0; z is more than or equal to 1.0 and less than or equal to 3.0, weighing, performing wet ball milling treatment, drying after ball milling, and then presintering to obtain presintering ceramic powder;
step (2): and (2) performing secondary wet ball milling treatment on the pre-sintered ceramic powder obtained in the step (1), drying, adding a binder for granulation, tabletting and sintering to obtain the microwave dielectric ceramic.
As a specific implementation mode, in the wet ball milling treatment in the step (1), deionized water with a dispersant of 300wt% and zirconium balls as a medium are used as the wet ball milling dispersing agent, and the ball milling process is to perform ball milling at a speed of 360r/min for 5 hours.
In a specific embodiment, the pre-sintering in step (1) is performed at a temperature of 1000 ℃ to 1100 ℃ for 5 to 10 hours, and the pre-sintering is performed to obtain a pre-sintered phase of the ceramic powder.
As a specific implementation mode, the binder in the step (2) is PVA or paraffin, and the mass fraction of the added binder is 5-10%.
As a specific implementation mode, the sintering temperature in the step (2) is 1150-1250 ℃, and the sintering time is 5-10 hours.
The novel microwave dielectric ceramic prepared by the invention has low dielectric constant and excellent comprehensive microwave dielectric property. The low dielectric constant is favorable for improving the transmission rate of electric signals in a dielectric material, the excellent comprehensive microwave dielectric property reduces the loss of system work and improves the stability, and the low-dielectric constant material does not contain variable-price elements, has low raw material cost and sintering temperature below the melting point of a Ni electrode, and is suitable for the field of BME-MLCC.
The following are examples:
examples 1 to 5
The preparation method of the microwave dielectric ceramic comprises the following steps:
(1) Will analyze pure BaCO 3 、CaCO 3 、SrCO 3 And SiO 2 Respectively mixing according to the stoichiometric proportion, mixing and stirring the powder for 5 hours by using a ball mill with zirconium balls as a medium and deionized water as a dispersing agent, wherein the rotating speed is 360r/min; drying the obtained slurry, and presintering for 5 hours at 1050 ℃ to obtain presintering ceramic powder;
(2) Performing wet ball milling treatment on the pre-sintered ceramic powder obtained in the step (1), drying the dispersant by using deionized water, adding 8wt% of polyvinyl alcohol (PVA) adhesive into the dried powder for granulation, and pressing the powder into a cylindrical green compact sample with the thickness-to-diameter ratio of 0.4-0.6 under the pressure of 150 MPa; and sintering the pressed ceramic in air at 1150-1250 ℃ for 5 hours to obtain the microwave dielectric ceramic shown in the table 1.
TABLE 1 examples 1 to 5, sintering temperatures and microwave dielectric Properties
From the examples 1 to 5, the novel silicon-based microwave dielectric ceramic material has low dielectric constant and good microwave dielectric property, the dielectric constant is between 7.30 and 11.0, the quality factor is between 5370 and 40500GHz, the phase components are single, the material does not contain variable valence elements, the sintering temperature is lower than the melting point of a Ni electrode, and the like, and the novel silicon-based microwave dielectric ceramic material can be applied to the field of BME-MLCC.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (3)
1. A silicon-based low-dielectric microwave dielectric ceramic is characterized in that: comprises a ceramic body, the ceramic body
The porcelain body is prepared from a compound having the chemical formulaxBaO-yMO-zSiO 2 In which
M=Ca,Sr; 0<x≤1.0; 1.0≤y≤2.0; 1.0≤z≤3.0；
The silicon-based low-dielectric microwave dielectric ceramic has excellent microwave dielectric property and relative dielectric constant
7.3 to 11.0, quality factorQ×f5370 to 40500GHz and a resonant frequency temperature coefficient of-76.6
ppm/°C ≤ τf ≤-36.3 ppm/°C。
2. The method of claim 1, wherein the dielectric ceramic is prepared from silicon-based low-k microwave dielectric ceramic
The method comprises the following steps:
(1) According to the chemical expression asxBaO-yMO-zSiO 2 (M=Ca,Sr; 0<x≤1.0; 1.0≤y≤2.0;
Z is more than or equal to 1.0 and less than or equal to 3.0) and weighing BaCO according to the stoichiometric ratio 3 、CaCO 3 、SrCO 3 And SiO 2 Wet method after weighing
Performing ball milling treatment, drying after ball milling, and then presintering to obtain presintering ceramic powder;
(2) Carrying out secondary wet ball milling treatment on the pre-sintered ceramic powder obtained in the step (1), and drying
Adding a bonding agent for granulation after drying, and sintering after tabletting to obtain the microwave dielectric ceramic;
(3) The wet ball milling treatment in the steps (1) and (2) is carried out, and the ball milling dispersing agent accounts for 300wt%
The deionized water and the medium are zirconium balls, and the ball milling process comprises the steps of ball milling for 5 hours at the speed of 360r/min
The content of the adhesive in the step (2) is 5 to 10 wt%.
3. The method for preparing silicon-based low-dielectric microwave dielectric ceramic according to claim 2
Characterized in that: the temperature of the pre-sintering in the step (1) is 1000-1100 ℃, and the pre-sintering time is 5-10
Hours; the sintering temperature of the step (2) is 1150-1250 ℃, and the sintering time is 5-10 hours
When the user wants to use the device.
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| CN102030477A (en) * | 2009-10-07 | 2011-04-27 | 旭硝子株式会社 | Ceramic material composition |
| CN101805172A (en) * | 2010-02-05 | 2010-08-18 | 华中科技大学 | Microwave dielectric ceramic material with ultra-low dielectric constant |
| CN102214775A (en) * | 2010-04-02 | 2011-10-12 | 旭硝子株式会社 | Substrate for mounting light-emitting element and light-emitting device employing the substrate |
| CN101863655A (en) * | 2010-06-08 | 2010-10-20 | 杭州电子科技大学 | Microwave dielectric ceramic material and preparation method thereof |
| CN104496442A (en) * | 2014-11-27 | 2015-04-08 | 中国计量学院 | Microwave dielectric ceramic powder with low dielectric constant, and preparation method thereof |
| CN107637185A (en) * | 2015-06-29 | 2018-01-26 | 株式会社村田制作所 | The manufacture method of multilayer ceramic substrate and multilayer ceramic substrate |
| CN106927804A (en) * | 2017-03-15 | 2017-07-07 | 华中科技大学 | A kind of microwave-medium ceramics temperature frequency characteristic adjusting control agent and its LTCC materials |
| CN109320225A (en) * | 2018-09-30 | 2019-02-12 | 天津大学 | A kind of preparation method of ultralow dielectric loss calcium and magnesium silicon systems microwave-medium ceramics |
| CN109928753A (en) * | 2019-03-14 | 2019-06-25 | 杭州电子科技大学 | A kind of low-k silicon substrate microwave dielectric ceramic materials and preparation method thereof |
| CN112279632A (en) * | 2020-10-31 | 2021-01-29 | 林玉婷 | Microwave dielectric ceramic and preparation method thereof |
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