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CN113354409A - Microwave dielectric ceramic and preparation method thereof - Google Patents

Microwave dielectric ceramic and preparation method thereof Download PDF

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Publication number
CN113354409A
CN113354409A CN202110634264.2A CN202110634264A CN113354409A CN 113354409 A CN113354409 A CN 113354409A CN 202110634264 A CN202110634264 A CN 202110634264A CN 113354409 A CN113354409 A CN 113354409A
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microwave dielectric
main material
dielectric ceramic
ceramic
mass fraction
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宿金栋
蒋韶华
范宇
余亮
郭槐
梁宝龙
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Zhenjin New Materials Shenzhen Co ltd
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Zhenjin New Materials Shenzhen Co ltd
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Abstract

The invention discloses a microwave dielectric ceramic and a preparation method thereof, wherein the microwave dielectric ceramic is RO doped magnesium-calcium-titanium system ceramic, and the chemical composition expression of the microwave dielectric ceramic is aMgTiO3‑bCaTiO3-RO; wherein, the magnesium-calcium-titanium system ceramic is taken as a main material, and the chemical expression thereof is aMgTiO3‑bCaTiO3A and b respectively represent a molar ratio, a is more than or equal to 0.90 and less than or equal to 0.99, b is more than or equal to 0.01 and less than or equal to 0.1, and a + b is equal to 1; the RO is a sintering aid comprising MnO2、Fe2O3、ZnO、SiO2、Nb2O5、Cr2O3、La2O3、NiO、ZrO2And Nd2O3At least one of them. The microwave dielectric ceramic is formed by using RO (reverse osmosis) doped magnesium-calcium-titanium system ceramic as a sintering aid and has excellent performanceThe microwave dielectric property is high, the quality factor is high, the dielectric constant is moderate, the microwave dielectric property has good temperature stability and excellent mechanical property, the microwave dielectric property has wide application prospect, the preparation process is simple, the operation is convenient, and the repeatability is good.

Description

Microwave dielectric ceramic and preparation method thereof
Technical Field
The invention relates to the technical field of ceramic materials, in particular to a microwave dielectric ceramic and a preparation method thereof.
Background
As a novel functional ceramic, the microwave dielectric ceramic has the characteristics of large dielectric constant, low dielectric loss, small temperature coefficient of resonant frequency and the like, can be made into components such as a filter, a resonator, an oscillator, a waveguide transmission line, a dielectric antenna and the like, has wide application in the microwave communication fields such as mobile communication, direct satellite broadcasting, radio remote control, radar, GPS and the like, and is a key material of the current communication technology. At present, microwave dielectric ceramic filter manufacturers in the industry adopt a solid-phase method for high-temperature sintering preparation, the process is complex, the mechanical property of the ceramic is poor, the temperature stability is poor after long-time use, cracks are easy to generate, and the ceramic cannot normally work, so that the practical application of the ceramic is greatly limited.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a microwave dielectric ceramic, which aims to solve the technical problems of poor temperature stability and mechanical property and complex process of the microwave dielectric ceramic in the prior art.
The invention also aims to provide a preparation method of the microwave dielectric ceramic.
The technical scheme adopted by the invention for solving the technical problems is as follows: providing a microwave dielectric ceramic, wherein the microwave dielectric ceramic is RO doped magnesium-calcium-titanium system ceramic, and the chemical composition expression of the microwave dielectric ceramic is aMgTiO3-bCaTiO3-RO；
Wherein the magnesium-calcium-titanium system ceramic is taken as a main material, and the chemical composition expression of the ceramic is aMgTiO3-bCaTiO3A and b respectively represent a molar ratio, a is more than or equal to 0.90 and less than or equal to 0.99, b is more than or equal to 0.01 and less than or equal to 0.1, and a + b is equal to 1; the RO is a sintering aid comprising MnO2、Fe2O3、ZnO、SiO2、Nb2O5、Cr2O3、La2O3、NiO、ZrO2And Nd2O3At least one of them.
Preferably, the RO comprises MnO2The mass fraction of the material relative to the main material is 0-1%.
Preferably, the RO comprises Fe2O3The mass fraction of the material relative to the main material is 0-1%.
Preferably, the RO comprises ZnO and the mass fraction of the ZnO relative to the main material is 0% -1%.
Preferably, the RO comprises SiO2The mass fraction of the material relative to the main material is 0-1%.
Preferably, the RO comprises Nb2O5The mass fraction of the material relative to the main material is 0-1%.
Preferably, the RO comprises Cr2O3The mass fraction of the material relative to the main material is 0-1%.
Preferably, the RO comprises La2O3The mass fraction of the material relative to the main material is 0-1%.
Preferably, the RO comprises NiO, and the mass fraction of the NiO relative to the main material is 0-1%.
Preferably, the RO comprises ZrO2The mass fraction of the material relative to the main material is 0-1%.
Preferably, the RO comprises Nd2O3The mass fraction of the material relative to the main material is 0-1%.
Preferably, the particle size of the powder of the magnesium-calcium-titanium system ceramic is 1-10 μm.
The invention also provides a preparation method of the microwave dielectric ceramic, which comprises the following steps:
(1) MgO and TiO with the purity of more than 99 percent2、CaCO3The raw materials are subjected to ball milling, fully mixed, dried and presintered to obtain the magnesium-calcium-titanium system ceramic serving as a main material of the microwave dielectric ceramic;
(2) doping with sintering aid with purity over 99.9%: mixing the main material and the sintering aid, then fully ball-milling, drying, granulating and sieving, pressing and molding the sieved mixed powder, and finally sintering to obtain the microwave dielectric ceramic.
Preferably, in the step (1), the temperature for drying is 200 ℃.
Preferably, in the step (1), the pre-sintering process parameters are as follows: the presintering temperature is 1000-1200 ℃, and the presintering time is 2-6 hours.
Preferably, in the step (2), the sintering process parameters are as follows: the sintering temperature is 1300-1360 ℃, and the sintering time is 3-6 hours.
Preferably, in the step (2), the granulation is to mix the dried powder with purified water and then make the mixture into micron-sized spherical particles.
Preferably, in the step (2), the sieved powder mixture is pressed into a cylinder with a diameter of 10mm and a height of 8 mm.
Preferably, the pre-firing in the step (1) and the sintering in the step (2) are performed in an air atmosphere.
The invention has the beneficial effects that: the microwave dielectric ceramic formed by the RO doped magnesium-calcium-titanium system ceramic used as the sintering aid has excellent microwave dielectric property, high quality factor, moderate dielectric constant, good temperature stability, excellent mechanical property, wide application prospect, simple preparation process, convenient operation and good repeatability.
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.
The microwave dielectric ceramic is RO doped Mg-Ca-Ti system ceramic, and the chemical composition expression is aMgTiO3-bCaTiO3-RO。
Wherein, the magnesium-calcium-titanium system ceramic is taken as a main material, and the chemical composition expression is aMgTiO3-bCaTiO3A and b respectively represent a molar ratio, a is more than or equal to 0.90 and less than or equal to 0.99, b is more than or equal to 0.01 and less than or equal to 0.1, and a + b is equal to 1. The particle size of the powder of the magnesium-calcium-titanium system ceramic is preferably 1-10 mu m.
RO is a sintering aid, which may include MnO2、Fe2O3、ZnO、SiO2、Nb2O5、Cr2O3、La2O3、NiO、ZrO2And Nd2O3At least one of them. When the RO comprises any one of the above components, the mass fraction of the RO relative to the main material is 0-1%; when the RO comprises a plurality of the above, the mass fraction of each material relative to the main material is 0% to 1%.
The preparation method of the microwave dielectric ceramic can comprise the following steps:
(1) MgO and TiO with the purity of more than 99 percent2、CaCO3Is taken as raw material and is expressed by composition expression aMgTiO3-bCaTiO3The molar ratio of the elements is proportioned, dissolved in deionized water, ball-milled, mixed evenly, dried and presintered to obtain the magnesium-calcium-titanium system ceramic as the main material of the microwave dielectric ceramic.
Wherein the drying temperature is 200 ℃. The pre-sintering process parameters are as follows: the presintering temperature is 1000-1200 ℃, and the presintering time is 2-6 hours.
(2) Doping with sintering aid with purity over 99.9%: respectively weighing MnO according to mass fraction relative to the mass of the main material2、Fe2O3、ZnO、SiO2、Nb2O5、Cr2O3、La2O3、NiO、ZrO2And Nd2O3Mixing the main material and the sintering aid, fully ball-milling, drying, granulating, sieving, pressing and molding the sieved mixed powder, and finally sintering to obtain the microwave dielectric ceramic.
Wherein, the granulation is to mix the dried powder with purified water and then prepare micron-sized spherical particles. The sieved mixed powder was pressed into a cylinder with a diameter of 10mm and a height of 8 mm. The sintering process parameters are as follows: the sintering temperature is 1300-1360 ℃, and the sintering time is 3-6 hours.
The calcination in the step (1) and the sintering in the step (2) are both performed in an air atmosphere.
The present invention will be described in detail with reference to specific examples.
Example 1
Microwave dielectric ceramic 0.955MgTiO3-0.045CaTiO3-MnO2-SiO2MnO being a sintering aid2And SiO2Doped Mg-Ca-Ti ceramics, in which MnO is20.955MgTiO relative to the main material3-0.045CaTiO3The mass fraction of (A) is 0.21%; SiO 220.955MgTiO relative to the main material3-0.045CaTiO3The mass fraction is 0.13%.
The preparation method of the microwave dielectric ceramic comprises the following steps:
(1) MgO and TiO with the purity of more than 99 percent2、CaCO3Dissolving the raw materials in deionized water, then performing ball milling, fully and uniformly mixing, placing the prepared mixed solution in a drying oven at 200 ℃, drying, crushing and sieving; presintering the powder obtained by sieving at the presintering temperature of 1000 ℃ for 2 hours to obtain main material magnesium-calcium-titanium ceramic powder;
(2) adding sintering aid MnO into magnesium-calcium-titanium ceramic powder2And SiO2Spraying granulation and compression molding are carried out on the dispersing agent, the release agent and the binder; and sintering the formed blank in a muffle furnace at 1360 ℃ for 4 hours to obtain the microwave dielectric ceramic.
Example 2
Microwave dielectric ceramic 0.955MgTiO3-0.045CaTiO3-SiO2-ZrO2-Fe2O3Is SiO as a sintering aid2、ZrO2And Fe2O3Doped Mg-Ca-Ti ceramics, in which SiO is20.955MgTiO relative to the main material3-0.045CaTiO3The mass fraction of (A) is 0.15%; ZrO (ZrO)20.955MgTiO relative to the main material3-0.045CaTiO3The mass fraction is 0.91%; fe2O30.955MgTiO relative to the main material3-0.045CaTiO3The mass fraction is 0.18%.
The preparation method of the microwave dielectric ceramic comprises the following steps:
(1) MgO and TiO with the purity of more than 99 percent2、CaCO3Dissolving the raw materials in deionized water, and then performing ball milling to fully and uniformly mix; drying the prepared mixed solution in a drying oven at 200 ℃, crushing and sieving; presintering the powder obtained by sieving at 1050 ℃ for 2 hours to obtain main material magnesium calcium titanium ceramic powder;
(2) adding sintering aid SiO into the magnesium-calcium-titanium ceramic powder2、ZrO2And Fe2O3Spraying granulation and compression molding are carried out on the dispersing agent, the release agent and the binder; and sintering the formed blank in a muffle furnace at 1340 ℃ for 3 hours to obtain the microwave dielectric ceramic.
Example 3
Microwave dielectric ceramic 0.955MgTiO3-0.045CaTiO3-Cr2O3-ZrO2-Fe2O3-Nd2O3Sintering aid Cr2O3、ZrO2、Fe2O3、Nd2O3Doped Mg-Ca-Ti ceramics in which Cr is2O30.955MgTiO relative to the main material3-0.045CaTiO3The mass fraction is 0.05 percent; ZrO2 relative to 0.955MgTiO of main material3-0.045CaTiO3The mass fraction is 0.15%; fe2O30.955MgTiO relative to the main material3-0.045CaTiO3The mass fraction is 0.23%; nd (neodymium)2O3The mass fraction of the main material is 0.955MgTiO3-0.045CaTiO 3.
The preparation method of the microwave dielectric ceramic comprises the following steps:
(1) MgO and TiO with the purity of more than 99 percent2、CaCO3Dissolving the raw materials in deionized water, and then performing ball milling to fully and uniformly mix; drying the prepared mixed solution in a drying oven at 200 ℃, crushing and sieving; presintering the sieved powder at 1100 deg.C for 3 deg.CObtaining the main material magnesium calcium titanium ceramic powder after hours;
(2) adding a sintering aid Cr into the magnesium-calcium-titanium ceramic powder2O3、ZrO2、Fe2O3And Nd2O3Spraying granulation and compression molding are carried out on the dispersing agent, the release agent and the binder; and sintering the formed blank in the step (A) in a muffle furnace at 1360 ℃ for 3.5 hours to obtain the microwave dielectric ceramic.
Example 4
Microwave dielectric ceramic 0.955MgTiO3-0.045CaTiO3-MnO2-Nb2O5-NiO-La2O3MnO as sintering aid2、Nb2O5、NiO、La2O3Doped Mg-Ca-Ti ceramics, in which MnO is20.955MgTiO relative to the main material3-0.045CaTiO3The mass fraction of (A) is 0.16%; nb2O50.955MgTiO relative to the main material3-0.045CaTiO3The mass fraction is 0.2%; NiO 0.955MgTiO relative to the main material3-0.045CaTiO3The mass fraction is 0.12%; la2O30.955MgTiO relative to the main material3-0.045CaTiO3The mass fraction is 0.75%.
The preparation method of the microwave dielectric ceramic comprises the following steps:
(1) dissolving MgO, TiO2 and CaCO3 with the purity of more than 99 percent as raw materials in deionized water, and then fully and uniformly mixing by ball milling; drying the prepared mixed solution in a drying oven at 200 ℃, crushing and sieving; presintering the powder obtained by sieving at the presintering temperature of 1000 ℃ for 2 hours to obtain main material magnesium-calcium-titanium ceramic powder;
(2) adding sintering aid MnO into magnesium-calcium-titanium ceramic powder2、Nb2O5NiO and La2O3Spraying granulation and compression molding are carried out on the dispersing agent, the release agent and the binder; and sintering the formed blank in a muffle furnace at 1340 ℃ for 5 hours to obtain the microwave dielectric ceramic.
The performance of the microwave dielectric ceramic samples prepared in examples 1 to 4 was measured, including the relative dielectric constant ε r, the quality factor (Qxf), the temperature coefficient of resonance frequency τ f, and the mechanical properties, and the results are shown in Table 1.
TABLE 1
Figure BDA0003104771450000071
The detection results in table 1 show that the microwave dielectric ceramics prepared in embodiments 1 to 4 of the present invention have very high quality factor, near-zero temperature coefficient of resonant frequency, and appropriate relative dielectric constant, and are excellent in mechanical properties, good in reliability, free from cracks after long-term use, improved in service life, reduced in cost, excellent in microwave dielectric properties, simple in preparation process, and convenient to operate, and good in repeatability.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the present specification, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.

Claims (10)

1. The microwave dielectric ceramic is characterized by being RO doped magnesium-calcium-titanium system ceramic, and the chemical composition expression of the microwave dielectric ceramic is aMgTiO3-bCaTiO3-RO；
Wherein the magnesium-calcium-titanium system ceramic is taken as a main material, and the chemical composition expression of the ceramic is aMgTiO3-bCaTiO3A and b respectively represent a molar ratio, a is more than or equal to 0.90 and less than or equal to 0.99, b is more than or equal to 0.01 and less than or equal to 0.1, and a + b is equal to 1; the RO is a sintering aid comprising MnO2、Fe2O3、ZnO、SiO2、Nb2O5、Cr2O3、La2O3、NiO、ZrO2And Nd2O3At least one of them.
2. A microwave dielectric ceramic as claimed in claim 1,wherein the RO comprises MnO2The mass fraction of the main material is 0-1%; or the like, or, alternatively,
the RO comprises Fe2O3The mass fraction of the main material is 0-1%; or the like, or, alternatively,
the RO comprises ZnO and the mass fraction of the ZnO relative to the main material is 0-1%; or the like, or, alternatively,
the RO comprises SiO2The mass fraction of the main material is 0-1%; or the like, or, alternatively,
the RO comprises Nb2O5The mass fraction of the main material is 0-1%; or the like, or, alternatively,
the RO comprises Cr2O3The mass fraction of the main material is 0-1%; or the like, or, alternatively,
the RO comprises La2O3The mass fraction of the main material is 0-1%; or the like, or, alternatively,
the RO comprises NiO, and the mass fraction of the NiO relative to the main material is 0-1%; or the like, or, alternatively,
the RO comprises ZrO2The mass fraction of the main material is 0-1%; or the like, or, alternatively,
the RO comprises Nd2O3The mass fraction of the material relative to the main material is 0-1%.
3. A microwave dielectric ceramic as claimed in claim 1 or 2, wherein the powder particle size of the MgCaTi system ceramic is 1 to 10 μm.
4. A preparation method of a microwave dielectric ceramic as claimed in any one of claims 1 to 3, characterized by comprising the following steps:
(1) MgO and TiO with the purity of more than 99 percent2、CaCO3The raw materials are subjected to ball milling, fully mixed, dried and presintered to obtain the magnesium-calcium-titanium system ceramic serving as a main material of the microwave dielectric ceramic;
(2) doping with sintering aid with purity over 99.9%: mixing the main material and the sintering aid, then fully ball-milling, drying, granulating and sieving, pressing and molding the sieved mixed powder, and finally sintering to obtain the microwave dielectric ceramic.
5. A microwave dielectric ceramic preparation method as claimed in claim 4 wherein in step (1), the temperature of said oven drying is 200 ℃.
6. A preparation method of microwave dielectric ceramic according to claim 4, wherein in the step (1), the pre-sintering process parameters are as follows: the presintering temperature is 1000-1200 ℃, and the presintering time is 2-6 hours.
7. A method for preparing microwave dielectric ceramic according to claim 4, wherein in the step (2), the sintering process parameters are as follows: the sintering temperature is 1300-1360 ℃, and the sintering time is 3-6 hours.
8. A method for preparing microwave dielectric ceramic according to claim 4, wherein in the step (2), the granulation is to mix the dried powder with purified water and then to prepare micron-sized spherical particles.
9. A microwave dielectric ceramic preparation method as claimed in claim 4 wherein in step (2), the sieved mixed powder is pressed into a cylinder having a diameter of 10mm and a height of 8 mm.
10. A method for preparing a microwave dielectric ceramic according to claim 4 wherein the pre-firing in step (1) and the sintering in step (2) are performed in an air atmosphere.
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