CN112573914A - Microwave dielectric ceramic for low-temperature sintering temperature-stable dielectric waveguide and preparation method thereof - Google Patents
Microwave dielectric ceramic for low-temperature sintering temperature-stable dielectric waveguide and preparation method thereof Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 56
- 238000009766 low-temperature sintering Methods 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims description 12
- 238000005245 sintering Methods 0.000 claims abstract description 50
- 239000000463 material Substances 0.000 claims abstract description 36
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 27
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 22
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 18
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium oxide Inorganic materials [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 claims abstract description 16
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 9
- 229910002971 CaTiO3 Inorganic materials 0.000 claims abstract description 8
- 229910010252 TiO3 Inorganic materials 0.000 claims abstract description 7
- 229910017676 MgTiO3 Inorganic materials 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims description 37
- 238000000498 ball milling Methods 0.000 claims description 36
- 239000000843 powder Substances 0.000 claims description 36
- 238000007873 sieving Methods 0.000 claims description 29
- 238000001035 drying Methods 0.000 claims description 27
- 229910052593 corundum Inorganic materials 0.000 claims description 19
- 239000010431 corundum Substances 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- 239000000126 substance Substances 0.000 claims description 9
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 229910052681 coesite Inorganic materials 0.000 claims description 6
- 229910052906 cristobalite Inorganic materials 0.000 claims description 6
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000012798 spherical particle Substances 0.000 claims description 6
- 229910052682 stishovite Inorganic materials 0.000 claims description 6
- 229910052905 tridymite Inorganic materials 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 5
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 3
- 238000000748 compression moulding Methods 0.000 claims description 2
- 239000004615 ingredient Substances 0.000 claims description 2
- 230000000717 retained effect Effects 0.000 claims 1
- 230000000052 comparative effect Effects 0.000 description 10
- 238000004891 communication Methods 0.000 description 7
- 238000003825 pressing Methods 0.000 description 6
- 239000011230 binding agent Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 2
- 238000005469 granulation Methods 0.000 description 2
- 230000003179 granulation Effects 0.000 description 2
- 238000009740 moulding (composite fabrication) Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910000859 α-Fe Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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Abstract
The invention discloses a microwave dielectric ceramic for a low-temperature sintering temperature stable type dielectric waveguide, which comprises a main component and a sintering aid, wherein the phase of the main component comprises MgTiO3、CaTiO3And Li0.5Nd0.5TiO3The microwave dielectric ceramic is prepared from MgO and TiO2、CaCO3、Li2CO3、Nd2O3The molar ratio of MgO is a, TiO2In a molar ratio of b, CaCO3In a molar ratio of c, Li2CO3In a molar ratio of d, Nd2O3The molar ratio of e is more than or equal to 0.20 and less than or equal to 0.30, b is more than or equal to 0.5 and less than or equal to 0.7, c is more than or equal to 0.03 and less than or equal to 0.05, d is more than or equal to 0.02 and less than or equal to 0.04, e is more than or equal to 0.05 and less than or equal to 0.15, and a + b + c + d + e is equal to 1. The microwave dielectric ceramic has the dielectric constant of about 20, low loss, good temperature stability and lower sintering temperature, and can meet the requirements of dielectric waveguide device materials.
Description
Technical Field
The invention belongs to the technical field of electronic ceramics and preparation thereof, and particularly relates to a microwave dielectric ceramic for a low-temperature sintering temperature-stable dielectric waveguide and a preparation method thereof.
Background
The microwave dielectric ceramic is a novel functional ceramic developed in recent decades and is a key material for manufacturing microwave dielectric resonators and filters. On the basis of the original microwave ferrite, the formula and the manufacturing process are greatly upgraded and updated, so that the microwave ferrite has the excellent performances of proper dielectric constant, low microwave loss, near-zero temperature coefficient and the like, is suitable for manufacturing various modern microwave devices, such as frequency-stabilizing oscillators, filters, duplexers and the like in equipment such as electronic countermeasure, navigation, communication, radar, household satellite direct broadcast television receivers, mobile phones and the like, and can meet the requirements of miniaturization, integration, high reliability and low cost of microwave circuits.
With the development of scientific technology, the amount of communication information is rapidly increased, and the requirements of people on wireless communication, the use of microwave communication systems such as satellite communication and satellite direct broadcast television becomes a necessary trend for the development of current communication technology. A filter and a resonator are required to be used in a mobile communication base station system, and with the arrival of the 5G era, a microwave dielectric ceramic having a dielectric constant of about 20, a quality factor value of 70000 or more and a resonant frequency temperature coefficient of near zero is a most core material for producing the filter and the resonator. At present, the microwave dielectric ceramic material for dielectric waveguide is mostly MgO-TiO2The ceramic is mainly used, so that the loss is low, the synthesis process is simple, the raw materials are low in price, but the temperature stability of the ceramic is poor, and the sintering temperature is high, so that the practical application of the ceramic is limited.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a microwave dielectric ceramic for a low-temperature sintering temperature-stable dielectric waveguide and a preparation method thereof; the microwave dielectric ceramic has the advantages of dielectric constant of about 20, low loss, near-zero temperature coefficient of resonant frequency, good temperature stability, excellent microwave dielectric property and lower sintering temperature, and can meet the high requirements of dielectric waveguide device materials.
In order to achieve the technical purpose and achieve the technical effect, the invention is realized by the following technical scheme:
a low-temperature sintering temperature stable type microwave dielectric ceramic for dielectric waveguide is characterized in that: the microwave dielectric ceramic comprises a main component and a sintering aid, wherein the phase of the main component comprises MgTiO3、CaTiO3And Li0.5Nd0.5TiO3The microwave ofThe dielectric ceramic is MgO or TiO2、CaCO3、Li2CO3、Nd2O3The molar ratio of MgO is a, TiO2In a molar ratio of b, CaCO3In a molar ratio of c, Li2CO3In a molar ratio of d, Nd2O3E, a, b, c, d, e satisfy the following conditions: a is more than or equal to 0.20 and less than or equal to 0.30, b is more than or equal to 0.5 and less than or equal to 0.7, c is more than or equal to 0.03 and less than or equal to 0.05, d is more than or equal to 0.02 and less than or equal to 0.04, e is more than or equal to 0.05 and less than or equal to 0.15, and a + b + c + d + e is equal to 1;
the chemical composition of the sintering aid is xLi2CO3-ySiO2Wherein x and y represent molar ratios, respectively, and x is 0.6-0.8, y is 0.2-0.4, and x + y is 1.
Further, the mass ratio of the main component to the sintering aid is 1: 0.1-0.2.
Furthermore, the relative dielectric constant of the microwave dielectric ceramic is 18.0-22, the quality factor Qxf is 55000 GHz-85000 GHz, and the temperature coefficient of the resonance frequency is-10 ppm/DEG C to +10 ppm/DEG C.
The invention also provides a preparation method of the microwave dielectric ceramic for the low-temperature sintering temperature-stable dielectric waveguide, which comprises the following steps:
(1) mixing MgO and TiO2、CaCO3、Li2CO3、Nd2O3Mixing according to a molar ratio of a, TiO and MgO2In a molar ratio of b, CaCO3In a molar ratio of c, Li2CO3In a molar ratio of d, Nd2O3E, a, b, c, d, e satisfy the following conditions: a is more than or equal to 0.20 and less than or equal to 0.30, b is more than or equal to 0.5 and less than or equal to 0.7, c is more than or equal to 0.03 and less than or equal to 0.05, d is more than or equal to 0.02 and less than or equal to 0.04, e is more than or equal to 0.05 and less than or equal to 0.15, and a + b + c + d + e is equal to 1; fully mixing all the powder materials, then carrying out ball milling, drying and sieving after ball milling, and then putting the powder materials into a corundum crucible for roasting to obtain the main component of the microwave dielectric ceramic;
(2) according to chemical composition xLi2CO3-ySiO2Stoichiometric ratio of (A) to (B) Li2CO3And SiO2Preparing materials, wherein x and y respectively represent a molar ratio, x is more than or equal to 0.6 and less than or equal to 0.8, y is more than or equal to 0.2 and less than or equal to 0.4, and x + y is equal to 1; mixing the materialsFully mixing, performing ball milling, drying and sieving after ball milling, and then putting into a corundum crucible for roasting to obtain a sintering aid;
(3) mixing the main component and the sintering aid, performing ball milling, drying, granulating, sieving, performing compression molding on the sieved granular powder, and finally sintering to obtain the microwave dielectric ceramic for the low-temperature sintering temperature stable type dielectric waveguide.
Further, in the step (3), the mass ratio of the main component to the sintering aid is 1: 0.1-0.2.
Further, the drying temperature in the step (1), the drying temperature in the step (2) and the drying temperature in the step (3) are all 100-120 ℃, and the ball milling time is all 4-8 h.
Further, the sieving in the step (1) and the sieving in the step (2) are both 60-mesh sieving screens, the sieving in the step (3) is double-layer sieving screens, namely 60-mesh sieving screens and 120-mesh sieving screens, and the particles remained on the 120-mesh sieving screens are taken.
Further, in the granulation in the step (3), the dried powder is mixed with a polyvinyl alcohol aqueous solution with the mass fraction of 5%, and then micron-sized spherical particles are prepared.
Further, the roasting temperature in the step (1) is 1000-1050 ℃, the roasting temperature in the step (2) is 600-800 ℃, and the roasting heat preservation time in the step (1) and the step (2) is 3-5 hours.
Further, the sintering temperature in the step (3) is 1100-1250 ℃, and the sintering heat preservation time is 4-6 h.
Compared with the prior art, the invention has the following beneficial effects: the invention uses MgO and TiO2、CaCO3、Li2CO3、Nd2O3The raw materials are mixed, the specific molar ratio of each component is designed, and the specific sintering aid is added to obtain the MgTiO powder with the main component composition3+CaTiO3+Li0.5Nd0.5TiO3The microwave dielectric ceramic of (3); the addition of the specific sintering aid can improve the temperature stability and reduce the sintering temperature; in which a small amount of CaTiO3The temperature stability of the whole microwave dielectric ceramic can be improved; from MgTiO3、CaTiO3、Li0.5Nd0.5TiO3The three microwave dielectric ceramics matched with each other have the dielectric constant epsilon r of about 20, higher quality factor (Qxf), lower loss, nearly zero temperature coefficient tau f of resonance frequency, good temperature stability, lower sintering temperature and excellent microwave dielectric comprehensive performance, can meet the high requirement of dielectric waveguide device materials, is used for producing dielectric waveguide devices for 5G communication antennas, and has higher practical use value. In addition, the preparation process is simple, the production cost is low, no pollution is caused, and the industrialization prospect is good.
Detailed Description
The technical solutions in the present invention will be described clearly and completely with reference to specific embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a microwave dielectric ceramic for a low-temperature sintering temperature stable type dielectric waveguide, which comprises a main component and a sintering aid, wherein the phase of the main component comprises MgTiO3、CaTiO3And Li0.5Nd0.5TiO3The microwave dielectric ceramic is prepared from MgO and TiO2、CaCO3、Li2CO3、Nd2O3The molar ratio of MgO is a, TiO2In a molar ratio of b, CaCO3In a molar ratio of c, Li2CO3In a molar ratio of d, Nd2O3E, a, b, c, d, e satisfy the following conditions: a is more than or equal to 0.20 and less than or equal to 0.30, b is more than or equal to 0.5 and less than or equal to 0.7, c is more than or equal to 0.03 and less than or equal to 0.05, d is more than or equal to 0.02 and less than or equal to 0.04, e is more than or equal to 0.05 and less than or equal to 0.15, and a + b + c + d + e is equal to 1;
the chemical composition of the sintering aid is xLi2CO3-ySiO2Wherein x and y represent molar ratios, respectively, and x is 0.6-0.8, y is 0.2-0.4, and x + y is 1.
Wherein the mass ratio of the main component to the sintering aid is 1: 0.1-0.2.
The relative dielectric constant of the microwave dielectric ceramic is 18.0-22, the quality factor Qxf is 55000 GHz-85000 GHz, and the temperature coefficient of the resonance frequency is-10 ppm/DEG C to +10 ppm/DEG C.
The invention also provides a preparation method of the microwave dielectric ceramic for the low-temperature sintering temperature stable type dielectric waveguide, which comprises the following steps:
(1) mixing MgO and TiO2、CaCO3、Li2CO3、Nd2O3Mixing according to a molar ratio of a, TiO and MgO2In a molar ratio of b, CaCO3In a molar ratio of c, Li2CO3In a molar ratio of d, Nd2O3E, a, b, c, d, e satisfy the following conditions: a is more than or equal to 0.20 and less than or equal to 0.30, b is more than or equal to 0.5 and less than or equal to 0.7, c is more than or equal to 0.03 and less than or equal to 0.05, d is more than or equal to 0.02 and less than or equal to 0.04, e is more than or equal to 0.05 and less than or equal to 0.15, and a + b + c + d + e is equal to 1; fully mixing all the powder materials, then carrying out ball milling, drying and sieving after ball milling, and then putting the powder materials into a corundum crucible for roasting to obtain the main component of the microwave dielectric ceramic;
(2) according to chemical composition xLi2CO3-ySiO2Stoichiometric ratio of (A) to (B) Li2CO3And SiO2Preparing materials, wherein x and y respectively represent a molar ratio, x is more than or equal to 0.6 and less than or equal to 0.8, y is more than or equal to 0.2 and less than or equal to 0.4, and x + y is equal to 1; fully mixing the ingredients, performing ball milling, drying and sieving after ball milling, and then putting into a corundum crucible for roasting to obtain a sintering aid;
(3) the microwave dielectric ceramic for the low-temperature sintering temperature stable type dielectric waveguide is prepared by fully mixing the main components and the sintering aid according to the mass ratio of 1: 0.1-0.2, then carrying out ball milling, drying, granulating, sieving, pressing and forming sieved granular powder, and finally sintering.
The drying temperature in the step (1), the drying temperature in the step (2) and the drying temperature in the step (3) are all 100-120 ℃, and the ball milling time is all 4-8 h.
Sieving in the step (1) and the step (2) are both 60-mesh sieves, sieving in the step (3) is a double-layer sieve, namely sieving with 60-mesh and 120-mesh sieves respectively, and taking particles remained on the 120-mesh sieve.
And (3) mixing the dried powder with a polyvinyl alcohol aqueous solution (binder) with the mass fraction of 5% during granulation, and then preparing micron-sized spherical particles.
The roasting temperature in the step (1) is 1000-1050 ℃, the roasting temperature in the step (2) is 600-800 ℃, and the roasting heat preservation time in the step (1) and the step (2) is 3-5 hours; the sintering temperature in the step (3) is 1100-1250 ℃, and the sintering heat preservation time is 4-6 h.
And (3) pressing and forming, namely pressing the granular powder into a cylinder with the diameter of 10mm and the height of 6 mm.
The roasting process in the step (1), the step (2) and the sintering process in the step (3) are all carried out in an air atmosphere.
In the step (1) and the step (2), when the sieved powder is placed in a corundum crucible, the crucible is vibrated or knocked to enable the powder to be tightly stacked.
The following are specific examples of the present invention.
Examples 1 to 8:
the preparation method of the microwave dielectric ceramic for the low-temperature sintering temperature-stable dielectric waveguide comprises the following steps:
(1) mixing MgO and TiO2、CaCO3、Li2CO3、Nd2O3Blending according to the molar ratio (a, b, c, d, e) in the table 1; mixing all the powder materials fully, ball-milling for 5h, drying at 110 ℃ after ball-milling, then sieving by a 60-mesh sieve, putting the sieved powder materials into a corundum crucible, roasting at 1000 ℃ and keeping the temperature for 4h to obtain the MgTiO powder3+CaTiO3+Li0.5Nd0.5TiO3The main component of (1);
(2) according to chemical composition 0.6Li2CO3-0.4SiO2Stoichiometric ratio of (A) to (B) Li2CO3And SiO2Mixing the materials, fully mixing the materials, performing ball milling for 5 hours, drying the materials at the temperature of 110 ℃ after ball milling, then sieving the materials by a 60-mesh sieve, putting the sieved powder into a corundum crucible, and then putting the corundum crucible into the corundum crucible to be roasted and insulated for 4 hours at the temperature of 800 ℃ to obtain a sintering aid;
(3) fully mixing the main components and the sintering aid according to the mass ratio of 1:0.15, carrying out ball milling for 6 hours, drying at the temperature of 110 ℃ after ball milling, mixing the dried powder with a polyvinyl alcohol aqueous solution (binder) with the mass fraction of 5%, then preparing micron-sized spherical particles, sieving with 60-mesh and 120-mesh sieves, taking the particles left on the 120-mesh sieves, pressing the sieved particle powder into cylinders with the diameter of 10mm and the height of 6mm, and finally sintering at the sintering temperature in the table 1 and keeping the temperature for 5 hours to obtain the microwave dielectric ceramic for the low-temperature sintering temperature stable type dielectric waveguide.
TABLE 1 respective ratios, sintering temperatures and microwave dielectric properties of the microwave dielectric ceramics of examples 1-8
Comparative example 1
The preparation method of the microwave dielectric ceramic of the comparative example 1 comprises the following steps:
(1) mixing MgO and TiO2、CaCO3According to a molar ratio of 0.2: 0.6: 0.2, batching; fully mixing all the powder materials, performing ball milling for 5 hours, drying the powder materials at the temperature of 110 ℃ after ball milling, then sieving the powder materials by a 60-mesh sieve, putting the sieved powder materials into a corundum crucible, and roasting and preserving heat for 4 hours at the temperature of 1000 ℃ to obtain the main component of the microwave dielectric ceramic;
(2) according to chemical composition 0.6Li2CO3-0.4SiO2Stoichiometric ratio of (A) to (B) Li2CO3And SiO2Mixing the materials, fully mixing the materials, performing ball milling for 5 hours, drying the materials at the temperature of 110 ℃ after ball milling, then sieving the materials by a 60-mesh sieve, putting the sieved powder into a corundum crucible, and then putting the corundum crucible into the corundum crucible to be roasted and insulated for 4 hours at the temperature of 800 ℃ to obtain a sintering aid;
(3) fully mixing the main components and the sintering aid according to the mass ratio of 1:0.15, carrying out ball milling for 6h, drying at the temperature of 110 ℃ after ball milling, mixing the dried powder with a polyvinyl alcohol aqueous solution (binder) with the mass fraction of 5%, then preparing micron-sized spherical particles, sieving with 60-mesh and 120-mesh sieves, taking the particles remained on the 120-mesh sieves, pressing the sieved particle powder into cylinders with the diameter of 10mm and the height of 6mm, and finally sintering at 1350 ℃ and keeping the temperature for 5h to obtain the microwave dielectric ceramic of the comparative example 1.
Comparative example 2
The preparation method of the microwave dielectric ceramic of the comparative example 2 comprises the following steps:
(1) mixing MgO and TiO2、CaCO3According to a molar ratio of 0.2: 0.7: 0.1, batching; fully mixing all the powder materials, performing ball milling for 5 hours, drying the powder materials at the temperature of 110 ℃ after ball milling, then sieving the powder materials by a 60-mesh sieve, putting the sieved powder materials into a corundum crucible, and roasting and preserving heat for 4 hours at the temperature of 1000 ℃ to obtain the main component of the microwave dielectric ceramic;
(2) according to chemical composition 0.6Li2CO3-0.4SiO2Stoichiometric ratio of (A) to (B) Li2CO3And SiO2Mixing the materials, fully mixing the materials, performing ball milling for 5 hours, drying the materials at the temperature of 110 ℃ after ball milling, then sieving the materials by a 60-mesh sieve, putting the sieved powder into a corundum crucible, and then putting the corundum crucible into the corundum crucible to be roasted and insulated for 4 hours at the temperature of 800 ℃ to obtain a sintering aid;
(3) fully mixing the main components and the sintering aid according to the mass ratio of 1:0.15, carrying out ball milling for 6h, drying at the temperature of 110 ℃ after ball milling, mixing the dried powder with a polyvinyl alcohol aqueous solution (binder) with the mass fraction of 5%, then preparing micron-sized spherical particles, sieving with 60-mesh and 120-mesh sieves, taking the particles remained on the 120-mesh sieves, pressing the sieved particle powder into cylinders with the diameter of 10mm and the height of 6mm, and finally sintering at 1350 ℃ and keeping the temperature for 5h to obtain the microwave dielectric ceramic of the comparative example 2.
The microwave dielectric properties of the microwave dielectric ceramics of comparative example 1 and comparative example 2 are shown in table 2.
TABLE 2 microwave dielectric Properties of the microwave dielectric ceramics of comparative examples 1 and 2
As can be seen from the comparison between examples 1-8 and comparative examples 1 and 2, the microwave dielectric ceramics of examples 1-8 of the present invention has a dielectric constant of about 20, and has a high quality factor and a near-zero temperature coefficient of resonant frequency, a good temperature stability, an excellent microwave dielectric combination property, and a low sintering temperature, and can meet the high requirements of dielectric waveguide device materials.
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 and equivalents made by the contents of the present invention or directly or indirectly applied to other related technical fields are included in the scope of the present invention.
Claims (10)
1. A low-temperature sintering temperature stable type microwave dielectric ceramic for dielectric waveguide is characterized in that: the microwave dielectric ceramic comprises a main component and a sintering aid, wherein the phase of the main component comprises MgTiO3、CaTiO3And Li0.5Nd0.5TiO3The microwave dielectric ceramic is prepared from MgO and TiO2、CaCO3、Li2CO3、Nd2O3The molar ratio of MgO is a, TiO2In a molar ratio of b, CaCO3In a molar ratio of c, Li2CO3In a molar ratio of d, Nd2O3E, a, b, c, d, e satisfy the following conditions: a is more than or equal to 0.20 and less than or equal to 0.30, b is more than or equal to 0.5 and less than or equal to 0.7, c is more than or equal to 0.03 and less than or equal to 0.05, d is more than or equal to 0.02 and less than or equal to 0.04, e is more than or equal to 0.05 and less than or equal to 0.15, and a + b + c + d + e is equal to 1;
the chemical composition of the sintering aid is xLi2CO3-ySiO2Wherein x and y represent molar ratios, respectively, and x is 0.6-0.8, y is 0.2-0.4, and x + y is 1.
2. A low temperature sintered temperature stable microwave dielectric ceramic for dielectric waveguides as claimed in claim 1, wherein: the mass ratio of the main component to the sintering aid is 1: 0.1-0.2.
3. A low temperature sintered temperature stable microwave dielectric ceramic for dielectric waveguides as claimed in claim 1, wherein: the relative dielectric constant of the microwave dielectric ceramic is 18.0-22, the quality factor Qxf is 55000 GHz-85000 GHz, and the temperature coefficient of the resonance frequency is-10 ppm/DEG C to +10 ppm/DEG C.
4. A preparation method of microwave dielectric ceramic for low-temperature sintering temperature-stable dielectric waveguide is characterized by comprising the following steps:
(1) mixing MgO and TiO2、CaCO3、Li2CO3、Nd2O3Mixing according to a molar ratio of a, TiO and MgO2In a molar ratio of b, CaCO3In a molar ratio of c, Li2CO3In a molar ratio of d, Nd2O3E, a, b, c, d, e satisfy the following conditions: a is more than or equal to 0.20 and less than or equal to 0.30, b is more than or equal to 0.5 and less than or equal to 0.7, c is more than or equal to 0.03 and less than or equal to 0.05, d is more than or equal to 0.02 and less than or equal to 0.04, e is more than or equal to 0.05 and less than or equal to 0.15, and a + b + c + d + e is equal to 1; fully mixing all the powder materials, then carrying out ball milling, drying and sieving after ball milling, and then putting the powder materials into a corundum crucible for roasting to obtain the main component of the microwave dielectric ceramic;
(2) according to chemical composition xLi2CO3-ySiO2Stoichiometric ratio of (A) to (B) Li2CO3And SiO2Preparing materials, wherein x and y respectively represent a molar ratio, x is more than or equal to 0.6 and less than or equal to 0.8, y is more than or equal to 0.2 and less than or equal to 0.4, and x + y is equal to 1; fully mixing the ingredients, performing ball milling, drying and sieving after ball milling, and then putting into a corundum crucible for roasting to obtain a sintering aid;
(3) mixing the main component and the sintering aid, performing ball milling, drying, granulating, sieving, performing compression molding on the sieved granular powder, and finally sintering to obtain the microwave dielectric ceramic for the low-temperature sintering temperature stable type dielectric waveguide.
5. The method for preparing a microwave dielectric ceramic for a low-temperature sintering temperature stable dielectric waveguide according to claim 4, wherein in the step (3), the mass ratio of the main component to the sintering aid is 1: 0.1-0.2.
6. The method for preparing a microwave dielectric ceramic for a low-temperature sintering temperature stable type dielectric waveguide according to claim 4, wherein the drying temperature in the step (1), the drying temperature in the step (2) and the drying temperature in the step (3) are 100 ℃ to 120 ℃, and the ball milling time is 4h to 8 h.
7. The method of claim 4, wherein the screens in step (1) and step (2) are 60 mesh screens, and the screens in step (3) are double layer screens, namely 60 mesh screens and 120 mesh screens, respectively, and the particles retained on the 120 mesh screens are collected.
8. The method according to claim 4, wherein the step (3) of granulating comprises mixing the dried powder with 5% by weight of aqueous solution of polyvinyl alcohol, and then granulating into micron-sized spherical particles.
9. The method for preparing a microwave dielectric ceramic for a low-temperature sintering temperature stable dielectric waveguide according to claim 4, wherein the sintering temperature in the step (1) is 1000-1050 ℃, the sintering temperature in the step (2) is 600-800 ℃, and the sintering heat preservation time in the step (1) and the step (2) is 3-5 h.
10. The method for preparing a microwave dielectric ceramic for a low-temperature sintering temperature stable type dielectric waveguide according to claim 4, wherein the sintering temperature in the step (3) is 1100-1250 ℃, and the sintering holding time is 4-6 h.
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Inventor after: Ji An Inventor after: Jin Zhenlong Inventor before: Ji An Inventor before: Wang Xiaohui Inventor before: Jin Zhenlong |