CN114163242B - Microwave dielectric ceramic with low dielectric constant and high quality factor and preparation method thereof - Google Patents
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Abstract
The invention discloses a microwave dielectric ceramic with low dielectric constant and high quality factor and a preparation method thereof 5 The relative dielectric constant of the microwave dielectric ceramic is 6.5-7.7, the quality factor is 31400-40500 GHz, and the microwave dielectric ceramic has excellent performance combination of low dielectric constant and high quality factor, and has wide application prospect in the passive devices of the microwave communication system in the future. The preparation method of the microwave dielectric ceramic with low dielectric constant and high quality factor adopts a solid-phase reaction preparation process, and has the advantages of simple process, good repeatability and stable and single synthesized phase. In addition, the preparation method of the microwave dielectric ceramic with low dielectric constant and high quality factor takes perfluorinated compounds as reaction raw materials, and the sintering temperature is not higher than 1200 ℃ compared with other oxide ceramics, such as MgAl 2 O 4 The sintering temperature (1450 ℃) and the like is reduced by more than 275 ℃, and the cost of large-scale industrial production can be greatly saved.
Description
Technical Field
The invention relates to the technical field of electronic information materials, in particular to a microwave dielectric ceramic with low dielectric constant and high quality factor and a preparation method thereof.
Background
The microwave dielectric ceramic is a key dielectric material applied to microwave frequency band (300MHz to 300GHz) circuits as passive devices (such as resonators, filters, antennas and the like) in a microwave communication system. The two most important performance evaluation indexes of the microwave dielectric ceramic are respectively the dielectric constant and the dielectric loss of the ceramic (generally, quality factor of the product is used)QfThe value representing the inverse of the dielectric loss, i.e.QfThe larger the value, the lower the dielectric loss).
In recent decades, as people have continuously improved requirements on information transmission content, speed, quality and the like, wireless communication technology has been developed rapidly, new-generation information technologies such as 5G mobile communication, internet of things (IoT) technology and the like are emerging continuously, and the frequency of use of the emerging technologies gradually develops towards a higher frequency band. The classic theory of dielectric medium shows that the dielectric loss of the material gradually increases with the increase of frequency, the excessive dielectric loss easily causes the energy of electromagnetic wave signals to be dissipated in the form of heat in the process of propagation, the communication signals are shortened in propagation distance due to the dissipation of the energy, the device is heated seriously, and the service life of the device is shortened. Therefore, microwave dielectric ceramic materials with high quality factors are urgently needed in future communication systems. On the other hand, the delay time of signals is required to be less than 1ms in future 5G communication, internet of things technology and the like. Since the signal delay time is proportional to the dielectric constant of the material, a ceramic system with a low dielectric constant needs to be researched to meet the technical requirement of low time delay. In view of the above, the search for microwave dielectric ceramic materials with low dielectric constant and high quality factor is a leading issue to meet the future wireless communication requirements.
In this context, microwave dielectric ceramics have been extensively studied, resulting in a large array of dielectric ceramic systems. However, the current scientific and industrial research and development concepts are fixed, and the material system is basically a compound synthesized by using common oxides as raw materials: such as aluminate, silicate, titanate, etc. (e.g. Chinese patent CN202011445549.3, CN 111592348A), the sintering temperature is usually 1400 deg.C o And C is about. However, ceramic systems synthesized entirely from fluorides are less studied. Compared with oxides, the sintering temperature of fluoride is generally lower, which is beneficial to reducing the sintering temperature of ceramics, thereby saving energy required by industrial production and reducing cost. In addition, compared with the corresponding oxide, the common fluoride has a better quality factor, so that the common fluoride has a better application prospect in the field of microwave dielectric ceramics. Therefore, the research on the novel fluoride-based microwave dielectric ceramic has very important scientific research and practical application values.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a microwave dielectric ceramic with low dielectric constant and high quality factor and a preparation method thereof.
In order to solve the problems, the invention adopts the following technical scheme:
the invention provides a microwave dielectric ceramic with low dielectric constant and high quality factor, wherein the chemical composition expression of the microwave dielectric ceramic is MgAlF 5 Relative dielectric constant of the microwave dielectric ceramic
6.5 to 7.7, quality factorQfIs 31400-40500 GHz.
The invention also provides a preparation method of the microwave dielectric ceramic with low dielectric constant and high quality factor, which comprises the following steps:
(1) Preparing materials: according to MgAlF 5 Weighing MgF according to the molar stoichiometric ratio of 1 2 And AlF 3 Raw materials;
(2) Mixing materials: carrying out wet ball milling on the mixed raw material obtained by burdening and absolute ethyl alcohol to obtain a slurry raw material;
(3) Drying: drying the slurry raw material to constant weight to obtain a dry mixture;
(4) Pre-burning: sieving and dispersing the mixture, then pre-burning the mixture, and reacting to obtain MgAlF 5 Powder;
(5) Ball milling: to the MgAlF 5 Adding absolute ethyl alcohol into the powder, and grinding for the second time to form uniformly dispersed MgAlF 5 Sizing agent;
(6) Drying: subjecting the MgAlF to 5 Drying the slurry to constant weight to obtain MgAlF 5 A compound powder;
(7) And (3) sintering: subjecting the MgAlF to 5 Pressing compound powder into a green body, and sintering the green body to obtain the microwave dielectric ceramic MgAlF 5 ；
(8) Grinding and polishing the surface of the ceramic: the sintered microwave dielectric ceramic MgAlF 5 Surface ofAnd grinding and polishing.
Preferably, in the step (4), the pre-sintering treatment temperature is 900-1000 ℃ and the time is 1-4 h.
Preferably, in the step (7), the sintering treatment temperature is 1100-1175 ℃, and the time is 1-4 h.
Further, in the step (4), the temperature rise rate of the pre-sintering treatment is 5 ℃/min to 10 ℃/min, and the pre-sintering treatment is followed by natural cooling to room temperature.
Further, in the step (7), the temperature rise rate of the sintering treatment is 1 ℃/min to 5 ℃/min.
Furthermore, in the step (7), after the sintering treatment, the temperature is reduced to 800-1000 ℃ at the speed of 1-5 ℃/min, and then the temperature is naturally cooled to the room temperature.
Preferably, in the step (2) and the step (5), the ball milling beads are ZrO 2 。
Preferably, the raw materials, zrO are mixed 2 The mass ratio of the ball milling beads to the absolute ethyl alcohol solvent is 1.
Preferably, in the step (7), the pressing pressure of the green body is 95 to 100mpa.
Compared with the prior art, the invention has the technical effects that:
the chemical composition expression of the microwave dielectric ceramic is MgAlF 5 Relative dielectric constant of microwave dielectric ceramic
6.5 to 7.7, quality factorQf31400-40500 GHz, the microwave dielectric ceramic has excellent performance combination of low dielectric constant and high quality factor, and has wide application prospect in passive devices of microwave communication systems in the future.
The preparation method of the microwave dielectric ceramic with low dielectric constant and high quality factor adopts a solid-phase reaction preparation process, and has the advantages of simple process, good repeatability and stable and single synthesized phase. In addition, the invention is a low dielectric constant high quality factor microThe preparation method of the wave dielectric ceramic completely takes fluoride as a reaction raw material, and the fluoride raw material MgF 2 And AlF 3 The price is relatively low, precious elements such as Nb, ta, rare earth elements and the like are not contained, and the cost of raw materials is low; on the other hand, when perfluoro-compound is used as the reaction raw material, the sintering temperature of the microwave dielectric ceramic is not higher than 1200 ℃, compared with other oxide ceramics, such as MgAl 2 O 4 The sintering temperature (1450 ℃) and the like is reduced by more than 275 ℃, and the cost of large-scale industrial production can be greatly saved.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
It will be appreciated by those skilled in the art that the objects and advantages that can be achieved with the present invention are not limited to the specific details set forth above, and that these and other objects that can be achieved with the present invention will be more clearly understood from the detailed description that follows.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
It is to be understood that the processing equipment or apparatus not specifically identified in the following examples is conventional in the art.
Furthermore, it is to be understood that one or more method steps recited in the present disclosure are not exclusive of other method steps that may also be present before or after the recited combination of steps or that other method steps may also be inserted between the explicitly recited steps, unless otherwise indicated; moreover, unless otherwise indicated, the numbering of the method steps is only a convenient tool for identifying each method step, and is not intended to limit the order of the method steps or the scope of the invention, and changes or modifications in the relative relationship thereof may be regarded as the scope of the invention without substantial change in the technical content.
The embodiment of the invention provides a microwave dielectric ceramic with low dielectric constant and high quality factor, and the chemical composition expression of the microwave dielectric ceramic is MgAlF 5 Relative dielectric constant of the microwave dielectric ceramic
6.5 to 7.7, quality factorQfIs 31400-40500 GHz.
The embodiment of the invention also provides a preparation method of the microwave dielectric ceramic with low dielectric constant and high quality factor, which comprises the following steps:
(1) Preparing materials: according to MgAlF 5 Weighing MgF according to the molar stoichiometric ratio of 1 2 And AlF 3 Raw materials; preferably, a high-purity chemical raw material, mgF, is selected 2 The purity of the raw material was 99.9%, alF 3 The purity of the starting material was 99.9%.
(2) Mixing materials: carrying out wet ball milling on the mixed raw material obtained by burdening and absolute ethyl alcohol to obtain a slurry raw material; the ball milling is carried out by using a planetary ball mill, the rotating speed range is 150 r/min-200 r/min, and the ball milling beads are ZrO 2 . Mixed raw material, zrO 2 The mass ratio of the ball milling beads to the absolute ethyl alcohol solvent is preferably 1.
(3) And (3) drying: putting the slurry raw material into a drying oven to be dried to constant weight to obtain a dry mixture;
(4) Pre-burning: sieving and dispersing the mixture, placing the mixture into a high-temperature furnace for presintering treatment, and obtaining MgAlF after reaction 5 Powder; the pre-sintering treatment temperature can be 900-1000 ℃, such as 920 ℃, 940 ℃, 960 ℃ and the like; the pre-sintering treatment time is 1-4h, such as 2h and 3 h. The temperature rising rate of the pre-sintering treatment can be selected to be 5-10 ℃/min, and the pre-sintering treatment is carried out and then the product is naturally cooled to the room temperature.
(5) Ball milling: to MgAlF 5 Adding absolute ethyl alcohol into the powder, placing the powder in a ball mill for secondary grinding to form uniformly dispersed MgAlF 5 Sizing agent; the rotating speed range of the ball mill is 150r/min to 200r/min, the ball milling beads are ZrO 2 。MgAlF 5 Powder of ZrO 2 The mass ratio of the ball milling beads to the absolute ethyl alcohol solvent is preferably 1.
(6) Drying: mgAlF 5 The slurry is placed in an oven to be dried to constant weight to obtain MgAlF 5 A compound powder;
(7) And (3) sintering: mgAlF 5 Pressing the compound powder into a cylindrical green body under the pressure of 95-100MPa, and then sintering the cylindrical green body to obtain the microwave dielectric ceramic MgAlF 5 (ii) a The sintering temperature can be 1100-1175 deg.C, such as 1525 deg.C, 1550 deg.C, 1575 deg.C, etc.; the time is 1 to 4h, such as 2h and 3 h. The temperature rise rate of the sintering treatment can be selected to be 1-5 ℃/min. After sintering treatment, firstly cooling to 800-1000 ℃ at the speed of 1-5 ℃/min, and then naturally cooling to room temperature;
(8) Grinding and polishing the surface of the ceramic: the sintered microwave dielectric ceramic MgAlF is sintered 5 And grinding and polishing the surface.
The chemical composition expression of the microwave dielectric ceramic is MgAlF 5 Relative dielectric constant of microwave dielectric ceramic
6.5 to 7.7, quality factorQf31400-40500 GHz, the microwave dielectric ceramic has excellent combination of low dielectric constant and high quality factor performance, and has wide application prospect in the passive devices of microwave communication systems in the future.
The preparation method of the microwave dielectric ceramic with low dielectric constant and high quality factor adopts a solid-phase reaction preparation process, and has the advantages of simple process, good repeatability and stable and single synthesized phase. In addition, the preparation method of the microwave dielectric ceramic with low dielectric constant and high quality factor completely takes fluoride as a reaction raw material, and the fluoride raw material MgF 2 And AlF 3 The price is relatively low, precious elements such as Nb, ta, rare earth elements and the like are not contained, and the cost of raw materials is low; on the other hand, when perfluoro-compound is used as the reaction raw material, the sintering temperature of the microwave dielectric ceramic is not higher than 1200 ℃,compared with other oxide ceramics, e.g. MgAl 2 O 4 The sintering temperature of (1450 ℃) and the like is reduced by more than 275 ℃, and the cost of large-scale industrial production can be greatly saved.
The following is a further description with reference to specific examples.
Example 1
The embodiment 1 of the invention provides a microwave dielectric ceramic with low dielectric constant and high quality factor and a preparation method thereof, comprising the following steps:
(1) Preparing materials: according to MgAlF 5 Weighing MgF according to the molar stoichiometric ratio of 1 2 And AlF 3 Raw materials;
(2) Mixing materials: putting the raw materials obtained by the burdening in the step (1), zirconia ball-milling beads and an absolute ethyl alcohol solvent into a planetary ball mill according to the mass ratio of 1;
(3) Drying: putting the slurry raw material in the step (2) into an oven to be dried to constant weight to obtain a dry mixture;
(4) Pre-burning: dispersing the mixture obtained in the step (3) through a 120-mesh screen, then placing the mixture into a high-temperature furnace, heating the mixture to 950 ℃ at the speed of 5 ℃/min, pre-sintering the mixture for 3 hours, and obtaining MgAlF after reaction 5 Powder;
(5) Ball milling: mgAlF obtained by pre-sintering in the step (4) 5 Adding absolute ethyl alcohol into the powder, and placing the powder in a ball mill for secondary grinding to form uniformly dispersed MgAlF 5 The slurry and ball milling process is consistent with the step (2);
(6) Drying: mgAlF of the step (5) 5 The slurry is placed in an oven to be dried to constant weight to obtain MgAlF 5 A compound powder;
(7) And (3) sintering: pressing the powder dried in the step (6) into a cylindrical green body under the pressure of 98MPa, then raising the temperature of the green body to 1100 ℃ at the speed of 5 ℃/min for sintering for 3h, cooling to 900 ℃ at the speed of 2 ℃/min after sintering, and finally naturally cooling to obtain the microwave dielectric ceramic MgAlF 5 ；
(8) Ceramic surface grinding and polishingLight: mgAlF is sintered as microwave dielectric ceramic 5 And grinding and polishing.
Example 2
The embodiment 2 of the invention provides a microwave dielectric ceramic with low dielectric constant and high quality factor and a preparation method thereof, and the preparation method comprises the following steps:
(1) Preparing materials: according to MgAlF 5 Weighing MgF according to the molar stoichiometric ratio of 1 2 And AlF 3 Raw materials;
(2) Mixing materials: putting the raw materials obtained by the burdening in the step (1), zirconia ball-milling beads and an absolute ethyl alcohol solvent into a planetary ball mill according to the mass ratio of 1;
(3) Drying: putting the slurry raw material in the step (2) into an oven to be dried to constant weight to obtain a dry mixture;
(4) Pre-burning: dispersing the mixture obtained in the step (3) through a 120-mesh screen, then placing the mixture into a high-temperature furnace, heating the mixture to 950 ℃ at the speed of 5 ℃/min, pre-burning the mixture for 3 hours, and obtaining MgAlF after reaction 5 Powder;
(5) Ball milling: mgAlF obtained by pre-sintering in the step (4) 5 Adding anhydrous ethanol into the powder, and placing the powder in a ball mill for secondary grinding to form uniformly dispersed MgAlF 5 Slurry, the ball milling process is consistent with the step (2);
(6) And (3) drying: mgAlF of the step (5) 5 The slurry is placed in an oven to be dried to constant weight to obtain MgAlF 5 A compound powder;
(7) And (3) sintering: pressing the powder dried in the step (6) into a cylindrical green body under the pressure of 98MPa, then raising the temperature of the green body to 1125 ℃ at the speed of 5 ℃/min for sintering for 3h, cooling to 900 ℃ at the speed of 2 ℃/min after sintering, and finally naturally cooling to obtain the microwave dielectric ceramic MgAlF 5 ；
(8) Grinding and polishing the surface of the ceramic: mgAlF is sintered microwave dielectric ceramic 5 And grinding and polishing.
Example 3
The embodiment 3 of the invention provides a microwave dielectric ceramic with low dielectric constant and high quality factor and a preparation method thereof, comprising the following steps:
(1) Preparing materials: according to MgAlF 5 Weighing MgF according to the molar stoichiometric ratio of 1 2 And AlF 3 Raw materials;
(2) Mixing materials: putting the raw materials obtained by the burdening in the step (1), zirconia ball-milling beads and an absolute ethyl alcohol solvent into a planetary ball mill according to the mass ratio of 1;
(3) And (3) drying: putting the slurry raw material in the step (2) into an oven to be dried to constant weight to obtain a dry mixture;
(4) Pre-burning: dispersing the mixture obtained in the step (3) through a 120-mesh screen, then placing the mixture into a high-temperature furnace, heating the mixture to 950 ℃ at the speed of 5 ℃/min, pre-sintering the mixture for 3 hours, and obtaining MgAlF after reaction 5 Powder;
(5) Ball milling: pre-burning the MgAlF obtained in the step (4) 5 Adding anhydrous ethanol into the powder, and placing the powder in a ball mill for secondary grinding to form uniformly dispersed MgAlF 5 Slurry, the ball milling process is consistent with the step (2);
(6) And (3) drying: mgAlF of the step (5) 5 The slurry is placed in an oven to be dried to constant weight to obtain MgAlF 5 A compound powder;
(7) And (3) sintering: pressing the powder dried in the step (6) into a cylindrical green body under the pressure of 98MPa, then raising the temperature of the green body to 1150 ℃ at the speed of 5 ℃/min for sintering for 3h, cooling to 900 ℃ at the speed of 2 ℃/min after sintering, and finally naturally cooling to obtain the microwave dielectric ceramic MgAlF 5 ；
(8) Grinding and polishing the surface of the ceramic: mgAlF is sintered as microwave dielectric ceramic 5 And grinding and polishing.
Example 4
The embodiment 4 of the invention provides a microwave dielectric ceramic with low dielectric constant and high quality factor and a preparation method thereof, comprising the following steps:
(1) Preparing materials: according to MgAlF 5 Weighing MgF according to the molar stoichiometric ratio of 1 2 And AlF 3 Raw materials;
(2) Mixing materials: putting the raw materials obtained by the burdening in the step (1), zirconia ball-milling beads and an absolute ethyl alcohol solvent into a planetary ball mill according to the mass ratio of 1;
(3) And (3) drying: putting the slurry raw material in the step (2) into an oven to be dried to constant weight to obtain a dry mixture;
(4) Pre-burning: dispersing the mixture obtained in the step (3) through a 120-mesh screen, then placing the mixture into a high-temperature furnace, heating the mixture to 950 ℃ at the speed of 5 ℃/min, pre-sintering the mixture for 3 hours, and obtaining MgAlF after reaction 5 Powder;
(5) Ball milling: adding the MgAlF5 powder obtained by pre-sintering in the step (4) into absolute ethyl alcohol, and placing the mixture into a ball mill for secondary grinding to form uniformly dispersed MgAlF 5 Slurry, the ball milling process is consistent with the step (2);
(6) And (3) drying: mgAlF of the step (5) 5 The slurry is placed in an oven to be dried to constant weight to obtain MgAlF 5 A compound powder;
(7) And (3) sintering: pressing the powder dried in the step (6) into a cylindrical green body under the pressure of 98MPa, then raising the temperature of the green body to 1175 ℃ at the speed of 5 ℃/min, sintering for 3h, cooling to 900 ℃ at the speed of 2 ℃/min after sintering, and finally naturally cooling to obtain the microwave dielectric ceramic MgAlF 5 ；
(8) Grinding and polishing the surface of the ceramic: mgAlF is sintered microwave dielectric ceramic 5 And grinding and polishing.
The dielectric properties of the cylindrical microwave dielectric ceramics prepared in the above examples 1 to 4 were measured by using a dielectric resonant cavity method proposed by Hakki-Coleman, and the measured specific performance parameters are listed in table 1 below.
As shown in table 1 above, the dielectric constant of the fluoride microwave dielectric ceramic prepared in embodiments 1 to 4 of the present invention obtained by adjusting the sintering temperature is 6.5 to 7.7; in addition, the quality factors of the ceramics obtained in all the embodiments are all up to more than 30000GHz, and the ultralow dielectric loss is shown, so that the microwave dielectric ceramics have wide application prospects in the field of millimeter wave communication in the future.
The present invention is not limited to the above-described specific embodiments, and various modifications and variations are possible. Any modifications, equivalent substitutions, improvements and the like of the above embodiments according to the technical essence of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The microwave dielectric ceramic with low dielectric constant and high quality factor is characterized in that the chemical composition expression of the microwave dielectric ceramic is MgAlF 5 Relative dielectric constant of the microwave dielectric ceramic
6.5 to 7.7, quality factorQfIs 31400-40500 GHz.
2. The method for preparing a microwave dielectric ceramic with low dielectric constant and high quality factor as claimed in claim 1, comprising the steps of:
(1) Preparing materials: according to MgAlF 5 Weighing MgF according to the molar stoichiometric ratio of 1 2 And AlF 3 Raw materials;
(2) Mixing materials: carrying out wet ball milling on the mixed raw material obtained by burdening and absolute ethyl alcohol to obtain a slurry raw material;
(3) And (3) drying: drying the slurry-like raw material to constant weight to obtain a dry mixture;
(4) Pre-burning: sieving and dispersing the mixture, then pre-burning the mixture, and reacting to obtain MgAlF 5 Powder;
(5) Ball milling: to the MgAlF 5 Adding absolute ethyl alcohol into the powder to carry outSecondary grinding to form uniformly dispersed MgAlF 5 Sizing agent;
(6) Drying: subjecting the MgAlF to 5 Drying the slurry to constant weight to obtain MgAlF 5 A compound powder;
(7) And (3) sintering: subjecting the MgAlF to 5 Pressing compound powder into a green body, and sintering the green body to obtain the microwave dielectric ceramic MgAlF 5 ；
(8) Grinding and polishing the surface of the ceramic: the sintered microwave dielectric ceramic MgAlF 5 And grinding and polishing the surface.
3. The method for preparing the microwave dielectric ceramic with low dielectric constant and high quality factor as claimed in claim 2, wherein in the step (4), the pre-sintering treatment temperature is 900-1000 ℃ and the time is 1-4 h.
4. The preparation method of the microwave dielectric ceramic with low dielectric constant and high quality factor as claimed in claim 2, wherein in the step (7), the sintering temperature is 1100-1175 ℃ and the sintering time is 1-4 h.
5. The method for preparing a microwave dielectric ceramic with low dielectric constant and high quality factor as claimed in claim 3, wherein in the step (4), the temperature rise rate of the pre-sintering treatment is 5 ℃/min to 10 ℃/min, and the microwave dielectric ceramic is naturally cooled to room temperature after the pre-sintering treatment.
6. The method for preparing a microwave dielectric ceramic with low dielectric constant and high quality factor as claimed in claim 4, wherein in the step (7), the temperature rise rate of the sintering treatment is 1 ℃/min to 5 ℃/min.
7. The method for preparing the microwave dielectric ceramic with low dielectric constant and high quality factor as claimed in claim 6, wherein in the step (7), the temperature is reduced to 800-1000 ℃ at a speed of 1-5 ℃/min after the sintering treatment, and then the ceramic is naturally cooled to room temperature.
8. The method as claimed in claim 2, wherein in the steps (2) and (5), the ball milling beads are ZrO 2 。
9. The method according to claim 8, wherein the raw materials, zrO, are mixed 2 The mass ratio of the ball milling beads to the absolute ethyl alcohol solvent is 1.
10. The method for preparing the microwave dielectric ceramic with low dielectric constant and high quality factor as claimed in claim 2, wherein in the step (7), the pressing pressure of the green body is 95 to 100mpa.
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