CN111943675A - Preparation method of neodymium-calcium-aluminum-titanate microwave dielectric material based on reaction sintering - Google Patents
Preparation method of neodymium-calcium-aluminum-titanate microwave dielectric material based on reaction sintering Download PDFInfo
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Abstract
The invention discloses a preparation method of a neodymium-calcium aluminum titanate microwave dielectric material based on reaction sintering, which comprises the following steps: CaCO with the purity of more than or equal to 99 percent3、TiO2、Nd2O3And Al2O3According to Ca1.15Nd0.85Al0.85Ti0.15O4(CNAT for short) batching, then carrying out wet ball milling and mixing on the materials for 4 hours, taking ethanol as a ball milling medium, drying, then pressing and molding by adopting a hand pressing mode, and finally sintering the porcelain at 1450-1550 ℃ for 6 hours; the microwave dielectric ceramic prepared by the method has moderate dielectric constant r =17.1~19.2,Q ×fValue is high,Up to 74920GHzTemperature coefficient of resonant frequency near zeroτ f =‑3.2~‑1.2ppm/℃The method can be used for manufacturing microwave devices such as resonators, antennas, filters and the like.
Description
Technical Field
The invention relates to a reactive sintering-based neodymium-calcium-aluminum-titanate microwave dielectric material preparation method, and belongs to the technical field of microwave dielectric material preparation.
Background
The microwave dielectric material is ceramic which is used as a medium and can complete one or more functions in a microwave frequency band (300 MHz-300 GHz) circuit, and is mainly used for preparing microwave components such as a resonator, a filter, a dielectric antenna, a dielectric guided wave loop and the like. In recent years, with the development of low cost, miniaturization and light weight of microwave components, microwave dielectric materials are required to have excellent microwave dielectric properties (high Q × f value, moderate dielectric constant, near-zero τ f value), low production cost and low density.
For calcium neodymium aluminium titanate Ca1.15Nd0.85Al0.85Ti0.15O4The traditional solid phase method has the defects of high sintering temperature, large grain size and the like, and has adverse effect on the performance of the microwave dielectric ceramic.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the preparation method of the neodymium-calcium-aluminum-titanate microwave dielectric material based on reaction sintering is provided, the pre-sintering process of ceramics is omitted, the preparation process is simpler, the preparation period of the ceramics is greatly shortened, and the preparation cost of the ceramics is effectively reduced.
The technical scheme adopted by the invention is as follows: a preparation method of neodymium-calcium-aluminum-titanate microwave dielectric material based on reaction sintering comprises the following steps:
s1 CaCO with purity more than or equal to 99%3、TiO2、Nd2O3And Al2O3According to Ca1.15Nd0.85Al0.85Ti0.15O4Weighing and then mixing materials; according to the mass ratio of the absolute ethyl alcohol to the powder of 1: 1, adding absolute ethyl alcohol into the powder, mixing for 4 hours by a wet grinding method, drying at 120-140 ℃ after grinding, and sieving by a 80-mesh sieve;
s2, pressing the powder obtained in the step (1) after granulation into a small cylinder with the diameter of 12mm and the thickness of 6mm, and sintering a sample of the small cylinder at 1450-1550 ℃ for 6 hours to obtain the required microwave dielectric ceramic material.
The invention has the beneficial effects that: compared with the prior art, the invention combines the two processes of pre-sintering and sintering in the ceramic preparation process into a whole, and omits the pre-sintering process of ceramic powder compared with the traditional solid-phase reaction method, thereby greatly shortening the preparation process, saving the cost, and having excellent microwave performance of the material: moderate dielectric constantr17.1 to 19.2, high Q multiplied by f value up to 74920GHz, and nearly zero temperature coefficient of resonance frequency tauf-3.2 to-1.2 ppm/deg.C, and can be used for resonator, antenna and filterThe manufacture of microwave devices such as wave filters.
Detailed Description
The invention is further described below with reference to specific examples.
Example 1: a preparation method of neodymium-calcium-aluminum-titanate microwave dielectric material based on reaction sintering comprises the following steps:
s1 CaCO with purity more than or equal to 99%3、TiO2、Nd2O3And Al2O3According to Ca1.15Nd0.85Al0.85Ti0.15O4Weighing and then mixing materials; according to the mass ratio of the absolute ethyl alcohol to the powder of 1: 1, adding absolute ethyl alcohol into the powder, mixing for 4 hours by a wet grinding method, drying at 120-140 ℃ after grinding, and sieving by a 80-mesh sieve;
s2, pressing the powder obtained in the step (1) after granulation into a small cylinder with the diameter of 12mm and the thickness of 6mm, and sintering a sample of the small cylinder at 1450-1550 ℃ for 6 hours to obtain the required microwave dielectric ceramic material. The invention combines the two processes of pre-sintering and sintering in the ceramic preparation process into a whole, and saves the pre-sintering process of ceramic powder while ensuring excellent performance of the ceramic compared with the traditional solid-phase reaction method, thereby greatly shortening the preparation process and saving the cost.
The main difference between reactive sintering and other sintering processes is that before sintering and heating, particles in the pressed pellets do not have highly agglomerated clusters like a calcination process or a high-energy ball mill, and compared with a traditional solid phase method, the method has the advantages of simple process and high densification degree.
Table 1 lists 10 specific examples of different sintering temperatures constituting the invention and their microwave dielectric properties, where Ca1.15Nd0.85Al0.85Ti0.15O4Abbreviated CNAT. The preparation method is as described above, and the evaluation of the microwave dielectric property is carried out by the cylindrical dielectric resonator method.
The ceramic can be widely used for manufacturing microwave electronic components such as various dielectric substrates, antennas, filters and the like, and meets the technical requirements of modern mobile communication systems.
Table 1:
examples of the invention | Composition of | Sintering temperature (. degree. C.) | εr | Q×f(GHz) | τf(ppm/℃) |
1 | CNAT | 1450℃ | 17.1 | 62240 | -1.2 |
2 | CNAT | 1475℃ | 18.8 | 74920 | -2.7 |
3 | CNAT | 1500℃ | 19.2 | 74090 | -1.3 |
4 | CNAT | 1525℃ | 19.2 | 44580 | -3.2 |
5 | CNAT | 1550℃ | 18.6 | 60570 | -3.0 |
The above description is only an embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of changes or substitutions within the technical scope of the present invention, and therefore, the scope of the present invention should be determined by the scope of the claims.
Claims (1)
1. A preparation method of neodymium calcium aluminum titanate microwave dielectric material based on reaction sintering is characterized by comprising the following steps: the method comprises the following steps:
s1 CaCO with purity more than or equal to 99%3、TiO2、Nd2O3And Al2O3According to Ca1.15Nd0.85Al0.85Ti0.15O4Weighing and then mixing materials; according to the mass ratio of the absolute ethyl alcohol to the powder of 1: 1, adding absolute ethyl alcohol into the powder, mixing for 4 hours by a wet grinding method, drying at 120-140 ℃ after grinding, and sieving by a 80-mesh sieve;
s2, pressing the powder obtained in the step (1) after granulation into a small cylinder with the diameter of 12mm and the thickness of 6mm, and sintering a sample of the small cylinder at 1450-1550 ℃ for 6 hours to obtain the required microwave dielectric ceramic material.
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Citations (7)
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US6403053B1 (en) * | 1997-12-15 | 2002-06-11 | National Science Council | Preparation of translucent strontium barium niobate ceramics using reaction sintering |
CN102153343A (en) * | 2011-01-10 | 2011-08-17 | 天津大学 | Method for preparing high Q-value magnesium titanate base microwave medium ceramics by adopting reactive sintering method |
CN104387057A (en) * | 2014-11-12 | 2015-03-04 | 桂林理工大学 | Temperature-stable titanium-based spinel microwave dielectric ceramic and low-temperature preparation method thereof |
CN105272245A (en) * | 2015-10-30 | 2016-01-27 | 天津大学 | Low-loss zinc zirconium and niobium series microwave dielectric ceramic prepared by reaction sintering method |
CN107253856A (en) * | 2017-06-26 | 2017-10-17 | 桂林理工大学 | A kind of microwave dielectric material of near-zero resonance frequency temperature coefficient and preparation method thereof |
CN110423117A (en) * | 2019-07-15 | 2019-11-08 | 深圳顺络电子股份有限公司 | A kind of high q-factor microwave dielectric ceramic materials and preparation method thereof |
CN110723968A (en) * | 2019-11-06 | 2020-01-24 | 苏州博恩希普新材料科技有限公司 | Microwave dielectric ceramic with high dielectric constant and preparation method thereof |
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US6403053B1 (en) * | 1997-12-15 | 2002-06-11 | National Science Council | Preparation of translucent strontium barium niobate ceramics using reaction sintering |
CN102153343A (en) * | 2011-01-10 | 2011-08-17 | 天津大学 | Method for preparing high Q-value magnesium titanate base microwave medium ceramics by adopting reactive sintering method |
CN104387057A (en) * | 2014-11-12 | 2015-03-04 | 桂林理工大学 | Temperature-stable titanium-based spinel microwave dielectric ceramic and low-temperature preparation method thereof |
CN105272245A (en) * | 2015-10-30 | 2016-01-27 | 天津大学 | Low-loss zinc zirconium and niobium series microwave dielectric ceramic prepared by reaction sintering method |
CN107253856A (en) * | 2017-06-26 | 2017-10-17 | 桂林理工大学 | A kind of microwave dielectric material of near-zero resonance frequency temperature coefficient and preparation method thereof |
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