CN113979743A - high-Q light microwave dielectric ceramic for 5G base station ceramic filter and preparation method thereof - Google Patents
high-Q light microwave dielectric ceramic for 5G base station ceramic filter and preparation method thereof Download PDFInfo
- Publication number
- CN113979743A CN113979743A CN202111170462.4A CN202111170462A CN113979743A CN 113979743 A CN113979743 A CN 113979743A CN 202111170462 A CN202111170462 A CN 202111170462A CN 113979743 A CN113979743 A CN 113979743A
- Authority
- CN
- China
- Prior art keywords
- microwave dielectric
- base station
- ceramic
- light
- dielectric ceramic
- 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.)
- Pending
Links
- 239000000919 ceramic Substances 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title abstract description 16
- 238000000498 ball milling Methods 0.000 claims abstract description 26
- 239000010955 niobium Substances 0.000 claims abstract description 24
- 239000010936 titanium Substances 0.000 claims abstract description 22
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000002994 raw material Substances 0.000 claims abstract description 14
- 238000005245 sintering Methods 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 7
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium dioxide Chemical compound O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 5
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 claims abstract description 4
- QZQVBEXLDFYHSR-UHFFFAOYSA-N gallium(III) oxide Inorganic materials O=[Ga]O[Ga]=O QZQVBEXLDFYHSR-UHFFFAOYSA-N 0.000 claims abstract description 4
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 4
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 4
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims abstract description 4
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 4
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 4
- 229940119177 germanium dioxide Drugs 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 18
- 239000002002 slurry Substances 0.000 claims description 6
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 239000012188 paraffin wax Substances 0.000 claims description 3
- 230000003179 granulation Effects 0.000 claims description 2
- 238000005469 granulation Methods 0.000 claims description 2
- 238000003786 synthesis reaction Methods 0.000 claims description 2
- 229910010252 TiO3 Inorganic materials 0.000 abstract description 3
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 3
- -1 niobium ions Chemical class 0.000 abstract description 3
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052733 gallium Inorganic materials 0.000 abstract description 2
- 150000002500 ions Chemical class 0.000 abstract description 2
- 238000000465 moulding Methods 0.000 abstract 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 23
- 229910052744 lithium Inorganic materials 0.000 description 23
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 22
- 239000003989 dielectric material Substances 0.000 description 8
- 229910007848 Li2TiO3 Inorganic materials 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 230000007547 defect Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- 229910019704 Nb2O Inorganic materials 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 229910004688 Ti-V Inorganic materials 0.000 description 1
- 229910010968 Ti—V Inorganic materials 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000002639 sodium chloride Nutrition 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
Images
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
- C04B35/46—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
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01P—WAVEGUIDES; RESONATORS, LINES, OR OTHER DEVICES OF THE WAVEGUIDE TYPE
- H01P1/00—Auxiliary devices
- H01P1/20—Frequency-selective devices, e.g. filters
-
- 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
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3251—Niobium oxides, niobates, tantalum oxides, tantalates, 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
- C04B2235/3286—Gallium oxides, gallates, indium oxides, indates, thallium oxides, thallates or oxide forming salts thereof, e.g. zinc gallate
-
- 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
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Insulating Materials (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention belongs to the technical field of ceramic materials, and discloses a high-Q light microwave dielectric ceramic for a 5G base station ceramic filter and a preparation method thereof, wherein the chemical formula is Li2Ti1‑x(Ga1/2Nb1/2)xO3‑y w.t.％Nb2O5(ii) a Wherein x is 0.015-0.03, and y is 0-1.5; the preparation process comprises the steps of respectively preparing raw materials of lithium carbonate, titanium dioxide, germanium dioxide, gallium sesquioxide and niobium pentoxide, carrying out ball milling by taking absolute ethyl alcohol as a ball milling agent, and drying; pre-synthesizing dried powder; adding Nb into the pre-synthesized powder2O, carrying out secondary ball milling by taking absolute ethyl alcohol as a ball milling agent, and drying; drying the powder, granulating and molding into a blank; sintering the blank to obtain the target product. The invention improves Li by ion codoping (gallium and niobium ions)2TiO3The dielectric property of the microwave dielectric ceramic is light, and the microwave dielectric ceramic has high quality factor, low temperature coefficient of resonance frequency and proper dielectric constant.
Description
Technical Field
The invention belongs to the technical field of ceramic materials, and particularly relates to a ceramic composition characterized by components and a preparation method thereof.
Technical Field
Under the standard of the fifth generation mobile communication technology (5G), the 3GPP proposes a reconfiguration scheme to introduce a CU-DU-AAU architecture into a 5G access network, an RRU upward movement and an antenna feed system are combined into an AAU (active antenna unit), and a microwave filter is used as a core device at the connection position of the RRU and an antenna in the AAU unit, thereby playing a role in bringing great importance to the performance of a base station.
In addition to the AAU, Massive MIMO (large-scale antenna array technology) used in 5G base stations makes the base station antenna develop from 2T2R and 4T4R in 4G period to 64T64R, and the increase of the number and weight of the antennas makes the AAU and Massive MIMO technologies and the filters require miniaturization and light weight, so that the manufacturers tend to select ceramic filters with smaller size, lighter weight and lower cost (low insertion loss, good stability and high carrying power). Therefore, high-performance microwave dielectric materials have become one of the most active research directions in recent years as key materials for developing high-quality ceramic filters.
Among various microwave dielectric materials, Li2TiO3The microwave dielectric ceramic is a lithium-based rock salt material with low volume density (rho)bul～3.1g/cm3) The filters with the same volume are made, and the weight is light; the raw materials are relatively cheap, and the sintering temperature is relatively low (T)s1230 ℃); has moderate dielectric constant (epsilon) in millimeter wave bandr19.80) belonging to the K20 series microwave dielectric material, ensures the miniaturization of the filter and keeps low transmission loss, and is the preferable material for 5G base station filters and future wearable devices. However, it has a low quality factor (Qxf 23,600GHz) and a slightly higher temperature coefficient of resonance frequency (τ)f+38.5 ppm/. degree.C.).
Disclosure of Invention
The present invention is directed to existing Li2TiO3The microwave dielectric material has low quality factor (Qxf-23,600 GHz) and high resonant frequencyThe coefficient of degree is slightly higher (tau)f+38.5 ppm/DEG C), provides a high-Q light microwave dielectric ceramic for a 5G base station ceramic filter and a preparation method thereof, improves Li by ion co-doping (gallium and niobium ions)2TiO3The dielectric property of the microwave dielectric ceramic is light, and the microwave dielectric ceramic has high quality factor, low temperature coefficient of resonance frequency and proper dielectric constant.
The invention is realized by the following technical scheme:
according to one aspect of the invention, the invention provides a high-Q light microwave dielectric ceramic for a 5G base station ceramic filter, which has a chemical formula of Li2Ti1-x(Ga1/2Nb1/2)xO3-y w.t.％Nb2O5(ii) a Wherein x is 0.015 to 0.03 and y is 0 to 1.5.
Further, the quality factor Qf is 75,310-136,569 GHz, and the temperature coefficient tau of the resonance frequencyfIs + 18.61- +23.08 ppm/DEG C, and the dielectric constant epsilonrIs 20.49 to 23.38.
Further, the density is 3.09-3.23 g/cm3。
Further, when x is 0.025 and y is 0.5, the quality factor Qf is 136,569 GHz.
Further, when x is 0.025 and y is 1, the temperature coefficient of resonance frequency is 18.61 ppm/deg.c.
According to another aspect of the invention, a preparation method of the high-Q light-weight microwave dielectric ceramic for the 5G base station ceramic filter is provided, and the method comprises the following steps:
(1) according to Li2Ti1-x(Ga1/2Nb1/2)xO3The chemical formula of the method is that raw materials of lithium carbonate, titanium dioxide, germanium dioxide, gallium sesquioxide and niobium pentoxide are respectively prepared; ball-milling the raw materials by using absolute ethyl alcohol as a ball-milling agent, and drying the slurry after the ball-milling is finished; wherein x is 0.015-0.03;
(2) pre-synthesizing the dried powder obtained in the step (1);
(3) pre-synthesized powder obtained in the step (2)Addition of y w.t.% Nb2O, ball milling is carried out by taking absolute ethyl alcohol as a ball milling agent, and the slurry is dried after the ball milling is finished; wherein y is 0-1.5, and y w.t.% represents adding Nb2O5Occupying the pre-synthesized powder Li obtained in the step (2)2Ti1-x(Ga1/2Nb1/2)xO3Mass percent;
(4) granulating the dried powder obtained in the step (3) and forming a blank;
(5) sintering the blank formed in the step (4) at 1150-1200 ℃, and preserving heat for 3-6 h to obtain Li2Ti1-x(Ga1/2Nb1/2)xO3-y w.t.％Nb2O5Microwave dielectric ceramics.
Further, the step (1) and the step (3) are dried in the air atmosphere, and the step (5) is sintered in the air atmosphere.
Further, the pre-synthesis temperature in the step (2) is 800 ℃, and the heat preservation time is 4 hours.
Further, the granulation in the step (3) is carried out by adding 6 wt% of paraffin wax.
Further, the sintering temperature in the step (4) is 1150 ℃, and the heat preservation time is 4 hours.
The invention has the beneficial effects that:
the invention adopts the traditional solid phase synthesis method to prepare the high-Q light microwave dielectric material Ga for the 5G base station ceramic filter3+、Nd5+Doped substituted Ti of4+Formation of Li2Ti1-x(Ga1/2Nb1/2)xO3Solid solution, inhibition of V'Li、Ti′TiAnd
equal defect and (V'LI-V¨o-V′Li) And (Ti'Ti-V¨o-Vi′TiThe generation of the equal-defect dipoles reduces lattice non-resonance vibration caused by the defects and relaxation loss caused by the defect dipoles, and improves the quality factor of the material; and by adding a stabilizer Nb2O5Using Ti4+＝1/2(Ga3++Nd5+) The structural stability is adjusted by a mechanism, the temperature coefficient of the resonant frequency of the material is improved, and finally Li is obtained2Ti1-x(Ga1/2Nb1/2)xO3-y w.t.％Nb2O5(x is 0.015 to 0.03 and y is 0 to 1.5). The high-Q light microwave dielectric material for the lithium titanate-based base station ceramic filter has light density (3.09-3.23 g/cm)3) Has a high quality factor (Qf:75,310-136,569 GHz) and a small temperature coefficient (tau) of resonance frequencyf+18.61 to +23.08 ppm/. degree.C.), and an appropriate dielectric constant (. epsilon.) (E.)r:20.49～23.38)。
Drawings
FIG. 1 is a graph showing the Qf changes of the lithium titanate-based microwave dielectric ceramics obtained in examples 1 to 8;
FIG. 2 is a graph showing the change in dielectric constant of the lithium titanate-based microwave dielectric ceramics obtained in examples 1 to 8;
FIG. 3 is a graph showing the temperature coefficient change of the resonance frequency of the lithium titanate-based microwave dielectric ceramics obtained in examples 1 to 8.
Detailed Description
The invention is described in further detail below by means of specific examples and comparative examples:
example 1
(1) According to Li2Ti1-x(Ga1/2Nb1/2)xO3Respectively preparing raw materials of lithium carbonate, titanium dioxide, gallium trioxide and niobium pentoxide according to a chemical formula (x is 0.025), putting the raw materials into a ball milling tank, ball milling for 12 hours by taking absolute ethyl alcohol as a ball milling agent, and then putting the slurry into an oven to dry in an air atmosphere;
(2) sieving the dried powder obtained in the step (1), pre-synthesizing at 800 ℃, and keeping the temperature for 4 hours;
(3) sieving the pre-synthesized raw materials obtained in the step (2), placing the sieved pre-synthesized raw materials into a ball milling tank, ball milling the pre-synthesized raw materials for 12 hours by using absolute ethyl alcohol as a ball milling agent, and then placing the slurry into an oven to dry in an air atmosphere;
(4) granulating the dried powder obtained in the step (3) by using 6 wt% of paraffin, and forming into a blank;
(5) and (4) sintering the blank formed in the step (4) at 1150 ℃ in an air atmosphere, and preserving heat for 4 hours to obtain the lithium titanate-based microwave dielectric ceramic.
Example 2
The preparation of lithium titanate-based microwave dielectric ceramic was carried out by the method of example 1, except that 0.5 w.t.% Nb was added to the presynthesized raw material of step (3) while ball milling2O。
Example 3
The preparation of lithium titanate-based microwave dielectric ceramic was carried out by the method of example 1, except that 1 w.t.% of Nb was added during ball milling of the pre-synthesized raw material of step (3)2O。
Example 4
The preparation of lithium titanate-based microwave dielectric ceramic was carried out by the method of example 1, except that 1.5 w.t.% Nb was added to the presynthesized raw material of step (3) while ball milling2O。
Example 5
The preparation of a lithium titanate-based microwave dielectric ceramic was carried out by the method of example 1 except that the sintering temperature in step (5) was 1200 ℃.
Example 6
The preparation of lithium titanate-based microwave dielectric ceramic was carried out by the method of example 2, except that the sintering temperature in step (5) was 1200 ℃.
Example 7
The preparation of a lithium titanate-based microwave dielectric ceramic was carried out by the method of example 3, except that the sintering temperature in step (5) was 1200 ℃.
Example 8
The preparation of lithium titanate-based microwave dielectric ceramic was carried out by the method of example 4, except that the sintering temperature in step (5) was 1200 ℃.
Example 9
The preparation of a lithium titanate-based microwave dielectric ceramic was carried out using the method of example 2, except that x was 0.015.
Example 10
The preparation of lithium titanate-based microwave dielectric ceramic was carried out by the method of example 3, except that x was 0.03 and the sintering temperature in step (5) was 1125 ℃.
Li obtained in test examples 1 to 102Ti1-x(Ga1/2Nb1/2)xO3-y w.t.％Nb2The dielectric properties of the microwave dielectric ceramic material (after annealing treatment) are shown in table 1, wherein O (x is 0.015 to 0.03, and y is 0 to 1.5).
TABLE 1
As can be seen from Table 1, Li in phase-pure form2TiO3Performance (quality factor Qxf 23,600GHz, temperature coefficient of resonance frequency τ)fTo +38.5 ppm/DEG C), the density of the lithium titanate-based microwave dielectric ceramic is lighter (3.09-3.23 g/cm)3) High quality factor (Qf:75,310-136,569 GHz), and small temperature coefficient of resonance frequency (tau)f+18.61 to +23.08 ppm/. degree.C) and a suitable dielectric constant (. epsilon.) (E)r:20.49～23.38)。
The optimal formula and the performance are as follows:
x＝0.025，y＝0.5；
sintering temperature: 1150 deg.C
Bulk density: 3.21g/cm3
Dielectric constant: 20.49 of the total weight of the mixture;
quality factor: 136,569 GHz;
temperature coefficient of resonance frequency: 19.8 ppm/. degree.C
FIG. 1 is a graph showing the Qf changes of the lithium titanate-based microwave dielectric ceramics obtained in examples 1 to 8. As can be seen from FIG. 1, with pure phase Li2TiO3Compared with microwave dielectric material Qf (23,600 GHz), the lithium titanate-based microwave dielectric ceramic Qf prepared by the invention is obviously improved and is above 75,061 GHz. Wherein, the ball milling is carried out for the second timeAddition of Nb2O5The Qf value of the system reaches the highest value of 136,569GHz when the Qf is 0.5 w.t.% and the sintering temperature is 1150 ℃. Shows a chemical formula of Li2Ti1-x(Ga1/2Nb1/2)xO3-yw.t.％Nb2O5The lithium titanate-based high-Q light microwave dielectric ceramic (x is 0.025 and y is 0.5) has good Qf.
FIG. 2 is a graph showing the change of dielectric constant of the lithium titanate-based microwave dielectric ceramics prepared in examples 1 to 8, the dielectric constants of which are about 21 to 22, indicating the formula Li prepared by the present invention2Ti1-x(Ga1/2Nb1/2)xO3-y w.t.％Nb2O5The lithium titanate-based high-Q light microwave dielectric ceramic (x is 0.015-0.03, y is 0-1.5) belongs to K20 series microwave dielectric materials, and can ensure low transmission loss and realize filter miniaturization.
FIG. 3 is a graph showing the temperature coefficient change of the resonance frequency of the lithium titanate-based microwave dielectric ceramics obtained in examples 1 to 8. As can be seen from FIG. 3, the temperature coefficient of the resonance frequency is between +18.6 ppm/DEG C and +23.08 ppm/DEG C, and is equal to the pure phase Li2TiO3The frequency is more stable under temperature changes than (+ 38.5 ppm/. degree.C.). Wherein for Li2Ti1-x(Ga1/2Nb1/2)xO3-yw.t.％Nb2O5The temperature coefficient of the resonance frequency reached a minimum of 18.6 ppm/c when x is 0.025 and y is 1.
In conclusion, with pure phase Li2TiO3Performance (Density ρ)bul～3.1g/cm3Dielectric constant εr19.80, Q multiplied by f 23,600GHz, temperature coefficient of resonance frequency taufTo +38.5 ppm/DEG C) is higher than that of the lithium titanate-based high-Q light microwave dielectric ceramic (Qf:75,310-136,569 GHz) and has smaller resonance frequency temperature coefficient (tau)f+18.61 to +23.08 ppm/. degree.C) and a suitable dielectric constant (. epsilon.) (E)r20.95 to 23.38) and retains Li2TiO3Lower density (3.09-3.23 g/cm)3) The characteristics of (1).
Although the preferred embodiments of the present invention have been described, the present invention is not limited to the above-mentioned embodiments, which are only illustrative and not restrictive, and those skilled in the art can make various modifications without departing from the spirit and scope of the present invention, which falls within the protection scope of the present invention.
Claims (10)
1. A high-Q light microwave dielectric ceramic for a 5G base station ceramic filter is characterized in that the chemical formula is Li2Ti1-x(Ga1/2Nb1/2)xO3-y w.t.％Nb2O5(ii) a Wherein x is 0.015 to 0.03 and y is 0 to 1.5.
2. The high-Q light-weight microwave dielectric ceramic for the 5G base station ceramic filter as claimed in claim 1, wherein the quality factor Qf is 75,310-136,569 GHz, and the temperature coefficient of resonance frequency τ isfIs + 18.61- +23.08 ppm/DEG C, and the dielectric constant epsilonrIs 20.49 to 23.38.
3. The high-Q light-weight microwave dielectric ceramic for the 5G base station ceramic filter as claimed in claim 1, wherein the density is 3.09-3.23G/cm3。
4. The high-Q light-weight microwave dielectric ceramic for the 5G base station ceramic filter is characterized in that when x is 0.025 and y is 0.5, the quality factor Qf is 136,569 GHz.
5. The high-Q light-weight microwave dielectric ceramic for the 5G base station ceramic filter is characterized in that when x is 0.025 and y is 1, the temperature coefficient of the resonance frequency is 18.61ppm/° C.
6. A method for preparing a high-Q lightweight microwave dielectric ceramic for a 5G base station ceramic filter according to claims 1-5, which comprises the following steps:
(1) according to Li2Ti1-x(Ga1/2Nb1/2)xO3The chemical formula of the method is that raw materials of lithium carbonate, titanium dioxide, germanium dioxide, gallium sesquioxide and niobium pentoxide are respectively prepared; ball-milling the raw materials by using absolute ethyl alcohol as a ball-milling agent, and drying the slurry after the ball-milling is finished; wherein x is 0.015-0.03;
(2) pre-synthesizing the dried powder obtained in the step (1);
(3) adding y w.t.% Nb into the pre-synthesized powder obtained in the step (2)2O, ball milling is carried out by taking absolute ethyl alcohol as a ball milling agent, and the slurry is dried after the ball milling is finished; wherein y is 0-1.5, and y w.t.% represents adding Nb2O5Occupying the pre-synthesized powder Li obtained in the step (2)2Ti1-x(Ga1/2Nb1/2)xO3Mass percent;
(4) granulating the dried powder obtained in the step (3) and forming a blank;
(5) sintering the blank formed in the step (4) at 1150-1200 ℃, and preserving heat for 3-6 h to obtain Li2Ti1-x(Ga1/ 2Nb1/2)xO3-y w.t.％Nb2O5Microwave dielectric ceramics.
7. The method for preparing the high-Q light-weight microwave dielectric ceramic for the 5G base station ceramic filter according to claim 6, wherein the step (1) and the step (3) are dried in an air atmosphere, and the step (5) is sintered in the air atmosphere.
8. The method for preparing a high-Q light microwave dielectric ceramic for a 5G base station ceramic filter according to claim 6, wherein the pre-synthesis temperature in step (2) is 800 ℃ and the holding time is 4 h.
9. The method for preparing a high-Q light microwave dielectric ceramic for a 5G base station ceramic filter as claimed in claim 6, wherein the granulation in step (3) is carried out by adding 6 wt% of paraffin wax.
10. The method for preparing a high-Q light microwave dielectric ceramic for a 5G base station ceramic filter as claimed in claim 6, wherein the sintering temperature in step (4) is 1150 ℃ and the holding time is 4 h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111170462.4A CN113979743A (en) | 2021-10-08 | 2021-10-08 | high-Q light microwave dielectric ceramic for 5G base station ceramic filter and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111170462.4A CN113979743A (en) | 2021-10-08 | 2021-10-08 | high-Q light microwave dielectric ceramic for 5G base station ceramic filter and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113979743A true CN113979743A (en) | 2022-01-28 |
Family
ID=79737728
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111170462.4A Pending CN113979743A (en) | 2021-10-08 | 2021-10-08 | high-Q light microwave dielectric ceramic for 5G base station ceramic filter and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113979743A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20150111719A1 (en) * | 2012-03-22 | 2015-04-23 | Holy Stone Enterprise Co., Ltd. | Dielectric ceramic material |
| CN107500750A (en) * | 2017-08-04 | 2017-12-22 | 天津大学 | Magnesium niobium is co-doped with preparing high q-factor lithium-based microwave dielectric material |
| CN111606705A (en) * | 2020-04-16 | 2020-09-01 | 天津大学 | high-Q light microwave dielectric material for 5G base station ceramic filter |
-
2021
- 2021-10-08 CN CN202111170462.4A patent/CN113979743A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20150111719A1 (en) * | 2012-03-22 | 2015-04-23 | Holy Stone Enterprise Co., Ltd. | Dielectric ceramic material |
| CN107500750A (en) * | 2017-08-04 | 2017-12-22 | 天津大学 | Magnesium niobium is co-doped with preparing high q-factor lithium-based microwave dielectric material |
| CN111606705A (en) * | 2020-04-16 | 2020-09-01 | 天津大学 | high-Q light microwave dielectric material for 5G base station ceramic filter |
Non-Patent Citations (3)
| Title |
|---|
| DONG WANG ET AL.: "A low-sintering temperature microwave dielectric ceramic for 5G LTCC applications with ultralow loss", 《CERAMICS INTERNATIONAL》 * |
| DONG WANG ET AL.: "Ultra-low dielectric loss lithium-based, temperature stable microwave dielectric ceramics", 《CERAMICS INTERNATIONAL》 * |
| RAZ MUHAMMAD ET AL.: "Microwave dielectric properties of CaTi1-x(Nb0.5Ga0.5)xO3 ceramics", 《MATERIALS LETTERS》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107117967B (en) | Low-temperature sintered composite microwave dielectric ceramic material and preparation method thereof | |
| CN110092655B (en) | Barium samarium-titanium series low-loss microwave dielectric ceramic and preparation method thereof | |
| CN112851346B (en) | Ultralow-loss zirconium magnesium niobate system microwave dielectric ceramic material and preparation method thereof | |
| CN108059454B (en) | Temperature-stable high-dielectric-constant microwave dielectric ceramic and preparation method and application thereof | |
| CN108358633B (en) | Low-temperature sintered Ca5Mn4-xMgxV6O24Microwave dielectric material and preparation method thereof | |
| CN108147809B (en) | Medium-low temperature sintered barium-titanium series microwave dielectric material and preparation method thereof | |
| CN103833351B (en) | Microwave dielectric ceramic and preparation method thereof | |
| CN111606705A (en) | high-Q light microwave dielectric material for 5G base station ceramic filter | |
| CN102731092A (en) | Zr-Ti-based microwave dielectric ceramic material and preparation method thereof | |
| CN107721421B (en) | Zn-Nb-Ti LTCC material and preparation method thereof | |
| CN103467084B (en) | A kind of high-k series of lithium, niobium and titanium low-temperature sintered ceramics and preparation method thereof | |
| CN113979743A (en) | high-Q light microwave dielectric ceramic for 5G base station ceramic filter and preparation method thereof | |
| CN106938924B (en) | Microwave composite ceramic with small dielectric constant and high Q value and preparation method thereof | |
| CN110734284A (en) | medium high Q microwave medium ceramic material and preparation method thereof | |
| CN106866143B (en) | Microwave complex phase ceramic AWO4-TiO2 and preparation method thereof | |
| CN105399413A (en) | Microwave dielectric ceramic with low dielectric constant and low loss and preparation method | |
| CN104692792A (en) | Low-temperature sintering temperature stable stannate microwave dielectric ceramic material | |
| CN113956033A (en) | Medium high-Q-value microwave dielectric ceramic and preparation method thereof | |
| CN109650886B (en) | Ba-Mg-Ta LTCC material and preparation method thereof | |
| CN112898012A (en) | Microwave dielectric ceramic material and preparation method thereof | |
| CN111825445B (en) | High-dielectric-constant microwave dielectric ceramic material, preparation and application thereof | |
| CN112028621A (en) | Medium dielectric constant dielectric ceramic for filter and preparation method thereof | |
| CN113387695A (en) | Low-dielectric high-quality microwave dielectric ceramic for 5G communication and preparation method thereof | |
| CN112745106A (en) | Low-expansion-coefficient microwave dielectric ceramic material and preparation method thereof | |
| CN112266238A (en) | Low dielectric constant ceramic material for microwave device and preparation method thereof |
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 | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20220128 |