CN113004028A - Silicon-based low-dielectric microwave dielectric ceramic and preparation method thereof - Google Patents
Silicon-based low-dielectric microwave dielectric ceramic and preparation method thereof Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 53
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 20
- 239000010703 silicon Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
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- 238000000034 method Methods 0.000 claims description 12
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 8
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical group [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 4
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
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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-zSiO2(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)r7.3-11.0), excellent quality factor (Qxf 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 ≦ taufLess 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 required efforts in the MLCC field in China.
In order to prepare a competitive MLCC product, it is important to research a microwave dielectric ceramic which can resist reduction (does not contain elements easy to change price), has low price (is rich in Si, Ba, Ca and the like) 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 the preparation of 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 the formula xBaO-yMO-zSiO for preparing a microwave dielectric ceramic2Wherein 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 5370-40500 GHz, and the temperature coefficient tau of the resonant frequency isfThe range of (A) is as follows: -76.6 ppm/. degree.C.ltoreq.tauf≤-36.3ppm/℃。
Preferably, the microwave dielectric ceramic is prepared according to the following method:
step (1): according to the chemical expression of xBaO-yMO-zSiO2Weighing BaCO according to the stoichiometric ratio3、CaCO3、SrCO3And SiO2Weighing 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 300 wt% 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 pre-sintering temperature 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-zSiO2(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 are not intended to limit the invention. In addition, the technical features involved in the 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-zSiO2Wherein 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 (Qxf is 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 is less than or equal to tau and less than or equal to tau)f≤-36.3ppm/℃)。
The microwave dielectric ceramic is prepared according to the following method:
step (1): according to the chemical expression of xBaO-yMO-zSiO2Weighing BaCO according to the stoichiometric ratio3、CaCO3、SrCO3And SiO2Wherein 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, wet ball milling treatment is carried out after weighing, drying is carried out after ball milling, and then presintering is carried out 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 300 wt% 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.
As a specific implementation mode, the pre-sintering temperature in the step (1) is 1000-1100 ℃, the pre-sintering time is 5-10 hours, and the pre-sintering aims to obtain a pre-sintering 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 BaCO3、CaCO3、SrCO3And SiO2Respectively mixing according to a stoichiometric proportion, taking zirconium balls as a medium and deionized water as a dispersing agent, and mixing and stirring the powder for 5 hours by using a ball mill at the rotating speed of 360 r/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 8 wt% 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 1-5, the novel silicon-based microwave dielectric ceramic material has a low dielectric constant and good microwave dielectric property, the dielectric constant of the novel silicon-based microwave dielectric ceramic material is 7.30-11.0, the quality factor of the novel silicon-based microwave dielectric ceramic material is 5370-40500 GHz, the novel silicon-based microwave dielectric ceramic material is single in phase component, free of variable-valence elements, low in sintering temperature lower than the melting point of a Ni electrode and the like, and 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 (6)
1. A silicon-based low-dielectric microwave dielectric ceramic is characterized in that: comprises a ceramic body, wherein the ceramic body is prepared from a compound with a chemical formula of xBaO-yMO-zSiO2Wherein M ═ Ca, Sr; 0<x≤1.0；1.0≤y≤2.0；1.0≤z≤3.0。
2. The silicon-based low dielectric microwave dielectric ceramic of claim 1, wherein: the dielectric constant of the microwave dielectric ceramic prepared by the compound is between 7.3 and 11.0, the quality factor Qxf is 5370-40500 GHz, and the temperature coefficient tau of the resonant frequency isfThe range of (A) is as follows: -76.6 ppm/. degree.C.ltoreq.tauf≤-36.3ppm/℃。
3. The preparation method of the silicon-based low-dielectric microwave dielectric ceramic according to claim 1, wherein the microwave dielectric ceramic is prepared according to the following method:
step (1): according to the chemical expression of xBaO-yMO-zSiO2(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 weighed3、CaCO3、SrCO3And SiO2Weighing, 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.
4. The method for preparing a silicon-based low-dielectric microwave dielectric ceramic according to claim 3, wherein the method comprises the following steps: and (3) performing wet ball milling treatment in the steps (1) and (2), wherein a ball milling dispersing agent is 300 wt% of deionized water and a medium is zirconium balls, and the ball milling process is ball milling at a speed of 360r/min for 5 hours.
5. The method for preparing a silicon-based low-dielectric microwave dielectric ceramic according to claim 3, wherein the method comprises the following steps: the pre-sintering temperature in the step (1) is 1000-1100 ℃, and the pre-sintering time is 5-10 hours; the sintering temperature in the step (2) is 1150-1250 ℃, and the sintering time is 5-10 hours.
6. The method for preparing a silicon-based low-dielectric microwave dielectric ceramic according to claim 3, wherein the method comprises the following steps: the content of the adhesive in the step (2) is 5-10 wt%.
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