CN112830775B - Low-dielectric-constant microwave dielectric ceramic and preparation method thereof - Google Patents
Low-dielectric-constant microwave dielectric ceramic and preparation method thereof Download PDFInfo
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Abstract
The invention provides a low-dielectric-constant microwave dielectric ceramic and a preparation method thereof, wherein the microwave dielectric ceramic comprises the following components in parts by weight: 100 parts of titanate silicate complex and 0.1 to 0.3 part of rare metal oxide; the titanate silicate complex is [ (Zn) x Mg 1‑x ) 2 SiO 4 ] z ‑(Sr y Ca 1‑y TiO 3 ) 1‑z The method comprises the steps of carrying out a first treatment on the surface of the The rare metal oxide is CeO 2 、Nb 2 O 5 And/or Ta 2 O 5 The method comprises the steps of carrying out a first treatment on the surface of the Wherein x is more than or equal to 0 and less than or equal to 1, y is more than or equal to 0 and less than or equal to 0.2,0.75, and z is more than or equal to 0.95. The microwave dielectric ceramic can be prepared at a lower sintering temperature, has a larger sintering window, namely good stability when the performance fluctuates with the sintering temperature, has higher Qf value and adjustable frequency temperature coefficient, has a simple preparation process, and can realize large-scale mass production.
Description
[ field of technology ]
The invention relates to the technical field of microwave dielectric ceramic materials, in particular to a low-dielectric-constant microwave dielectric ceramic and a preparation method thereof.
[ background Art ]
The dielectric filter is made of microwave dielectric ceramic materials, and the microwave dielectric ceramic is used as a key material in modern communication and can be applied to microwave frequency band circuits as a dielectric material.
Among the existing low-dielectric-constant microwave dielectric ceramic materials, mg2SiO4/Zn2SiO4 series silicate microwave ceramic has wide application, low dielectric loss at very high microwave frequency, is a negative-frequency temperature coefficient material, can adjust the frequency temperature coefficient of the composite material to be near zero by adding a positive-frequency temperature coefficient material, and is a typical low-dielectric-constant material which is more studied and mature. However, the severe sintering temperature makes the material difficult to sinter, the sintering window is generally only within 20 ℃, the mass production is very unfavorable, and the dielectric property of the material is deteriorated due to the fact that Zn is easy to volatilize during the high-temperature sintering process. And the material is fixed and not easy to adjust under the condition that the frequency temperature coefficient needs to be determined.
Accordingly, there is a need for an improved low dielectric constant microwave dielectric ceramic and method of making the same.
[ invention ]
The invention mainly aims to provide the low-dielectric-constant microwave dielectric ceramic and the preparation method thereof, which can be prepared at a lower sintering temperature, and have the advantages of larger sintering window, namely good stability when the performance fluctuates with the sintering temperature, higher Qf value, adjustable frequency temperature coefficient, simple preparation process and capability of realizing large-scale mass production.
In order to achieve the above object, the first aspect of the present invention provides a low dielectric constant microwave dielectric ceramic, which comprises the following components in parts by weight: 100 parts of titanate silicate complex and 0.1 to 0.3 part of rare metal oxide; the titanate silicate complex is [ (Zn) x Mg 1-x ) 2 SiO 4 ] z -(Sr y Ca 1-y TiO 3 ) 1-z The method comprises the steps of carrying out a first treatment on the surface of the The rare metal oxide is CeO 2 、Nb 2 O 5 And/or Ta 2 O 5 The method comprises the steps of carrying out a first treatment on the surface of the Wherein x is more than or equal to 0 and less than or equal to 1, y is more than or equal to 0 and less than or equal to 0.2,0.75, and z is more than or equal to 0.95.
As a preferable technical scheme, the dielectric constant is 8.0-9.0, the temperature coefficient of resonance frequency is-15- +20ppm/DEG C, and the Qf value is 35000-40000 GHz.
The technical scheme provided by the second aspect of the invention is that the preparation method of the low-dielectric-constant microwave dielectric ceramic comprises the following steps: preparing composite powder: in a molar ratio of [2xz ]]：[2z-2xz]：[z]：[y-yz]：[1-y-z+yz]：[1-z]Respectively weighing ZnO, mgO, siO with purity of more than 99.5% 2 、SrCO 3 、CaCO 3 、TiO 2 Ball milling the powder, fully mixing, drying and grinding, and presintering at high temperature to obtain [ (Zn) x Mg 1-x ) 2 SiO 4 ] z -(Sr y Ca 1-y TiO 3 ) 1-z A composite powder; preparing ceramic powder: adding 0.1-0.3% of rare metal oxide by weight into the composite powder, performing secondary ball milling, adding a binder, and granulating to obtain ceramic powder; blank manufacturing: adding a release agent into the ceramic powder, sieving, and pressing into a ceramic blank on a pressing machine; sintering and forming: sintering the pressed ceramic blank at high temperature to form porcelain; wherein x is more than or equal to 0 and less than or equal to 1, y is more than or equal to 0 and less than or equal to 0.2,0.75, and z is more than or equal to 0.95; the rare metal oxide is CeO 2 、Nb 2 O 5 And/or Ta 2 O 5 。
As a preferable technical scheme, the binder is polyvinyl alcohol, and the addition amount is 5-10% of the weight of the composite powder.
As a preferable technical scheme, the release agent is calcium stearate, zinc stearate or magnesium stearate, and the addition amount is 1-5% of the weight of the composite powder.
As a preferable technical scheme, the presintering temperature is 800-900 ℃ and the presintering time is 1.8-2.5 hours.
As a preferable technical scheme, the high-temperature sintering temperature is 1050-1100 ℃ and the sintering time is 4-5 hours.
The microwave dielectric ceramic of the invention is prepared by adopting ZnO, mgO, siO 2 、SrCO 3 、CaCO 3 、TiO 2 Powder combination solid solution to form titanate silicate complex [ (Zn) x Mg 1-x ) 2 SiO 4 ] z -(Sr y Ca 1-y TiO 3 ) 1-z Then through rare metal oxide (CeO) 2 、Nb 2 O 5 And/or Ta 2 O 5 ) The doping of the material can be prepared at a lower sintering temperature, the sintering window is larger, namely the stability of the performance is good along with the fluctuation of the sintering temperature, the preparation process is simple, the mass production can be realized, meanwhile, the Qf value is higher, the better microwave dielectric performance can be obtained, and the temperature coefficient of the resonant frequency can be adjusted as required.
[ detailed description ] of the invention
The invention is further described below with reference to examples.
The low-dielectric-constant microwave dielectric ceramic provided by the embodiment comprises the following components in parts by weight: 100 parts of titanate silicate complex and 0.1 to 0.3 part of rare metal oxide. The titanate silicate complex is [ (Zn) x Mg 1-x ) 2 SiO 4 ] z -(Sr y Ca 1-y TiO 3 ) 1-z . The rare metal oxide is CeO 2 、Nb 2 O 5 And/or Ta 2 O 5 . Wherein x is more than or equal to 0 and less than or equal to 1, y is more than or equal to 0 and less than or equal to 0.2,0.75, and z is more than or equal to 0.95.
The embodiment also provides a preparation method of the low-dielectric-constant microwave dielectric ceramic.
Example 1
The specific steps of this embodiment are as follows:
(1) Preparing composite powder: at a molar ratio of [ 2.0.5.0.86]：[2*0.86-2*0.5*0.86]：[0.86]：[0.05-0.05*0.86]：[1-0.05-0.86+0.05*0.86]：[1-0.86]Respectively weighing ZnO, mgO, siO with purity of more than 99.5% 2 、SrCO 3 、CaCO 3 、TiO 2 Ball milling the powder in a high-speed ball mill, fully mixing, drying and grinding, and presintering at high temperature to obtain [ (Zn) 0.5 Mg 0.5 ) 2 SiO 4 ] 0.86 -(Sr 0.05 Ca 0.95 TiO 3 ) 0.14 The presintering temperature is 800 ℃ and the presintering time is 1.8 hours.
(2) Preparing ceramic powder: 0.2% by weight (i.e., 0.2% by weight) of rare metal oxide CeO was added to the composite powder 2 And (3) performing secondary ball milling in a high-speed ball mill, adding 5% (i.e. 5 wt%) of binder by weight of the composite powder, and granulating to obtain the ceramic powder. The ceramic powder has the composition of [ (Zn) 0.5 Mg 0.5 ) 2 SiO 4 ] 0.86 -(Sr 0.05 Ca 0.95 TiO 3 ) 0.14 +0.2wt％CeO 2 . The binder is polyvinyl alcohol (PVA).
(3) Blank manufacturing: adding a release agent which is 3 percent (namely 3 weight percent) of the weight of the composite powder into the ceramic powder, then passing through an 80-mesh screen, and pressing into a cylindrical ceramic blank body on a press. It will be appreciated that the shape of the blank may also be other. The release agent is calcium stearate.
(4) Sintering and forming: sintering the pressed ceramic blank at high temperature into porcelain to obtain the microwave dielectric ceramic, wherein the high-temperature sintering temperature is 1090 ℃ and the sintering time is 4 hours. The dielectric constant epsilon of the microwave dielectric ceramic r At a resonant frequency temperature coefficient τ of 8.5 f The Qf value (Q is the quality factor, f is the resonance frequency, and Qf is the product of the quality factor Q and the resonance frequency f) was 38000GHz at +1.5ppm/. Degree.C.
Example 2
The specific steps of this embodiment are as follows:
(1) Preparing composite powder: at a molar ratio of [ 2.0.86]：[2*0.86-2*0*0.86]：[0.86]：[0.05-0.05*0.86]：[1-0.05-0.86+0.05*0.86]：[1-0.86]Respectively weighing ZnO, mgO, siO with purity of more than 99.5% 2 、SrCO 3 、CaCO 3 、TiO 2 Ball milling the powder in a high-speed ball mill, fully mixing, drying, grinding, and presintering at high temperature to obtain (Mg) 2 SiO 4 ) 0.86 -(Sr 0.05 Ca 0.95 TiO 3 ) 0.14 The presintering temperature is 850 ℃, and the presintering time is 2 hours.
(2) Preparing ceramic powder: 0.1% by weight (i.e., 0.1% by weight) of rare metal oxide CeO was added to the composite powder 2 And (3) performing secondary ball milling in a high-speed ball mill, adding an adhesive accounting for 10% of the weight of the composite powder, and granulating to obtain the ceramic powder. The ceramic powder has a composition of (Mg 2 SiO 4 ) 0.86 -(Sr 0.05 Ca 0.95 TiO 3 ) 0.14 +0.1wt％CeO 2 . The binder is polyvinyl alcohol (PVA).
(3) Blank manufacturing: adding a release agent accounting for 3 percent of the weight of the composite powder into the ceramic powder, then passing through an 80-mesh screen, and pressing into a cylindrical ceramic blank on a press. It will be appreciated that the shape of the blank may also be other. The release agent is zinc stearate.
(4) Sintering and forming: sintering the pressed ceramic blank at high temperature into porcelain to obtain the microwave dielectric ceramic, wherein the high-temperature sintering temperature is 1090 ℃ and the sintering time is 4.5 hours. The dielectric constant epsilon of the microwave dielectric ceramic r At a resonant frequency temperature coefficient τ of 8.4 f The Qf value was 35500GHz at +3.5 ppm/. Degree.C.
Example 3
The specific steps of this embodiment are as follows:
(1) Preparing composite powder: at a molar ratio of [ 2.0.86]：[2*0.86-2*0*0.86]：[0.86]：[0-0*0.86]：[1-0-0.86+0*0.86]：[1-0.86]Respectively weighing ZnO, mgO, siO with purity of more than 99.5% 2 、SrCO 3 、CaCO 3 、TiO 2 Ball milling the powder in a high-speed ball mill, fully mixing, drying, grinding, and presintering at high temperature to obtain (Mg) 2 SiO 4 ) 0.86 -(CaTiO 3 ) 0.14 The presintering temperature is 900 ℃ and the presintering time is 2.5 hours.
(2) Preparing ceramic powder: 0.3% by weight (i.e., 0.3% by weight) of rare metal oxide CeO was added to the composite powder 2 And (3) performing secondary ball milling in a high-speed ball mill, adding an adhesive accounting for 8% of the weight of the composite powder, and granulating to obtain the ceramic powder. The ceramic powder has a composition of (Mg 2 SiO 4 ) 0.86 -(CaTiO 3 ) 0.14 +0.3wt％CeO 2 . The binder is polyvinyl alcohol (PVA).
(3) Blank manufacturing: adding a release agent accounting for 1 percent of the weight of the composite powder into the ceramic powder, then passing through an 80-mesh screen, and pressing into a cylindrical ceramic blank on a press. It will be appreciated that the shape of the blank may also be other. The release agent is magnesium stearate.
(4) Sintering and forming: sintering the pressed ceramic blank into porcelain at high temperature to obtain the microwave dielectric ceramic, wherein the high-temperature sintering temperature is 1050 ℃, and the sintering time is 5 hours. The dielectric constant epsilon of the microwave dielectric ceramic r At a resonant frequency temperature coefficient τ of 8.4 f The Qf value was 38000GHz at +0.5 ppm/. Degree.C.
Example 4
The specific steps of this embodiment are as follows:
(1) Preparing composite powder: at a molar ratio of [ 2.0.5.0.86]：[2*0.86-2*0.5*0.86]：[0.86]：[0-0*0.86]：[1-0-0.86+0*0.86]：[1-0.86]Respectively weighing ZnO, mgO, siO with purity of more than 99.5% 2 、SrCO 3 、CaCO 3 、TiO 2 Ball milling the powder in a high-speed ball mill, fully mixing, drying and grinding, and presintering at high temperature to obtain [ (Zn) 0.5 Mg 0.5 ) 2 SiO 4 ] 0.86 -(CaTiO 3 ) 0.14 The composite powder has presintering temperature of 850 deg.c and presintering period of 2 hr。
(2) Preparing ceramic powder: 0.2% by weight (i.e., 0.2% by weight) of rare metal oxide CeO was added to the composite powder 2 And (3) performing secondary ball milling in a high-speed ball mill, adding an adhesive accounting for 8% of the weight of the composite powder, and granulating to obtain the ceramic powder. The ceramic powder has the composition of [ (Zn) 0.5 Mg 0.5 ) 2 SiO 4 ] 0.86 -(CaTiO 3 ) 0.14 +0.2wt％CeO 2 . The binder is polyvinyl alcohol (PVA).
(3) Blank manufacturing: adding a release agent accounting for 5 percent of the weight of the composite powder into the ceramic powder, then passing through an 80-mesh screen, and pressing into a cylindrical ceramic blank on a press. It will be appreciated that the shape of the blank may also be other. The release agent is calcium stearate.
(4) Sintering and forming: sintering the pressed ceramic blank into porcelain at high temperature to obtain the microwave dielectric ceramic, wherein the high-temperature sintering temperature is 1080 ℃ and the sintering time is 4 hours. The dielectric constant epsilon of the microwave dielectric ceramic r At a resonant frequency temperature coefficient τ of 8.5 f The Qf value was 38500GHz at +4ppm/. Degree.C.
Example 5
The specific steps of this embodiment are as follows:
(1) Preparing composite powder: at a molar ratio of [ 2.0.5.0.83]：[2*0.83-2*0.5*0.83]：[0.83]：[0.05-0.05*0.83]：[1-0.05-0.83+0.05*0.83]：[1-0.83]Respectively weighing ZnO, mgO, siO with purity of more than 99.5% 2 、SrCO 3 、CaCO 3 、TiO 2 Ball milling the powder in a high-speed ball mill, fully mixing, drying and grinding, and presintering at high temperature to obtain [ (Zn) 0.5 Mg 0.5 ) 2 SiO 4 ] 0.83 -(Sr 0.05 Ca 0.95 TiO 3 ) 0.17 The presintering temperature is 850 ℃, and the presintering time is 2 hours.
(2) Preparing ceramic powder: 0.1% by weight (i.e., 0.1% by weight) of rare metal oxide CeO was added to the composite powder 2 Secondary ball milling in a high-speed ball mill, and adding bonding of 8% of the weight of the composite powderGranulating after the preparation to obtain ceramic powder. The ceramic powder has the composition of [ (Zn) 0.5 Mg 0.5 ) 2 SiO 4 ] 0.83 -(Sr 0.05 Ca 0.95 TiO 3 ) 0.17 +0.1wt％CeO 2 . The binder is polyvinyl alcohol (PVA).
(3) Blank manufacturing: adding a release agent accounting for 3 percent of the weight of the composite powder into the ceramic powder, then passing through an 80-mesh screen, and pressing into a cylindrical ceramic blank on a press. It will be appreciated that the shape of the blank may also be other. The release agent is calcium stearate.
(4) Sintering and forming: sintering the pressed ceramic blank at high temperature into porcelain to obtain the microwave dielectric ceramic, wherein the high-temperature sintering temperature is 1090 ℃ and the sintering time is 4 hours. The dielectric constant epsilon of the microwave dielectric ceramic r At 9.0, resonant frequency temperature coefficient τ f The Qf value was 37000GHz at +16 ppm/. Degree.C.
Example 6
The specific steps of this embodiment are as follows:
(1) Preparing composite powder: at a molar ratio of [ 2.0.5.0.89]：[2*0.89-2*0.5*0.89]：[0.89]：[0.05-0.05*0.89]：[1-0.05-0.89+0.05*0.89]：[1-0.89]Respectively weighing ZnO, mgO, siO with purity of more than 99.5% 2 、SrCO 3 、CaCO 3 、TiO 2 Ball milling the powder in a high-speed ball mill, fully mixing, drying and grinding, and presintering at high temperature to obtain [ (Zn) 0.5 Mg 0.5 ) 2 SiO 4 ] 0.89 -(Sr 0.05 Ca 0.95 TiO 3 ) 0.11 The presintering temperature is 850 ℃, and the presintering time is 2 hours.
(2) Preparing ceramic powder: 0.1% by weight (i.e., 0.1% by weight) of rare metal oxide CeO was added to the composite powder 2 And (3) performing secondary ball milling in a high-speed ball mill, adding an adhesive accounting for 6% of the weight of the composite powder, and granulating to obtain the ceramic powder. The ceramic powder has the composition of [ (Zn) 0.5 Mg 0.5 ) 2 SiO 4 ] 0.89 -(Sr 0.05 Ca 0.95 TiO 3 ) 0.11 +0.1wt％CeO 2 . The binder is polyvinyl alcohol (PVA).
(3) Blank manufacturing: adding a release agent accounting for 2 percent of the weight of the composite powder into the ceramic powder, then passing through an 80-mesh screen, and pressing into a cylindrical ceramic blank on a press. It will be appreciated that the shape of the blank may also be other. The release agent is calcium stearate.
(4) Sintering and forming: sintering the pressed ceramic blank at high temperature into porcelain to obtain the microwave dielectric ceramic, wherein the high-temperature sintering temperature is 1090 ℃ and the sintering time is 4 hours. The dielectric constant epsilon of the microwave dielectric ceramic r At a resonant frequency temperature coefficient τ of 8.1 f The Qf value was 40000GHz at-15 ppm/. Degree.C.
Example 7
The specific steps of this embodiment are as follows:
(1) Preparing composite powder: at a molar ratio of [ 2.0.5.0.86]：[2*0.86-2*0.5*0.86]：[0.86]：[0.05-0.05*0.86]：[1-0.05-0.86+0.05*0.86]：[1-0.86]Respectively weighing ZnO, mgO, siO with purity of more than 99.5% 2 、SrCO 3 、CaCO 3 、TiO 2 Ball milling the powder in a high-speed ball mill, fully mixing, drying and grinding, and presintering at high temperature to obtain [ (Zn) 0.5 Mg 0.5 ) 2 SiO 4 ] 0.86 -(Sr 0.05 Ca 0.95 TiO 3 ) 0.14 The presintering temperature is 850 ℃, and the presintering time is 2 hours.
(2) Preparing ceramic powder: adding 0.1% by weight (i.e., 0.1% by weight) of rare metal oxide Nb to the composite powder 2 O 5 And (3) performing secondary ball milling in a high-speed ball mill, adding an adhesive accounting for 8% of the weight of the composite powder, and granulating to obtain the ceramic powder. The ceramic powder has the composition of [ (Zn) 0.5 Mg 0.5 ) 2 SiO 4 ] 0.86 -(Sr 0.05 Ca 0.95 TiO 3 ) 0.14 +0.1wt％Nb 2 O 5 . The binder is polyvinyl alcohol (PVA).
(3) Blank manufacturing: adding a release agent accounting for 3 percent of the weight of the composite powder into the ceramic powder, then passing through an 80-mesh screen, and pressing into a cylindrical ceramic blank on a press. It will be appreciated that the shape of the blank may also be other. The release agent is calcium stearate.
(4) Sintering and forming: sintering the pressed ceramic blank at high temperature into porcelain to obtain the microwave dielectric ceramic, wherein the high-temperature sintering temperature is 1090 ℃ and the sintering time is 4 hours. The dielectric constant epsilon of the microwave dielectric ceramic r At a resonant frequency temperature coefficient τ of 8.5 f The Qf value was 38500GHz at +1ppm/. Degree.C.
Example 8
The specific steps of this embodiment are as follows:
(1) Preparing composite powder: at a molar ratio of [ 2.0.5.0.86]：[2*0.86-2*0.5*0.86]：[0.86]：[0.05-0.05*0.86]：[1-0.05-0.86+0.05*0.86]：[1-0.86]Respectively weighing ZnO, mgO, siO with purity of more than 99.5% 2 、SrCO 3 、CaCO 3 、TiO 2 Ball milling the powder in a high-speed ball mill, fully mixing, drying and grinding, and presintering at high temperature to obtain [ (Zn) 0.5 Mg 0.5 ) 2 SiO 4 ] 0.86 -(Sr 0.05 Ca 0.95 TiO 3 ) 0.14 The presintering temperature is 850 ℃, and the presintering time is 2 hours.
(2) Preparing ceramic powder: adding 0.2% by weight (i.e., 0.2% by weight) of rare metal oxide Nb to the composite powder 2 O 5 And 0.1wt% of rare metal oxide Ta 2 O 5 And (3) performing secondary ball milling in a high-speed ball mill, adding an adhesive accounting for 8% of the weight of the composite powder, and granulating to obtain the ceramic powder. The ceramic powder has the composition of [ (Zn) 0.5 Mg 0.5 ) 2 SiO 4 ] 0.86 -(Sr 0.05 Ca 0.95 TiO 3 ) 0.14 +0.2wt％Nb 2 O 5 +0.1wt％Ta 2 O 5 . The binder is polyvinyl alcohol (PVA).
(3) Blank manufacturing: adding a release agent accounting for 3 percent of the weight of the composite powder into the ceramic powder, then passing through an 80-mesh screen, and pressing into a cylindrical ceramic blank on a press. It will be appreciated that the shape of the blank may also be other. The release agent is calcium stearate.
(4) Sintering and forming: sintering the pressed ceramic blank into porcelain at high temperature to obtain the microwave dielectric ceramic, wherein the high-temperature sintering temperature is 1060 ℃, and the sintering time is 4 hours. The dielectric constant epsilon of the microwave dielectric ceramic r At a resonant frequency temperature coefficient τ of 8.5 f The Qf value was 39500GHz at +1.5 ppm/. Degree.C.
Example 9
The specific steps of this embodiment are as follows:
(1) Preparing composite powder: at a molar ratio of [ 2.0.5.0.86]：[2*0.86-2*0.5*0.86]：[0.86]：[0.05-0.05*0.86]：[1-0.05-0.86+0.05*0.86]：[1-0.86]Respectively weighing ZnO, mgO, siO with purity of more than 99.5% 2 、SrCO 3 、CaCO 3 、TiO 2 Ball milling the powder in a high-speed ball mill, fully mixing, drying and grinding, and presintering at high temperature to obtain [ (Zn) 0.5 Mg 0.5 ) 2 SiO 4 ] 0.86 -(Sr 0.05 Ca 0.95 TiO 3 ) 0.14 The presintering temperature is 850 ℃, and the presintering time is 2 hours.
(2) Preparing ceramic powder: 0.2% by weight (i.e., 0.2% by weight) of rare metal oxide CeO was added to the composite powder 2 And 0.1wt% of rare metal oxide Ta 2 O 5 And (3) performing secondary ball milling in a high-speed ball mill, adding an adhesive accounting for 8% of the weight of the composite powder, and granulating to obtain the ceramic powder. The ceramic powder has the composition of [ (Zn) 0.5 Mg 0.5 ) 2 SiO 4 ] 0.86 -(Sr 0.05 Ca 0.95 TiO 3 ) 0.14 +0.2wt％CeO 2 +0.1wt％Ta 2 O 5 . The binder is polyvinyl alcohol (PVA).
(3) Blank manufacturing: adding a release agent accounting for 3 percent of the weight of the composite powder into the ceramic powder, then passing through an 80-mesh screen, and pressing into a cylindrical ceramic blank on a press. It will be appreciated that the shape of the blank may also be other. The release agent is calcium stearate.
(4) Sintering and forming: sintering the pressed ceramic blank into porcelain at high temperature to obtain the microwave dielectric ceramic, wherein the high-temperature sintering temperature is 1060 ℃, and the sintering time is 4 hours. The dielectric constant epsilon of the microwave dielectric ceramic r At a resonant frequency temperature coefficient τ of 8.4 f The Qf value was 39000GHz at-0.5 ppm/. Degree.C.
Example 10
The specific steps of this embodiment are as follows:
(1) Preparing composite powder: at a molar ratio of [ 2.0.5.0.86]：[2*0.86-2*0.5*0.86]：[0.86]：[0.05-0.05*0.86]：[1-0.05-0.86+0.05*0.86]：[1-0.86]Respectively weighing ZnO, mgO, siO with purity of more than 99.5% 2 、SrCO 3 、CaCO 3 、TiO 2 Ball milling the powder in a high-speed ball mill, fully mixing, drying and grinding, and presintering at high temperature to obtain [ (Zn) 0.5 Mg 0.5 ) 2 SiO 4 ] 0.86 -(Sr 0.05 Ca 0.95 TiO 3 ) 0.14 The presintering temperature is 850 ℃, and the presintering time is 2 hours.
(2) Preparing ceramic powder: 0.1% by weight (i.e., 0.1% by weight) of rare metal oxide CeO was added to the composite powder 2 0.1wt% of rare metal oxide Ta 2 O 5 And 0.1wt% of rare metal oxide Nb 2 O 5 And (3) performing secondary ball milling in a high-speed ball mill, adding an adhesive accounting for 8% of the weight of the composite powder, and granulating to obtain the ceramic powder. The ceramic powder has the composition of [ (Zn) 0.5 Mg 0.5 ) 2 SiO 4 ] 0.86 -(Sr 0.05 Ca 0.95 TiO 3 ) 0.14 +0.1wt％CeO 2 +0.1wt％Ta 2 O 5 +0.1wt％
Nb 2 O 5 . The binder is polyvinyl alcohol (PVA).
(3) Blank manufacturing: adding a release agent accounting for 3 percent of the weight of the composite powder into the ceramic powder, then passing through an 80-mesh screen, and pressing into a cylindrical ceramic blank on a press. It will be appreciated that the shape of the blank may also be other. The release agent is calcium stearate.
(4) Sintering and forming: sintering the pressed ceramic blank into porcelain at high temperature to obtain the microwave dielectric ceramic, wherein the high-temperature sintering temperature is 1050 ℃, and the sintering time is 4 hours. The dielectric constant epsilon of the microwave dielectric ceramic r At a resonant frequency temperature coefficient τ of 8.6 f The Qf value was 38500GHz at-1 ppm/. Degree.C.
Example 11
The specific steps of this embodiment are as follows:
(1) Preparing composite powder: at a molar ratio of [ 2.1.0.75]：[2*0.75-2*1*0.75]：[0.75]：[0.2-0.2*0.75]：[1-0.2-0.75+0.2*0.75]：[1-0.75]Respectively weighing ZnO, mgO, siO with purity of more than 99.5% 2 、SrCO 3 、CaCO 3 、TiO 2 Ball milling the powder in a high-speed ball mill, fully mixing, drying, grinding, and presintering at high temperature to obtain (Zn) 2 SiO 4 ) 0.75 -(Sr 0.2 Ca 0.8 TiO 3 ) 0.25 The presintering temperature is 850 ℃, and the presintering time is 2 hours.
(2) Preparing ceramic powder: adding 0.1% by weight (i.e., 0.1% by weight) of rare metal oxide Ta to the composite powder 2 O 5 And (3) performing secondary ball milling in a high-speed ball mill, adding an adhesive accounting for 8% of the weight of the composite powder, and granulating to obtain the ceramic powder. The ceramic powder has a composition of (Zn) 2 SiO 4 ) 0.75 -(Sr 0.2 Ca 0.8 TiO 3 ) 0.25 +0.1wt％Ta 2 O 5 . The binder is polyvinyl alcohol (PVA).
(3) Blank manufacturing: adding a release agent accounting for 3 percent of the weight of the composite powder into the ceramic powder, then passing through an 80-mesh screen, and pressing into a cylindrical ceramic blank on a press. It will be appreciated that the shape of the blank may also be other. The release agent is calcium stearate.
(4) Sintering and forming: sintering the pressed ceramic blank into porcelain at high temperature to obtain the microwave dielectric ceramic, wherein the high-temperature sintering temperature is 1100 ℃ and the sintering time is 4 hours. The dielectric constant epsilon of the microwave dielectric ceramic r At a temperature coefficient of resonance frequency τ of 8.9 f The Qf value was 35000GHz at +20 ppm/. Degree.C.
Example 12
The specific steps of this embodiment are as follows:
(1) Preparing composite powder: at a molar ratio of [ 2.1.0.95]：[2*0.95-2*1*0.95]：[0.95]：[0.2-0.2*0.95]：[1-0.2-0.95+0.2*0.95]：[1-0.95]Respectively weighing ZnO, mgO, siO with purity of more than 99.5% 2 、SrCO 3 、CaCO 3 、TiO 2 Ball milling the powder in a high-speed ball mill, fully mixing, drying, grinding, and presintering at high temperature to obtain (Zn) 2 SiO 4 ) 0.95 -(Sr 0.2 Ca 0.8 TiO 3 ) 0.05 The presintering temperature is 850 ℃, and the presintering time is 2 hours.
(2) Preparing ceramic powder: adding 0.2% by weight (i.e., 0.2% by weight) of rare metal oxide Ta to the composite powder 2 O 5 And (3) performing secondary ball milling in a high-speed ball mill, adding an adhesive accounting for 8% of the weight of the composite powder, and granulating to obtain the ceramic powder. The ceramic powder has a composition of (Zn) 2 SiO 4 ) 0.95 -(Sr 0.2 Ca 0.8 TiO 3 ) 0.05 +0.2wt％Ta 2 O 5 . The binder is polyvinyl alcohol (PVA).
(3) Blank manufacturing: adding a release agent accounting for 3 percent of the weight of the composite powder into the ceramic powder, then passing through an 80-mesh screen, and pressing into a cylindrical ceramic blank on a press. It will be appreciated that the shape of the blank may also be other. The release agent is calcium stearate.
(4) Sintering and forming: sintering the pressed ceramic blank into porcelain at high temperature to obtain the microwave dielectric ceramic, wherein the high-temperature sintering temperature is 1100 ℃, and the sintering time is 4 hours. The dielectric constant epsilon of the microwave dielectric ceramic r At a temperature coefficient of resonance frequency τ of 8.0 f The Qf value was 40000GHz at-15 ppm/. Degree.C.
Example 13
The specific steps of this embodiment are as follows:
(1) Preparing composite powder: at a molar ratio of [ 2.0.5.0.86]：[2*0.86-2*0.5*0.86]：[0.86]：[0.05-0.05*0.86]：[1-0.05-0.86+0.05*0.86]：[1-0.86]Respectively weighing ZnO, mgO, siO with purity of more than 99.5% 2 、SrCO 3 、CaCO 3 、TiO 2 Ball milling the powder in a high-speed ball mill, fully mixing, drying and grinding, and presintering at high temperature to obtain [ (Zn) 0.5 Mg 0.5 ) 2 SiO 4 ] 0.86 -(Sr 0.05 Ca 0.95 TiO 3 ) 0.14 The presintering temperature is 850 ℃, and the presintering time is 2 hours.
(2) Preparing ceramic powder: adding 0.1% by weight (i.e., 0.1% by weight) of rare metal oxide Ta to the composite powder 2 O 5 And (3) performing secondary ball milling in a high-speed ball mill, adding an adhesive accounting for 8% of the weight of the composite powder, and granulating to obtain the ceramic powder. The ceramic powder has the composition of [ (Zn) 0.5 Mg 0.5 ) 2 SiO 4 ] 0.86 -(Sr 0.05 Ca 0.95 TiO 3 ) 0.14 +0.1wt％Ta 2 O 5 . The binder is polyvinyl alcohol (PVA).
(3) Blank manufacturing: adding a release agent accounting for 3 percent of the weight of the composite powder into the ceramic powder, then passing through an 80-mesh screen, and pressing into a cylindrical ceramic blank on a press. It will be appreciated that the shape of the blank may also be other. The release agent is calcium stearate.
(4) Sintering and forming: sintering the pressed ceramic blank into porcelain at high temperature to obtain the microwave dielectric ceramic, wherein the high-temperature sintering temperature is 1070 ℃ and the sintering time is 4 hours. The dielectric constant epsilon of the microwave dielectric ceramic r At a resonant frequency temperature coefficient τ of 8.5 f The Qf value was 38500GHz at +0.5 ppm/. Degree.C.
Example 14
The specific steps of this embodiment are as follows:
(1) Preparing composite powder: at a molar ratio of [ 2.0.5.0.86]：[2*0.86-2*0.5*0.86]：[0.86]：[0.05-0.05*0.86]：[1-0.05-0.86+0.05*0.86]：[1-0.86]Respectively weighing ZnO, mgO, siO with purity of more than 99.5% 2 、SrCO 3 、CaCO 3 、TiO 2 Ball milling the powder in a high-speed ball mill, fully mixing, drying and grinding, and presintering at high temperature to obtain [ (Zn) 0.5 Mg 0.5 ) 2 SiO 4 ] 0.86 -(Sr 0.05 Ca 0.95 TiO 3 ) 0.14 The presintering temperature is 850 ℃, and the presintering time is 2 hours.
(2) Preparing ceramic powder: adding 0.1% by weight (i.e., 0.1% by weight) of rare metal oxide Nb to the composite powder 2 O 5 And 0.1wt% of rare metal oxide CeO 2 And (3) performing secondary ball milling in a high-speed ball mill, adding an adhesive accounting for 8% of the weight of the composite powder, and granulating to obtain the ceramic powder. The ceramic powder has the composition of [ (Zn) 0.5 Mg 0.5 ) 2 SiO 4 ] 0.86 -(Sr 0.05 Ca 0.95 TiO 3 ) 0.14 +0.1wt％Nb 2 O 5 +0.1wt％CeO 2 . The binder is polyvinyl alcohol (PVA).
(3) Blank manufacturing: adding a release agent accounting for 3 percent of the weight of the composite powder into the ceramic powder, then passing through an 80-mesh screen, and pressing into a cylindrical ceramic blank on a press. It will be appreciated that the shape of the blank may also be other. The release agent is calcium stearate.
(4) Sintering and forming: sintering the pressed ceramic blank at high temperature into porcelain to obtain the microwave dielectric ceramic, wherein the high-temperature sintering temperature is 1075 ℃ and the sintering time is 4 hours. The dielectric constant epsilon of the microwave dielectric ceramic r At a resonant frequency temperature coefficient τ of 8.5 f The Qf value was 38000GHz at +0.5 ppm/. Degree.C.
Table 1 shows the microwave dielectric ceramic composition, sintering temperature, dielectric constant ε of several embodiments of the invention r Temperature coefficient of resonant frequency τ f Qf value, composition of the existing microwave dielectric ceramic, sintering temperature, dielectric constant epsilon r Temperature coefficient of resonant frequency τ f Qf value.
TABLE 1
As can be seen from Table 1, the microwave dielectric ceramic of the present invention can be prepared at a lower sintering temperature, and has a larger sintering window, i.e., good stability of performance with fluctuation of sintering temperature, a higher Qf value, and a better microwave dielectric property, dielectric constant ε r Is 8.0-9.0, and the resonant frequency temperature coefficient tau f At-15 to +20ppm/DEG C, qf value of 35000-40000 GHz, resonant frequency temperature coefficient tau f Can be adjusted according to the requirement, and the resonant frequency temperature coefficient tau f The adjustable range is wide.
The foregoing examples illustrate only a few embodiments of the invention and are described in detail herein without thereby limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (5)
1. The low-dielectric-constant microwave dielectric ceramic is characterized by comprising the following components in parts by weight:
100 parts of titanate silicate complex
0.1 parts of rare metal oxide;
the titanate silicate complex is [ (Zn) prepared by presintering at 850 ℃ for 2 hours x Mg 1-x ) 2 SiO 4 ] z -(Sr y Ca 1-y TiO 3 ) 1-z The method comprises the steps of carrying out a first treatment on the surface of the The rare metal oxide is Nb 2 O 5 ；
Wherein x=0.5, y=0.05, and z=0.86.
2. The microwave dielectric ceramic of claim 1, having a dielectric constant of 8.5, a temperature coefficient of resonance frequency of +1ppm/°c, and a Qf value of 38500GHz.
3. The method for preparing the low-dielectric-constant microwave dielectric ceramic according to claim 1, which comprises the following steps:
preparing composite powder: in a molar ratio of [2xz ]]：[2z-2xz]：[z]：[y-yz]：[1-y-z+yz]：[1-z]Respectively weighing ZnO, mgO, siO with purity of more than 99.5% 2 、SrCO 3 、CaCO 3 、TiO 2 Ball milling the powder, fully mixing, drying and grinding, and presintering at 800-900 ℃ for 1.8-2.5 hours to obtain [ (Zn) x Mg 1-x ) 2 SiO 4 ] z -(Sr y Ca 1- y TiO 3 ) 1-z A composite powder;
preparing ceramic powder: adding 0.1% by weight of rare metal oxide Nb to the composite powder 2 O 5 Performing secondary ball milling, adding a binder, and granulating to obtain ceramic powder;
blank manufacturing: adding a release agent into the ceramic powder, sieving, and pressing into a ceramic blank on a pressing machine;
sintering and forming: sintering the pressed ceramic blank into porcelain at a high-temperature sintering temperature of 1090 ℃ for 4 hours to obtain the ceramic;
wherein x=0.5, y=0.05, and z=0.86.
4. The method according to claim 3, wherein the binder is polyvinyl alcohol and the amount of the binder added is 8% by weight of the composite powder.
5. The method according to claim 3, wherein the release agent is calcium stearate and the amount added is 3% by weight of the composite powder.
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