CN112898010B - Microwave dielectric ceramic material for 5G communication base station and preparation method and application thereof - Google Patents
Microwave dielectric ceramic material for 5G communication base station and preparation method and application thereof Download PDFInfo
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 58
- 238000004891 communication Methods 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000000919 ceramic Substances 0.000 claims abstract description 85
- 239000000843 powder Substances 0.000 claims abstract description 68
- 238000005245 sintering Methods 0.000 claims abstract description 39
- 238000005469 granulation Methods 0.000 claims abstract description 20
- 230000003179 granulation Effects 0.000 claims abstract description 20
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- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 8
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 8
- 229910010413 TiO 2 Inorganic materials 0.000 claims abstract description 8
- 238000013001 point bending Methods 0.000 claims abstract description 7
- 239000002002 slurry Substances 0.000 claims description 30
- 238000010438 heat treatment Methods 0.000 claims description 18
- 239000002202 Polyethylene glycol Substances 0.000 claims description 15
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 15
- 239000002270 dispersing agent Substances 0.000 claims description 15
- 229920001223 polyethylene glycol Polymers 0.000 claims description 15
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- 238000000498 ball milling Methods 0.000 claims description 14
- 238000003825 pressing Methods 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
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- 238000002156 mixing Methods 0.000 claims description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-O ammonium group Chemical group [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 8
- 229920000058 polyacrylate Polymers 0.000 claims description 8
- 238000000465 moulding Methods 0.000 claims description 7
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- 229910052709 silver Inorganic materials 0.000 abstract description 15
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- 239000000203 mixture Substances 0.000 abstract description 7
- 238000003754 machining Methods 0.000 abstract description 3
- 238000007599 discharging Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 19
- 239000011230 binding agent Substances 0.000 description 18
- 238000012360 testing method Methods 0.000 description 17
- 239000002994 raw material Substances 0.000 description 13
- 238000000034 method Methods 0.000 description 8
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- 238000004154 testing of material Methods 0.000 description 6
- 239000003153 chemical reaction reagent Substances 0.000 description 5
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- 230000000052 comparative effect Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000011777 magnesium Substances 0.000 description 3
- 239000012776 electronic material Substances 0.000 description 2
- 229910052573 porcelain Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
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- 239000011521 glass Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 1
- 229910052919 magnesium silicate Inorganic materials 0.000 description 1
- 235000019792 magnesium silicate Nutrition 0.000 description 1
- 239000000391 magnesium silicate Substances 0.000 description 1
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- 239000008204 material by function Substances 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
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- 238000011056 performance test Methods 0.000 description 1
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- 229910052761 rare earth metal Inorganic materials 0.000 description 1
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- 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
- C04B35/44—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 aluminates
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Abstract
The invention discloses a microwave dielectric ceramic material for a 5G communication base station, a preparation method and application thereof, wherein the microwave dielectric ceramic material comprises the following chemical compositions: (1-y) (Ca) 1+x Sb 1‑x )(Al 1‑x Ti x )O 4 +yMg 2 SiO 4 Wherein x is more than or equal to 0 and less than or equal to 0.4, and y is more than 0 and less than or equal to 0.3; and with CaCO 3 、Sb 2 O 3 、Al 2 O 3 、TiO 2 、MgO、SiO 2 Grinding, pre-sintering to prepare powder, re-dispersing and grinding, preparing the powder and an adhesive into microwave dielectric ceramic granulation powder, preparing a green body, discharging glue, and sintering to prepare the ceramic material; and the application of the microwave dielectric ceramic material in the preparation of microwave devices; the microwave dielectric ceramic has high three-point bending strength and excellent machining characteristics; the matching with a metal silver electrode is good, and the metallization is easy; and has dielectric tunable characteristics, high Q x f, and excellent temperature coefficient of resonance frequency τ f.
Description
Technical Field
The invention belongs to the technical field of electronic information functional materials and devices, and particularly relates to a microwave dielectric ceramic material for a 5G communication base station, which has the characteristics of adjustable dielectric constant, low dielectric loss, small temperature coefficient of resonant frequency and the like, and a preparation method and application thereof, and can be used for manufacturing microwave devices such as dielectric resonators, filters and the like and applied to the communication field.
Background
With the rapid development of modern communication technology, especially the rapid advance of 5G networks, miniaturization, integration and low cost become the development direction of mobile communication and mobile terminals, the traditional metal resonant cavity and metal waveguide have too large volume and weight, which limits the development of microwave integrated circuits, and therefore, a series of electronic materials and components with high performance and high reliable operating characteristics suitable for the microwave range need to be developed. The microwave dielectric ceramic is a novel electronic material, has the characteristics of adjustable dielectric constant, low dielectric loss, small temperature coefficient of resonant frequency and the like, is very suitable for the requirements of 5G communication base stations on the material, and is widely concerned by people.
The frequency band of 5G communication deployment mainly comprises Sub-6GHz and high-frequency millimeter waves, wherein Sub-6GHz utilizes bandwidth resources below 6GHz to develop 5G, the initial construction of domestic 5G has confirmed to use the frequency band, and a microwave dielectric ceramic material with a dielectric constant of about 20 is the best choice for a 5G base station dielectric filter applied to the frequency band. In addition, in order to meet the requirements of people on ultrahigh flow density, ultrahigh mobility and ultrahigh connection number density, the 5G base station dielectric filter needs microwave dielectric ceramics with a high quality factor Qxf value and a near-zero resonant frequency temperature coefficient. A higher Q x f value represents lower loss, so that the signal has a small absorption effect and a good frequency selection characteristic. The temperature coefficient tau f of the resonance frequency is close to zero, and the aim is to meet the temperature stability requirement of the device during working.
At present, microwave ceramic materials with dielectric constants of 20 +/-1 are generally used in the market by two systems, one is Mg 0.95 TiO 3 -Ca 0.05 TiO 3 The system has the advantages of high bonding strength with a metal silver electrode and low sintering density, but after the system material is made into porcelain, the machinability of the product is poor due to excessive glass phase content and three-point bending strength of about 50MPa, and the phenomena of breakage and edge breakage are easy to occur when the porcelain body is polished or drilled, so that the qualification rate of the product is extremely low; the other is (Ca) 1+x Sm 1-x )(Al 1-x Ti x )O 4 The microwave dielectric ceramic has excellent microwave dielectric property, but the system is poor in matching with a metallic silver electrode, the problem of metallization silver plating is difficult to solve, the bonding strength of a product and the silver electrode is low, and the phenomena of peeling and stripping are easy to occur, so that the product cannot be normally used.
Disclosure of Invention
The invention aims to overcome one or more defects in the prior art and provides a novel microwave dielectric ceramic material (1-y) (Ca) for a 5G communication base station 1+x Sb 1-x )(Al 1-x Ti x )O 4 +yMg 2 SiO 4 (x is more than or equal to 0 and less than or equal to 0.4, y is more than 0 and less than or equal to 0.3), the material system has high three-point bending strengthThe processing characteristics are excellent; the matching with a metal silver electrode is good, and the metallization is easy; and has dielectric tunable characteristics, a high Q x f value, an excellent temperature coefficient of resonance frequency τ f, and the like.
The invention also provides a preparation method of the microwave dielectric ceramic material for the 5G communication base station.
The invention also provides application of the microwave dielectric ceramic material for the 5G communication base station in preparation of microwave devices.
In order to achieve the purpose, the invention adopts a technical scheme that:
a microwave dielectric ceramic material for a 5G communication base station comprises the following chemical components: (1-y) (Ca) 1+x Sb 1-x )(Al 1-x Ti x )O 4 +y Mg 2 SiO 4 Wherein x is more than or equal to 0 and less than or equal to 0.4, and y is more than 0 and less than or equal to 0.3.
According to some preferred aspects of the invention, y is 0.01 or greater and 0.25 or less. In some embodiments of the invention y is 0.01, 0.02, 0.03, 0.05, 0.06, 0.09, 0.10, 0.12, 0.13, 0.14, 0.16, 0.18, 0.20, 0.21, 0.22, 0.23, 0.24, or 0.25, and the like.
According to some preferred aspects of the invention, x is 0.05 or greater and 0.30 or less. In some embodiments of the invention, x is 0.05, 0.06, 0.07, 0.08, 0.09, 0.10, 0.13, 0.15, 0.16, 0.17, 0.18, 0.19, 0.20, 0.21, 0.22, 0.23, 0.25, 0.26, 0.28, 0.30, or the like.
According to the microwave dielectric ceramic material, the three-point bending strength can be more than or equal to 150 MPa.
The invention provides another technical scheme that: a preparation method of the microwave dielectric ceramic material for the 5G communication base station comprises the following steps:
(1) with CaCO 3 、Sb 2 O 3 、Al 2 O 3 、TiO 2 、MgO、SiO 2 As a raw material according to (1-y) (Ca) 1+x Sb 1-x )(Al 1-x Ti x )O 4 +y Mg 2 SiO 4 Of (2) aPreparing materials according to the general formula, and mixing and ball-milling to obtain ball-milled slurry; wherein x is more than or equal to 0 and less than or equal to 0.4, and y is more than 0 and less than or equal to 0.3;
(2) drying and pre-burning the ball-milling slurry obtained in the step (1) to prepare microwave dielectric ceramic pre-burning powder;
(3) adding water and a dispersing agent into the microwave dielectric ceramic pre-sintering powder obtained in the step (2), carrying out ball milling, then adding an adhesive into the slurry, uniformly mixing, and carrying out spray granulation to prepare microwave dielectric ceramic granulation powder;
(4) dry-pressing and molding the granulated powder obtained in the step (3) to obtain a microwave medium ceramic green body;
(5) and (4) carrying out glue discharging treatment on the microwave dielectric ceramic green body obtained in the step (4), then heating and sintering.
According to some preferred aspects of the invention, in step (1), the average particle size of the powder particles in the ball milling slurry is 0.5 to 1.6 μm.
According to some preferred aspects of the present invention, in the step (2), the pre-sintering temperature is 1150-1200 ℃, and the pre-sintering time is 2-6 h.
According to some preferred aspects of the invention, in the step (3), the mass ratio of the addition amount of the water to the addition amount of the microwave dielectric ceramic pre-sintered powder is 0.8-1.2: 1.
According to some preferred aspects of the invention, in the step (3), the dispersant is ammonium polyacrylate, and the addition amount of the ammonium polyacrylate accounts for 0.8-1.5% of the addition amount of the microwave dielectric ceramic pre-sintering powder.
According to some preferred aspects of the invention, in step (3), D of the particles in the milled slurry 50 Is 0.5-1.2 μm.
According to some preferred aspects of the present invention, in the step (3), the binder comprises polyvinyl alcohol and polyethylene glycol, and the feeding mass ratio of the polyvinyl alcohol to the polyethylene glycol is 3-5: 1. In some embodiments of the invention, the addition may be in the form of an aqueous solution of both polyvinyl alcohol, polyethylene glycol.
According to some preferred aspects of the invention, in the step (3), the microwave dielectric ceramic pre-sintered powder accounts for 95 to 99.7 percent and the binder accounts for 0.3 to 5 percent based on 100 percent of the total amount of the microwave dielectric ceramic pre-sintered powder and the binder.
According to some preferred aspects of the present invention, in the step (3), the temperature of the inlet of the spray drying tower is 190 ℃ to 240 ℃, the temperature of the outlet is 90 to 120 ℃, and the obtained microwave dielectric ceramic granulated powder has an average particle size of 50 to 90 μm and a bulk density of 1.1 to 1.5g/cm 3 。
According to some preferred aspects of the present invention, in the step (4), the pressure of the dry-pressing is 100-200 MPa.
According to some preferred aspects of the invention, in the step (5), the microwave dielectric ceramic green body obtained in the step (4) is subjected to heat preservation at 600-700 ℃ for 1-3 hours for glue removal treatment.
According to some preferred aspects of the present invention, in the step (5), the sintering temperature is 1350-. Further, the heating rate is 100-; further, the temperature rise rate is 120-.
The invention provides another technical scheme that: the application of the microwave dielectric ceramic material for the 5G communication base station in the preparation of microwave devices.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:
based on the problems that the microwave dielectric ceramic material in the prior art is difficult to give consideration to better machining performance, the matching property of the metal silver electrode and the like, the invention innovatively provides a novel microwave dielectric ceramic material (1-y) (Ca) for a 5G communication base station 1+x Sb 1-x )(Al 1-x Ti x )O 4 +yMg 2 SiO 4 (wherein x is more than or equal to 0 and less than or equal to 0.4, and y is more than 0 and less than or equal to 0.3), the material is prepared by mixing magnesium silicate and (Ca) 1+x Sb 1-x )(Al 1-x Ti x )O 4 The interaction of the components not only realizes excellent three-point bending strength (more than or equal to 150MPa) of a material system, so that the machining performance is good, and the phenomena of edge breakage and ceramic shortage can not occur when the sintered microwave dielectric ceramic is processed; meanwhile, the material is easy to generate an intermediate transition layer after silver is burnt with a metal silver electrode, so that the microwave mediumThe ceramic and silver electrode has high bonding strength and is easy to metalize.
In addition, the microwave dielectric ceramic material (1-y) (Ca) for the 5G communication base station of the invention 1+x Sb 1-x )(Al 1-x Ti x )O 4 +yMg 2 SiO 4 (x is more than or equal to 0 and less than or equal to 0.4, y is more than 0 and less than or equal to 0.3), the dielectric constant and the temperature coefficient of the resonant frequency can be continuously adjusted in a wider range along with the chemical component ratio, the structure and the performance can be adjusted according to the requirements of a designed device, meanwhile, the microwave dielectric ceramic material does not contain rare earth elements, the raw material price is low, and the process route is simple and easy to implement.
Detailed Description
The above scheme is further explained by combining with specific embodiments; it is to be understood that these embodiments are provided to illustrate the general principles, essential features and advantages of the present invention, and the present invention is not limited in scope by the following embodiments; the implementation conditions used in the examples can be further adjusted according to specific requirements, and the implementation conditions not noted are generally those in routine experiments.
Not specifically illustrated in the following examples, all starting materials are commercially available or prepared by methods conventional in the art.
Example 1
The embodiment provides a microwave dielectric ceramic material for a 5G communication base station and a preparation method thereof. The chemical composition of the microwave dielectric ceramic material for the 5G communication base station is 0.95 (Ca) 1.1 Sb 0.9 )(Al 0.9 Ti 0.1 )O 4 +0.05Mg 2 SiO 4 。
The preparation method comprises the following steps:
(1) using analytically pure chemical reagents CaCO 3 、Sb 2 O 3 、Al 2 O 3 、TiO 2 、MgO、SiO 2 As raw material, 0.95 (Ca) 1.1 Sb 0.9 )(Al 0.9 Ti 0.1 )O 4 +0.05Mg 2 SiO 4 The chemical general formula (2) is prepared according to the molar ratio, and the prepared raw materials are put into a ball mill for ball milling for 16 hours to obtain slurry with the average particle size of about 0.8 mu m;
(2) after the ball-milled slurry is spray-dried, the temperature is raised to 1200 ℃ at the heating rate of 3 ℃/min for presintering for 4 hours to obtain microwave dielectric ceramic presintering powder;
(3) adding water and dispersant into the microwave dielectric ceramic pre-sintering powder, grinding with a sand mill to obtain slurry D 50 Adding adhesive into the slurry, uniformly mixing and stirring for 4 hours, and then carrying out spray granulation to obtain the dielectric adjustable characteristic, high Q x f and resonance frequency temperature coefficient tau with the dielectric adjustable characteristic f Excellent microwave dielectric ceramic granulated powder. Wherein the mass ratio of the added water to the feeding of the microwave dielectric ceramic pre-sintered powder is 1:1, the dispersing agent is ammonium polyacrylate, the adding amount is 1% of the microwave dielectric ceramic pre-sintered powder, the binder is a mixed solution (prepared into an 8% aqueous solution form) of polyethylene glycol and polyvinyl alcohol, the mass ratio of the polyethylene glycol to the polyvinyl alcohol is 1: 4, and the microwave dielectric ceramic pre-sintered powder accounts for 98.5% and the binder accounts for 1.5% of the total amount of the microwave dielectric ceramic pre-sintered powder and the binder. The inlet temperature of a spray drying tower for spray granulation is 220 ℃, the outlet temperature is 100 ℃, the average grain diameter of the obtained microwave medium ceramic granulation powder is 75 +/-10 mu m, and the bulk density is 1.3 +/-0.1 g/cm 3 。
(4) And dry-pressing and molding the granulated powder to obtain the microwave dielectric ceramic green body. Wherein the pressure of dry pressing is 150 MPa.
(5) And (3) preserving the heat of the microwave dielectric ceramic green body at 650 ℃ for 2 hours for glue removal treatment, then heating for sintering, wherein the sintering temperature is 1420 ℃, the heat preservation time is 4 hours, the heating rate is 130 +/-5 ℃/h, preparing the microwave dielectric ceramic material for the 5G communication base station, and finally finishing according to the size requirement of the device.
Testing the bending strength of the microwave dielectric ceramic material by adopting a WDW-50 universal material testing machine; the relative dielectric constant and the quality factor of the material are analyzed by an Agilent 8722ET network analyzer (open cavity method), the resonance frequency temperature coefficient of the material is measured by the Agilent 8722ET network analyzer and a precise constant temperature box, and the test temperature range is-50 ℃ to 125 ℃. The test results are shown in Table 1.
The application comprises the following steps: the processed microwave dielectric ceramic is metallized (silver paste is coated and sintered) by adopting a conventional metallization treatment mode to obtain the metallized microwave dielectric ceramic material for the 5G communication base station.
Example 2
The embodiment provides a microwave dielectric ceramic material for a 5G communication base station and a preparation method thereof. The chemical composition of the microwave dielectric ceramic material for the 5G communication base station is 0.9 (Ca) 1.2 Sb 0.8 )(Al 0.8 Ti 0.2 )O 4 +0.1Mg 2 SiO 4 。
The preparation method comprises the following steps:
(1) using analytically pure chemical reagents CaCO 3 、Sb 2 O 3 、Al 2 O 3 、TiO 2 、MgO、SiO 2 As raw material, 0.9 (Ca) 1.2 Sb 0.8 )(Al 0.8 Ti 0.2 )O 4 +0.1Mg 2 SiO 4 The chemical general formula (2) is prepared according to the molar ratio, and the prepared raw materials are put into a ball mill for ball milling for 16 hours to obtain slurry with the average particle size of about 0.8 mu m;
(2) after the ball-milled slurry is spray-dried, the temperature is raised to 1200 ℃ at the heating rate of 3 ℃/min for presintering for 4 hours to obtain microwave dielectric ceramic presintering powder;
(3) adding water and dispersant into the microwave dielectric ceramic pre-sintering powder, grinding with a sand mill to obtain slurry D 50 Adding adhesive into the slurry, uniformly mixing and stirring for 4 hours, and then carrying out spray granulation to obtain the dielectric adjustable characteristic, high Q x f and high resonant frequency temperature coefficient tau with dielectric adjustable characteristic f Excellent microwave dielectric ceramic granulated powder. Wherein the mass ratio of the added water to the microwave dielectric ceramic pre-sintering powder is 1:1, the dispersant is ammonium polyacrylate, the added amount is 1% of the microwave dielectric ceramic pre-sintering powder, the binder is a mixed solution (prepared into an 8% aqueous solution) of polyethylene glycol and polyvinyl alcohol, the mass ratio of the polyethylene glycol to the polyvinyl alcohol is 1: 4, and the total amount of the microwave dielectric ceramic pre-sintering powder and the binder is 100%The microwave dielectric ceramic pre-sintering powder accounts for 98.5 percent, and the binder accounts for 1.5 percent. The inlet temperature of a spray drying tower for spray granulation is 220 ℃, the outlet temperature is 100 ℃, the average grain diameter of the obtained microwave medium ceramic granulation powder is 75 +/-10 mu m, and the bulk density is 1.3 +/-0.1 g/cm 3 。
(4) And dry-pressing and molding the granulated powder to obtain the microwave dielectric ceramic green body. Wherein the pressure of dry pressing is 150 MPa.
(5) And (3) preserving the heat of the microwave dielectric ceramic green body at 650 ℃ for 2 hours for glue removal treatment, then heating for sintering, wherein the sintering temperature is 1400 ℃, the heat preservation time is 4 hours, the heating rate is 135 +/-5 ℃/h, preparing the microwave dielectric ceramic material for the 5G communication base station, and finally finishing according to the size requirement of the device.
Adopting a WDW-50 universal material testing machine to test the bending strength of the microwave dielectric ceramic material; the relative dielectric constant and the quality factor of the material are analyzed by an Agilent 8722ET network analyzer (open cavity method), the resonance frequency temperature coefficient of the material is measured by the Agilent 8722ET network analyzer and a precise constant temperature box, and the test temperature range is-50 ℃ to 125 ℃. The test results are shown in Table 1.
The application comprises the following steps: the processed microwave dielectric ceramic is metallized (silver paste is coated and sintered) by adopting a conventional metallization treatment mode to obtain the metallized microwave dielectric ceramic material for the 5G communication base station.
Example 3
The embodiment provides a microwave dielectric ceramic material for a 5G communication base station and a preparation method thereof. The chemical composition of the microwave dielectric ceramic material for the 5G communication base station is 0.88 (Ca) 1.3 Sb 0.7 )(Al 0.7 Ti 0.3 )O 4 +0.12Mg 2 SiO 4 。
The preparation method comprises the following steps:
(1) using analytically pure chemical reagents CaCO 3 、Sb 2 O 3 、Al 2 O 3 、TiO 2 、MgO、SiO 2 As raw material, 0.88 (Ca) 1.3 Sb 0.7 )(Al 0.7 Ti 0.3 )O 4 +0.12Mg 2 SiO 4 The chemical general formula (2) is prepared according to the molar ratio, and the prepared raw materials are put into a ball mill for ball milling for 16 hours to obtain slurry with the average particle size of about 0.8 mu m;
(2) after the ball-milled slurry is spray-dried, the temperature is raised to 1200 ℃ at the heating rate of 3 ℃/min for presintering for 4 hours to obtain microwave dielectric ceramic presintering powder;
(3) adding water and dispersant into the microwave dielectric ceramic pre-sintering powder, grinding with a sand mill to obtain slurry D 50 Adding adhesive into the slurry, uniformly mixing and stirring for 4 hours, and then carrying out spray granulation to obtain the dielectric adjustable characteristic, high Q x f and resonance frequency temperature coefficient tau with the dielectric adjustable characteristic f Excellent microwave dielectric ceramic granulated powder. Wherein the mass ratio of the added water to the feeding of the microwave dielectric ceramic pre-sintered powder is 1:1, the dispersing agent is ammonium polyacrylate, the adding amount is 1% of the microwave dielectric ceramic pre-sintered powder, the binder is a mixed solution (prepared into an 8% aqueous solution form) of polyethylene glycol and polyvinyl alcohol, the mass ratio of the polyethylene glycol to the polyvinyl alcohol is 1: 4, and the microwave dielectric ceramic pre-sintered powder accounts for 99.5% and the binder accounts for 0.5% of the total amount of the microwave dielectric ceramic pre-sintered powder and the binder. The inlet temperature of a spray drying tower for spray granulation is 220 ℃, the outlet temperature is 100 ℃, the average grain diameter of the obtained microwave medium ceramic granulation powder is 75 +/-10 mu m, and the bulk density is 1.3 +/-0.1 g/cm 3 。
(4) And dry-pressing and molding the granulated powder to obtain the microwave dielectric ceramic green body. Wherein the pressure of the dry pressing is 200 MPa.
(5) And (3) preserving the heat of the microwave dielectric ceramic green body at 650 ℃ for 2 hours for glue removal treatment, then heating for sintering, wherein the sintering temperature is 1400 ℃, the heat preservation time is 4 hours, the heating rate is 120 +/-5 ℃/h, preparing the microwave dielectric ceramic material for the 5G communication base station, and finally finishing according to the size requirement of the device.
Testing the bending strength of the microwave dielectric ceramic material by adopting a WDW-50 universal material testing machine; the relative dielectric constant and the quality factor of the material are analyzed by an Agilent 8722ET network analyzer (open cavity method), the resonance frequency temperature coefficient of the material is measured by the Agilent 8722ET network analyzer and a precise constant temperature box, and the test temperature range is-50 ℃ to 125 ℃. The test results are shown in Table 1.
The application comprises the following steps: the processed microwave dielectric ceramic is metallized (silver paste is coated and sintered) by adopting a conventional metallization treatment mode to obtain the metallized microwave dielectric ceramic material for the 5G communication base station.
Example 4
The embodiment provides a microwave dielectric ceramic material for a 5G communication base station and a preparation method thereof. The chemical composition of the microwave dielectric ceramic material for the 5G communication base station is 0.85 (Ca) 1.2 Sb 0.8 )(Al 0.8 Ti 0.2 )O 4 +0.15Mg 2 SiO 4 。
The preparation method comprises the following steps:
(1) using analytically pure chemical reagents CaCO 3 、Sb 2 O 3 、Al 2 O 3 、TiO 2 、MgO、SiO 2 As raw material, 0.85 (Ca) 1.2 Sb 0.8 )(Al 0.8 Ti 0.2 )O 4 +0.15Mg 2 SiO 4 The chemical general formula of (1) is a molar ratio, and the prepared raw materials are put into a ball mill for ball milling for 16 hours to obtain slurry with the average particle size of about 1.2 mu m;
(2) after the ball-milled slurry is spray-dried, the temperature is raised to 1200 ℃ at the heating rate of 3 ℃/min for presintering for 4 hours to obtain microwave dielectric ceramic presintering powder;
(3) adding water and dispersant into the microwave dielectric ceramic pre-sintering powder, grinding with a sand mill to obtain slurry D 50 Adding adhesive into the slurry, uniformly mixing and stirring for 4 hours, and then carrying out spray granulation to obtain the dielectric adjustable characteristic, the Q x f high and resonant frequency temperatureCoefficient τ f Excellent microwave dielectric ceramic granulated powder. Wherein the mass ratio of the added water to the feeding of the microwave dielectric ceramic pre-sintered powder is 1:1, the dispersing agent is ammonium polyacrylate, the adding amount is 1% of the microwave dielectric ceramic pre-sintered powder, the binder is a mixed solution (prepared into an 8% aqueous solution form) of polyethylene glycol and polyvinyl alcohol, the mass ratio of the polyethylene glycol to the polyvinyl alcohol is 1: 4, and the microwave dielectric ceramic pre-sintered powder accounts for 98.2% and the binder accounts for 1.8% of the total amount of the microwave dielectric ceramic pre-sintered powder and the binder. The inlet temperature of a spray drying tower for spray granulation is 220 ℃, the outlet temperature is 100 ℃, the average grain diameter of the obtained microwave medium ceramic granulation powder is 75 +/-10 mu m, and the bulk density is 1.3 +/-0.1 g/cm 3 。
(4) And dry-pressing and molding the granulated powder to obtain the microwave dielectric ceramic green body. Wherein the pressure of the dry pressing is 200 MPa.
(5) And (3) preserving the heat of the microwave dielectric ceramic green body at 650 ℃ for 2 hours to remove the glue, then heating for sintering, wherein the sintering temperature is 1380 ℃, the heat preservation time is 4 hours, the heating rate is 135 +/-5 ℃/h, preparing the microwave dielectric ceramic material for the 5G communication base station, and finally finishing according to the size requirement of the device.
Testing the bending strength of the microwave dielectric ceramic material by adopting a WDW-50 universal material testing machine; the relative dielectric constant and the quality factor of the material are analyzed by an Agilent 8722ET network analyzer (open cavity method), the resonance frequency temperature coefficient of the material is measured by the Agilent 8722ET network analyzer and a precise constant temperature box, and the test temperature range is-50 ℃ to 125 ℃. The test results are shown in Table 1.
The application comprises the following steps: the processed microwave dielectric ceramic is metallized (silver paste is coated and sintered) by adopting a conventional metallization treatment mode to obtain the metallized microwave dielectric ceramic material for the 5G communication base station.
Example 5
This example provides aA microwave dielectric ceramic material for a 5G communication base station and a preparation method thereof. The chemical composition of the microwave dielectric ceramic material for the 5G communication base station is 0.76 (Ca) 1.2 Sb 0.8 )(Al 0.8 Ti 0.2 )O 4 +0.24Mg 2 SiO 4 。
The preparation method comprises the following steps:
(1) using analytically pure chemical reagents CaCO 3 、Sb 2 O 3 、Al 2 O 3 、TiO 2 、MgO、SiO 2 As raw material, 0.76 (Ca) 1.2 Sb 0.8 )(Al 0.8 Ti 0.2 )O 4 +0.24Mg 2 SiO 4 The chemical general formula of (1) is a molar ratio, and the prepared raw materials are put into a ball mill for ball milling for 16 hours to obtain slurry with the average particle size of about 1.2 mu m;
(2) after the ball-milled slurry is spray-dried, the temperature is raised to 1200 ℃ at the heating rate of 3 ℃/min for presintering for 4 hours to obtain microwave dielectric ceramic presintering powder;
(3) adding water and dispersant into the microwave dielectric ceramic pre-sintering powder, grinding with a sand mill to obtain slurry D 50 Adding adhesive into the slurry, uniformly mixing and stirring for 4 hours, and then carrying out spray granulation to obtain the dielectric adjustable characteristic, high Q x f and resonance frequency temperature coefficient tau with the dielectric adjustable characteristic f Excellent microwave dielectric ceramic granulated powder. Wherein the mass ratio of the added water to the feeding of the microwave dielectric ceramic pre-sintered powder is 1:1, the dispersing agent is ammonium polyacrylate, the adding amount is 1% of the microwave dielectric ceramic pre-sintered powder, the binder is a mixed solution (prepared into an 8% aqueous solution form) of polyethylene glycol and polyvinyl alcohol, the mass ratio of the polyethylene glycol to the polyvinyl alcohol is 1: 4, and the microwave dielectric ceramic pre-sintered powder accounts for 99.5% and the binder accounts for 0.5% of the total amount of the microwave dielectric ceramic pre-sintered powder and the binder. The inlet temperature of a spray drying tower for spray granulation is 220 ℃, the outlet temperature is 100 ℃, the average grain diameter of the obtained microwave medium ceramic granulation powder is 75 +/-10 mu m, and the bulk density is 1.3 +/-0.1 g/cm 3 。
(4) And dry-pressing and molding the granulated powder to obtain the microwave dielectric ceramic green body. Wherein the pressure of dry pressing is 150 MPa.
(5) And then, preserving the heat of the microwave dielectric ceramic green body at 650 ℃ for 2 hours for glue removal treatment, then heating for sintering, wherein the sintering temperature is 1370 ℃, the heat preservation time is 4 hours, the heating rate is 140 +/-5 ℃/h, preparing the microwave dielectric ceramic material for the 5G communication base station, and finally finishing according to the size requirement of the device.
Adopting a WDW-50 universal material testing machine to test the bending strength of the microwave dielectric ceramic material; the relative dielectric constant and the quality factor of the material are analyzed by an Agilent 8722ET network analyzer (open cavity method), the resonance frequency temperature coefficient of the material is measured by the Agilent 8722ET network analyzer and a precise constant temperature box, and the test temperature range is-50 ℃ to 125 ℃. The test results are shown in Table 1.
The application comprises the following steps: the processed microwave dielectric ceramic is metallized (silver paste is coated and sintered) by adopting a conventional metallization treatment mode to obtain the metallized microwave dielectric ceramic material for the 5G communication base station.
Comparative example
The present embodiment provides a microwave dielectric ceramic material and a preparation method thereof, wherein the microwave dielectric ceramic material comprises the following chemical compositions: 0.85 (Ca) 1.2 Sm 0.8 )(Al 0.8 Ti 0.2 )O 4 +0.15Mg 2 SiO 4 The preparation method is basically the same as example 4, and only the raw material Sb 2 O 3 Sm is replaced by Sm 2 O 3 。
Performance test
The microwave dielectric ceramics obtained in the above examples 1-5 and comparative examples are tested for bending strength by adopting a WDW-50 universal material testing machine; the relative dielectric constant and the quality factor of the material are analyzed by an Agilent 8722ET network analyzer (open cavity method), the resonance frequency temperature coefficient of the material is measured by the Agilent 8722ET network analyzer and a precise constant temperature box, and the test temperature range is-50 ℃ to 125 ℃. The test results are shown in Table 1.
TABLE 1
| Sintering temperature (. degree. C.) | Three point bending strength (MPa) | ε r | Q×f(GHz) | τ f (ppm/℃) | |
| Example 1 | 1420 | 230 | 21.8 | 97247 | 7.6 |
| Example 2 | 1400 | 215 | 21.6 | 92189 | 4.2 |
| Example 3 | 1400 | 200 | 21.3 | 85164 | 3.5 |
| Example 4 | 1380 | 175 | 20.8 | 81000 | 1.2 |
| Example 5 | 1370 | 150 | 20.4 | 78682 | -2.3 |
| Comparative example | 1380 | 180 | 21.2 | 26000 | 8.5 |
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
Claims (9)
1. A microwave dielectric ceramic material for a 5G communication base station is characterized by comprising the following chemical components: (1-y) (Ca) 1+x Sb 1-x )(Al 1-x Ti x )O 4 + y Mg 2 SiO 4 Wherein x is more than 0 and less than or equal to 0.4, and y is more than 0 and less than or equal to 0.3;
the preparation method of the microwave dielectric ceramic material for the 5G communication base station comprises the following steps:
(1) with CaCO 3 、Sb 2 O 3 、Al 2 O 3 、TiO 2 、MgO、SiO 2 As a starting material, according to (1-y) (Ca) 1+x Sb 1-x )(Al 1-x Ti x )O 4 + y Mg 2 SiO 4 The chemical formula is prepared, and ball milling is carried out to obtain ball milling slurry; wherein x is more than 0 and less than or equal to 0.4, and y is more than 0 and less than or equal to 0.3;
(2) drying and pre-burning the ball-milling slurry obtained in the step (1) to prepare microwave dielectric ceramic pre-burning powder;
(3) adding water and a dispersing agent into the microwave dielectric ceramic pre-sintering powder obtained in the step (2), carrying out ball milling, then adding an adhesive into the slurry, uniformly mixing, and carrying out spray granulation to prepare microwave dielectric ceramic granulation powder;
(4) dry-pressing and molding the granulated powder obtained in the step (3) to obtain a microwave medium ceramic green body;
(5) and (4) carrying out glue removal treatment on the microwave dielectric ceramic green body obtained in the step (4), then heating up, and sintering, wherein the sintering temperature is 1350-.
2. A microwave dielectric ceramic material for a 5G communication base station as claimed in claim 1, wherein y is 0.01 or more and 0.25 or less.
3. A microwave dielectric ceramic material for a 5G communication base station as claimed in claim 1, wherein x is 0.05 or more and 0.30 or less.
4. The microwave dielectric ceramic material for the 5G communication base station as claimed in claim 1, wherein the three-point bending strength of the microwave dielectric ceramic material is 150MPa or more.
5. The microwave dielectric ceramic material for the 5G communication base station as claimed in claim 1, wherein in the step (1), the average particle size of the powder particles in the ball-milling slurry is 0.5-1.6 μm; and/or, in the step (2), the pre-sintering temperature is 1150-1200 ℃, and the pre-sintering time is 2-6 h.
6. The microwave dielectric ceramic material for the 5G communication base station as claimed in claim 1, wherein in the step (3), the mass ratio of the addition amount of the water to the addition amount of the microwave dielectric ceramic pre-sintering powder is 0.8-1.2: 1; in the step (3), the dispersant is ammonium polyacrylate, and the addition amount of the dispersant accounts for 0.8-1.5% of the addition amount of the microwave dielectric ceramic pre-sintering powder; in the step (3), D of the powder particles in the ground slurry 50 0.5-1.2 μm; and/or, in the step (3), the adhesive comprises polyvinyl alcohol and polyethylene glycol, and the feeding mass ratio of the polyvinyl alcohol to the polyethylene glycol is 3-5: 1; in the step (3), the microwave dielectric ceramic pre-sintering powder accounts for 95-99.7% and the adhesive accounts for 0.3-5% of the total amount of the microwave dielectric ceramic pre-sintering powder and the adhesive by 100%.
7. The microwave dielectric ceramic material for the 5G communication base station as claimed in claim 1, wherein in the step (3), the temperature of the inlet of the spray drying tower is 190- 3 (ii) a And/or in the step (4), the pressure of the dry pressing is 100-200 MPa.
8. The microwave dielectric ceramic material for the 5G communication base station as claimed in claim 1, wherein in the step (5), the microwave dielectric ceramic green compact obtained in the step (4) is subjected to heat preservation at 600-700 ℃ for 1-3 hours for glue removal treatment; and/or, in the step (5), the sintering temperature is 1350-.
9. Use of the microwave dielectric ceramic material for the 5G communication base station in any one of claims 1 to 8 in the preparation of microwave devices.
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