CN114920551A - Method for reducing cracking failure by reinforcing 5G ceramic filter material - Google Patents
Method for reducing cracking failure by reinforcing 5G ceramic filter material Download PDFInfo
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Abstract
The invention belongs to the technical field of ceramic materials, and particularly relates to a method for reducing cracking failure by reinforcing a 5G ceramic filter material. A 5G ceramic filter material comprising a ceramic material and optional dopants, the ceramic material having the chemical formula: (1-x) MgTiO 3 ‑xCaTiO 3 Wherein x is 0.005-0.10 and includes doping with Bi 2 O 3 、CuO、MnO 2 And one or more of CoO, wherein the total weight percentage of various doping components is not more than 3%. And the trace doping component is used for adjusting the grain boundary characteristics of the ceramic, increasing the mechanical strength of the ceramic and improving the thermal shock resistance of the filter.
Description
Technical Field
The invention belongs to the technical field of ceramic materials, and particularly relates to a method for reducing cracking failure by reinforcing a 5G ceramic filter material.
Background
With the gradual implementation of the 5G communication technology, the signal transmission frequency is higher, the speed is faster, and the data density is higher, so that the current 3G/4G base station cannot meet the requirements, and therefore, the 5G base station needs to be built. The greater density and number of 5G base stations requires the base stations to be miniaturized and intensive. Accordingly, the amount of filters used is sharply increased as one of the devices used in large numbers in the base station. That is to say the filter must also be miniaturized. The solution is to replace the original metal cavity filter, 5G ceramic filter for short, with a dielectric ceramic filter. According to the principles of electromagnetism, the size of a resonator is inversely proportional to the square root of the dielectric constant of the dielectric material. The larger the dielectric constant of the dielectric material, the smaller the volume of dielectric ceramic required for a given frequency filter, that is, the smaller the size of the filter. Therefore, the high dielectric constant of the microwave dielectric ceramic material enables the miniaturization and integration of the microwave dielectric filter.
At present, 5G ceramic filters face a plurality of problems, and the station building speed of a 5G base station is seriously influenced. Among other problems, the cracking phenomenon of the filter during use restricts the operating efficiency of the 5G base station. On one hand, the 5G base station belongs to an open-air facility and is subjected to climate change, and on the other hand, a large amount of heat generated in the working process of the filter cannot be dissipated in time. The two brought consequences are that the filter is subjected to thermal shock caused by temperature difference, when stress generated by the thermal shock exceeds the mechanical strength of the material, cracks are generated, the material is damaged until the material is broken when the cracks are gradually accumulated to reach a certain threshold, and the device fails.
As a kind of electronic ceramic, the past research mainly focuses on its electrical properties, while the research on its mechanical properties has been neglected for a long time, so that the data on the mechanical properties of ceramic filter materials are seriously lacking and few reports are reported. However, the main reason for the severe cracking of the current 5G ceramic filter is that the mechanical strength of the material is too low to resist damage from thermal shock.
Disclosure of Invention
Based on the above background, the present invention aims to provide a method for reinforcing a 5G ceramic filter material to reduce cracking failure.
In order to achieve the above object, the present invention provides the following technical solutions:
A5G ceramic filter material comprising a ceramic material and, where necessary, a dopant,
the chemical formula of the ceramic material is as follows: (1-x) MgTiO 3-x CaTiO 3 Wherein x is 0.005-0.10 and includes doping with Bi 2 O 3 、CuO、MnO 2 And one or more of CoO, wherein the weight percentage of the total amount of various doping components is not more than 3 percent based on 100 percent of the weight of the ceramic material. And the trace doping component is used for adjusting the grain boundary characteristics of the ceramic, increasing the mechanical strength of the ceramic and improving the thermal shock resistance of the filter.
Preferably, the ceramic material is Mg 0.95 Ca 0.05 TiO 3 Doped with 0.25 wt% MnO 2 0.25 wt% of CoO and 0.2 wt% to 2.5 wt% of Bi 2 O 3 . Bi in 5G ceramic material 2 O 3 The content of (B) is preferably 0.2 wt% to 2.5 wt%, preferably 0.5 wt% to 2.0 wt%, and most preferably 1.0 wt%.
A method of reinforcing a 5G ceramic filter material to reduce cracking failure, the method comprising the steps of:
s1, batching the raw materials according to the stoichiometric ratio of the ceramic material;
s2, performing primary ball milling treatment and primary presintering treatment on the raw materials, wherein the temperature of the primary presintering treatment is controlled to be 900-1100 ℃, and primary ceramic powder is obtained;
s3, performing secondary ball milling treatment on the primary ceramic powder to obtain secondary ceramic powder;
s4, sequentially granulating, pressing and sintering the secondary ceramic powder to obtain the 5G ceramic filter material;
the primary ball milling and the secondary ball milling are wet ball milling by taking absolute ethyl alcohol as a medium; the rotation speed of the first-stage ball milling treatment and the second-stage ball milling treatment is 200-400 rpm, and the time is 4-24 hours;
the first-stage ball milling and the second-stage ball milling are carried out by adopting mixed zirconium balls containing large zirconium balls and small zirconium balls, the diameter of each large zirconium ball is 8-10 mm, and the diameter of each small zirconium ball is 4-6 mm.
The density of the ceramic sample of the filter ceramic material is measured by adopting an Archimedes method, the surrounding structure and the crystal boundary morphology of the ceramic sample of the filter ceramic material are observed by adopting a scanning electron microscope, and the mechanical property of the ceramic sample of the filter ceramic material is measured by adopting a standard three-point bending method.
Preferably, the ratio of the large zirconium balls to the small zirconium balls adopted by the first-stage ball milling and the second-stage ball milling is 2: 1, and the weight ratio is 1: 1.
Preferably, the particle size of the mixed powder obtained by the primary ball milling treatment is 0.1-0.6 μm, and more preferably 0.2-0.3 μm; the particle size of the mixed powder obtained by the secondary ball milling treatment is 0.2-1.0 μm, and the preferable particle size is 0.3-0.5 μm.
Preferably, after the first-stage ball milling treatment in step S2 is completed, before the first-stage pre-sintering, the mixed powder obtained by ball milling is sequentially dried and sieved; the drying treatment is drying in an electric furnace at 70-80 ℃, and the mesh number of the screen for sieving treatment is 100 meshes.
Preferably, the temperature of the first-stage pre-sintering is 950-1000 ℃, the time is 2-6 h, and the temperature rising rate from room temperature to the first-stage pre-sintering treatment is 2-10 ℃/min.
Preferably, the step S4 is to press-form the green compact under a pressure of 20MPa or more with the addition of the PVA binder; and after the pressing treatment in the step S4, placing the formed green body on an alumina setter plate for sintering.
Preferably, in step S4, the temperature is slowly increased to 1150-1350 ℃ during sintering, the temperature increase rate is 2 ℃/min, the temperature is maintained for 2-8 hours, the temperature is reduced to 600 ℃ at 2 ℃/min, and then the temperature is reduced to room temperature along with the furnace.
In the invention, the balls for the primary ball milling treatment are preferably zirconium balls, and more preferably, the balls are firstly ball milled by using mixed zirconium balls containing zirconium balls with different sizes, wherein the diameter of the large zirconium ball is preferably 8-10 mm, and the diameter of the small zirconium ball is preferably 4-6 mm; the ratio of the diameters of the large zirconium balls and the small zirconium balls is preferably 2: 1, and the weight ratio is preferably 1: 1. In the invention, the first-stage ball milling treatment is preferably wet ball milling; the medium of the wet ball milling is preferably absolute ethyl alcohol.
In the invention, the rotation speed of the primary ball milling treatment is preferably 200-400 rpm, and more preferably 300 rpm; the time of the first-stage ball milling treatment is preferably 4-24 h, and further preferably 2-12 h. The equipment adopted by the primary ball milling treatment is not particularly limited, and the ball milling equipment well known in the field can be adopted; in the embodiment of the present invention, the primary ball milling treatment is preferably performed in a tumbling ball mill. The wet ball milling of the combined zirconium balls with different diameters can further improve the dispersibility and uniformity of powder. In the invention, the particle size of the mixed powder obtained by the primary ball milling treatment is preferably less than 0.1-0.6 μm, and more preferably 0.2-0.3 μm.
After the first-stage ball milling treatment is finished, the first-stage ball milling powder obtained by the first-stage ball milling treatment is preferably dried and sieved in sequence. In the invention, the drying treatment is preferably to screen and separate the zirconium balls and the powder slurry through a screen with the aperture smaller than 2mm, the powder slurry is stored in a glass drying dish, and the drying dish is placed in an oven for drying, wherein the drying temperature is preferably 60-80 ℃, the temperature is further preferably 70 ℃, the time is preferably 2-12 h, and the time is further preferably 6 h; the invention can remove the organic solvent absolute ethyl alcohol in the wet ball milling process by drying. In the present invention, the mesh number of the screen used for the sieving treatment is preferably 100 mesh.
In the present invention, the temperature of the primary pre-firing treatment is preferably 900 to 1100 ℃, and more preferably 1000 ℃. In the invention, the heating rate from room temperature to the first-stage pre-sintering treatment temperature is preferably 2-10/min, and more preferably 5/min; after the temperature is raised to the first-stage pre-sintering treatment temperature, the heat preservation time is preferably 2-6 hours, and more preferably 4 hours.
In the present invention, the specific operations of the primary pre-firing treatment are preferably: and placing the primary powder in a corundum crucible for presintering treatment.
After the primary pre-sintering treatment is completed, the invention preferably cools the primary pre-sintering powder obtained by the primary pre-sintering treatment to obtain the primary ceramic powder. In the present invention, the cooling is preferably performed by taking the product out of the oven and naturally cooling the product at room temperature.
After the first-stage ceramic powder is obtained, the first-stage ceramic powder is sequentially subjected to second-stage ball milling treatment to obtain second-stage ceramic powder.
In the present invention, the balls for the secondary ball-milling treatment are preferably zirconium balls, and are further preferably ball-milled using mixed zirconium balls comprising large zirconium balls and small zirconium balls, wherein the diameter of the large zirconium balls is preferably 8 to 10mm, and the diameter of the small zirconium balls is preferably 4 to 6 mm; the ratio of the diameters of the large zirconium balls and the small zirconium balls is preferably 2: 1, and the weight ratio is preferably 1: 1. In the invention, the secondary ball milling treatment is preferably wet ball milling; the medium for wet ball milling is preferably absolute ethyl alcohol.
In the invention, the rotation speed of the secondary ball milling treatment is preferably 200-400 rpm, and more preferably 300 rpm; the time of the secondary ball milling treatment is preferably 2-12 h, and further preferably 4 h. The equipment adopted by the secondary ball milling treatment is not particularly limited, and the ball milling equipment well known in the field can be adopted; in the embodiments of the present invention, the secondary ball milling treatment is preferably performed in a tumbling ball mill. The invention leads the crystal grains of the first-grade ceramic powder to be more refined through the second-grade ball milling treatment. In the present invention, the particle size of the mixed powder obtained by the secondary ball milling treatment is preferably 0.2 to 1.0 μm, and more preferably 0.3 to 0.5 μm.
After the secondary ball milling treatment is finished, the secondary ball milling powder obtained by the secondary ball milling treatment is preferably dried and sieved in sequence. In the invention, the drying treatment is preferably to screen and separate the zirconium balls and the powder slurry through a screen with the aperture of 1-2mm, the powder slurry is stored in a drying dish, and the drying dish is placed in an oven for drying, wherein in the invention, the drying temperature is preferably 60-80 ℃, and more preferably 70 ℃; the time is preferably 2-8 h; further preferably 4 hours. The invention can remove the organic solvent absolute ethyl alcohol in the wet ball milling process by drying. In the present invention, the mesh number of the screen used for the sieving treatment is preferably 100 meshes, and the secondary ceramic powder is obtained.
After secondary ceramic powder is obtained, the secondary ceramic powder is sequentially pressed and sintered to obtain a ceramic sample of the 5G ceramic filter material.
In the present invention, dry press molding is used for the press molding, and the pressure is 20MPa or more, preferably 60 to 120MPa, and more preferably 80 MPa. In the present invention, the pressing is preferably performed in a mold. The mold of the present invention is not particularly limited, and a mold known in the art may be used. In the embodiment of the present invention, the mold is preferably a cylindrical mold or a rectangular parallelepiped mold. In the present invention, in the pressing process, the secondary ceramic powder is preferably made into a high-density and high-strength ceramic green body by using a mold. The present invention does not require any particular pressing operation, and may employ pressing operations known to those skilled in the art.
In the invention, the sintering treatment is preferably to slowly raise the temperature to 1200-1400 ℃ during sintering, more preferably to 1250-1350 ℃, and the temperature is kept for 2-12 hours, preferably 4 hours, and the temperature raising rate is 1-5 ℃/min, preferably 4 ℃/min; and cooling to 400-600 ℃, preferably 600 ℃, at a cooling rate of 4-20 ℃/min, preferably 10 ℃/min, and then cooling to room temperature along with the furnace. The invention preferably controls the heating rate within the range, and the cooling mode is preferably adopted in view of the fact that the reduction of the porosity is not influenced, so that the finally obtained ceramic material has a more compact structure, and on the premise that the problems of too high cooling rate and too large internal stress of the ceramic, which causes defects, can be prevented, the time of each link is shortened as much as possible, the process progress is accelerated, the process period is shortened, and the process efficiency is improved.
The 5G ceramic filter material or the 5G ceramic filter material prepared by the method is applied as a filter in a 5G communication base station.
Compared with the prior art, the invention has the following advantages:
1. the method of the invention achieves the purpose of improving the mechanical property of the material by controlling and adjusting the grain boundary characteristic of the ceramic material of the filter so as to resist the thermal shock caused by the temperature difference of the device in the working process, thereby reducing the probability of cracking failure.
2. The invention utilizes the doped oxide to form a second phase after being directly segregated at the grain boundary of the ceramic during the sintering process or being segregated at the boundary with the main crystal phase, and the segregation from the grain boundary formed after optimization enhances the bonding force between grains.
3. Because the doping process of the oxide is highly matched with the ceramic process, the preparation process of the filter is not influenced.
Drawings
FIG. 1 scanning electron micrograph of ceramic sample of example 2;
FIG. 2 SEM of a ceramic sample of example 6.
Detailed Description
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The chemical general formula of the ceramic material provided by the invention is as follows: (1-x) MgTiO 3-x CaTiO 3 . The present invention provides a ceramic material and (Mg) 0.95 Ca 0.05 )TiO 3 Is a base material and comprises Bi 2 O 3 、CuO、MnO 2 And trace doping components such as CoO and the like are used for adjusting and modifying the grain boundary characteristics of the ceramic so as to enhance the mechanical strength of the material, provide thermal shock resistance and reduce the cracking failure probability.
In the present invention, in the chemical formula, x is preferably 0.005 to 0.10, and the total weight percentage of each trace doping component is not more than 3%.
The 5G ceramic filter material provided by the invention is (Mg) 0.95 Ca 0.05 )TiO 3 Is used as matrix and the trace doped component is used for material modification.
In the present invention, all the raw materials are commercially available products known to those skilled in the art, and the purity of the raw materials is preferably 99% or more, unless otherwise specified.
In the present invention, the magnesium material is preferably magnesium oxide, the purity is preferably 99.8%, the calcium material is preferably calcium carbonate, the purity is preferably 99%, the titanium material is preferably titanium dioxide, the purity is preferably 99%, the purity of bismuth trioxide is preferably 99%, the purity of copper oxide is preferably 99%, the purity of manganese dioxide is preferably 99%, and the purity of cobalt oxide is preferably 99%.
In the invention, the 5G ceramic filter is used for a 5G communication base station.
Example 1
5G ceramic material composition: mg (Mg) 0.95 Ca 0.05 TiO 3 The method for reducing cracking failure by reinforcing the 5G ceramic filter material comprises the following specific steps:
(1) preparing materials: weighing MgO and CaCO according to the molecular formula of the ceramic material and the stoichiometric ratio 3 、TiO 2 Weighing raw materials required for preparing 0.1mol of ceramic powder, and simultaneously adding 0.25 wt% of MnO 2 、0.25wt％CoO、0.25wt％ CuO。
(2) In addition, 0.05 wt% Bi was added 2 O 3 The raw materials of (1).
(3) Ball milling: the weighed raw materials are put into a ball milling tank with zirconium balls (the diameter is 5 mm and 10mm) with different sizes, the weight ratio of the large zirconium balls to the small zirconium balls is 1: 1 (the same below), and then absolute ethyl alcohol is added as a ball milling medium, and the addition amount is just to submerge powder and the milling balls. And then ball-milling for 4h on a roller ball mill.
(4) Drying and sieving: separating the ball-milled protomer slurry into a drying dish by using a screen, and then placing the drying dish into an oven to dry at 70 ℃ until the powder in the drying dish is volatilized and dried by alcohol. And sieving the dried powder by using a 100-mesh sieve.
(5) Pre-burning: and (3) putting the dried and sieved raw material powder into a crucible, heating to 1000 ℃ at a heating rate of 4 to/min, and keeping the temperature for 4 hours to finally obtain the first-level powder of the embodiment.
(6) Secondary ball milling: the obtained first-stage powder of the embodiment is filled into a ball milling tank with zirconium balls with different sizes again, absolute alcohol is added into the ball milling tank to completely submerge the powder and the milling balls, and then ball milling is carried out for 4 hours.
(7) Drying and sieving: separating the ball-milled protomer slurry into a drying dish by using a screen, and then placing the drying dish into an oven to dry at 70 ℃ until the alcohol is volatilized and dried. After the drying, the powder was sieved with a 100-mesh sieve to obtain the second-level powder of this example.
(8) Dry pressing and forming: the secondary powder of this example was dry-pressed with an appropriate amount of PVA binder to obtain a green compact of two shapes, i.e., a wafer shape and a rectangular parallelepiped shape.
(9) And (3) sintering: and (3) placing the ceramic green body formed by pressing on a corundum setter plate, and sintering for 2 hours at 1300 ℃. The heating rate was 2 ℃/min. Then, the temperature was decreased to 600 ℃ at a rate of 10 ℃/min, and then cooled to room temperature along with the furnace, thereby obtaining a sample of example 1.
Example 2
5G ceramic material composition: mg (Mg) 0.95 Ca 0.05 TiO 3 The method for reducing cracking failure by reinforcing the 5G ceramic filter material comprises the following specific steps:
(1) preparing materials: weighing MgO and CaCO according to the molecular formula of the ceramic material and the stoichiometric ratio 3 、TiO 2 Weighing raw materials required for preparing 0.1mol of ceramic powder, and simultaneously adding 0.25 wt% of MnO 2 、0.25wt％CoO。
(2) In addition, 0.07 wt% of Bi was added 2 O 3 The raw materials of (1).
(3) Steps (9) to (9) were the same as in example 1, and example 2 was obtained after sintering.
Example 3
5G ceramic material composition: mg (Mg) 0.95 Ca 0.05 TiO 3 The method for reducing cracking failure by reinforcing the 5G ceramic filter material comprises the following specific steps:
(1) preparing materials: weighing MgO and CaCO according to the molecular formula of the ceramic material and the stoichiometric ratio 3 、TiO 2 Weighing raw materials for preparing 0.1mol of ceramic powder, and adding 0.25 wt% of MnO 2 、0.25wt％CoO。
(2) In addition, 0.1 wt% Bi was added 2 O 3 The raw materials of (1).
(3) Steps (9) were the same as in example 1, and the sample of example 3 was obtained after sintering.
Example 4
5G ceramic material composition: mg (Mg) 0.95 Ca 0.05 TiO 3 The method for reducing cracking failure by reinforcing the 5G ceramic filter material comprises the following specific steps:
(1) preparing materials: weighing MgO and CaCO according to the molecular formula of the ceramic material and the stoichiometric ratio 3 、TiO 2 Weighing raw materials required for preparing 0.1mol of ceramic powder, and simultaneously adding 0.25 wt% of MnO 2 、0.25wt％CoO。
(2) In addition, 0.2 wt% Bi was added 2 O 3 The raw materials of (1).
(3) Steps (9) to (9) were the same as in example 1, and example 4 was obtained after sintering.
Example 5
5G ceramic material composition: mg (magnesium) 0.95 Ca 0.05 TiO 3 The method for reducing cracking failure by reinforcing the 5G ceramic filter material comprises the following specific steps:
(1) preparing materials: weighing MgO and CaCO according to the molecular formula of the ceramic material and the stoichiometric ratio 3 、TiO 2 Weighing raw materials for preparing 0.1mol of ceramic powder, and adding 0.25 wt% of MnO 2 、0.25wt％CoO。
(2) In addition, 0.5 wt% Bi was added 2 O 3 The raw materials of (1).
(3) Steps (9) were the same as in example 1, and the sample of example 5 was obtained after sintering.
Example 6
5G ceramic material composition: mg (magnesium) 0.95 Ca 0.05 TiO 3 The method for reducing cracking failure by reinforcing the 5G ceramic filter material comprises the following specific steps:
(1) preparing materials: weighing MgO and CaCO according to the molecular formula of the ceramic material and the stoichiometric ratio 3 、TiO 2 Weighing raw materials required for preparing 0.1mol of ceramic powder, and simultaneously adding 0.25 wt% of MnO 2 、0.25wt％CoO。
(2) In addition, 1.0 wt% Bi was added 2 O 3 The raw materials of (1).
(3) Steps (9) to (9) were the same as in example 1, and a sample of example 6 was obtained after sintering.
Example 7
5G ceramic material composition: mg (magnesium) 0.95 Ca 0.05 TiO 3 The method for reducing cracking failure by reinforcing the 5G ceramic filter material comprises the following specific steps:
(1) preparing materials: weighing MgO and CaCO according to the molecular formula of the ceramic material and the stoichiometric ratio 3 、TiO 2 Weighing raw materials required for preparing 0.1mol of ceramic powder, and simultaneously adding 0.25 wt% of MnO 2 、0.25wt％CoO。
(2) In addition, 2.0 wt% Bi was added 2 O 3 The raw materials of (1).
(3) Steps (9) were the same as in example 1, and example 7 was obtained after sintering.
Example 8
5G ceramic material composition: mg (Mg) 0.95 Ca 0.05 TiO 3 The method for reducing cracking failure by reinforcing the 5G ceramic filter material comprises the following specific steps:
(1) preparing materials: weighing MgO and CaCO according to the molecular formula of the ceramic material and the stoichiometric ratio 3 、TiO 2 Weighing raw materials required for preparing 0.1mol of ceramic powder, and simultaneously adding 0.25 wt% of MnO 2 、0.25wt％CoO。
(2) In addition, 2.5 wt% Bi was added 2 O 3 The raw materials of (1).
(3) Steps (9) were the same as in example 1, and example 8 was obtained after sintering.
Example 9
5G ceramic material composition: mg (Mg) 0.95 Ca 0.05 TiO 3 The method for reducing cracking failure by reinforcing the 5G ceramic filter material comprises the following specific steps:
(1) preparing materials: weighing MgO and CaCO according to the molecular formula of the ceramic material and the stoichiometric ratio 3 、TiO 2 Weighing raw materials required for preparing 0.1mol of ceramic powder, and simultaneously adding 0.25 wt% of MnO 2 、0.25wt％CoO。
(2) In addition, 3 wt% of Bi was added 2 O 3 The raw materials of (1).
(3) Steps (9) were the same as in example 1, and example 9 was obtained after sintering.
The samples obtained in examples 1 to 9 were subjected to density measurement, microstructure analysis and strength measurement tests, respectively, in the following specific methods:
1. density measurement: the density of the sintered sample was measured using archimedes' method.
2. And (3) microstructure analysis: and analyzing the natural section of the ceramic sample by adopting a scanning electron microscope to obtain a structural picture, and analyzing the grain size and size distribution.
3. And (3) measuring the strength: the mechanical strength of the cuboid sample was measured by a three-point bending method.
The density and mechanical strength of each of the samples of examples 1-9 are shown in Table 1.
TABLE 1 Density and mechanical Strength of the samples
As can be seen from the data in table 1, the bending strength of the filter ceramic samples gradually increased from example 1 to example 9 until example 6 reached the maximum value and then began to decrease. This indicates that the strength of the filter ceramic can be controlled by controlling Bi 2 O 3 The dosage of the composition is optimized. Since Bi 2 O 3 The melting point of (2) is lower, and the material is melted into a liquid phase in the sintering process to realize liquid phase sintering. Thus, Bi 2 O 3 On the one hand, the additive has a promoting effect on sintering, and on the other hand, the additive can be segregated in a grain boundary during cooling after sintering. In Bi 2 O 3 At a low content, the liquid phase is not sufficient to fill all grain boundaries, so the strength follows Bi 2 O 3 The content is increased gradually; when the grain boundaryWhen completely filled, the intensity reached a maximum (example 6); then Bi 2 O 3 Further increase in the content results in a decrease in the mechanical strength of the ceramic. Thus, Bi in 5G ceramic materials 2 O 3 The content of (B) is preferably 0.2 to 2.5% by weight, more preferably 0.5 to 2.0% by weight, most preferably 1.0% by weight of example 6.
FIGS. 1 and 2 are SEM photographs of the ceramic samples of examples 2 and 6, respectively, showing that Bi is present 2 O 3 At lower contents, the grain boundaries are not completely filled, and the grain boundary strength of the ceramic is low, so that sample fracture occurs along the grain boundaries (fig. 1). When Bi is present 2 O 3 The content reaches its optimum value, the grain boundary strength is sufficiently high, and fracture of the sample occurs both along the grain boundary and through the grains, so that the fracture strength of the sample reaches the maximum value.
In summary, the grain boundary characteristics of the 5G ceramic filter material can be effectively controlled by the trace amount of the dopant, thereby improving the mechanical strength. Under the condition of given material composition, Bi can be controlled 2 O 3 The content of (a) optimizes the fracture strength of the filter ceramic.
In the present specification, the embodiments are described in a progressive manner, and each embodiment focuses on differences from other embodiments, and the same or similar parts between the embodiments are referred to each other. The device disclosed by the embodiment corresponds to the method disclosed by the embodiment, so that the description is simple, and the relevant points can be referred to the method part for description.
The method for reinforcing the 5G ceramic filter material to reduce the cracking failure provided by the invention is described in detail above. The principles and embodiments of the present invention are explained herein using specific examples, which are presented only to assist in understanding the method and its core concepts. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
Claims (10)
1. A 5G ceramic filter material, characterized by: the material comprises a ceramic material and necessary doping, wherein the chemical formula of the ceramic material is as follows: (1-x) MgTiO 3-x CaTiO 3 Wherein x is 0.005-0.10 and includes doping with Bi 2 O 3 、CuO、MnO 2 And one or more of CoO, wherein the weight percentage of the total amount of various doping components is not more than 3 percent based on 100 percent of the weight of the ceramic material.
2. The 5G ceramic filter material of claim 1, wherein: the ceramic material is Mg 0.95 Ca 0.05 TiO 3 Doped with 0.25 wt% MnO 2 0.25 wt% of CoO and 0.2 wt% to 2.5 wt% of Bi 2 O 3 。
3. A method of reinforcing a 5G ceramic filter material to reduce cracking failure according to claim 1, the method comprising the steps of:
s1, mixing the raw materials according to the stoichiometric ratio of the ceramic material;
s2, performing primary ball milling treatment and primary presintering treatment on the raw materials, wherein the temperature of the primary presintering treatment is controlled to be 900-1100 ℃, and obtaining primary ceramic powder;
s3, carrying out secondary ball milling treatment on the primary ceramic powder to obtain secondary ceramic powder;
s4, sequentially granulating, pressing and sintering the secondary ceramic powder to obtain the 5G ceramic filter material;
the primary ball milling and the secondary ball milling are wet ball milling by taking absolute ethyl alcohol as a medium; the rotation speed of the first-stage ball milling treatment and the second-stage ball milling treatment is 200-400 rpm, and the time is 4-24 hours;
the first-stage ball milling and the second-stage ball milling are carried out by adopting mixed zirconium balls containing large zirconium balls and small zirconium balls, the diameter of each large zirconium ball is 8-10 mm, and the diameter of each small zirconium ball is 4-6 mm.
4. The method of 5G ceramic filter material reinforcement to reduce cracking failure of claim 3, wherein: the ratio of the large zirconium balls to the small zirconium balls adopted by the first-stage ball milling and the second-stage ball milling is 2: 1, and the weight ratio is 1: 1.
5. The method of 5G ceramic filter material reinforcement to reduce cracking failure of claim 3, wherein: the granularity of the mixed powder obtained by the primary ball milling treatment is 0.1-0.6 mu m; the granularity of the mixed powder obtained by the secondary ball milling treatment is 0.2-1.0 mu m.
6. The method of 5G ceramic filter material reinforcement to reduce cracking failure of claim 3, wherein: after the primary ball milling treatment in the step S2 is finished, drying and sieving the mixed powder obtained by ball milling in sequence before primary presintering; the drying treatment is drying in an electric furnace at 70-80 ℃, and the mesh number of the screen for sieving treatment is 100 meshes.
7. The method of 5G ceramic filter material reinforcement to reduce cracking failure of claim 1, wherein: the temperature of the first-stage pre-sintering is 950-1000 ℃, the time is 2-6 h, and the heating rate from room temperature to the first-stage pre-sintering treatment is 2-10 ℃/min.
8. The method of 5G ceramic filter material reinforcement to reduce cracking failure of claim 1, wherein: the step S4 is to press and shape under the pressure of more than 20MPa and under the condition of adding PVA binder to form a green body; and after the pressing treatment in the step S4, placing the molded green body on an alumina setter plate for sintering.
9. The method of 5G ceramic filter material reinforcement to reduce cracking failure of claim 1, wherein: in the step S4, the temperature is slowly raised to 1150-1350 ℃ during sintering, the heating rate is 2 ℃/min, the temperature is kept for 2-8 hours, and the temperature is lowered to 600 ℃ at 2 ℃/min and then is lowered to room temperature along with the furnace.
10. Use of the 5G ceramic filter material of claim 1 or the 5G ceramic filter material produced by the method of any one of claims 3 to 9 as a filter device in a 5G communication base station.
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Denomination of invention: Method of enhancing 5G ceramic filter materials to reduce cracking failure Granted publication date: 20230711 Pledgee: Zhejiang Tailong Commercial Bank Co.,Ltd. Jiaxing Pinghu Sub branch Pledgor: Zhejiang Tiersai New Material Co.,Ltd. Registration number: Y2024980033157 |
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