CN106986636B - Low-temperature sintered microwave ceramic material and preparation method thereof - Google Patents

Low-temperature sintered microwave ceramic material and preparation method thereof Download PDF

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CN106986636B
CN106986636B CN201710236375.1A CN201710236375A CN106986636B CN 106986636 B CN106986636 B CN 106986636B CN 201710236375 A CN201710236375 A CN 201710236375A CN 106986636 B CN106986636 B CN 106986636B
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李波
郑景国
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University of Electronic Science and Technology of China
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Abstract

The invention belongs to the technical field of electronic functional ceramics and components, relates to a microwave device and a circuit, and particularly provides a low-temperature sintered microwave ceramic material and a preparation method thereof, which are used for overcoming the defect that the temperature coefficient of the existing low-temperature sintered microwave ceramic is not zeroed; the chemical expression of the microwave ceramic material is as follows: ca5+ACo4+BV6+ CO24－XCaTiO3Wherein A + B + C is-0.05-0.0, and-0.05-0.2 wt%<X is less than or equal to 10 wt%; the microwave ceramic can be co-fired with metal silver and does not chemically react with the silver, and can realize the following resonant frequency temperature coefficients: -10 ppm/DEG C to +10 ppm/DEG C, namely a zero temperature coefficient; meanwhile, the material has the characteristic of low sintering temperature, does not need to add any sintering aid, effectively prevents the dielectric property of the material from deteriorating due to the sintering aid, keeps higher density and ceramic strength, has simple preparation process, is environment-friendly and energy-saving, has good repeatability and low cost, and is easy to realize industrial production.

Description

Low-temperature sintered microwave ceramic material and preparation method thereof
Technical Field
The invention belongs to the technical field of electronic functional ceramics and components, in particular to a microwave device and a circuit, and relates to a low-temperature sintered microwave ceramic material and a preparation method thereof.
Background
The rapid development of microelectronic devices and integrated devices puts high demands on the miniaturization and light weight of electronic equipment, the integration of a single active device cannot meet the generation and application, and the miniaturization of a passive device becomes a trend, but the integration of a microstrip circuit is difficult due to a large-volume metal resonant cavity used in the prior art. Microwave multi-chip module (MMCM) modules are widely used because of their technical features of light weight, small size, low cost and high reliability, and an effective way to implement this technology is to develop multi-layer components. Low Temperature Co-fired Ceramics (LTCC) technology has become a main way to realize the integration of current electronic components because of its advantages such as higher integration density and better high frequency property. The multilayer wiring structure adopted by the LTCC technology is a passive device integration and passive device hybrid integration technology of three-dimensional assembly, can realize the integration of passive elements (resistors, capacitors, inductors and filters) and transmission lines, can be used for surface mounting of an IC (integrated circuit), and plays an important role in realizing miniaturization, multi-function modularization and improving the reliability of signals.
The interconnection conductor used in LTCC technology generally has silver metal with excellent conductivity, and its melting point is about 961 ℃, which requires that the ceramic material applied in LTCC technology must be sintered to be compact below 950 ℃, and in addition, the microwave ceramic material applied in LTCC technology should have the following characteristics: (1) a suitable dielectric constant to facilitate miniaturization of the device; (2) high quality factor to reduce loss, generally requiring Q x f ≥ 20000 GHz; (3) a near-zero temperature coefficient (10 to +10 ppm/. degree. C.) to facilitate temperature stability. However, in order to meet the temperature requirement of LTCC (sintering densification temperature is lower than 950 ℃), many high-temperature sintering microwave ceramics must be added with sintering aid (B)2O3Glass and V2O5Lower melting point oxides) such as in Ohsato H, Ohhashi T, Kato H, et al, microwave Dielectric Properties and Structure of the Ba6-3xSm8+2xTi18O54Solid Solutions[J]Ba is reported in Japanese Journal of Applied Physics,1995,34(1):187-1916-3xSm8+2xTi18O54By adding 0.5 wt% of B2O3Lowering the sintering temperature from 1733K to 1473K also lowers the quality factor and dielectric constant, which is typical of low temperature sintering in exchange for sacrificing microwave dielectric properties. Therefore, although the sintering aid can play a role in reducing sintering, the addition of the sintering aid can deteriorate the microwave dielectric property and reduce the density and the strength of the ceramic body; the structure formed by adding the sintering aid is difficult to control, the preparation process is relatively complex, the sintering aid generally needs to be prepared separately, such as through a glass melting process, the complexity of the process is increased, a large amount of energy is consumed, and the energy consumption is increased. Therefore, there has been a trend toward the development of low-temperature sintered microwave ceramics.
The vanadate system is a novel LTCC microwave dielectric material, has the advantages of low sintering temperature and high Q x f value, and is gradually concerned in recent years. For example, in Journal of the American Ceramic Society,2013,96(6):1691-1693《Novel Series of Low‐Firing Microwave Dielectric Ceramics:Ca5A4(VO4)6(A2+ ═ Mg, Zn) reported that Ca5Zn4(VO4)6And Ca5Mg4(VO4)6Microwave dielectric property of microwave ceramic sintered at 725 ℃ and 800 ℃: dielectric constants 11.7 and 9.2, quality factor Q × f 49400GHz and 53300GHz, temperature coefficients-83 ppm/° c and-50 ppm/° c; in Journal of Materials Science: Materials in Electronics 2016,27(7):7292-5Mn4(VO4)6In the report of diabetes mellitus, Ca5Mn4(VO4)6The microwave dielectric property of (2): dielectric constant 11.7, quality factor Qxf 33800GHz, temperature coefficient-70 ppm/deg.C. Although the vanadate system microwave ceramic can meet the temperature requirement of LTCC (sintering densification temperature is lower than 950 ℃), the vanadate system microwave ceramic cannot meet the requirement of near-zero temperature coefficient, and the application of the vanadate system microwave ceramic in microwave devices is severely limited, so that the research of the microwave ceramic meeting various requirements of LTCC technology is urgent.
Disclosure of Invention
The invention aims to provide a low-temperature sintering microwave ceramic material and a preparation method thereof, which are used for overcoming the defect that the temperature coefficient of the existing low-temperature sintering microwave ceramic is not zeroed; the chemical expression of the microwave ceramic material is as follows: ca5+ACo4+BV6+ CO24－XCaTiO3Wherein A + B + C is-0.05, -0.05. ltoreq. A.ltoreq.0, -0.05. ltoreq. B.ltoreq.0, -0.05. ltoreq. C.ltoreq.0, 0<X is less than or equal to 15; the microwave ceramic can be co-fired with metal silver and does not chemically react with the silver, and can realize the following resonant frequency temperature coefficients: the concentration of the active carbon is-10 ppm/DEG C to +10 ppm/DEG C, and meanwhile, the preparation process is simple, the cost is low, the repeatability is good, and the industrial production is easy.
In order to achieve the purpose, the invention adopts the technical scheme that:
the low-temperature sintering microwave ceramic material is characterized by comprising the following chemical expressions:Ca5+ACo4+BV6+CO24－XCaTiO3wherein A + B + C is-0.05-0.0, and-0.05-0.2 wt%<X is less than or equal to 10 wt% (especially 4 wt%)<X≤8wt％)。
The main crystal phase of the microwave dielectric ceramic is Ca5Co4(VO4)6The paracrystalline phase is CaTiO3。
The preparation method of the low-temperature sintering microwave ceramic material comprises the following steps:
step 1: with CaCO3、Co2O3、V2O5And CaTiO3As raw material, according to the mol ratio of CaCO3：Co2O3：V2O55+ a: 4+ B: 6+ C are mixed and evenly mixed to obtain a mixture, wherein A + B + C is-0.05 and 0, B is-0.05 and 0, C is-0.05 and 0, and 2 wt%<X≤10wt％；
Step 2: sequentially carrying out ball milling, drying and sieving on the mixture obtained in the step 1 to obtain dry powder; pre-burning for 4-6 h at the temperature of 750-850 ℃ to obtain a pre-burning material;
and step 3: performing ball milling, drying and sieving on the pre-sintered material obtained in the step 2 in sequence to obtain a secondary ball grinding material;
and 4, step 4: adding 5-10 wt% of binder PVA into the secondary ball grinding material obtained in the step (3), mixing, granulating, and forming to obtain a green body;
and 5: and (4) sintering the green body obtained in the step (4) for 1-7 hours under the conditions that the temperature is 900-950 ℃ and the atmosphere is air to obtain the microwave ceramic material.
Further, in the step 2 and the step 3, the ball milling time is as follows: 4-7 h, the drying temperature is: 80-100 ℃.
In the step 4, the granulation size is 100-250 meshes, and the molding is carried out under the pressure of 20 MPa.
The invention has the beneficial effects that:
the invention provides a low-temperature sintering microwave ceramic material and a preparation method thereof, wherein the microwave ceramic material can realize the following resonant frequency temperature coefficients: -10 ppm/DEG C to +10 ppm/DEG C, namely a zero temperature coefficient; the material has the characteristic of low sintering temperature (the sintering temperature is lower than 950 ℃), and no sintering aid is added, so that the dielectric property deterioration caused by the sintering aid is effectively prevented, and higher density and ceramic strength are kept; meanwhile, the problems that a complex phase structure formed by adding the sintering aid is difficult to control, the preparation process is complex (the sintering aid needs to be prepared separately, such as through a glass melting process) and the like are effectively avoided; in conclusion, the invention provides the low-temperature sintering microwave medium with the zero temperature coefficient, and meanwhile, the microwave ceramic material has the advantages of simple preparation process, environmental protection, energy conservation, good repeatability, low cost and easy realization of industrial production.
Drawings
FIG. 1 shows a microwave ceramic material Ca prepared in example 15+ACo4+BV6+CO24－XCaTiO3XRD diffractogram of (a).
FIG. 2 shows a microwave ceramic material Ca prepared in example 15+ACo4+BV6+CO24－XCaTiO3SEM electron micrograph of (a).
Detailed Description
The invention will be further illustrated with reference to the following specific examples:
examples 1 to 5
The chemical expression of the microwave medium provided in the above embodiment is:
the specific implementation steps for preparing the microwave ceramics of the implementation examples are as follows: ca5+ACo4+BV6+CO24－XCaTiO3Wherein, A ═ B ═ 0, C ═ 0.05, X ═ 6 wt%; the specific preparation process of the microwave ceramic material is as follows:
step 1: weighing CaCO as the raw material in accordance with the chemical formula of the invention as claimed in claim 13、Co2O3、V2O5And CaTiO3Burdening and mixing to obtain a mixture;
step 2: ball-milling the mixture obtained in the step 1 for 7 hours, drying at 100 ℃, sieving by a 40-mesh sieve, and presintering at 775 ℃ for 3 hours to obtain a presintering material;
and step 3: carrying out secondary ball milling on the obtained pre-sintered material for 7 hours, and drying the ball grinding material at 100 ℃ after the ball milling is finished to obtain a secondary ball grinding material;
and 4, step 4: adding 5-10 wt% of binder PVA into the obtained secondary ball-milled material, mixing, granulating, controlling the granulation size to be 100-250 meshes, and forming under the pressure of 20MPa to obtain a green body;
and 5: and (4) sintering the green body obtained in the step (4) for 1-7 hours under the conditions that the temperature is 900-950 ℃ and the atmosphere is air to obtain the finally required microwave ceramic.
Step 6: and (3) testing: and testing the microwave medium performance of the sample by using a network analyzer according to a Hakki-Coleman medium resonance method.
The specific composition, process parameters and microwave dielectric properties of examples 1-5 are shown in the following table:
Figure BDA0001268089130000041
while the invention has been described with reference to specific embodiments, any feature disclosed in this specification may be replaced by alternative features serving the same, equivalent or similar purpose, unless expressly stated otherwise; all of the disclosed features, or all of the method or process steps, may be combined in any combination, except mutually exclusive features and/or steps.

Claims (4)

1. The low-temperature sintering microwave ceramic material is characterized by comprising the following chemical expressions: ca5+ ACo4+BV6+CO24－XCaTiO3Wherein A + B + C is-0.05-0.0, and-0.05-0.2 wt%<X is less than or equal to 10 wt%; the main crystal phase of the microwave ceramic material is Ca5Co4(VO4)6The paracrystalline phase is CaTiO3(ii) a The resonant frequency temperature coefficient of the microwave ceramic material is as follows: -10ppm/° C to +10ppm/° C.
2. The method for preparing a low-temperature sintered microwave ceramic material according to claim 1, comprising the steps of:
step 1: with CaCO3、Co2O3、V2O5And CaTiO3As raw material, according to the mol ratio of CaCO3：Co2O3：V2O55+ a: 4+ B: 6+ C are mixed and evenly mixed to obtain a mixture, wherein A + B + C is-0.05 and 0, B is-0.05 and 0, C is-0.05 and 0, and 2 wt%<X≤10wt％；
Step 2: sequentially carrying out ball milling, drying and sieving on the mixture obtained in the step 1 to obtain dry powder; pre-burning for 4-6 h at the temperature of 750-850 ℃ to obtain a pre-burning material;
and step 3: performing ball milling, drying and sieving on the pre-sintered material obtained in the step 2 in sequence to obtain a secondary ball grinding material;
and 4, step 4: adding 5-10 wt% of binder PVA into the secondary ball grinding material obtained in the step (3), mixing, granulating, and forming to obtain a green body;
and 5: and (4) sintering the green body obtained in the step (4) for 1-7 hours under the conditions that the temperature is 900-950 ℃ and the atmosphere is air to obtain the microwave ceramic material.
3. The method for preparing the low-temperature sintered microwave ceramic material as claimed in claim 2, wherein in the step 2 and the step 3, the ball milling time is as follows: 4-7 h, the drying temperature is: 80-100 ℃.
4. The preparation method of the low-temperature sintered microwave ceramic material as claimed in claim 2, wherein in the step 4, the granulation size is 100-250 meshes, and the molding is performed under the pressure of 20 MPa.
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Low-temperature sintering and microwave dielectric properties of Ca5C4（VO4）6 ceramics;Guoguang Yao.etc;《Journal of the European Ceramic Society》;20140426;第2983-2987页 *

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