CN111995383B - Mg2-xMxSiO4-CaTiO3Composite microwave dielectric ceramic and preparation method thereof - Google Patents
Mg2-xMxSiO4-CaTiO3Composite microwave dielectric ceramic and preparation method thereof Download PDFInfo
- Publication number
- CN111995383B CN111995383B CN202010936202.2A CN202010936202A CN111995383B CN 111995383 B CN111995383 B CN 111995383B CN 202010936202 A CN202010936202 A CN 202010936202A CN 111995383 B CN111995383 B CN 111995383B
- Authority
- CN
- China
- Prior art keywords
- putting
- catio
- sio
- ball milling
- temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
- C04B35/20—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in magnesium oxide, e.g. forsterite
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
- C04B35/462—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates
- C04B35/465—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/6261—Milling
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3208—Calcium oxide or oxide-forming salts thereof, e.g. lime
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3275—Cobalt oxides, cobaltates or cobaltites or oxide forming salts thereof, e.g. bismuth cobaltate, zinc cobaltite
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3279—Nickel oxides, nickalates, or oxide-forming salts thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3281—Copper oxides, cuprates or oxide-forming salts thereof, e.g. CuO or Cu2O
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3284—Zinc oxides, zincates, cadmium oxides, cadmiates, mercury oxides, mercurates or oxide forming salts thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
Abstract
The invention discloses Mg2‑xMxSiO4‑CaTiO3The composite microwave dielectric ceramic and the preparation method thereof are disclosed, wherein: x is not less than 0.01 and not more than 0.03, M is Zn, Cu, Co, Ni, CaTiO3The mass fraction of the components is 10-50%, and the steps are as follows: (1) will (MgCO)3)4·Mg(OH)2·5H2O、ZnO、CuO、CoO、NiO、TiO2Weighing and ball-milling with CaCO3 according to the chemical ratio; (2) drying and sieving; (3) pre-sintering at 1300 ℃; (4) mixing Mg2‑xMxSiO4And CaTiO3Weighing according to the mass ratio of the mixture ratio and performing secondary ball milling; (5) drying and sieving; (6) adding polyvinyl alcohol for granulation and compression molding; (7) sintering at 1225-1275 deg.c; (8) and (5) testing the dielectric property. The invention reduces Mg by doping different ions2SiO4Sintering temperature of microwave dielectric ceramic, and addition of the ceramic and CaTiO3Compounding, and adjusting the temperature coefficient to obtain the near-zero temperature coefficient microwave dielectric ceramic.
Description
Technical Field
The invention relates to the technical field of microwave dielectric ceramics, in particular to Mg with high quality factor2-xMxSiO4-CaTiO3The composite microwave dielectric ceramic is suitable for preparing microwave components such as filters, antennas, capacitors and the like, and belongs to the field of microwave dielectric ceramics.
Background
With the development of 5G technology standards, the need for miniaturization of components and low power consumption of components is becoming more apparent in the construction of 5G base stations. Compared with a metal cavity, the microwave ceramic powder has the material characteristic of high Q value, so that the insertion loss is greatly reduced, and the microwave ceramic powder has the characteristics of high out-of-band rejection, good temperature drift characteristic, wide temperature application range, various packaging structures and output interface forms, and meets the development trend of miniaturization and low power consumption of a base station filter, so that the ceramic dielectric filter gradually replaces the traditional metal cavity filter.
Mg2SiO4The microwave dielectric ceramic has the characteristic of high quality factor and is suitable for being used as a ceramic filter. However, Mg2SiO4Tau of the systemfNegative values are not beneficial to the stability of the microwave device in practical application. Therefore, it is required to have positive τfThe dielectric ceramic material with the value is compounded according to a certain proportion to reach a temperature coefficient close to zero, thereby ensuring the temperature stability of the material and meeting the actual requirements of a microwave circuit. In which CaTiO3(εr≈170，Q×f≈3600GHz，τf≈800×10-6/℃)、SrTiO3(εr≈300， Q×f≈3000GHz，τf≈1650×10-6/° c) is a commonly used material for adjusting a negative temperature coefficient due to a large positive temperature coefficient. Researchers use sol-gel method to deposit Mg2SiO4With CaTiO3Composite, formed Mg2SiO4@CaTiO3The microwave dielectric property of the composite dielectric ceramic material is that epsilon r is approximately equal to 9.4, Q multiplied by f is approximately equal to 19000 GHz, tauf≈0×10-6/° C, satisfy τfA value approaching zero. However, Mg2SiO4–CaTiO3The preparation of the system material often requires high sintering temperatures (1300-1350 ℃).
Disclosure of Invention
The purpose of the invention is to overcome Mg2SiO4The system has a negative temperature coefficient, Mg2SiO4–CaTiO3The sintering temperature of the system is high, and Mg is improved2-xMxSiO4–CaTiO3Dielectric property of the system, lowering sintering temperature to (MgCO)3)4·Mg(OH)2·5H2O、ZnO、CuO、CoO、NiO、TiO2And CaCO3As raw material, providing Mg2-xMxSiO4-CaTiO3A method for preparing composite microwave dielectric ceramic and a preparation method thereof.
The invention is realized by the following technical scheme.
Mg2-xMxSiO4-CaTiO3A composite microwave dielectric ceramic, wherein: x is not less than 0.01 and not more than 0.03, M is Zn, Cu, Co, Ni, CaTiO3The mass fraction of the active carbon is 10-50%, and the preparation method comprises the following steps:
(1) will (MgCO)3)4·Mg(OH)2·5H2O、ZnO、CuO、CoO、NiO、TiO2And CaCO3Weighing according to a chemical ratio, putting deionized water and zirconia balls as a solvent and a ball milling medium into a polyurethane ball milling tank to perform ball milling for 8-24 hours on a planetary ball mill;
(2) putting the ball-milled raw materials in the step (1) into a drying oven, drying at 100 ℃, and then crushing and sieving with a 100-mesh sieve;
(3) putting the powder sieved in the step (2) into an alumina crucible, putting the alumina crucible into a sintering furnace, heating the alumina crucible to 1300 ℃ at the heating rate of 10 ℃ per minute, and preserving the heat at the temperature of 1300 ℃ for 2 hours to respectively obtain Mg2-xMxSiO4And CaTiO3；
(4) Mixing Mg2-xMxSiO4And CaTiO3Weighing the components according to the ratio of mass fraction, taking deionized water and zirconia balls as a solvent and a ball milling medium, and putting the solvent and the zirconia balls into a polyurethane ball milling tank to perform ball milling for 4 to 8 hours on a planetary ball mill;
(5) putting the powder subjected to ball milling in the step (4) into a drying oven, drying at 100 ℃, and then crushing and sieving with a 200-mesh sieve;
(6) putting the powder sieved in the step (5) into a mortar, adding a PVA solution with the mass of 8 wt% of the powder and the concentration of 5 wt%, grinding and granulating, and then pressing and forming by using a tablet press;
(7) Putting the green body formed by pressing in the step (6) into a sintering furnace, sintering at the temperature of 1225-1275 ℃, and preserving heat for 4 hours to obtain microwave dielectric ceramic;
and (5) carrying out dielectric property test on the microwave dielectric ceramic prepared in the step (7).
The ball grinding material obtained in the step (1) and the step (4): water: the mass ratio of the balls is 1:8:8, and the rotating speed is 400 r/min.
The heating rate of the step (3) is 5 ℃/min.
The forming pressure of the step (6) is 4MPa, the diameter of the green body is 16mm, and the height of the green body is 8 mm.
The sintering system in the step (7) is that the temperature is raised to 200 ℃ at the speed of 3 ℃/min and is preserved for 1h, and the temperature is raised to 500 ℃ at the speed of 3 ℃/min and is preserved for 2 h; heating to the target temperature at the speed of 2 ℃/min and preserving the heat for 4 h.
The preferable time of the step (1) is 12 hours, the preferable time of the step (4) is 6 hours, and the preferable sintering temperature of the step (7) is 1250 ℃.
The invention has the beneficial effect that the Mg is reduced by certain doping2SiO4–CaTiO3The microwave dielectric ceramic is sintered at the medium temperature of 1225 ℃ to successfully prepare high-performance Mg2SiO4–CaTiO3Microwave dielectric ceramic having a dielectric constant εr8.12 to 15.23, Q × f 42000 to 56000GHz, and temperature coefficient of resonance frequency τf＝-10～5×10-6/° c; can be used for preparing microwave devices such as filters, antennas and the like, and has good application prospect.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the present invention is not limited to the examples.
Example 1-1
16.592g (MgCO) is weighed according to the formula proportion3)4·Mg(OH)2·5H2O，0.163g ZnO，6g SiO2And 10g of CaCO3,.7.99g TiO2Respectively putting the mixed powder into a polyurethane ball milling tank, adding 180g of deionized water, 180g of zirconia balls, 140g of deionized water and 140g of zirconia balls, and carrying out ball milling on a planetary ball mill for 12 hours at the rotating speed of 400 r/min; putting the ball-milled raw materials into a drying oven, drying at 100 ℃, and then crushing and sieving by a 100-mesh sieve; placing the sieved powder into a sintering furnace, and adding Mg2-0.01Zn0.01SiO4And CaTiO3Heating to 1300 ℃ according to the heating rate of 5 ℃/min for presintering, and keeping the temperature for 2 h; weighing 12g of Mg2-0.01Zn0.01SiO4And 8g of CaTiO3Putting the mixture into a polyurethane ball milling tank, adding 160g of deionized water and 160g of zirconia balls,ball-milling for 6 hours on a planetary ball mill at the rotating speed of 400 r/min; putting the ball-milled powder into a drying oven to be dried at 100 ℃, and then crushing and sieving the powder by a 200-mesh sieve; putting the sieved powder into a mortar, adding a PVA solution with the mass of 8 wt% and the concentration of 5 wt% of the powder, grinding and granulating, and pressing into a green body with the diameter of 16mm and the height of 8mm by using a tablet press under the pressure of 4 MPa; putting the pressed and molded blank into a sintering furnace, heating to 200 ℃ at the heating rate of 3 ℃/min, and keeping the temperature for 1h, and heating to 500 ℃ at the heating rate of 3 ℃/min, and keeping the temperature for 2 h; heating up to 1250 ℃ at the heating rate of 2 ℃/min and preserving heat for 4h to prepare the microwave dielectric ceramic.
Examples 1 to 2
16.425g (MgCO) is weighed according to the formula proportion3)4·Mg(OH)2·5H2O，0.326g ZnO，6g SiO2And 10g of CaCO3,.7.99g TiO2Respectively putting the mixed powder into a polyurethane ball milling tank, adding 180g of deionized water, 180g of zirconia balls, 140g of deionized water and 140g of zirconia balls, and carrying out ball milling on a planetary ball mill for 12 hours at the rotating speed of 400 r/min; putting the ball-milled raw materials into a drying oven, drying at 100 ℃, and then crushing and sieving by a 100-mesh sieve; placing the sieved powder into a sintering furnace, and adding Mg2-0.02Zn0.02SiO4And CaTiO3Heating to 1300 ℃ according to the heating rate of 5 ℃/min for presintering, and keeping the temperature for 2 h; weighing 12g of Mg2-0.02Zn0.02SiO4And 8g of CaTiO3Putting the mixture into a polyurethane ball milling tank, adding 160g of deionized water and 160g of zirconia balls, and ball milling the mixture for 6 hours on a planetary ball mill at the rotating speed of 400 r/min; putting the ball-milled powder into a drying oven to be dried at 100 ℃, and then crushing and sieving the powder by a 200-mesh sieve; putting the sieved powder into a mortar, adding a PVA solution with the mass of 8 wt% and the concentration of 5 wt% of the powder, grinding and granulating, and pressing into a green body with the diameter of 16mm and the height of 8mm by using a tablet press under the pressure of 4 MPa; putting the pressed and molded blank into a sintering furnace, heating to 200 ℃ at the heating rate of 3 ℃/min, and keeping the temperature for 1h, and heating to 500 ℃ at the heating rate of 3 ℃/min, and keeping the temperature for 2 h; heating up to 1250 ℃ at the heating rate of 2 ℃/min and preserving heat for 4h to prepare the microwave dielectric ceramic.
Examples 1 to 3
16.257g (MgCO) is weighed according to the formula proportion3)4·Mg(OH)2·5H2O，0.488g ZnO，6g SiO2And 10g of CaCO3,.7.99g TiO2Respectively putting the mixed powder into a polyurethane ball milling tank, adding 180g of deionized water, 180g of zirconia balls, 140g of deionized water and 140g of zirconia balls, and carrying out ball milling on a planetary ball mill for 12 hours at the rotating speed of 400 r/min; putting the ball-milled raw materials into a drying oven, drying at 100 ℃, and then crushing and sieving by a 100-mesh sieve; placing the sieved powder into a sintering furnace, and adding Mg2-0.03Zn0.03SiO4And CaTiO3Heating to 1300 ℃ according to the heating rate of 5 ℃/min for presintering, and keeping the temperature for 2 h; weighing 12g of Mg2-0.03Zn0.03SiO4And 8g of CaTiO3Putting the mixture into a polyurethane ball milling tank, adding 160g of deionized water and 160g of zirconia balls, and ball milling the mixture for 6 hours on a planetary ball mill at the rotating speed of 400 r/min; putting the ball-milled powder into a drying oven to be dried at 100 ℃, and then crushing and sieving the powder by a 200-mesh sieve; putting the sieved powder into a mortar, adding a PVA solution with the mass of 8 wt% and the concentration of 5 wt% of the powder, grinding and granulating, and pressing into a green body with the diameter of 16mm and the height of 8mm by using a tablet press under the pressure of 4 MPa; putting the pressed and molded blank into a sintering furnace, heating to 200 ℃ at the heating rate of 3 ℃/min, and keeping the temperature for 1h, and heating to 500 ℃ at the heating rate of 3 ℃/min, and keeping the temperature for 2 h; heating up to 1250 ℃ at the heating rate of 2 ℃/min and preserving heat for 4h to prepare the microwave dielectric ceramic.
Example 2-1
16.592g (MgCO) is weighed according to the formula proportion3)4·Mg(OH)2·5H2O，0.159g CuO，6g SiO2And 10g of CaCO3,.7.99g TiO2Respectively putting the mixed powder into a polyurethane ball milling tank, adding 180g of deionized water, 180g of zirconia balls, 140g of deionized water and 140g of zirconia balls, and carrying out ball milling on a planetary ball mill for 12 hours at the rotating speed of 400 r/min; putting the ball-milled raw materials into a drying oven, drying at 100 ℃, and then crushing and sieving by a 100-mesh sieve; placing the sieved powder into a sintering furnace, and adding Mg2-0.01Cu0.01SiO4And CaTiO3Heating to 1300 ℃ according to the heating rate of 5 ℃/min for presintering, and keeping the temperature for 2 h;weighing 12g of Mg2-0.01Cu0.01SiO4And 8g of CaTiO3Putting the mixture into a polyurethane ball milling tank, adding 160g of deionized water and 160g of zirconia balls, and ball milling the mixture for 6 hours on a planetary ball mill at the rotating speed of 400 r/min; putting the ball-milled powder into a drying oven to be dried at 100 ℃, and then crushing and sieving the powder by a 200-mesh sieve; putting the sieved powder into a mortar, adding a PVA solution with the mass of 8 wt% and the concentration of 5 wt% of the powder, grinding and granulating, and pressing into a green body with the diameter of 16mm and the height of 8mm by using a tablet press under the pressure of 4 MPa; putting the pressed and molded blank into a sintering furnace, heating to 200 ℃ at the heating rate of 3 ℃/min, and keeping the temperature for 1h, and heating to 500 ℃ at the heating rate of 3 ℃/min, and keeping the temperature for 2 h; heating up to 1250 ℃ at the heating rate of 2 ℃/min and preserving heat for 4h to prepare the microwave dielectric ceramic.
Examples 2 to 2
16.592g (MgCO) is weighed according to the formula proportion3)4·Mg(OH)2·5H2O，0.318g CuO，6g SiO2And 10g of CaCO3,.7.99g TiO2Respectively putting the mixed powder into a polyurethane ball milling tank, adding 180g of deionized water, 180g of zirconia balls, 140g of deionized water and 140g of zirconia balls, and carrying out ball milling on a planetary ball mill for 12 hours at the rotating speed of 400 r/min; putting the ball-milled raw materials into a drying oven, drying at 100 ℃, and then crushing and sieving by a 100-mesh sieve; placing the sieved powder into a sintering furnace, and adding Mg2-0.02Cu0.02SiO4And CaTiO3Heating to 1300 ℃ according to the heating rate of 5 ℃/min for presintering, and keeping the temperature for 2 h; weighing 12g of Mg2-0.02Cu0.02SiO4And 8g of CaTiO3Putting the mixture into a polyurethane ball milling tank, adding 160g of deionized water and 160g of zirconia balls, and ball milling the mixture for 6 hours on a planetary ball mill at the rotating speed of 400 r/min; putting the ball-milled powder into a drying oven to be dried at 100 ℃, and then crushing and sieving the powder by a 200-mesh sieve; putting the sieved powder into a mortar, adding a PVA solution with the mass of 8 wt% and the concentration of 5 wt% of the powder, grinding and granulating, and pressing into a green body with the diameter of 16mm and the height of 8mm by using a tablet press under the pressure of 4 MPa; putting the pressed and molded blank into a sintering furnace, heating to 200 ℃ at the heating rate of 3 ℃/min, and keeping the temperature for 1h, and heating to 500 ℃ at the heating rate of 3 ℃/min, and keeping the temperature for 2 h; Heating up to 1250 ℃ at the heating rate of 2 ℃/min and preserving the heat for 4h to prepare the microwave dielectric ceramic.
Examples 2 to 3
16.592g (MgCO) is weighed according to the formula proportion3)4·Mg(OH)2·5H2O，0.477g CuO，6g SiO2And 10g of CaCO3,.7.99g TiO2Respectively putting the mixed powder into a polyurethane ball milling tank, adding 180g of deionized water, 180g of zirconia balls, 140g of deionized water and 140g of zirconia balls, and carrying out ball milling on a planetary ball mill for 12 hours at the rotating speed of 400 r/min; putting the ball-milled raw materials into a drying oven, drying at 100 ℃, and then crushing and sieving by a 100-mesh sieve; placing the sieved powder into a sintering furnace, and adding Mg2-0.03Cu0.03SiO4And CaTiO3Heating to 1300 ℃ according to the heating rate of 5 ℃/min for presintering, and keeping the temperature for 2 h; weighing 12g of Mg2-0.03Cu0.03SiO4And 8g of CaTiO3Putting the mixture into a polyurethane ball milling tank, adding 160g of deionized water and 160g of zirconia balls, and ball milling the mixture for 6 hours on a planetary ball mill at the rotating speed of 400 r/min; putting the ball-milled powder into a drying oven to be dried at 100 ℃, and then crushing and sieving the powder by a 200-mesh sieve; putting the sieved powder into a mortar, adding a PVA solution with the mass of 8 wt% and the concentration of 5 wt% of the powder, grinding and granulating, and pressing into a green body with the diameter of 16mm and the height of 8mm by using a tablet press under the pressure of 4 MPa; putting the pressed and molded blank into a sintering furnace, heating to 200 ℃ at the heating rate of 3 ℃/min, and keeping the temperature for 1h, and heating to 500 ℃ at the heating rate of 3 ℃/min, and keeping the temperature for 2 h; heating up to 1250 ℃ at the heating rate of 2 ℃/min and preserving heat for 4h to prepare the microwave dielectric ceramic.
Example 3-1
16.592g (MgCO) is weighed according to the formula proportion3)4·Mg(OH)2·5H2O，0.150g CoO，6g SiO2And 10g of CaCO3,.7.99g TiO2Respectively putting the mixed powder into a polyurethane ball milling tank, adding 180g of deionized water, 180g of zirconia balls, 140g of deionized water and 140g of zirconia balls, and carrying out ball milling on a planetary ball mill for 12 hours at the rotating speed of 400 r/min; putting the ball-milled raw materials into a drying oven, drying at 100 ℃, and then crushing and sieving by a 100-mesh sieve; discharging the sieved powderPutting into a sintering furnace, and Mg2-0.01Co0.01SiO4And CaTiO3Heating to 1300 ℃ according to the heating rate of 5 ℃/min for presintering, and keeping the temperature for 2 h; weighing 12g of Mg2-0.01Co0.01SiO4And 8g of CaTiO3Putting the mixture into a polyurethane ball milling tank, adding 160g of deionized water and 160g of zirconia balls, and ball milling the mixture for 6 hours on a planetary ball mill at the rotating speed of 400 r/min; putting the ball-milled powder into a drying oven to be dried at 100 ℃, and then crushing and sieving the powder by a 200-mesh sieve; putting the sieved powder into a mortar, adding a PVA solution with the mass of 8 wt% and the concentration of 5 wt% of the powder, grinding and granulating, and pressing into a green body with the diameter of 16mm and the height of 8mm by using a tablet press under the pressure of 4 MPa; putting the pressed and molded blank into a sintering furnace, heating to 200 ℃ at the heating rate of 3 ℃/min, and keeping the temperature for 1h, and heating to 500 ℃ at the heating rate of 3 ℃/min, and keeping the temperature for 2 h; heating up to 1250 ℃ at the heating rate of 2 ℃/min and preserving heat for 4h to prepare the microwave dielectric ceramic.
Example 3-2
16.592g (MgCO) is weighed according to the formula proportion3)4·Mg(OH)2·5H2O，0.300g CoO，6g SiO2And 10g of CaCO3,.7.99g TiO2Respectively putting the mixed powder into a polyurethane ball milling tank, adding 180g of deionized water, 180g of zirconia balls, 140g of deionized water and 140g of zirconia balls, and carrying out ball milling on a planetary ball mill for 12 hours at the rotating speed of 400 r/min; putting the ball-milled raw materials into a drying oven, drying at 100 ℃, and then crushing and sieving by a 100-mesh sieve; placing the sieved powder into a sintering furnace, and adding Mg2-0.02Co0.02SiO4And CaTiO3Heating to 1300 ℃ according to the heating rate of 5 ℃/min for presintering, and keeping the temperature for 2 h; weighing 12g of Mg2-0.02Co0.02SiO4And 8g of CaTiO3Putting the mixture into a polyurethane ball milling tank, adding 160g of deionized water and 160g of zirconia balls, and ball milling the mixture for 6 hours on a planetary ball mill at the rotating speed of 400 r/min; putting the ball-milled powder into a drying oven to be dried at 100 ℃, and then crushing and sieving the powder by a 200-mesh sieve; placing the sieved powder into a mortar, adding a 5 wt% PVA solution with the mass of 8 wt% of the powder, grinding and granulating, and pressing with a tablet press under the pressure of 4MPa to obtain the powder with the diameter of 16mm and the height of 8mm green bodies; putting the pressed and molded blank into a sintering furnace, heating to 200 ℃ at the heating rate of 3 ℃/min, and keeping the temperature for 1h, and heating to 500 ℃ at the heating rate of 3 ℃/min, and keeping the temperature for 2 h; heating up to 1250 ℃ at the heating rate of 2 ℃/min and preserving heat for 4h to prepare the microwave dielectric ceramic.
Examples 3 to 3
16.592g (MgCO) is weighed according to the formula proportion3)4·Mg(OH)2·5H2O，0.450g CoO，6g SiO2And 10g of CaCO3,.7.99g TiO2Respectively putting the mixed powder into a polyurethane ball milling tank, adding 180g of deionized water, 180g of zirconia balls, 140g of deionized water and 140g of zirconia balls, and carrying out ball milling on a planetary ball mill for 12 hours at the rotating speed of 400 r/min; the ball-milled raw materials are put into a drying oven to be dried at 100 ℃, and then are crushed and sieved by a 100-mesh sieve; placing the sieved powder into a sintering furnace, and adding Mg2-0.03Co0.03SiO4And CaTiO3Heating to 1300 ℃ according to the heating rate of 5 ℃/min for presintering, and keeping the temperature for 2 h; weighing 12g of Mg2-0.03Co0.03SiO4And 8g of CaTiO3Putting the mixture into a polyurethane ball milling tank, adding 160g of deionized water and 160g of zirconia balls, and ball milling the mixture for 6 hours on a planetary ball mill at the rotating speed of 400 r/min; putting the ball-milled powder into a drying oven to be dried at 100 ℃, and then crushing and sieving the powder by a 200-mesh sieve; putting the sieved powder into a mortar, adding a PVA solution with the mass of 8 wt% and the concentration of 5 wt% of the powder, grinding and granulating, and pressing into a green body with the diameter of 16mm and the height of 8mm by using a tablet press under the pressure of 4 MPa; putting the pressed and molded blank into a sintering furnace, heating to 200 ℃ at the heating rate of 3 ℃/min, and keeping the temperature for 1h, and heating to 500 ℃ at the heating rate of 3 ℃/min, and keeping the temperature for 2 h; heating up to 1250 ℃ at the heating rate of 2 ℃/min and preserving heat for 4h to prepare the microwave dielectric ceramic.
Example 4-1
16.592g (MgCO) is weighed according to the formula proportion3)4·Mg(OH)2·5H2O，0.149g NiO，6g SiO2And 10g of CaCO3,.7.99g TiO2The mixed powder is respectively put into a polyurethane ball milling tank, and 180g of deionized water, 180g of zirconia balls, 140g of deionized water and 140g of zirconia balls are added into the polyurethane ball milling tankBall-milling for 12 hours on a planetary ball mill at the rotating speed of 400 r/min; putting the ball-milled raw materials into a drying oven, drying at 100 ℃, and then crushing and sieving by a 100-mesh sieve; placing the sieved powder into a sintering furnace, and adding Mg2-0.01Ni0.01SiO4And CaTiO3Heating to 1300 ℃ according to the heating rate of 5 ℃/min for presintering, and keeping the temperature for 2 h; weighing 12g of Mg2-0.01Ni0.01SiO4And 8g of CaTiO3Putting the mixture into a polyurethane ball milling tank, adding 160g of deionized water and 160g of zirconia balls, and ball milling the mixture for 6 hours on a planetary ball mill at the rotating speed of 400 r/min; putting the ball-milled powder into a drying oven to be dried at 100 ℃, and then crushing and sieving the powder by a 200-mesh sieve; putting the sieved powder into a mortar, adding a PVA solution with the mass of 8 wt% and the concentration of 5 wt% of the powder, grinding and granulating, and pressing into a green body with the diameter of 16mm and the height of 8mm by using a tablet press under the pressure of 4 MPa; putting the pressed and molded blank into a sintering furnace, heating to 200 ℃ at the heating rate of 3 ℃/min, and keeping the temperature for 1h, and heating to 500 ℃ at the heating rate of 3 ℃/min, and keeping the temperature for 2 h; heating up to 1250 ℃ at the heating rate of 2 ℃/min and preserving heat for 4h to prepare the microwave dielectric ceramic.
Example 4-2
16.592g (MgCO) is weighed according to the formula proportion3)4·Mg(OH)2·5H2O，0.299g NiO，6g SiO2And 10g of CaCO3,.7.99g TiO2Respectively putting the mixed powder into a polyurethane ball milling tank, adding 180g of deionized water, 180g of zirconia balls, 140g of deionized water and 140g of zirconia balls, and carrying out ball milling on a planetary ball mill for 12 hours at the rotating speed of 400 r/min; putting the ball-milled raw materials into a drying oven, drying at 100 ℃, and then crushing and sieving by a 100-mesh sieve; placing the sieved powder into a sintering furnace, and adding Mg2-0.02Ni0.02SiO4And CaTiO3Heating to 1300 ℃ according to the heating rate of 5 ℃/min for presintering, and keeping the temperature for 2 h; weighing 12g of Mg2-0.02Ni0.02SiO4And 8g of CaTiO3Putting the mixture into a polyurethane ball milling tank, adding 160g of deionized water and 160g of zirconia balls, and ball milling the mixture for 6 hours on a planetary ball mill at the rotating speed of 400 r/min; putting the ball-milled powder into a drying oven to be dried at 100 ℃, and then crushing and sieving the powder by a 200-mesh sieve; the sieved powder is put into a grinderAdding a PVA solution with the powder mass of 8 wt% and the concentration of 5 wt% into a pot, grinding and granulating, and pressing into a green body with the diameter of 16mm and the height of 8mm by using a tablet press under the pressure of 4 MPa; putting the pressed and molded blank into a sintering furnace, heating to 200 ℃ at the heating rate of 3 ℃/min, and keeping the temperature for 1h, and heating to 500 ℃ at the heating rate of 3 ℃/min, and keeping the temperature for 2 h; heating up to 1250 ℃ at the heating rate of 2 ℃/min and preserving heat for 4h to prepare the microwave dielectric ceramic.
Examples 4 to 3
16.592g (MgCO) is weighed according to the formula proportion3)4·Mg(OH)2·5H2O，0.448g NiO，6g SiO2And 10g of CaCO3,.7.99g TiO2Respectively putting the mixed powder into a polyurethane ball milling tank, adding 180g of deionized water, 180g of zirconia balls, 140g of deionized water and 140g of zirconia balls, and carrying out ball milling on a planetary ball mill for 12 hours at the rotating speed of 400 r/min; the ball-milled raw materials are put into a drying oven to be dried at 100 ℃, and then are crushed and sieved by a 100-mesh sieve; placing the sieved powder into a sintering furnace, and adding Mg2-0.03Ni0.03SiO4And CaTiO3Heating to 1300 ℃ according to the heating rate of 5 ℃/min for presintering, and keeping the temperature for 2 h; weighing 12g of Mg2-0.03Ni0.03SiO4And 8g of CaTiO3Putting the mixture into a polyurethane ball milling tank, adding 160g of deionized water and 160g of zirconia balls, and ball milling the mixture for 6 hours on a planetary ball mill at the rotating speed of 400 r/min; putting the ball-milled powder into a drying oven to be dried at 100 ℃, and then crushing and sieving the powder by a 200-mesh sieve; putting the sieved powder into a mortar, adding a PVA solution with the mass of 8 wt% and the concentration of 5 wt% of the powder, grinding and granulating, and pressing into a green body with the diameter of 16mm and the height of 8mm by using a tablet press under the pressure of 4 MPa; putting the pressed and molded blank into a sintering furnace, heating to 200 ℃ at the heating rate of 3 ℃/min, and keeping the temperature for 1h, and heating to 500 ℃ at the heating rate of 3 ℃/min, and keeping the temperature for 2 h; heating up to 1250 ℃ at the heating rate of 2 ℃/min and preserving heat for 4h to prepare the microwave dielectric ceramic.
The detection results of various key parameters and dielectric properties of the embodiment of the invention are detailed in table 1.
Table 1 detection results of key parameters and dielectric properties of products in examples
The test result shows that the dielectric constant after doping is improved to 13.13-14.84 from epsilon r ≈ 9.4, the quality factor is improved to 46300-55900 from Q multiplied by f ≈ 19000GHz, and the temperature coefficient is close to zero. The dielectric constant and the quality factor after Zn doping are the highest, wherein epsilon r is 14.43-14.84, Q multiplied by f is 55000-55900 GHz, and the best Zn doping effect is shown. In addition, as the doping amount is increased, the dielectric constant and the quality factor are both increased and then decreased, which shows that the dielectric property is better when the doping amount is 0.02.
Claims (5)
1.Mg2-xMxSiO4-CaTiO3The preparation method of the composite microwave dielectric ceramic is characterized by comprising the following steps:
(1) will (MgCO)3)4·Mg(OH)2·5H2O、ZnO、CuO、CoO、NiO、TiO2And CaCO3Weighing according to a chemical ratio, putting deionized water and zirconia balls as a solvent and a ball milling medium into a polyurethane ball milling tank to perform ball milling for 8-24 hours on a planetary ball mill;
(2) putting the ball-milled raw materials in the step (1) into a drying oven, drying at 100 ℃, and then crushing and sieving with a 100-mesh sieve;
(3) putting the powder sieved in the step (2) into an alumina crucible, putting the alumina crucible into a sintering furnace, heating the alumina crucible to 1300 ℃ at the heating rate of 5 ℃ per minute, and preserving the heat at the temperature of 1300 ℃ for 2 hours to respectively obtain Mg 2-xMxSiO4And CaTiO3(ii) a Wherein: x is more than or equal to 0.01 and less than or equal to 0.03, M = Zn, Cu, Co, Ni, CaTiO3The mass fraction of (A) is 10-50%;
(4) mixing Mg2-xMxSiO4And CaTiO3Weighing the components according to the ratio of mass fraction, taking deionized water and zirconia balls as a solvent and a ball milling medium, and putting the solvent and the zirconia balls into a polyurethane ball milling tank to perform ball milling for 4 to 8 hours on a planetary ball mill;
(5) putting the powder subjected to ball milling in the step (4) into a drying oven, drying at 100 ℃, and then crushing and sieving with a 200-mesh sieve;
(6) putting the powder sieved in the step (5) into a mortar, adding 8wt% of PVA solution with the concentration of 5wt% of the powder, grinding and granulating, and then pressing and forming by using a tablet press;
(7) putting the green body formed by pressing in the step (6) into a sintering furnace, sintering at the temperature of 1225-1275 ℃, and preserving heat for 4 hours to obtain microwave dielectric ceramic; the sintering system is that the temperature is raised to 200 ℃ at the speed of 3 ℃/min and is preserved for 1h, and the temperature is raised to 500 ℃ at the speed of 3 ℃/min and is preserved for 2 h; heating to the target temperature at the speed of 2 ℃/min and preserving heat for 4 h;
(8) and (4) carrying out dielectric property test on the microwave dielectric ceramic prepared in the step (7).
2. Mg of claim 12-xMxSiO4-CaTiO3The preparation method of the composite microwave dielectric ceramic is characterized in that in the ball milling in the steps (1) and (4), the following materials are used: water: the mass ratio of the balls is 1:8:8, and the rotating speed is 400 r/min.
3. Mg of claim 12-xMxSiO4-CaTiO3The preparation method of the composite microwave dielectric ceramic is characterized in that the forming pressure in the step (6) is 4MPa, the diameter of a green body is 16mm, and the height is 8 mm.
4. Mg of claim 12-xMxSiO4-CaTiO3The preparation method of the composite microwave dielectric ceramic is characterized in that the time of the step (1) is 12 hours, the time of the step (4) is 6 hours, and the sintering temperature of the step (7) is 1250 ℃.
5.Mg2-xMxSiO4-CaTiO3Composite microwave dielectric ceramic, characterized in that it is obtained by the method of preparation according to any one of claims 1 to 4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010936202.2A CN111995383B (en) | 2020-09-08 | 2020-09-08 | Mg2-xMxSiO4-CaTiO3Composite microwave dielectric ceramic and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010936202.2A CN111995383B (en) | 2020-09-08 | 2020-09-08 | Mg2-xMxSiO4-CaTiO3Composite microwave dielectric ceramic and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111995383A CN111995383A (en) | 2020-11-27 |
| CN111995383B true CN111995383B (en) | 2022-05-24 |
Family
ID=73469666
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010936202.2A Active CN111995383B (en) | 2020-09-08 | 2020-09-08 | Mg2-xMxSiO4-CaTiO3Composite microwave dielectric ceramic and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111995383B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112830775B (en) * | 2021-03-01 | 2023-06-23 | 南宁国人射频通信有限公司 | Low-dielectric-constant microwave dielectric ceramic and preparation method thereof |
| CN112919894B (en) | 2021-03-10 | 2022-02-22 | 嘉兴佳利电子有限公司 | Frequency-stable low-dielectric microwave dielectric ceramic material and preparation method thereof |
| CN113087507A (en) * | 2021-03-10 | 2021-07-09 | 无锡市高宇晟新材料科技有限公司 | Low-dielectric magnesium silicate microwave dielectric ceramic material and preparation method thereof |
| CN113563061B (en) * | 2021-09-26 | 2021-12-21 | 广东康荣高科新材料股份有限公司 | Low dielectric constant dielectric material for single-cavity filter and preparation method thereof |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000294447A (en) * | 1999-04-09 | 2000-10-20 | Unitika Ltd | High-permittivity film for film capacitor and manufacture thereof |
| KR20050058611A (en) * | 2003-12-12 | 2005-06-17 | 한국전자통신연구원 | Dielectric ceramic composition of forsterite system for microwave and millimeter-wave application and method for forming the same |
| CN1826299A (en) * | 2004-03-01 | 2006-08-30 | 株式会社村田制作所 | Insulating ceramic composition, insulating ceramic sintered body, and multilayer ceramic electronic component |
| CN1921038A (en) * | 2005-11-18 | 2007-02-28 | 广东风华高新科技股份有限公司 | Non-magnetism high-voltage sheet type multilayer ceramic capacitor and its producing method |
| CN101397206A (en) * | 2007-09-28 | 2009-04-01 | Tdk株式会社 | Dielectric ceramic composition |
| CN103641469A (en) * | 2013-12-02 | 2014-03-19 | 电子科技大学 | Low-loss microwave dielectric ceramic material and preparation method thereof |
| CN109133912A (en) * | 2017-06-27 | 2019-01-04 | 深圳光启高等理工研究院 | A kind of microwave-medium ceramics and preparation method thereof |
| CN113087507A (en) * | 2021-03-10 | 2021-07-09 | 无锡市高宇晟新材料科技有限公司 | Low-dielectric magnesium silicate microwave dielectric ceramic material and preparation method thereof |
| CN113354399A (en) * | 2021-07-13 | 2021-09-07 | 宜宾红星电子有限公司 | Low-temperature co-fired composite ceramic material and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103864406B (en) * | 2014-02-12 | 2015-07-29 | 同济大学 | A kind of dielectric constant microwave ceramic medium and preparation method thereof |
-
2020
- 2020-09-08 CN CN202010936202.2A patent/CN111995383B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000294447A (en) * | 1999-04-09 | 2000-10-20 | Unitika Ltd | High-permittivity film for film capacitor and manufacture thereof |
| KR20050058611A (en) * | 2003-12-12 | 2005-06-17 | 한국전자통신연구원 | Dielectric ceramic composition of forsterite system for microwave and millimeter-wave application and method for forming the same |
| CN1826299A (en) * | 2004-03-01 | 2006-08-30 | 株式会社村田制作所 | Insulating ceramic composition, insulating ceramic sintered body, and multilayer ceramic electronic component |
| CN1921038A (en) * | 2005-11-18 | 2007-02-28 | 广东风华高新科技股份有限公司 | Non-magnetism high-voltage sheet type multilayer ceramic capacitor and its producing method |
| CN101397206A (en) * | 2007-09-28 | 2009-04-01 | Tdk株式会社 | Dielectric ceramic composition |
| CN103641469A (en) * | 2013-12-02 | 2014-03-19 | 电子科技大学 | Low-loss microwave dielectric ceramic material and preparation method thereof |
| CN109133912A (en) * | 2017-06-27 | 2019-01-04 | 深圳光启高等理工研究院 | A kind of microwave-medium ceramics and preparation method thereof |
| CN113087507A (en) * | 2021-03-10 | 2021-07-09 | 无锡市高宇晟新材料科技有限公司 | Low-dielectric magnesium silicate microwave dielectric ceramic material and preparation method thereof |
| CN113354399A (en) * | 2021-07-13 | 2021-09-07 | 宜宾红星电子有限公司 | Low-temperature co-fired composite ceramic material and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111995383A (en) | 2020-11-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111995383B (en) | Mg2-xMxSiO4-CaTiO3Composite microwave dielectric ceramic and preparation method thereof | |
| CN106587987B (en) | The preparation method of C0G microwave dielectric material and preparation method and ceramic material | |
| CN108358632B (en) | Ultralow-temperature sintered high-Q x f-value microwave dielectric material and preparation method thereof | |
| CN111763083B (en) | Low-temperature sintered ultralow-loss microwave dielectric ceramic and preparation method and application thereof | |
| CN107117967B (en) | Low-temperature sintered composite microwave dielectric ceramic material and preparation method thereof | |
| CN110282968A (en) | A kind of microwave dielectric ceramic materials and preparation method thereof | |
| CN105254293A (en) | Microwave dielectric ceramic material and preparation method thereof | |
| CN113087507A (en) | Low-dielectric magnesium silicate microwave dielectric ceramic material and preparation method thereof | |
| CN108147809B (en) | Medium-low temperature sintered barium-titanium series microwave dielectric material and preparation method thereof | |
| CN111004030B (en) | MgTiO (magnesium-titanium-oxide) powder3Microwave-based dielectric ceramic and preparation method thereof | |
| CN102850048A (en) | Niobium magnesium bismuth titanate ceramic material and preparation method thereof | |
| CN114031402B (en) | Low-temperature sintered microwave dielectric material MgZrNb 2 O 8 And method for preparing the same | |
| CN113896530A (en) | Modified NiO-Ta with stable temperature2O5Microwave-based dielectric ceramic material and preparation method thereof | |
| CN101811869A (en) | Low-temperature sintering microwave medium ceramic material and preparation method thereof | |
| CN111320473B (en) | Low-sintering microwave dielectric ceramic material and preparation method thereof | |
| CN107382314A (en) | A kind of microwave-medium ceramics of barium base complex perovskite structure | |
| CN113004026B (en) | LTCC microwave dielectric ceramic material and manufacturing method thereof | |
| CN104692792A (en) | Low-temperature sintering temperature stable stannate microwave dielectric ceramic material | |
| JP7238127B2 (en) | Doped perovskite-type barium stannate material, production method thereof, and use thereof | |
| CN111848154B (en) | Ceramic capacitor medium and preparation method thereof | |
| CN102030527B (en) | BaO-TiO2 microwave capacitor dielectric material and preparation method thereof | |
| CN113072373A (en) | Temperature-stable low-dielectric ceramic material suitable for 5G millimeter wave communication application and preparation method thereof | |
| CN104402430A (en) | Temperature-stable medium K value microwave dielectric ceramic and preparation method thereof | |
| CN111302795A (en) | Lithium-magnesium-niobium-aluminum-tungsten microwave dielectric ceramic and preparation method thereof | |
| CN104961459A (en) | Temperature-stable type magnesium titanate base microwave dielectric ceramic |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |