CN114315343A - Microwave dielectric material with high Q value and medium dielectric constant and preparation method thereof - Google Patents
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Abstract
The invention provides a microwave dielectric material with high Q value and medium dielectric constant and a preparation method thereof, wherein the material comprises the following components: CaCO3、TiO2、Y2O3、Al2O3、Sm2O3、Nd2O3、CeO2Mixing CaCO334 to 37 parts of TiO227 to 30 parts of Y2O325 to 29 parts of Al2O38-9 parts of the raw materials are subjected to batching, ball milling and presintering, and then La is added2O30 to 0.5 part of Sm2O30 to 0.5 parts of Nd2O30 to 0.5 part of CeO20 to 0.5 part of the mixture is subjected to secondary ball milling, drying and granulationDry pressing into green body, and sintering in box furnace to obtain the high Q value dielectric ceramic. The microwave dielectric material has high Q value, excellent thermal stability, simple components, low price and simple preparation process, and can be applied to satellite communication systems and mobile communication base stations in large batch.
Description
Technical Field
The invention belongs to the technical field of preparation of microwave dielectric ceramic compositions, and particularly relates to a microwave dielectric material with a high Q value and a medium dielectric constant and a preparation method thereof.
Background
The microwave dielectric ceramic is a novel functional ceramic material which is rapidly developed over two decades, is a ceramic which is used as a dielectric material and completes one or more functions in a microwave frequency band (mainly 300 MHz-300 GHz) circuit, is used as a dielectric material in a dielectric cavity filter, and generally has high dielectric constant
High Q and low temperature coefficient of resonance frequency
And the like, and is suitable for manufacturing various microwave components, such as filters, frequency stabilization oscillators, capacitors, antennas and other electronic components. In recent years, rapid development of microwave integrated circuits has brought great progress to communication technology, and higher requirements are made on the dielectric constant, the dielectric loss tangent value and the temperature coefficient of resonant frequency of microwave dielectric ceramic materials. And as for the microwave dielectric ceramic material with medium dielectric constant, there are many systems, but all have many disadvantages, and the use cost of many system raw materials is high, so that it is difficult to realize high dielectric constant together
High Q and low temperature coefficient of resonance frequency
And low cost.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a microwave dielectric material with high Q value and medium dielectric constant and a preparation method thereof.
The technical scheme adopted by the invention for solving the technical problems is as follows: a microwave dielectric material with high Q value and medium dielectric constant is composed of the following components in parts by mass: CaCO3 34 to 37 parts of TiO2 27 to 30 parts of Y2O3 25 to 29 parts of Al2O38 to 9 parts of Sm2O3 0 to 0.5 parts of Nd2O30 to 0.5 part of CeO2 0 to 0.5 portion.
Further, CaCO3、TiO2 、Y2O3 、Al2O3 、Sm2O3 、Nd2O3 、CeO2The purity of (A) was 99.9%.
A preparation method of a microwave dielectric material with high Q value and medium dielectric constant comprises the following preparation steps:
step one, calculating according to parts by mass, taking CaCO3 34 to 37 parts of TiO2 27 to 30 parts of Y2O3 25 to 29 parts of Al2O3Putting 8-9 parts of the mixture into a ball milling tank, adding deionized water and milling balls into the ball milling tank, performing ball milling for 20-30 hours, uniformly mixing, discharging, and drying to obtain powder for later use;
step two, calcining the powder prepared in the step one to synthesize ceramic powder in advance;
step three, adding Sm into the porcelain powder in the step two according to the mass parts2O3 0 to 0.5 parts of Nd2O30 to 0.5 part of CeO2 Pouring 0-0.5 parts of the mixture into a ball milling tank, adding deionized water and milling balls, discharging after ball milling, drying and sieving to obtain mixed powder;
step four, adding a polyvinyl alcohol aqueous solution into the mixed powder obtained in the step three for granulation, drying, grinding and sieving;
putting the powder granulated in the step four into a die, and performing dry pressing forming under the pressure of 100-120 MPa to form a cylinder to obtain a blank body;
and step six, sintering the pressed blank in a box-type furnace to obtain the microwave dielectric ceramic product.
Further, in the first step, the ball milling tank is a nylon ball milling tank, the grinding balls are zirconia grinding balls, and the weight ratio of the total amount of the mixed raw materials added into the ball milling tank, the deionized water and the grinding balls is 1 (1.5-2) to 1.8-2.2.
Further, the drying temperature in the first step is 95-105 ℃.
Furthermore, in the second step, the calcining temperature is 1200-1300 ℃, and the calcining time is 3.5-4.5 h.
Further, in the third step, the ball milling tank is a nylon ball milling tank, the grinding balls are zirconia grinding balls, the weight ratio of the mixture, the deionized water and the grinding balls added into the ball milling tank is 1 (1.2-1.8) to (1.8-2.2), the ball milling time is 18-22 hours, the drying temperature is 95-105 ℃, and the dried powder passes through a 40-80-mesh screen.
Furthermore, in the fourth step, the mass fraction of the polyvinyl alcohol aqueous solution is 18-22 wt%, the amount of the added polyvinyl alcohol aqueous solution is 4-6% of the total mass of the mixed powder, and the mixed powder is ground by a 40-80 mesh screen after being dried.
Further, in the fifth step, the die is cylindrical, the diameter of the die is 13-17 mm, and the obtained cylinder is phi (13-17) × (7-10).
Further, the sintering method in the sixth step is as follows: raising the temperature of the box-type furnace to 500-600 ℃ at a heating rate of 2.5-3.5 ℃/min, preserving the heat for 1.5-3 h, raising the temperature to 1480-1530 ℃ at a rate of 1.5-2.5 ℃/min, preserving the heat for 4-6 h, and finally cooling to room temperature at a rate of 1-3 min/DEG C.
The invention has the beneficial effects that: the microwave dielectric ceramic is prepared by using the traditional solid phase method, the preparation method is simple, the cost of raw materials is lower, and the ceramic prepared by using the microwave dielectric material has low cost, high dielectric constant, low dielectric loss and stable resonant frequency temperature coefficient; and isSimultaneously realizes high quality factor Q and low resonant frequency temperature coefficient
And low cost.
Detailed Description
The embodiments of the present invention are described in detail with reference to specific embodiments, and the embodiments and specific operations are provided in the present embodiment on the premise of the technical solution of the present invention, but the scope of the present invention is not limited to the following embodiments.
A microwave dielectric material with high Q value and medium dielectric constant is composed of the following components in parts by mass: CaCO3 34 to 37 parts of TiO2 27 to 30 parts of Y2O3 25 to 29 parts of Al2O38 to 9 parts of Sm2O3 0 to 0.5 parts of Nd2O30 to 0.5 part of CeO2 0 to 0.5 portion.
Further, CaCO3、TiO2 、Y2O3 、Al2O3 、Sm2O3 、Nd2O3 、CeO2The purity of (A) was 99.9%.
A preparation method of a microwave dielectric material with high Q value and medium dielectric constant comprises the following preparation steps:
step one, calculating according to parts by mass, taking CaCO3 34 to 37 parts of TiO2 27 to 30 parts of Y2O3 25 to 29 parts of Al2O3Putting 8-9 parts of the mixture into a ball milling tank, adding deionized water and milling balls into the ball milling tank, performing ball milling for 20-30 hours, uniformly mixing, discharging, and drying to obtain powder for later use;
step two, calcining the powder prepared in the step one to synthesize ceramic powder in advance;
step three, adding Sm into the porcelain powder in the step two according to the mass parts2O3 0 to 0.5 parts of Nd2O30 to 0.5 part of CeO2 Pouring 0-0.5 parts of the mixture into a ball milling tank, adding deionized water and milling balls, discharging after ball milling, drying and sieving to obtain mixed powder;
step four, adding a polyvinyl alcohol aqueous solution into the mixed powder obtained in the step three for granulation, drying, grinding and sieving;
putting the powder granulated in the step four into a die, and performing dry pressing forming under the pressure of 100-120 MPa to form a cylinder to obtain a blank body;
and step six, sintering the pressed blank in a box-type furnace to obtain the microwave dielectric ceramic product.
Further, in the first step, the ball milling tank is a nylon ball milling tank, the grinding balls are zirconia grinding balls, and the weight ratio of the total amount of the mixed raw materials added into the ball milling tank, the deionized water and the grinding balls is 1 (1.5-2) to 1.8-2.2.
Further, the drying temperature in the first step is 95-105 ℃.
Furthermore, in the second step, the calcining temperature is 1200-1300 ℃, and the calcining time is 3.5-4.5 h.
Further, in the third step, the ball milling tank is a nylon ball milling tank, the grinding balls are zirconia grinding balls, the weight ratio of the mixture, the deionized water and the grinding balls added into the ball milling tank is 1 (1.2-1.8) to (1.8-2.2), the ball milling time is 18-22 hours, the drying temperature is 95-105 ℃, and the dried powder passes through a 40-80-mesh screen.
Furthermore, in the fourth step, the mass fraction of the polyvinyl alcohol aqueous solution is 18-22 wt%, the amount of the added polyvinyl alcohol aqueous solution is 4-6% of the total mass of the mixed powder, and the mixed powder is ground by a 40-80 mesh screen after being dried.
Further, in the fifth step, the die is cylindrical, the diameter of the die is 13-17 mm, and the obtained cylinder is phi (13-17) × (7-10).
Further, the sintering method in the sixth step is as follows: raising the temperature of the box-type furnace to 500-600 ℃ at a heating rate of 2.5-3.5 ℃/min, preserving the heat for 1.5-3 h, raising the temperature to 1480-1530 ℃ at a rate of 1.5-2.5 ℃/min, preserving the heat for 4-6 h, and finally cooling to room temperature at a rate of 1-3 min/DEG C.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
A microwave dielectric material with high Q value and medium dielectric constant has the following chemical formula CaxTixY1-xAl1-xO3(0.29<x<0.34) and 0 to 0.5 weight percent of Sm2O30 to 0.5 percent of Nd2O3And 0 to 0.5 percent of CeO2(ii) a Wherein x is the mole fraction;
further, CaCO3、TiO2 、Y2O3 、Al2O3 、Sm2O3 、Nd2O3 、CeO2The purity of (A) was 99.9%.
A preparation method of a microwave dielectric material with high Q value and medium dielectric constant comprises the following preparation steps:
step one, calculating according to parts by mass, taking CaCO3 34 to 37 parts of TiO2 27 to 30 parts of Y2O3 25 to 29 parts of Al2O3Putting 8-9 parts of the mixture into a nylon ball milling tank, adding deionized water and zirconia grinding balls into the nylon ball milling tank, wherein the weight ratio of the total amount of the mixed raw materials, the deionized water and the grinding balls in the ball milling tank is 1: 1.7: 2; the ball milling time is 24 hours, the materials are discharged after being uniformly mixed, and the powder is obtained after drying, wherein the drying temperature is 100 ℃ for standby;
step two, calcining the powder prepared in the step one at 1250 ℃ for 4 hours to synthesize ceramic powder in advance;
step three, adding Sm into the porcelain powder in the step two according to the mass parts2O3 0 to 0.5 parts of Nd2O30 to 0.5 part of CeO2 Pouring 0-0.5 parts of the mixture into a nylon ball milling tank, adding deionized water and zirconia milling balls, wherein the weight ratio of the mixture, the deionized water and the milling balls added into the milling tank is 1:1.5:2, discharging after ball milling for 20 hours, and drying at 100 ℃ and screening by a 60-mesh screen to obtain mixed powder;
step four, adding a polyvinyl alcohol aqueous solution into the mixed powder obtained in the step three for granulation, drying, grinding and sieving;
putting the powder granulated in the step four into a phi 15 cylindrical mold, and performing dry pressing molding under the pressure of 100-120 MPa to form a phi 15 x 8 cylinder to obtain a blank body;
and step six, placing the pressed blank into a 1700 ℃ rapid heating box type furnace for sintering, raising the temperature to 550 ℃ at the heating rate of 3 ℃/min, preserving the heat for 2h, raising the temperature to 1480-1530 ℃ at the rate of 2 ℃/min, preserving the heat for 4-6 h, and finally reducing the temperature to room temperature at the rate of 1-3 min/DEG C to obtain the microwave dielectric ceramic product.
Further, in the first step, the ball milling tank is a nylon ball milling tank, the grinding balls are zirconia grinding balls, and the weight ratio of the total amount of the mixed raw materials added into the ball milling tank, the deionized water and the grinding balls is 1 (1.5-2) to 1.8-2.2.
Further, the drying temperature in the first step is 95-105 ℃.
Furthermore, in the second step, the calcining temperature is 1200-1300 ℃, and the calcining time is 3.5-4.5 h.
Further, in the third step, the ball milling tank is a nylon ball milling tank, the grinding balls are zirconia grinding balls, the weight ratio of the mixture, the deionized water and the grinding balls added into the ball milling tank is 1 (1.2-1.8) to (1.8-2.2), the ball milling time is 18-22 hours, the drying temperature is 95-105 ℃, and the dried powder passes through a 40-80-mesh screen.
Furthermore, in the fourth step, the mass fraction of the polyvinyl alcohol aqueous solution is 18-22 wt%, the amount of the added polyvinyl alcohol aqueous solution is 4-6% of the total mass of the mixed powder, and the mixed powder is ground by a 40-80 mesh screen after being dried.
Further, in the fifth step, the die is cylindrical, the diameter of the die is 13-17 mm, and the obtained cylinder is phi (13-17) × (7-10).
Further, the sintering method in the sixth step is as follows: raising the temperature of the box-type furnace to 500-600 ℃ at a heating rate of 2.5-3.5 ℃/min, preserving the heat for 1.5-3 h, raising the temperature to 1480-1530 ℃ at a rate of 1.5-2.5 ℃/min, preserving the heat for 4-6 h, and finally cooling to room temperature at a rate of 1-3 min/DEG C.
Example 1
The first embodiment is as follows: selection of Ca0.7Ti0.7Y0.3Al0.3O3Preparing the ceramic powder by chemical proportioning, and adopting high-purity Al with the purity of 99.99 percent2O3、Y2O3、TiO2And CaCO3Preparing raw materials according to the following ingredient table:
mixing materials by adopting a planetary ball milling mode, wherein a nylon ball milling tank is adopted as a tank body, the capacity of the tank body is 1L, and ZrO of two specifications are adopted2And (5) grinding balls. ZrO for each can2The number of balls is: 152g of large balls (middle and 5 columns), 76g of small balls (middle and 3 round balls), 324g of deionized water, 300 r/min of ball milling speed, 24 hours of ball milling time, discharging after uniform mixing, drying at 100 ℃, calcining at 1250 ℃ for 4 hours, and pre-synthesizing porcelain powder; 0.25 percent of Sm is added into the synthesized powder2O3And then pouring the mixture into a nylon ball milling tank, adding deionized water and zirconia grinding balls, wherein the weight ratio of the powder material to the deionized water to the grinding balls is 1:1.5:2, ball milling for 20 hours, discharging, drying at 100 ℃ and passing through a 60-mesh screen, adding 18wt% of polyvinyl alcohol aqueous solution with the mass fraction of 5% for granulation, drying and passing through the 60-mesh screen, dry-pressing under the pressure of 110MPa to form a cylinder with the diameter of 15 x 8, putting the cylinder into a 1700 ℃ rapid heating box furnace, raising the temperature to 550 ℃ according to the heating rate of 3 ℃/min, preserving the temperature for 2 hours, raising the temperature to 1500 ℃ according to the rate of 2 ℃/min, preserving the temperature for 4 hours, and lowering the temperature to room temperature according to the rate of 2 min/° C to obtain the microwave dielectric ceramic sample.
Through detection: the prepared ceramic sample has the dielectric constant of 45.68, the Qf value of about 33000GHz, the temperature coefficient of resonance frequency of 10 ppm/DEG C, compact and uniform structure and good mechanical property.
Example two: selection of Ca0.66Ti0.66Y0.34Al0.34O3Preparing the ceramic powder by chemical proportioning, and adopting high-purity Al with the purity of 99.99 percent2O3、Y2O3、TiO2And CaCO3Preparing raw materials according to the following ingredient table:
by means of planetary ballsMixing materials by grinding, wherein the tank body adopts a nylon ball-milling tank, the capacity of the tank body is 1L, and ZrO of two specifications2And (5) grinding balls. ZrO for each can2The number of balls is: 276g of large balls (which are the same as the columns of the main shaft 5), 138g of small balls (which are the same as the columns of the main shaft 3), and 650g of deionized water as a ball-milling dispersing agent. The material loading amount of each tank is 344.680g, the ball milling speed is about 300 rp/min, the ball milling time is 24 hours, the materials are discharged after being uniformly mixed, and the materials are dried at 100 ℃ and then calcined at 1250 ℃ for 4 hours to pre-synthesize porcelain powder; adding 0.25% of Nd into the synthesized powder2O3And then pouring the mixture into a nylon ball milling tank, adding deionized water and zirconia grinding balls, wherein the weight ratio of the materials to the deionized water to the grinding balls is 1:1.5:2, ball milling for 20 hours, discharging, drying at 100 ℃ and screening by a 60-mesh screen, adding 20wt% of polyvinyl alcohol aqueous solution with the mass fraction of 5% for granulation, drying and grinding by the 60-mesh screen, dry-pressing under the pressure of 110MPa to form a cylinder with phi of 15 x 8, putting the cylinder into a 1700 ℃ rapid heating chamber furnace, raising the temperature to 550 ℃ according to the heating rate of 3 ℃/min, preserving the temperature for 2 hours, raising the temperature to 1500 ℃ according to the rate of 2 ℃/min, preserving the temperature for 4 hours, and lowering the temperature to room temperature according to the rate of 2 min/° C to obtain the microwave dielectric ceramic sample.
Through detection: the prepared ceramic sample has the dielectric constant of 44.98, the Qf value of about 32000GHz, the temperature coefficient of resonance frequency of 2 ppm/DEG C, compact and uniform structure and good mechanical property.
The microwave dielectric material has high Q value, excellent thermal stability, simple components, low price and simple preparation process, and can be applied to satellite communication systems and mobile communication base stations in large batch.
It should be noted that while the invention has been described in terms of the above-mentioned embodiments, other embodiments are also possible. It will be apparent to those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention, and it is intended that all such changes and modifications be covered by the appended claims and their equivalents.
Claims (10)
1. Microwave with medium dielectric constant in high Q valueA dielectric material, characterized by: the material consists of the following components in parts by mass: CaCO3 34 to 37 parts of TiO2 27 to 30 parts of Y2O3 25 to 29 parts of Al2O38 to 9 parts of Sm2O3 0 to 0.5 parts of Nd2O30 to 0.5 part of CeO2 0 to 0.5 portion.
2. A high-Q medium dielectric constant microwave dielectric material as claimed in claim 1, wherein: CaCO3、TiO2 、Y2O3 、Al2O3 、Sm2O3 、Nd2O3 、CeO2The purity of (A) was 99.9%.
3. The method of any one of claims 1-2, wherein the step of preparing the microwave dielectric material with high Q value and medium dielectric constant comprises: the preparation method comprises the following preparation steps:
step one, calculating according to parts by mass, taking CaCO3 34 to 37 parts of TiO2 27 to 30 parts of Y2O3 25 to 29 parts of Al2O3Putting 8-9 parts of the mixture into a ball milling tank, adding deionized water and milling balls into the ball milling tank, performing ball milling for 20-30 hours, uniformly mixing, discharging, and drying to obtain powder for later use;
step two, calcining the powder prepared in the step one to synthesize ceramic powder in advance;
step three, adding Sm into the porcelain powder in the step two according to the mass parts2O3 0 to 0.5 parts of Nd2O30 to 0.5 part of CeO2 Pouring 0-0.5 parts of the mixture into a ball milling tank, adding deionized water and milling balls, discharging after ball milling, drying and sieving to obtain mixed powder;
step four, adding a polyvinyl alcohol aqueous solution into the mixed powder obtained in the step three for granulation, drying, grinding and sieving;
putting the powder granulated in the step four into a die, and performing dry pressing forming under the pressure of 100-120 MPa to form a cylinder to obtain a blank body;
and step six, sintering the pressed blank in a box-type furnace to obtain the microwave dielectric ceramic product.
4. The method of claim 3, wherein the step of preparing the high Q medium dielectric constant microwave dielectric material comprises: in the first step, the ball milling tank is a nylon ball milling tank, the grinding balls are zirconia grinding balls, and the weight ratio of the total amount of the mixed raw materials, deionized water and the grinding balls added into the ball milling tank is 1 (1.5-2) to 1.8-2.2.
5. The method of claim 3, wherein the step of preparing the high Q medium dielectric constant microwave dielectric material comprises: the drying temperature in the first step is 95-105 ℃.
6. The method of claim 3, wherein the step of preparing the high Q medium dielectric constant microwave dielectric material comprises: in the second step, the calcination temperature is 1200-1300 ℃, and the calcination time is 3.5-4.5 h.
7. The method of claim 3, wherein the step of preparing the high Q medium dielectric constant microwave dielectric material comprises: in the third step, the ball milling tank is a nylon ball milling tank, the grinding balls are zirconia grinding balls, the weight ratio of the mixture, the deionized water and the grinding balls added into the ball milling tank is 1 (1.2-1.8) to (1.8-2.2), the ball milling time is 18-22 h, the drying temperature is 95-105 ℃, and the dried powder passes through a screen mesh of 40-80 meshes.
8. The method of claim 3, wherein the step of preparing the high Q medium dielectric constant microwave dielectric material comprises: in the fourth step, the mass fraction of the polyvinyl alcohol aqueous solution is 18-22 wt%, the amount of the added polyvinyl alcohol aqueous solution is 4-6% of the total mass of the mixed powder, and the mixed powder is dried and ground by a screen mesh of 40-80 meshes.
9. The method of claim 3, wherein the step of preparing the high Q medium dielectric constant microwave dielectric material comprises: and fifthly, the mold is cylindrical, the diameter of the mold is 13-17 mm, and the obtained cylinder is phi (13-17) × (7-10).
10. The method of claim 3, wherein the step of preparing the high Q medium dielectric constant microwave dielectric material comprises: the sintering method in the sixth step comprises the following steps: raising the temperature of the box-type furnace to 500-600 ℃ at a heating rate of 2.5-3.5 ℃/min, preserving the heat for 1.5-3 h, raising the temperature to 1480-1530 ℃ at a rate of 1.5-2.5 ℃/min, preserving the heat for 4-6 h, and finally cooling to room temperature at a rate of 1-3 min/DEG C.
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| CN109704764A (en) * | 2019-01-15 | 2019-05-03 | 深圳顺络电子股份有限公司 | Dielectric high-Q microwave dielectric ceramic material, ceramic body and preparation method thereof |
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| JP2001199763A (en) * | 1999-11-12 | 2001-07-24 | Ube Ind Ltd | Dielectric porcelain composition |
| CN103172367A (en) * | 2011-12-22 | 2013-06-26 | 深圳市大富科技股份有限公司 | Preparation method of microwave dielectric ceramic material |
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