CN116023128A - Low-temperature sintered low-dielectric low-loss microwave dielectric ceramic and preparation method thereof - Google Patents
Low-temperature sintered low-dielectric low-loss microwave dielectric ceramic and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a low-temperature sintered low-dielectric low-loss microwave dielectric ceramic and a preparation method thereof, wherein the microwave dielectric ceramic consists of a main medium and an auxiliary medium, and the main medium consists of MgTiO with the molar ratio of (0.95-0.99) to (0.01-0.05) 3 And CaTiO 3 Constructing; the mass proportion of the auxiliary medium is 2-5% wt of the main medium, which is expressed as aBaO-bCAO-cSiO 2 -a zno glass ceramic, a, b, c and d each independently representing a mole percent, and satisfying the following conditions: a is more than or equal to 25% and less than or equal to 30%, b is more than or equal to 30% and less than or equal to 35%, c is more than or equal to 20% and less than or equal to 23%, d is more than or equal to 14% and less than or equal to 16%, and a+b+c+d=100%. The invention can be sintered and formed by using lower temperature, the sintered ceramic material has proper dielectric constant and near zero resonance frequency temperature coefficient, and the temperature coefficient is lowLower with low loss (i.e. with a higher Qf value), has important industrial application value in the fields of mobile communication, aerospace, military, modern medicine and the like.
Description
Technical field:
the invention belongs to the technical field of ceramic materials and preparation, and particularly relates to low-temperature sintered low-dielectric low-loss microwave dielectric ceramic and a preparation method thereof.
The background technology is as follows:
the microwave dielectric ceramic is a ceramic material which is used as a dielectric material in a microwave frequency band (mainly 300 MHz-300 GHz frequency band) circuit and can perform one or more functions, and is a key material for manufacturing a microwave dielectric filter and a resonator. With the rapid development of mobile communication industry, novel functional ceramic materials are widely used in a plurality of fields such as mobile communication, satellite television broadcast communication, scattering communication military radar, satellite navigation positioning systems and the like for manufacturing microwave elements such as a dielectric resonator, a dielectric antenna, a duplexer, a dielectric guided wave loop, a dielectric frequency stabilizing oscillator and the like. In recent years, due to the rapid development of fields such as mobile communication, aerospace, military, modern medicine and the like, higher requirements are also put forward on microwave dielectric ceramic materials, so that searching, preparing and researching a novel microwave dielectric ceramic with proper dielectric constant, low loss, near zero resonance frequency temperature coefficient and low cost and environmental protection becomes a hot spot and key point of current research of people.
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person of ordinary skill in the art.
The invention comprises the following steps:
the invention aims to provide low-temperature sintered low-dielectric low-loss microwave dielectric ceramic and a preparation method thereof, thereby overcoming the defects in the prior art.
In order to achieve the aim, the invention provides a low-temperature sintered low-dielectric low-loss microwave dielectric ceramic, which consists of a main medium and an auxiliary medium, wherein the main medium consists of MgTiO with the mol ratio of (0.95-0.99): 0.01-0.05 3 And CaTiO 3 Constructing; the mass proportion of the auxiliary medium is 2-5% wt of the main medium, which is expressed as aBaO-bCAO-cSiO 2 -a zno glass ceramic, a, b, c and d each independently representing a mole percent, and satisfying the following conditions: a is more than or equal to 25% and less than or equal to 30%, b is more than or equal to 30% and less than or equal to 35%, c is more than or equal to 20% and less than or equal to 23%, d is more than or equal to 14% and less than or equal to 16%, and a+b+c+d=100%.
Further, preferably, the host medium is composed of MgT in a molar ratio of 0.99:0.01iO 3 And CaTiO 3 The composition is formed.
Further, preferably, the mass proportion of the auxiliary medium is 5% of the main medium.
Further, in the expression of the auxiliary medium, preferably, a=28%, b=35%, c=22% and d=15%.
Further, preferably, the dielectric constant of the microwave dielectric ceramic material is 15.0.+ -. 1.0, the qf value is 102000 GHz-138000 GHz, and the temperature coefficient of resonance frequency is within.+ -. 30 ppm/. Degree.C.
The invention further provides a preparation method of the low-temperature sintered low-dielectric low-loss microwave dielectric ceramic, which is characterized by comprising the following steps of: the method comprises the following steps:
(1) According to MgTiO 3 The molar ratio of Mg to Ti is MgO to TiO 2 MgO and TiO 2 Ball milling, stoving and presintering to obtain MgTiO 3 ；
(2) According to CaTiO 3 The molar ratio of Ca to Ti is CaCO 3 And TiO 2 CaCO is processed by 3 And TiO 2 Ball milling, drying and presintering after mixing to obtain CaTiO 3 ；
(3) According to the composition expression aBaO-bCAO-cSiO 2 The mole percentages of the elements in dZnO are BaCO respectively 3 、CaCO 3 、SiO 2 Mixing the weighed materials, ball milling, drying and presintering to obtain glass ceramic, namely BCSZ glass ceramic;
wherein, in the composition expression aBaO-bCAO-cSiO 2 In dZnO, a, b, c and d each independently represent a mole percentage, and satisfy the following conditions: a is more than or equal to 25% and less than or equal to 30%, b is more than or equal to 30% and less than or equal to 35%, c is more than or equal to 20% and less than or equal to 23%, d is more than or equal to 14% and less than or equal to 16%, and a+b+c+d=100%;
(4) MgTiO obtained in the step (1) is processed 3 CaTiO obtained in step (2) 3 Mixing according to the mole ratio of (0.95-0.99) to (0.01-0.05), and then according to MgTiO 3 And CaTiO 3 Adding 2-5 wt% of the total weight into the BCSZ glass ceramic obtained in the step (3), ball milling, drying, granulating, pressing into cylinders, sintering into porcelain,obtaining the low-dielectric low-loss microwave dielectric ceramic.
Further, preferably, in the step (3), a=28%, b=35%, c=22%, and d=15%.
Further, preferably, the sintering process of the step (4) is sintering at 1200-1250 ℃.
Compared with the prior art, one aspect of the invention has the following beneficial effects:
(1) The invention uses MgTiO 3 And CaTiO 3 The synergistic effect of the (2) can ensure the range of dielectric constant and basic temperature coefficient, and after the (B) and the (B) are compounded with the BCSZ glass ceramic, the sintering temperature of the material can be obviously reduced, so that the material can be subjected to ceramic compact sintering at relatively low temperature, the process cost can be reduced, and the energy is saved;
(2) The composite material is compounded with BCSZ glass ceramic, so that the loss of a main material is not increased like a common low-temperature glass material, and the loss of the material can be greatly reduced while the low-frequency temperature coefficient is maintained;
(3) In the preparation process, a step solid phase reaction sintering method is adopted, and compared with a one-step mixed sintering method, the composition of the product is more stable, and the loss of the material under the same frequency temperature coefficient is lower.
The specific embodiment is as follows:
the following detailed description of specific embodiments of the invention is, but it should be understood that the invention is not limited to specific embodiments.
The following presents a simplified summary of one or more aspects in order to provide a basic understanding of such aspects. This summary is not an extensive overview of all contemplated aspects, and is intended to neither identify key or critical elements of all aspects nor delineate the scope of any or all aspects. Its sole purpose is to present some concepts of one or more aspects in a simplified form as a prelude to the more detailed description that is presented later.
Example 1:
a low-temperature sintered low-dielectric low-loss microwave dielectric ceramic is composed of main medium and auxiliary mediumThe main medium consists of MgTiO with the mol ratio of 0.95:0.05 3 And CaTiO 3 Constructing; the mass proportion of the auxiliary medium is 2% wt of the main medium, which is expressed as aBaO-bCAO-cSiO 2 The glass ceramics of dnos, a, b, c and d independently represent mole percentages, a=28%, b=35%, c=22% and d=15%, respectively.
The preparation method of the microwave dielectric ceramic comprises the following steps:
(1) According to MgTiO 3 The molar ratio of Mg to Ti is MgO to TiO 2 MgO and TiO 2 Ball milling, stoving and presintering to obtain MgTiO 3 ；
(2) According to CaTiO 3 The molar ratio of Ca to Ti is CaCO 3 And TiO 2 CaCO is processed by 3 And TiO 2 Ball milling, drying and presintering after mixing to obtain CaTiO 3 ；
(3) According to the composition expression 28BaO-35CaO-22SiO 2 The mole percentage of each element in-15 ZnO is BaCO 3 、CaCO 3 、SiO 2 Mixing the weighed materials, ball milling, drying and presintering to obtain glass ceramic, namely BCSZ glass ceramic;
(4) MgTiO obtained in the step (1) is processed 3 CaTiO obtained in step (2) 3 Mixing according to the mol ratio of 0.95:0.05, and then mixing according to MgTiO 3 And CaTiO 3 Adding 2 wt% of the total weight of the BCSZ glass ceramic obtained in the step (3) into the mixture, ball milling, drying, granulating, pressing into a cylinder, and sintering the cylinder into ceramic, wherein the sintering process of the ceramic is sintering at 1250 ℃ to obtain the low-dielectric low-loss microwave dielectric ceramic.
Example 2:
a low-temperature sintered low-dielectric low-loss microwave dielectric ceramic is composed of a main medium and an auxiliary medium, wherein the main medium is composed of MgTiO with the molar ratio of 0.96:0.04 3 And CaTiO 3 Constructing; the mass proportion of the auxiliary medium is 3% wt of the main medium, which is expressed as aBaO-bCAO-cSiO 2 -dnos glass ceramic, a, b, c and d each independently representing mole percent, a=27%, b=35%, c=23%, d=15%。
The preparation method of the microwave dielectric ceramic comprises the following steps:
(1) According to MgTiO 3 The molar ratio of Mg to Ti is MgO to TiO 2 MgO and TiO 2 Ball milling, stoving and presintering to obtain MgTiO 3 ；
(2) According to CaTiO 3 The molar ratio of Ca to Ti is CaCO 3 And TiO 2 CaCO is processed by 3 And TiO 2 Ball milling, drying and presintering after mixing to obtain CaTiO 3 ；
(3) According to the composition expression 27BaO-35CaO-23SiO 2 The mole percentage of each element in-15 ZnO is BaCO 3 、CaCO 3 、SiO 2 Mixing the weighed materials, ball milling, drying and presintering to obtain glass ceramic, namely BCSZ glass ceramic;
(4) MgTiO obtained in the step (1) is processed 3 CaTiO obtained in step (2) 3 Mixing according to the mol ratio of 0.96:0.04, and then mixing according to MgTiO 3 And CaTiO 3 Adding 3 wt% of the total weight of the BCSZ glass ceramic obtained in the step (3) into the mixture, ball milling, drying, granulating, pressing into a cylinder, and sintering the cylinder into ceramic, wherein the sintering process of the ceramic is sintering at 1230 ℃ to obtain the low-dielectric low-loss microwave dielectric ceramic.
Example 3:
a low-temperature sintered low-dielectric low-loss microwave dielectric ceramic is composed of a main medium and an auxiliary medium, wherein the main medium is composed of MgTiO with the molar ratio of 0.97:0.03 3 And CaTiO 3 Constructing; the mass proportion of the auxiliary medium is 4% wt of the main medium, which is expressed as aBaO-bCAO-cSiO 2 The glass ceramics of dnos, a, b, c and d independently represent mole percentages, a=29%, b=34%, c=23% and d=14%, respectively.
The preparation method of the microwave dielectric ceramic comprises the following steps:
(1) According to MgTiO 3 The molar ratio of Mg to Ti is MgO to TiO 2 MgO and TiO 2 Ball milling, stoving and presintering to obtain MgTiO 3 ；
(2) According to CaTiO 3 The molar ratio of Ca to Ti is CaCO 3 And TiO 2 CaCO is processed by 3 And TiO 2 Ball milling, drying and presintering after mixing to obtain CaTiO 3 ；
(3) According to the composition expression 29BaO-34CaO-23SiO 2 The mole percentage of each element in-14 ZnO is BaCO 3 、CaCO 3 、SiO 2 Mixing the weighed materials, ball milling, drying and presintering to obtain glass ceramic, namely BCSZ glass ceramic;
(4) MgTiO obtained in the step (1) is processed 3 CaTiO obtained in step (2) 3 Mixing according to the mol ratio of 0.97:0.03, and then mixing according to MgTiO 3 And CaTiO 3 Adding 4 wt% of the total weight of the BCSZ glass ceramic obtained in the step (3) into the mixture, ball milling, drying, granulating, pressing into a cylinder, and sintering the cylinder into ceramic, wherein the sintering process of the ceramic is sintering at 1210 ℃ to obtain the low-dielectric low-loss microwave dielectric ceramic.
Example 4:
a low-temperature sintered low-dielectric low-loss microwave dielectric ceramic is composed of a main medium and an auxiliary medium, wherein the main medium is composed of MgTiO with the molar ratio of 0.99:0.01 3 And CaTiO 3 Constructing; the mass proportion of the auxiliary medium is 5% wt of the main medium, which is expressed as aBaO-bCAO-cSiO 2 The glass ceramics of dnos, a, b, c and d independently represent mole percentages, a=30%, b=32%, c=23% and d=15%, respectively.
The preparation method of the microwave dielectric ceramic comprises the following steps:
(1) According to MgTiO 3 The molar ratio of Mg to Ti is MgO to TiO 2 MgO and TiO 2 Ball milling, stoving and presintering to obtain MgTiO 3 ；
(2) According to CaTiO 3 The molar ratio of Ca to Ti is CaCO 3 And TiO 2 CaCO is processed by 3 And TiO 2 Ball milling, drying and presintering after mixing to obtain CaTiO 3 ；
(3) 30BaO-32CaO-23SiO according to the composition expression 2 The mole percentage of each element in-15 ZnO is BaCO 3 、CaCO 3 、SiO 2 Mixing the weighed materials, ball milling, drying and presintering to obtain glass ceramic, namely BCSZ glass ceramic;
(4) MgTiO obtained in the step (1) is processed 3 CaTiO obtained in step (2) 3 Mixing according to the mol ratio of 0.99:0.01, and then mixing according to MgTiO 3 And CaTiO 3 Adding 5 wt% of the total weight of the BCSZ glass ceramic obtained in the step (3) into the mixture, ball milling, drying, granulating, pressing into a cylinder, and sintering the cylinder into ceramic, wherein the sintering process of the ceramic is sintering at 1200 ℃ to obtain the low-dielectric low-loss microwave dielectric ceramic.
Comparative example 1:
a low-temperature sintered low-dielectric low-loss microwave dielectric ceramic is prepared from MgTiO 3 The composition is formed.
The preparation method of the microwave dielectric ceramic comprises the following steps:
according to MgTiO 3 The molar ratio of Mg to Ti is MgO to TiO 2 MgO and TiO 2 Mixing, ball milling, drying, granulating, pressing into cylinders, sintering into porcelain, and sintering at 1340 ℃ to obtain the low-dielectric low-loss microwave dielectric ceramic.
Comparative example 2:
a low-temperature sintered low-dielectric low-loss microwave dielectric ceramic is prepared from MgTiO with a molar ratio of 0.96:0.04 3 And CaTiO 3 The composition is formed.
The preparation method of the microwave dielectric ceramic comprises the following steps:
(1) According to MgTiO 3 The molar ratio of Mg to Ti is MgO to TiO 2 MgO and TiO 2 Ball milling, stoving and presintering to obtain MgTiO 3 ；
(2) According to CaTiO 3 The molar ratio of Ca to Ti is CaCO 3 And TiO 2 CaCO is processed by 3 And TiO 2 Ball milling, drying and presintering after mixing to obtain CaTiO 3 ；
(3) MgTiO obtained in the step (1) is processed 3 CaTiO obtained in step (2) 3 Mixing, ball milling, drying, granulating and pressing into cylinders according to the mol ratio of 0.96:0.04, and sintering into porcelain, wherein the sintering process of the porcelain is sintering at 1250 ℃ to obtain the low-dielectric low-loss microwave dielectric ceramic.
Comparative example 3:
a low-temperature sintered low-dielectric low-loss microwave dielectric ceramic is prepared from MgTiO with a molar ratio of 0.99:0.01 3 And CaTiO 3 The composition is formed.
The preparation method of the microwave dielectric ceramic comprises the following steps:
(1) According to MgTiO 3 The molar ratio of Mg to Ti is MgO to TiO 2 MgO and TiO 2 Ball milling, stoving and presintering to obtain MgTiO 3 ；
(2) According to CaTiO 3 The molar ratio of Ca to Ti is CaCO 3 And TiO 2 CaCO is processed by 3 And TiO 2 Ball milling, drying and presintering after mixing to obtain CaTiO 3 ；
(3) MgTiO obtained in the step (1) is processed 3 CaTiO obtained in step (2) 3 Mixing, ball milling, drying, granulating and pressing into cylinders according to the mol ratio of 0.99:0.01, and sintering into porcelain, wherein the sintering process of the porcelain is sintering at 1200 ℃ to obtain the low-dielectric low-loss microwave dielectric ceramic.
The microwave dielectric ceramic materials prepared in examples 1 to 4 and comparative examples 1 to 3 were subjected to performance test, and the test results are shown in Table 1.
As can be seen from Table 1, compared with the microwave dielectric ceramics of comparative examples, the microwave dielectric ceramics of examples 1 to 4 of the present invention can be sintered and formed at a lower temperature, and the ceramic material has a suitable dielectric constant and a near-zero resonant frequency temperature coefficient, and has low loss (i.e., a higher Qf value) at a low frequency temperature coefficient, thus having important industrial application values in the fields of mobile communication, aerospace, military, modern medicine and the like.
The foregoing descriptions of specific exemplary embodiments of the present invention are presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain the specific principles of the invention and its practical application to thereby enable one skilled in the art to make and utilize the invention in various exemplary embodiments and with various modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents.
Claims (8)
1. A low temperature sintered low dielectric low loss microwave dielectric ceramic, characterized in that: comprises a main medium and an auxiliary medium, wherein the main medium is composed of MgTiO with the mol ratio of (0.95-0.99): 0.01-0.05 3 And CaTiO 3 Constructing; the mass proportion of the auxiliary medium is 2-5% wt of the main medium, which is expressed as aBaO-bCAO-cSiO 2 -a zno glass ceramic, a, b, c and d each independently representing a mole percent, and satisfying the following conditions: a is more than or equal to 25% and less than or equal to 30%, b is more than or equal to 30% and less than or equal to 35%, c is more than or equal to 20% and less than or equal to 23%, d is more than or equal to 14% and less than or equal to 16%, and a+b+c+d=100%.
2. A low temperature sintered low dielectric low loss microwave dielectric ceramic according to claim 1, wherein: the main medium consists of MgTiO with the mol ratio of 0.99:0.01 3 And CaTiO 3 The composition is formed.
3. A low temperature sintered low dielectric low loss microwave dielectric ceramic according to claim 1, wherein: the mass proportion of the auxiliary medium is 5% of that of the main medium.
4. A low temperature sintered low dielectric low loss microwave dielectric ceramic according to claim 1, wherein: in the expression of the auxiliary medium, a=28%, b=35%, c=22%, and d=15%.
5. A low temperature sintered low dielectric low loss microwave dielectric ceramic according to claim 1, wherein: the dielectric constant of the microwave dielectric ceramic material is 15.0+/-1.0, the qf value is 102000 GHz-138000 GHz, and the temperature coefficient of the resonant frequency is within +/-30 ppm/DEG C.
6. A preparation method of low-temperature sintered low-dielectric low-loss microwave dielectric ceramic is characterized by comprising the following steps: the method comprises the following steps:
(1) According to MgTiO 3 The molar ratio of Mg to Ti is MgO to TiO 2 MgO and TiO 2 Ball milling, stoving and presintering to obtain MgTiO 3 ；
(2) According to CaTiO 3 The molar ratio of Ca to Ti is CaCO 3 And TiO 2 CaCO is processed by 3 And TiO 2 Ball milling, drying and presintering after mixing to obtain CaTiO 3 ；
(3) According to the composition expression aBaO-bCAO-cSiO 2 The mole percentages of the elements in dZnO are BaCO respectively 3 、CaCO 3 、SiO 2 Mixing the weighed materials, ball milling, drying and presintering to obtain glass ceramic, namely BCSZ glass ceramic;
wherein, in the composition expression aBaO-bCAO-cSiO 2 In dZnO, a, b, c and d each independently represent a mole percentage, and satisfy the following conditions: a is more than or equal to 25% and less than or equal to 30%, b is more than or equal to 30% and less than or equal to 35%, c is more than or equal to 20% and less than or equal to 23%, d is more than or equal to 14% and less than or equal to 16%, and a+b+c+d=100%;
(4) MgTiO obtained in the step (1) is processed 3 CaTiO obtained in step (2) 3 Mixing according to the mole ratio of (0.95-0.99) to (0.01-0.05), and then according to MgTiO 3 And CaTiO 3 Adding 2-5 wt% of the total weight into the BCSZ glass ceramic obtained in the step (3), ball milling, drying, granulating, pressing into cylinders, and sintering into ceramic to obtain the low-dielectric low-loss microwave dielectric ceramic.
7. The method for preparing the low-temperature sintered low-dielectric low-loss microwave dielectric ceramic, according to claim 6, is characterized in that: in the step (3), a=28%, b=35%, c=22%, and d=15%.
8. The method for preparing the low-temperature sintered low-dielectric low-loss microwave dielectric ceramic, according to claim 6, is characterized in that: the sintering process of the step (4) is sintering at 1200-1250 ℃.
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| JPH07118060A (en) * | 1993-08-24 | 1995-05-09 | Nippon Electric Glass Co Ltd | High-dielectric constant glass ceramic |
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| CN109721340A (en) * | 2019-01-28 | 2019-05-07 | 深圳顺络电子股份有限公司 | A kind of high intensity low-loss LTCC material and preparation method thereof |
| CN110143814A (en) * | 2019-06-27 | 2019-08-20 | 无锡鑫圣慧龙纳米陶瓷技术有限公司 | A kind of intermediary's temperature-stable microwave-medium ceramics and preparation method thereof |
| CN112592174A (en) * | 2020-12-10 | 2021-04-02 | 无锡市高宇晟新材料科技有限公司 | Microwave dielectric ceramic material with high thermal shock resistance and preparation method thereof |
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- 2022-12-15 CN CN202211619482.XA patent/CN116023128A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH07118060A (en) * | 1993-08-24 | 1995-05-09 | Nippon Electric Glass Co Ltd | High-dielectric constant glass ceramic |
| JP2006290721A (en) * | 2005-03-16 | 2006-10-26 | Ngk Spark Plug Co Ltd | Low temperature firing porcelain composition, method of manufacturing the same and electronic component using the same |
| CN106631001A (en) * | 2016-11-18 | 2017-05-10 | 电子科技大学 | Mg-Ca-Ti-based dielectric material for microwave multilayer ceramic chip capacitor (MLCC) and preparation method of Mg-Ca-Ti-based dielectric material |
| CN109721340A (en) * | 2019-01-28 | 2019-05-07 | 深圳顺络电子股份有限公司 | A kind of high intensity low-loss LTCC material and preparation method thereof |
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