CN107805067B - Low-dielectric-constant microwave dielectric ceramic with zero-frequency temperature coefficient and ultralow loss and preparation method thereof - Google Patents
Low-dielectric-constant microwave dielectric ceramic with zero-frequency temperature coefficient and ultralow loss and preparation method thereof Download PDFInfo
- Publication number
- CN107805067B CN107805067B CN201711066157.4A CN201711066157A CN107805067B CN 107805067 B CN107805067 B CN 107805067B CN 201711066157 A CN201711066157 A CN 201711066157A CN 107805067 B CN107805067 B CN 107805067B
- Authority
- CN
- China
- Prior art keywords
- dielectric ceramic
- sio
- microwave dielectric
- mgta
- powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/495—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 vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3206—Magnesium oxides 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
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
-
- 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
- C04B2235/3232—Titanium oxides or titanates, e.g. rutile or anatase
-
- 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
- C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, 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
- C04B2235/3231—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
- C04B2235/3281—Copper oxides, cuprates or oxide-forming salts thereof, e.g. CuO or Cu2O
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3284—Zinc oxides, zincates, cadmium oxides, cadmiates, mercury oxides, mercurates or oxide forming salts thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—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
- C04B2235/02—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
- C04B2235/3293—Tin oxides, stannates or oxide forming salts thereof, e.g. indium tin oxide [ITO]
-
- 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
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3418—Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (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 relates to a low-dielectric constant microwave dielectric ceramic with zero frequency temperature coefficient and ultralow loss and a preparation method thereof, wherein the general chemical formula of the microwave dielectric ceramic is xMg2SiO4‑(1‑x)MgTa2O6+ y wt% of B, wherein B is ZnO, CuO or Al2O3、Ga2O3、TiO2、ZrO2、SnO2、MnO2、Nb2O5、Sb2O5And WO3Wherein x represents Mg2SiO4Occupy Mg2SiO4And MgTa2O6X is more than 0 and less than 1 in percentage of total molar weight; y represents B in Mg2SiO4And MgTa2O6Y is more than or equal to 0 and less than or equal to 5.
Description
Technical Field
The invention belongs to the technical field of microwave dielectric ceramics, and particularly relates to microwave dielectric ceramics with low dielectric constant, ultralow dielectric loss and near-zero frequency temperature coefficient and a preparation method thereof.
Background
In recent years, with the rapid development of 5G communication technology and global positioning technology, there is an increasing demand for high-performance microwave dielectric ceramics for wireless communication devices such as microwave filters, resonators, oscillators, and the like, especially for ceramics with ultra-low microwave dielectric loss and near-zero frequency temperature coefficient. The ceramic can meet the requirements of realizing mobility, portability, miniaturization and miniaturization of microwave communication equipment, and can meet the requirements of working characteristics of high performance, high reliability, large-capacity information transmission and the like in a microwave range, thereby gaining wide attention.
MgTa2O6Has high quality factor Qf value and medium and low dielectric constant epsilonrAnd positive temperature coefficient of resonance frequencyf(Qf＝60000GHz，εr＝30，τf30ppm/° c) cannot meet the actual requirements, whereas Mg does2SiO4Also has excellent microwave dielectric properties (Qf 270000GHz, epsilon)r＝6.8，τf-67ppm/° c), nor can it meet the application requirements.
Disclosure of Invention
In view of the above problems, the present invention aims to provide a microwave dielectric ceramic with low dielectric constant, ultra-low dielectric loss and near-zero frequency temperature coefficient and a preparation method thereof.
In one aspect, the invention provides a microwave dielectric ceramic with low dielectric constant and ultralow dielectric loss, wherein the chemical general formula of the microwave dielectric ceramic is xMg2SiO4-(1-x)MgTa2O6+ y wt% of B, wherein B is ZnO, CuO or Al2O3、Ga2O3、TiO2、ZrO2、SnO2、MnO2、Nb2O5、Sb2O5And WO3Wherein x represents Mg2SiO4Occupy Mg2SiO4And MgTa2O6X is more than 0 and less than 1 in percentage of total molar weight; y represents B in Mg2SiO4And MgTa2O6Y is more than or equal to 0 and less than or equal to 5.
The dielectric property of the dielectric ceramic is adjusted by utilizing a dielectric ceramic composite technology so as to meet the application requirement, and the mechanism is as follows: using two base materials (MgTa) with opposite frequency-temperature coefficients2O6Having a positive temperature coefficient of resonance frequency tauf30 ppm/DEG C, and Mg2SiO4Has the advantages ofNegative temperature coefficient of frequency taufAt-67 ppm/° c), the composition was adjusted by controlling the relative amounts of the two phases (i.e., molar ratio x: (1-x), wherein x is more than 0 and less than 1, and a result that the frequency temperature coefficient is close to zero is obtained. In addition, proper amount of B substances (B and Mg) are added into the two base materials2SiO4And MgTa2O6Y is more than or equal to 0 and less than or equal to 5), improves the sintering property of the material and stabilizes the dielectric property of the material.
Preferably, the dielectric constant of the microwave dielectric ceramic is 6.9 to 28.3, the quality factor Qf value is 60000 to 275000GHz, and the temperature coefficient of the resonant frequency is-70 to 55 ppm/DEG C.
Preferably, x is more than or equal to 0.5 and less than or equal to 0.7 or/and y is more than or equal to 1 and less than or equal to 3.
Also, preferably, when x is 0.5 ≦ x ≦ 0.7 and y is 1 ≦ y ≦ 3, the dielectric constant of the microwave dielectric ceramic is 12.1 to 15.2, preferably 13 to 15, the quality factor Qf is 120000 to 152000GHz, preferably 125000 to 140000GHz, and the temperature coefficient of the resonance frequency is-11 to 18 ppm/DEG C, preferably 0 to 4 ppm/DEG C.
In another aspect, the present invention provides a method for preparing a microwave dielectric ceramic, including:
mixing Mg2SiO4Powder and MgTa2O6Powder is as xMg2SiO4-(1-x)MgTa2O6Weighing and mixing stoichiometric compositions to obtain mixed powder;
adding B and a binder into the mixed powder, and crushing, granulating and molding to obtain a blank;
and sintering the obtained blank at 1300-1450 ℃ for 4-16 h to obtain the microwave dielectric ceramic.
Preferably, MgO, Ta2O5、SiO2Respectively synthesizing Mg in advance as raw materials2SiO4Powder and MgTa2O6And (3) powder.
Further, preferably, MgO and SiO are used2Mixing, calcining for 4-12 h at 1000-1250 ℃ to obtain Mg2SiO4。
Further, preferably, MgO and Ta2O5After mixingCalcining for 4-12 h at 1000-1250 ℃ to obtain MgTa2O6And (3) powder.
Preferably, the mass of B is 0 to 5 wt% of the mass of the mixed powder, and preferably 1 to 3 wt%.
Preferably, the binder is at least one of polyvinyl alcohol (PVA), polyvinyl butyral (PVB) and sodium carboxymethyl cellulose (CMC), and the amount of the binder is 2-4 wt% of the mass of the mixed powder.
The invention has the advantages that: xMg2SiO4-(1-x)MgTa2O6The + y wt% B composite microwave dielectric ceramic material has low dielectric constant and wide adjustable range of 6.9-28.3, high quality factor of 60000-275000 GHz, and continuously adjustable temperature coefficient of resonance frequency, and can meet the requirements of the new generation of communication.
Detailed Description
The present invention is further illustrated by the following examples, which are to be understood as merely illustrative and not restrictive.
In the invention, the chemical formula of the composite microwave dielectric ceramic with low dielectric constant, high quality factor and near-zero frequency temperature coefficient can be expressed as xMg2SiO4-(1-x)MgTa2O6+ y wt% of B. Wherein B can be ZnO, CuO, Al2O3、Ga2O3、TiO2、ZrO2、SnO2、MnO2、Nb2O5、Sb2O5And WO3At least one of (1). Wherein x represents Mg2SiO4Occupy Mg2SiO4And MgTa2O6X is more than 0 and less than 1 (preferably, x is more than or equal to 0.5 and less than or equal to 0.7) in percentage of the total molar weight; y represents B in Mg2SiO4And MgTa2O60. ltoreq. y.ltoreq.5 (preferably 1. ltoreq. y.ltoreq.3). If the addition amount of B exceeds 5 wt%, new compounds are generated, and various properties of the microwave dielectric ceramic deviate from predicted values.
In the invention, the dielectric constant of the microwave dielectric ceramic is 6.9-28.3, the quality factor Qf value is 60000-275000 GHz, and the temperature coefficient of the resonant frequency is-70-55 ppm/DEG C. When x is more than or equal to 0.5 and less than or equal to 0.7 and y is more than or equal to 1 and less than or equal to 3, the composite microwave dielectric ceramic has stable dielectric property and good repeatability, the dielectric constant of the microwave dielectric ceramic is 12.1-15.2, preferably 13-15, the quality factor Qf value is 120000-152000 GHz, preferably 125000-140000 GHz, the temperature coefficient of the resonance frequency is-11-18 ppm/DEG C, preferably 0-4 ppm/DEG C.
The microwave dielectric ceramic has the advantages of simple preparation process, good repeatability and excellent microwave dielectric property. The preparation method of the microwave dielectric ceramic with medium and low dielectric constant, extremely low dielectric loss and near-zero temperature coefficient of frequency provided by the invention is exemplarily described below.
Mg2SiO4Powder and MgTa2O6And (3) preparing powder. Specifically, MgO and Ta2O5、SiO2Respectively synthesizing Mg in advance as raw materials2SiO4Powder and MgTa2O6And (3) powder. Mixing MgO and SiO2Or MgO and Ta2O5Mixing, calcining for 4-12 h at 1000-1250 ℃ to obtain Mg2SiO4Or MgTa2O6And (3) powder. The mixing method may be ball milling. Note that Mg in the present invention2SiO4Powder and MgTa2O6The preparation of the powder is not limited to the above-mentioned preparation method. Mg prepared by other methods2SiO4Powder and MgTa2O6The powder can also be used for preparing the microwave dielectric ceramic.
Mixing Mg2SiO4Powder and MgTa2O6Powder is as xMg2SiO4-(1-x)MgTa2O6And (3) weighing the stoichiometric composition, adding B and a binder into the mixed powder, and crushing, granulating and molding to obtain the required blank. The mass of B is 0-5 wt% of the mass of the mixed powder, and preferably 1-3 wt%. The binder may be at least one of polyvinyl alcohol (PVA), polyvinyl butyral (PVB), sodium carboxymethyl cellulose (CMC), and the like. The dosage of the binder can be 2-4 wt% of the mass of the mixed powder. Said compositionThe molding method can be dry pressing, cold isostatic pressing and the like.
And sintering the obtained blank at 1300-1450 ℃ for 4-16 h to obtain the low-dielectric-constant microwave dielectric ceramic.
As an example of a method for preparing a microwave dielectric ceramic, a ceramic having high purity (purity)>99％)MgO、SiO2And Ta2O5Calcining the raw materials at 1000-1250 ℃ (preferably 1000-1200 ℃) for 4-12 h to synthesize Mg2SiO4Powder and MgTa2O6Powder of, then according to xMg2SiO4-(1-x)MgTa2O6Weighing stoichiometric components, adding B with the mass fraction of y wt%, crushing, adding a binder, granulating and molding to obtain a blank; and sintering the obtained blank at 1350-1450 ℃ for 4-16 h to obtain the microwave dielectric ceramic.
And testing the microwave dielectric property of the prepared ceramic. The diameter and thickness of the sample were measured using a micrometer. The dielectric constant and the dielectric loss of the prepared cylindrical ceramic material are measured by an Agilent E8363A PNA network analyzer through a cavity method, a test sample is placed into an ESPEC MC-710F type high-low temperature circulation box to measure the temperature coefficient of the resonant frequency, the temperature range is 20-85 ℃, and the test frequency is in the range of 9-16 GHz.
The present invention will be described in detail by way of examples. It is also to be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the invention, and that certain insubstantial modifications and adaptations of the invention by those skilled in the art in light of the foregoing description are intended to be included within the scope of the invention. The specific process parameters and the like of the following examples are also only one example of suitable ranges, i.e., those skilled in the art can select the appropriate ranges through the description herein, and are not limited to the specific values exemplified below.
The invention adopts high-purity MgO and Ta2O5、SiO2And B as raw materials for preparing xMg2SiO4-(1-x)MgTa2O6+ y wt% B ceramic, specific examples are as follows.
Example 1
(1) Mixing MgO and Ta2O5、SiO2According to the molar ratio of MgO to Ta2O51:1 and MgO SiO2Weigh 2:1, add zirconia balls and deionized water. Ball milling is carried out for 1-2 hours, the ball milled raw materials are dried in a drying oven and then calcined at 1100 ℃ for 4 hours to synthesize MgTa2O6And Mg2SiO4；
(2) Synthesized Mg2SiO4And MgTa2O6Weighing the raw materials according to the molar fraction ratio of 0.4:0.6, 0.5:0.5, 0.6:0.4, 0.7:0.3 and 0.8:0.2, adding the raw materials into a ball milling tank containing zirconia balls and deionized water, ball milling for 1-2 hours, drying, adding PVA (polyvinyl alcohol) with the mass fraction of 3% into powder serving as a binder for granulation, and pressing into a cylindrical blank;
(4) the cylindrical blank is sintered into ceramic at 1350 ℃ for 8h to obtain the required composite microwave dielectric ceramic;
(5) and (4) testing the microwave dielectric property of the composite microwave dielectric ceramic prepared in the step (4) by using a network analyzer and a resonant cavity. The results of the measurements of the relevant process parameters and microwave dielectric properties of the specific examples are detailed in table 1.
Table 1 shows the results of the experiments referred to in example 1:
example 2
The procedure is as in example 1 except that, in example 1, a 0.6-component x is selected, the amount of substance B added in step (2) is 1 wt%, and the remaining steps are the same as in example 1, and the test results are shown in table 2.
Table 2 shows the results of the experiments referred to in example 2:
example 3
Similar to example 2, on the basis of example 2, the material B is selected to be ZnO, the addition amount of the material B is changed, the rest steps are the same as example 1, and the test results are detailed in Table 3.
Table 3 shows the results of the experiments referred to in example 3:
Claims (8)
1. the microwave dielectric ceramic with low dielectric constant and ultralow dielectric loss is characterized in that the chemical general formula of the microwave dielectric ceramic is xMg2SiO4-(1-x)MgTa2O6+ y wt% of B, wherein B is ZnO, CuO or Al2O3、Ga2O3、TiO2、ZrO2、SnO2、MnO2、Nb2O5、Sb2O5And WO3At least one of; wherein x represents Mg2SiO4Occupy Mg2SiO4And MgTa2O6Percentage of total molar mass, y representing B in Mg2SiO4And MgTa2O6Percent of the total mass of; wherein x is 0.5-0.7, y is 1-3, x =0.5, y =0, x =0.6, y =0, or x =0.7, y = 0;
when x is more than or equal to 0.5 and less than or equal to 0.7 and y is more than or equal to 1 and less than or equal to 3, the dielectric constant of the microwave dielectric ceramic is 12.1-15.2, and the quality factorQfThe value is 120000-152000 GHz, and the temperature coefficient of the resonance frequency is-11-18 ppm/DEG C;
when x =0.5 and y =0, the dielectric constant of the microwave dielectric ceramic is 15.2, and the quality factor isQfThe value is 120000 GHz, and the temperature coefficient of the resonance frequency is 18 ppm/DEG C;
when x =0.6 and y =0, the dielectric constant of the microwave dielectric ceramic is 13.8, and the quality factor isQfThe value is 134000 GHz, the temperature coefficient of the resonance frequency is 4 ppm/DEG C;
when x =0.7 and y =0, the microwaveThe dielectric constant of the dielectric ceramic is 12.1, and the quality factorQfThe value is 152000GHz, and the temperature coefficient of the resonance frequency is-11 ppm/DEG C;
the preparation method of the microwave dielectric ceramic comprises the following steps:
mixing Mg2SiO4Powder and MgTa2O6Powder is as xMg2SiO4-(1-x)MgTa2O6Weighing and mixing stoichiometric compositions to obtain mixed powder;
adding B and a binder into the mixed powder, and crushing, granulating and molding to obtain a blank;
and sintering the obtained blank at 1300-1450 ℃ for 4-16 h to obtain the microwave dielectric ceramic.
2. The microwave dielectric ceramic of claim 1, wherein the microwave dielectric ceramic has a dielectric constant of 13 to 15 and a quality factorQfThe value is 125000-140000 GHz, and the temperature coefficient of resonance frequency is 0-4 ppm/DEG C.
3. A microwave dielectric ceramic according to claim 1 characterised in that MgO, Ta2O5、SiO2Respectively synthesizing Mg in advance as raw materials2SiO4Powder and MgTa2O6And (3) powder.
4. A microwave dielectric ceramic according to claim 3 wherein MgO and SiO are mixed2Mixing, calcining for 4-12 h at 1000-1250 ℃ to obtain Mg2SiO4。
5. A microwave dielectric ceramic according to claim 3 wherein MgO and Ta are mixed2O5After mixing, calcining for 4-12 h at 1000-1250 ℃ to obtain MgTa2O6And (3) powder.
6. A microwave dielectric ceramic according to claim 1, wherein the mass of B is 1 to 3 wt% of the mass of the mixed powder.
7. A microwave dielectric ceramic according to claim 1 wherein the binder is at least one of polyvinyl alcohol PVA, polyvinyl butyral PVB and sodium carboxymethyl cellulose CMC.
8. A microwave dielectric ceramic according to claim 7, wherein the binder is used in an amount of 2 to 4 wt% based on the mass of the mixed powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711066157.4A CN107805067B (en) | 2017-11-02 | 2017-11-02 | Low-dielectric-constant microwave dielectric ceramic with zero-frequency temperature coefficient and ultralow loss and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711066157.4A CN107805067B (en) | 2017-11-02 | 2017-11-02 | Low-dielectric-constant microwave dielectric ceramic with zero-frequency temperature coefficient and ultralow loss and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107805067A CN107805067A (en) | 2018-03-16 |
| CN107805067B true CN107805067B (en) | 2021-01-12 |
Family
ID=61591088
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711066157.4A Active CN107805067B (en) | 2017-11-02 | 2017-11-02 | Low-dielectric-constant microwave dielectric ceramic with zero-frequency temperature coefficient and ultralow loss and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107805067B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108439969B (en) * | 2018-06-29 | 2020-11-24 | 无锡鑫圣慧龙纳米陶瓷技术有限公司 | Low-dielectric-constant temperature-stable microwave medium and preparation method thereof |
| CN109503163A (en) * | 2018-12-20 | 2019-03-22 | 中国科学院上海硅酸盐研究所 | One kind having ultrahigh Q-value tantalic acid magnesium media ceramic and preparation method thereof |
| CN113563061B (en) * | 2021-09-26 | 2021-12-21 | 广东康荣高科新材料股份有限公司 | Low dielectric constant dielectric material for single-cavity filter and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100199301B1 (en) * | 1997-04-09 | 1999-06-15 | 김병규 | Dielectric ceramic composition |
| CN103319166A (en) * | 2013-05-28 | 2013-09-25 | 电子科技大学 | Microwave ceramic medium material and preparation method thereof |
-
2017
- 2017-11-02 CN CN201711066157.4A patent/CN107805067B/en active Active
Non-Patent Citations (1)
| Title |
|---|
| Microwave Dielectric Properties of MgTiO3, MgTa2O6 /Polytetrafluoroethylene Composite;Chang jun Jeon等;《Journal of The Korean Ceramic Society》;20121231;第49卷(第3期);第272-278页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107805067A (en) | 2018-03-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102442823B (en) | Microwave dielectric ceramic material and preparation method thereof | |
| CN102659396B (en) | Low-dielectric constant microwave ceramic dielectric material and preparation method thereof | |
| CN102603297B (en) | Novel low-temperature sintered microwave dielectric ceramic and preparation method thereof | |
| CN103265271B (en) | Low-temperature sintered alumina ceramic material with adjustable frequency temperature coefficient and preparation method thereof | |
| CN107805067B (en) | Low-dielectric-constant microwave dielectric ceramic with zero-frequency temperature coefficient and ultralow loss and preparation method thereof | |
| CN107382313B (en) | Microwave dielectric ceramic with ultrahigh quality factor, medium-low dielectric constant and near-zero temperature coefficient and preparation method thereof | |
| CN108911746B (en) | Low-loss tungsten-based ultralow-temperature sintered microwave dielectric ceramic material and preparation method and application thereof | |
| CN112125668B (en) | Medium low-loss LTCC microwave dielectric ceramic material and preparation method thereof | |
| CN110066169A (en) | A kind of oxidation silicon substrate dielectric constant microwave ceramic medium and preparation method | |
| CN105347781B (en) | A kind of ceramic material and preparation method thereof | |
| CN102887702A (en) | Low-temperature-sintered lithium-zinc-titanium microwave dielectric ceramic and preparation method thereof | |
| CN111377721B (en) | Low-temperature co-fired ceramic material and preparation method thereof | |
| CN112851347A (en) | Low-temperature sintered low-loss oxyfluoride microwave dielectric ceramic and preparation method thereof | |
| CN112174653A (en) | Microwave dielectric ceramic material with high Qf and low dielectric constant and preparation method thereof | |
| CN104710175B (en) | A kind of low-k magnesium zirconate lithium microwave dielectric ceramic materials and preparation method thereof | |
| CN108503353B (en) | Composite phosphate microwave dielectric ceramic and preparation method thereof | |
| CN114736012B (en) | Low dielectric microwave dielectric ceramic with ultrahigh Q value and LTCC material thereof | |
| CN110372347B (en) | Low-loss low-dielectric-constant microwave ceramic material and preparation method thereof | |
| CN114409396B (en) | High-temperature stable microwave dielectric ceramic for WIFI and preparation method thereof | |
| CN107056277B (en) | Low-temperature sintered medium-dielectric-constant microwave dielectric material and preparation method thereof | |
| CN112079631B (en) | Low-dielectric LTCC material with near-zero temperature coefficient and preparation method thereof | |
| CN104140260A (en) | Low-temperature sintering method of lithium-magnesium-titanium microwave dielectric ceramic | |
| KR100842854B1 (en) | Low temperature co-fired microwave dielectric ceramics and the manufacturing method thereof | |
| CN109650886B (en) | Ba-Mg-Ta LTCC material and preparation method thereof | |
| CN103951429B (en) | A kind of low-temperature sintering low-loss microwave dielectric ceramic materials |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |