CN113563072B - Microwave dielectric ceramic with medium dielectric constant - Google Patents
Microwave dielectric ceramic with medium dielectric constant Download PDFInfo
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- CN113563072B CN113563072B CN202110944011.5A CN202110944011A CN113563072B CN 113563072 B CN113563072 B CN 113563072B CN 202110944011 A CN202110944011 A CN 202110944011A CN 113563072 B CN113563072 B CN 113563072B
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
- C04B35/49—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates containing also titanium oxides or titanates
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
Abstract
The invention provides a medium dielectric constant microwave dielectric ceramic, the general expression of the formula is as follows: xHfO 2 •yTiO 2 . Wherein x is more than or equal to 35.0mol% and less than or equal to 65.0mol%, y is more than or equal to 35.0mol% and less than or equal to 65.0mol%, and x + y = 100%. The dielectric constant of the microwave dielectric ceramic provided by the invention is 30-50,Qthe value is as high as 5,000-11,000 (at 10GHz), and the temperature coefficient of the resonant frequency is near zero. The microwave dielectric ceramic provided by the invention can enable microwave components such as dielectric resonators, filters and the like to be simultaneously suitable for applications of decimetric waves and centimeter waves, and can be expected to solve the key material problems of 5G mobile communication and the like. Therefore, the present invention is industrially very valuable.
Description
Technical Field
The invention relates to the field of microwave communication, in particular to a medium dielectric constant microwave dielectric ceramic for a resonator and a filter.
Background
In recent years, with rapid development of mobile communication and satellite communication technologies, there has been an increasing demand for microwave dielectric ceramics for microwave devices such as dielectric resonators and filters. With the rapid development of 5G mobile communication, the microwave dielectric ceramic with ultralow dielectric constant and ultralow loss is required urgently. The basic performance requirements are as follows: dielectric constant of 30 ≤
Less than or equal to 50, quality factorQTemperature coefficient of resonance frequency of not less than 5,000 (at working frequency)
= 0 
5 ppm/℃。
The existing Ba-based composite perovskite ceramics and the like have medium dielectric constant, ultralow loss and near-zero temperature coefficient of fidelity frequency,however, it usually contains noble metals such as Ta and Nb, and has the disadvantages of too high process sensitivity of microwave dielectric property, difficult control, etc. And BaTi ４ O ９ ，Ｂa 2 Ti ９ O ２０ 、(Zr, Sn)TiO 4 The problem of low Q value exists in ceramics and the like, and the requirement of the development of 5G mobile communication to a higher frequency band is difficult to adapt.
Disclosure of Invention
A medium dielectric constant microwave dielectric ceramic has a general formula as follows: xHfO 2 • yTiO 2 . Wherein x is more than or equal to 35.0mol% and less than or equal to 65.0mol%, y is more than or equal to 35.0mol% and less than or equal to 65.0mol%, and x + y = 100%.
HfTiO 2 4 Microwave dielectric ceramics with a main crystal phase.
The microwave dielectric ceramic with the formula has a medium dielectric constant (30-50) and ultralow dielectric loss (Q=5,000-11,000 at 10GHz) and a temperature coefficient of near-zero resonance frequency (-10 ppm/DEG C. less than or equal to
Not more than +10 ppm/DEG C), is used as a key material of a microwave resonator and a filter, and is suitable for the field of microwave communication.
The invention has the advantages of
1. The existing (Zr, Sn) TiO 4 The ceramic and the like have the problems of low Q value and the like, and are difficult to adapt to the requirement of the development of 5G mobile communication to a higher frequency band. The dielectric ceramic provided by the invention has ultralow loss (Q=5,000-11,000 at 10GHz) and good temperature stability, and can provide key basic materials for 5G mobile communication and the like.
2. The microwave dielectric ceramic provided by the invention takes hafnium oxide as a grid material, and has good compatibility with semiconductor materials such as silicon and the like.
Due to the different electronic structure of Hf, Zr and Sn, HfTiO is used 4 Dielectric ceramics, which are the predominant crystalline phase, have low non-simple harmonic vibration terms and thus lower dielectric losses.
Drawings
FIG. 1 is an XRD pattern of a ceramic of different composition.
Detailed Description
Firstly, HfO with a purity of 99.9% or more is added 2 With TiO 2 Mixing at a certain ratio for 24 hr by wet ball milling (solvent is anhydrous ethanol), adding binder, granulating, and molding under uniaxial pressure at 1000 kg/cm 2 Preparing a ceramic blank with the diameter of 6 mm and the thickness of 3-6 mm under the pressure of the microwave dielectric ceramic, and finally sintering the ceramic blank for 3 hours at 1375-1450 ℃ in an atmospheric atmosphere to prepare the required microwave dielectric ceramic.
The sintered ceramic sample was subjected to phase analysis by powder X-ray diffraction method, and the microwave dielectric properties were evaluated at 10GHz by the cylindrical dielectric resonator method.
In the example, the XRD pattern of the ceramic is shown in FIG. 1, and HfTiO can be obtained 4 Single phase (x = y =50mol%; x =45mol%, y =55mol%) or a structure having it as a main crystal phase (x =65mol%, y =35 mol%). The microwave dielectric properties of the materials of the examples are shown in Table 1 in relation to the composition. As can be seen from Table 1, in the ceramic system of the present invention, TiO is accompanied by TiO 2 The content is increased, the dielectric constant of the material tends to increase, and tau f From negative to positive values, andQthe value increases first and then decreases slightly. In all component formulations of this example, HfO 2 =50.0 mol%，TiO 2 Formulation of = 50.0mol% has optimal microwave dielectric properties:
= 38.2, Q=11,000 in 10GHz,
= -4 ppm/℃。
TABLE 1 relationship between microwave dielectric properties and composition
Claims (2)
1. The microwave dielectric ceramic with medium dielectric constant is characterized by using HfTiO 4 Is a main crystal phase and is preparedThe expression is as follows: xHfO 2 • yTiO 2 (ii) a Wherein x is more than or equal to 35.0mol% and less than or equal to 65.0mol%, y is more than or equal to 35.0mol% and less than or equal to 65.0mol%, and x + y = 100%;
the preparation method of the microwave dielectric ceramic with the medium dielectric constant comprises the following steps:
HfO with purity of more than 99.9 percent 2 With TiO 2 Mixing at a certain ratio by wet ball milling method for 24 hr in anhydrous ethanol as solvent, adding binder, granulating, and molding under uniaxial pressure at 1000 kg/cm 2 Preparing a ceramic blank with the diameter of 6 mm and the thickness of 3-6 mm under the pressure of the microwave dielectric ceramic, and finally sintering the ceramic blank for 3 hours at 1375-1450 ℃ in an atmospheric atmosphere to prepare the required microwave dielectric ceramic.
2. The dielectric constant microwave dielectric ceramic of claim 1, which is used as a key material for microwave resonators and filters in the field of microwave communications.
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| CN202110944011.5A CN113563072B (en) | 2021-08-17 | 2021-08-17 | Microwave dielectric ceramic with medium dielectric constant |
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| CN113563072B true CN113563072B (en) | 2022-09-20 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1751415A (en) * | 2003-02-18 | 2006-03-22 | 大见忠弘 | Antenna for portable terminal and portable terminal using same |
| JP2008156214A (en) * | 2006-11-28 | 2008-07-10 | Ngk Insulators Ltd | Cordierite ceramic and method for manufacturing cordierite ceramic |
| FR2959505A1 (en) * | 2010-04-28 | 2011-11-04 | Saint Gobain Ct Recherches | COATED MULLITE GRAINS. |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7572695B2 (en) * | 2005-05-27 | 2009-08-11 | Micron Technology, Inc. | Hafnium titanium oxide films |
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2021
- 2021-08-17 CN CN202110944011.5A patent/CN113563072B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1751415A (en) * | 2003-02-18 | 2006-03-22 | 大见忠弘 | Antenna for portable terminal and portable terminal using same |
| JP2008156214A (en) * | 2006-11-28 | 2008-07-10 | Ngk Insulators Ltd | Cordierite ceramic and method for manufacturing cordierite ceramic |
| FR2959505A1 (en) * | 2010-04-28 | 2011-11-04 | Saint Gobain Ct Recherches | COATED MULLITE GRAINS. |
Non-Patent Citations (3)
| Title |
|---|
| Effects of Ti Doping on the Dielectric Properties of HfO2 Nanoparticles;S. Pokhriyal et al.;《AIP Conference Proceedings》;20160510;第1728卷(第1期);第020457-1至第020457-6页 * |
| HfTiO高k栅介质Ge MOS电容的制备及特性分析;朱秋玲等;《压电与声光》;20071015(第05期);第583-585页 * |
| HfxTi(1-x)O2电子结构与光学性质的第一性原理研究;段国玉等;《红外与毫米波学报》;20100815(第04期);第264-267页 * |
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