CN112830775A - Low-dielectric-constant microwave dielectric ceramic and preparation method thereof - Google Patents

Low-dielectric-constant microwave dielectric ceramic and preparation method thereof Download PDF

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CN112830775A
CN112830775A CN202110224129.0A CN202110224129A CN112830775A CN 112830775 A CN112830775 A CN 112830775A CN 202110224129 A CN202110224129 A CN 202110224129A CN 112830775 A CN112830775 A CN 112830775A
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CN112830775B (en
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周星星
盘耀东
吴成旺
王斌
谭伟能
陈明贵
郑酬
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Shenzhen Guoren Technology Co ltd
Nanning Guoren Radio Frequency Communication Co ltd
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Nanning Guoren Radio Frequency Communication Co ltd
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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 0.1-0.3 part of rare metal oxide; the titanate silicate complex is [ (Zn)xMg1‑x)2SiO4]z‑(SryCa1‑yTiO3)1‑z(ii) a The rare metal oxide is CeO2、Nb2O5And/or Ta2O5(ii) a 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, and z is more than or equal to 0.75 and less than or equal to 0.95. The microwave dielectric ceramic can be prepared at a lower sintering temperature, the sintering window is larger, namely the stability of the performance is good when the performance fluctuates along with the sintering temperature, the Qf value is higher, the frequency temperature coefficient is adjustable, and the preparation method is used for preparing the microwave dielectric ceramicThe process is simple, and large-scale mass production can be realized.

Description

Low-dielectric-constant microwave dielectric ceramic and preparation method thereof
[ technical field ] A method for producing a semiconductor device
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 of the invention ]
The dielectric filter is composed of microwave dielectric ceramic materials, and the microwave dielectric ceramic materials are used as key materials in modern communication and can be applied to microwave frequency band circuits as dielectric materials.
In the existing low-dielectric-constant microwave dielectric ceramic materials, Mg2SiO4/Zn2SiO4 series silicate microwave ceramics are widely applied, have low dielectric loss at very high microwave frequency and are negative frequency temperature coefficient materials, the frequency temperature coefficient of the composite material can be adjusted to be nearly zero by adding a positive frequency temperature coefficient material, and the low-dielectric-constant microwave dielectric ceramic material is a typical low-dielectric-constant material which is researched more and is mature. However, the severe sintering temperature makes the material difficult to sinter, the sintering window is generally only within 20 ℃, which is very unfavorable for large-scale mass production, and the dielectric property of the material is also deteriorated due to the easy volatilization of Zn in the high-temperature sintering process. And the material is fixed and not easily adjustable given the frequency temperature coefficient requirements.
Therefore, there is a need for an improved low dielectric constant microwave dielectric ceramic and a method for preparing the same.
[ summary of the invention ]
The invention mainly aims to provide a low-dielectric-constant microwave dielectric ceramic and a preparation method thereof, which can realize preparation at a lower sintering temperature, have a larger sintering window, namely have good stability when the performance fluctuates along with the sintering temperature, have a higher Qf value and an adjustable frequency temperature coefficient, have a simple preparation process and can realize large-scale mass production.
In order to achieve the above object, a first aspect of the present invention provides a low dielectric constant microwave dielectric ceramic, comprising the following components in parts by weight: 100 parts of titanate silicate complex and 0.1-0.3 part of rare metal oxide; the titanate silicate complex is [ (Zn)xMg1-x)2SiO4]z-(SryCa1-yTiO3)1-z(ii) a The rare metal oxide is CeO2、Nb2O5And/or Ta2O5(ii) a 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, and z is more than or equal to 0.75 and less than or equal to 0.95.
Preferably, the dielectric constant is 8.0 to 9.0, the temperature coefficient of the resonance frequency is-15 to +20 ppm/DEG C, and the Qf value is 35000 to 40000 GHz.
The second aspect of the present invention provides a method for preparing a low dielectric constant microwave dielectric ceramic, comprising the following steps: preparing composite powder: in molar ratio of [2xz ]]：[2z-2xz]：[z]：[y-yz]：[1-y-z+yz]：[1-z]Respectively weighing ZnO, MgO and SiO with the purity of more than 99.5 percent2、SrCO3、CaCO3、TiO2Ball milling, mixing, stoving, grinding and high temperature pre-sintering to obtain [ (Zn)xMg1-x)2SiO4]z-(SryCa1-yTiO3)1-zComposite powder; preparing ceramic powder: adding 0.1-0.3% by weight of rare metal oxide into the composite powder, performing secondary ball milling, adding a binder, and granulating to obtain ceramic powder; blank preparation: adding a release agent into the ceramic powder, sieving, and pressing into a ceramic green body on a pressing machine; sintering and forming: sintering the ceramic blank formed by pressing at high temperature into ceramic to obtain the ceramic; 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, and z is more than or equal to 0.75 and less than or equal to 0.95; the rare metal oxide is CeO2、Nb2O5And/or Ta2O5。
Preferably, the binder is polyvinyl alcohol, and the addition amount of the binder is 5-10% of the weight of the composite powder.
Preferably, the release agent is calcium stearate, zinc stearate or magnesium stearate, and the addition amount of the release agent is 1-5% of the weight of the composite powder.
According to the preferable technical scheme, the pre-sintering temperature is 800-900 ℃, and the pre-sintering time is 1.8-2.5 hours.
According to the 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 adopts ZnO, MgO and SiO2、SrCO3、CaCO3、TiO2The powder is combined and solid-dissolved to form titanate silicate complex [ (Zn)xMg1-x)2SiO4]z-(SryCa1-yTiO3)1-zThen through a rare metal oxide (CeO)2、Nb2O5And/or Ta2O5) The doping can realize preparation 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, large-scale mass production can be realized, meanwhile, the Qf value is higher, better microwave dielectric property can be obtained, and the temperature coefficient of the resonant frequency can be adjusted as required.
[ detailed description ] embodiments
The present invention will be further described with reference to the following examples.
The microwave dielectric ceramic with the low dielectric constant provided by the embodiment comprises the following components in parts by weight: 100 parts of titanate silicate complex and 0.1-0.3 part of rare metal oxide. The titanate silicate complex is [ (Zn)xMg1-x)2SiO4]z-(SryCa1-yTiO3)1-z. The rare metal oxide is CeO2、Nb2O5And/or Ta2O5. 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, and z is more than or equal to 0.75 and less 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 example are as follows:
(1) preparing composite powder: according to molar ratio [2X 0.5X 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 and SiO with the purity of more than 99.5 percent2、SrCO3、CaCO3、TiO2Ball-milling the powder in a high-speed ball mill, fully mixing, drying, grinding, and presintering at high temperature to obtain [ (Zn)0.5Mg0.5)2SiO4]0.86-(Sr0.05Ca0.95TiO3)0.14And (3) composite powder, wherein 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 powder2And performing secondary ball milling in a high-speed ball mill, adding a bonding agent accounting for 5 percent (namely 5 percent by weight) of the weight of the composite powder, and granulating to obtain the ceramic powder. The composition of the ceramic powder is [ (Zn)0.5Mg0.5)2SiO4]0.86-(Sr0.05Ca0.95TiO3)0.14+0.2wt％CeO2. The binder is polyvinyl alcohol (PVA).
(3) Blank preparation: adding a release agent accounting for 3 percent (namely 3 percent by weight) of the weight of the composite powder into the ceramic powder, then sieving the mixture by a 80-mesh sieve, and pressing the mixture on a press to form a cylindrical ceramic green body. It will be appreciated that the shape of the blank may also be other. The release agent is calcium stearate.
(4) Sintering and forming: and sintering the ceramic blank formed by pressing at a high temperature into a ceramic 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 ceramicrIs 8.5, temperature coefficient of resonance frequency taufIs +1.5 ppm/DEG C, and has a Qf value (Q is a quality factor, f is a resonance frequency, and Qf is a product of the quality factor Q and the resonance frequency f) of 38000GHz。
Example 2
The specific steps of this example are as follows:
(1) preparing composite powder: according to molar ratio [2x 0 x 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 and SiO with the purity of more than 99.5 percent2、SrCO3、CaCO3、TiO2Ball milling the powder in a high-speed ball mill, fully mixing, drying, grinding, and presintering at high temperature to obtain (Mg)2SiO4)0.86-(Sr0.05Ca0.95TiO3)0.14And (3) composite powder, wherein 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 powder2And performing secondary ball milling in a high-speed ball mill, adding a bonding agent accounting for 10 percent of the weight of the composite powder, and granulating to obtain the ceramic powder. The composition of the ceramic powder is (Mg)2SiO4)0.86-(Sr0.05Ca0.95TiO3)0.14+0.1wt％CeO2. The binder is polyvinyl alcohol (PVA).
(3) Blank preparation: adding a release agent accounting for 3 percent of the weight of the composite powder into the ceramic powder, then sieving the mixture by a 80-mesh sieve, and pressing the mixture on a press to form a cylindrical ceramic green body. It will be appreciated that the shape of the blank may also be other. The release agent is zinc stearate.
(4) Sintering and forming: and sintering the ceramic blank formed by pressing at a high temperature into a ceramic 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 ceramicrIs 8.4, temperature coefficient of resonance frequency taufIs +3.5 ppm/DEG C, and the Qf value is 35500 GHz.
Example 3
The specific steps of this example are as follows:
(1) preparing composite powder: according to molar ratio [2x 0 x 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 and SiO with the purity of more than 99.5 percent2、SrCO3、CaCO3、TiO2Ball milling the powder in a high-speed ball mill, fully mixing, drying, grinding, and presintering at high temperature to obtain (Mg)2SiO4)0.86-(CaTiO3)0.14And (3) composite powder, wherein 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 powder2And performing secondary ball milling in a high-speed ball mill, adding a bonding agent accounting for 8 percent of the weight of the composite powder, and granulating to obtain the ceramic powder. The composition of the ceramic powder is (Mg)2SiO4)0.86-(CaTiO3)0.14+0.3wt％CeO2. The binder is polyvinyl alcohol (PVA).
(3) Blank preparation: adding a release agent accounting for 1 percent of the weight of the composite powder into the ceramic powder, then sieving the mixture by a 80-mesh sieve, and pressing the mixture on a press to form a cylindrical ceramic green body. 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 ceramic blank formed by pressing into ceramic 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 ceramicrIs 8.4, temperature coefficient of resonance frequency taufIs +0.5 ppm/DEG C, and the Qf value is 38000 GHz.
Example 4
The specific steps of this example are as follows:
(1) preparing composite powder: according to molar ratio [2X 0.5X 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 and SiO with the purity of more than 99.5 percent2、SrCO3、CaCO3、TiO2Ball-milling the powder in a high-speed ball mill, fully mixing, drying, grinding, and presintering at high temperature to obtain [ (Zn)0.5Mg0.5)2SiO4]0.86-(CaTiO3)0.14And (3) composite powder, wherein 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 powder2And performing secondary ball milling in a high-speed ball mill, and adding an adhesive accounting for 8 percent of the weight of the composite powder for granulation to obtain the ceramic powder. The composition of the ceramic powder is [ (Zn)0.5Mg0.5)2SiO4]0.86-(CaTiO3)0.14+0.2wt％CeO2. The binder is polyvinyl alcohol (PVA).
(3) Blank preparation: adding a release agent accounting for 5 percent of the weight of the composite powder into the ceramic powder, then sieving the mixture by a 80-mesh sieve, and pressing the mixture on a press to form a cylindrical ceramic green body. 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 ceramic blank formed by pressing into ceramic 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 ceramicrIs 8.5, temperature coefficient of resonance frequency taufIs +4 ppm/DEG C, and the Qf value is 38500 GHz.
Example 5
The specific steps of this example are as follows:
(1) preparing composite powder: according to molar ratio [2x 0.5 x 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 and SiO with the purity of more than 99.5 percent2、SrCO3、CaCO3、TiO2Ball-milling the powder in a high-speed ball mill, fully mixing, drying, grinding, and presintering at high temperature to obtain [ (Zn)0.5Mg0.5)2SiO4]0.83-(Sr0.05Ca0.95TiO3)0.17And (3) composite powder, wherein 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 was added to the composite powderCeO2And performing secondary ball milling in a high-speed ball mill, adding a bonding agent accounting for 8 percent of the weight of the composite powder, and granulating to obtain the ceramic powder. The composition of the ceramic powder is [ (Zn)0.5Mg0.5)2SiO4]0.83-(Sr0.05Ca0.95TiO3)0.17+0.1wt％CeO2. The binder is polyvinyl alcohol (PVA).
(3) Blank preparation: adding a release agent accounting for 3 percent of the weight of the composite powder into the ceramic powder, then sieving the mixture by a 80-mesh sieve, and pressing the mixture on a press to form a cylindrical ceramic green body. It will be appreciated that the shape of the blank may also be other. The release agent is calcium stearate.
(4) Sintering and forming: and sintering the ceramic blank formed by pressing at a high temperature into a ceramic 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 ceramicrIs 9.0, temperature coefficient of resonance frequency taufIs +16 ppm/DEG C, and the Qf value is 37000 GHz.
Example 6
The specific steps of this example are as follows:
(1) preparing composite powder: according to molar ratio [2x 0.5 x 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 and SiO with the purity of more than 99.5 percent2、SrCO3、CaCO3、TiO2Ball-milling the powder in a high-speed ball mill, fully mixing, drying, grinding, and presintering at high temperature to obtain [ (Zn)0.5Mg0.5)2SiO4]0.89-(Sr0.05Ca0.95TiO3)0.11And (3) composite powder, wherein 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 powder2And performing secondary ball milling in a high-speed ball mill, adding a binder accounting for 6 percent of the weight of the composite powder, and granulating to obtain the ceramic powder. The composition of the ceramic powder is [ (Zn)0.5Mg0.5)2SiO4]0.89-(Sr0.05Ca0.95TiO3)0.11+0.1wt％CeO2. The binder is polyvinyl alcohol (PVA).
(3) Blank preparation: adding a release agent accounting for 2 percent of the weight of the composite powder into the ceramic powder, then sieving the mixture by a 80-mesh sieve, and pressing the mixture on a press to form a cylindrical ceramic green body. It will be appreciated that the shape of the blank may also be other. The release agent is calcium stearate.
(4) Sintering and forming: and sintering the ceramic blank formed by pressing at a high temperature into a ceramic 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 ceramicrIs 8.1, temperature coefficient of resonance frequency taufIs-15 ppm/DEG C, and the Qf value is 40000 GHz.
Example 7
The specific steps of this example are as follows:
(1) preparing composite powder: according to molar ratio [2X 0.5X 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 and SiO with the purity of more than 99.5 percent2、SrCO3、CaCO3、TiO2Ball-milling the powder in a high-speed ball mill, fully mixing, drying, grinding, and presintering at high temperature to obtain [ (Zn)0.5Mg0.5)2SiO4]0.86-(Sr0.05Ca0.95TiO3)0.14And (3) composite powder, wherein 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 a rare metal oxide Nb is added to the composite powder2O5And performing secondary ball milling in a high-speed ball mill, adding a bonding agent accounting for 8 percent of the weight of the composite powder, and granulating to obtain the ceramic powder. The composition of the ceramic powder is [ (Zn)0.5Mg0.5)2SiO4]0.86-(Sr0.05Ca0.95TiO3)0.14+0.1wt％Nb2O5. The binder is polyvinyl alcohol (PVA).
(3) Blank preparation: adding a release agent accounting for 3 percent of the weight of the composite powder into the ceramic powder, then sieving the mixture by a 80-mesh sieve, and pressing the mixture on a press to form a cylindrical ceramic green body. It will be appreciated that the shape of the blank may also be other. The release agent is calcium stearate.
(4) Sintering and forming: and sintering the ceramic blank formed by pressing at a high temperature into a ceramic 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 ceramicrIs 8.5, temperature coefficient of resonance frequency taufIs +1 ppm/DEG C, and the Qf value is 38500 GHz.
Example 8
The specific steps of this example are as follows:
(1) preparing composite powder: according to molar ratio [2X 0.5X 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 and SiO with the purity of more than 99.5 percent2、SrCO3、CaCO3、TiO2Ball-milling the powder in a high-speed ball mill, fully mixing, drying, grinding, and presintering at high temperature to obtain [ (Zn)0.5Mg0.5)2SiO4]0.86-(Sr0.05Ca0.95TiO3)0.14And (3) composite powder, wherein 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 a rare metal oxide Nb is added to the composite powder2O5And 0.1% by weight of a rare metal oxide Ta2O5And performing secondary ball milling in a high-speed ball mill, adding a bonding agent accounting for 8 percent of the weight of the composite powder, and granulating to obtain the ceramic powder. The composition of the ceramic powder is [ (Zn)0.5Mg0.5)2SiO4]0.86-(Sr0.05Ca0.95TiO3)0.14+0.2wt％Nb2O5+0.1wt％Ta2O5. The binder is polyvinyl alcohol (PVA).
(3) Blank preparation: adding a release agent accounting for 3 percent of the weight of the composite powder into the ceramic powder, then sieving the mixture by a 80-mesh sieve, and pressing the mixture on a press to form a cylindrical ceramic green body. It will be appreciated that the shape of the blank may also be other. The release agent is calcium stearate.
(4) Sintering and forming: and sintering the ceramic blank formed by pressing at a high temperature into ceramic 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 ceramicrIs 8.5, temperature coefficient of resonance frequency taufIs +1.5 ppm/DEG C, and the Qf value is 39500 GHz.
Example 9
The specific steps of this example are as follows:
(1) preparing composite powder: according to molar ratio [2X 0.5X 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 and SiO with the purity of more than 99.5 percent2、SrCO3、CaCO3、TiO2Ball-milling the powder in a high-speed ball mill, fully mixing, drying, grinding, and presintering at high temperature to obtain [ (Zn)0.5Mg0.5)2SiO4]0.86-(Sr0.05Ca0.95TiO3)0.14And (3) composite powder, wherein 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 powder2And 0.1% by weight of a rare metal oxide Ta2O5And performing secondary ball milling in a high-speed ball mill, adding a bonding agent accounting for 8 percent of the weight of the composite powder, and granulating to obtain the ceramic powder. The composition of the ceramic powder is [ (Zn)0.5Mg0.5)2SiO4]0.86-(Sr0.05Ca0.95TiO3)0.14+0.2wt％CeO2+0.1wt％Ta2O5. The binder is polyvinyl alcohol (PVA).
(3) Blank preparation: adding a release agent accounting for 3 percent of the weight of the composite powder into the ceramic powder, then sieving the mixture by a 80-mesh sieve, and pressing the mixture on a press to form a cylindrical ceramic green body. It will be appreciated that the shape of the blank may also be other. The release agent is calcium stearate.
(4) Sintering and forming: and sintering the ceramic blank formed by pressing at a high temperature into ceramic 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 ceramicrIs 8.4, temperature coefficient of resonance frequency taufIt was-0.5 ppm/DEG C, and the Qf value was 39000 GHz.
Example 10
The specific steps of this example are as follows:
(1) preparing composite powder: according to molar ratio [2X 0.5X 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 and SiO with the purity of more than 99.5 percent2、SrCO3、CaCO3、TiO2Ball-milling the powder in a high-speed ball mill, fully mixing, drying, grinding, and presintering at high temperature to obtain [ (Zn)0.5Mg0.5)2SiO4]0.86-(Sr0.05Ca0.95TiO3)0.14And (3) composite powder, wherein 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 powder20.1 wt% of rare metal oxide Ta2O5And 0.1 wt% of rare metal oxide Nb2O5And performing secondary ball milling in a high-speed ball mill, adding a bonding agent accounting for 8 percent of the weight of the composite powder, and granulating to obtain the ceramic powder. The composition of the ceramic powder is [ (Zn)0.5Mg0.5)2SiO4]0.86-(Sr0.05Ca0.95TiO3)0.14+0.1wt％CeO2+0.1wt％Ta2O5+0.1wt％
Nb2O5. The binder is polyvinyl alcohol (PVA).
(3) Blank preparation: adding a release agent accounting for 3 percent of the weight of the composite powder into the ceramic powder, then sieving the mixture by a 80-mesh sieve, and pressing the mixture on a press to form a cylindrical ceramic green body. 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 ceramic blank formed by pressing into ceramic 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 ceramicrIs 8.6, temperature coefficient of resonance frequency taufIs-1 ppm/DEG C, and the Qf value is 38500 GHz.
Example 11
The specific steps of this example are as follows:
(1) preparing composite powder: according to molar ratio [2x 1 x 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 and SiO with the purity of more than 99.5 percent2、SrCO3、CaCO3、TiO2Ball milling the powder in a high-speed ball mill, fully mixing, drying, grinding, and presintering at high temperature to obtain (Zn)2SiO4)0.75-(Sr0.2Ca0.8TiO3)0.25And (3) composite powder, wherein 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 Ta, a rare metal oxide, was added to the composite powder2O5And performing secondary ball milling in a high-speed ball mill, adding a bonding agent accounting for 8 percent of the weight of the composite powder, and granulating to obtain the ceramic powder. The composition of the ceramic powder is (Zn)2SiO4)0.75-(Sr0.2Ca0.8TiO3)0.25+0.1wt％Ta2O5. The binder is polyvinyl alcohol (PVA).
(3) Blank preparation: adding a release agent accounting for 3 percent of the weight of the composite powder into the ceramic powder, then sieving the mixture by a 80-mesh sieve, and pressing the mixture on a press to form a cylindrical ceramic green body. 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 ceramic blank formed by pressing at high temperature into ceramic to obtain the ceramicThe microwave dielectric ceramic has the high-temperature sintering temperature of 1100 ℃ and the sintering time of 4 hours. The dielectric constant epsilon of the microwave dielectric ceramicrIs 8.9, temperature coefficient of resonance frequency taufIs +20 ppm/DEG C, and the Qf value is 35000 GHz.
Example 12
The specific steps of this example are as follows:
(1) preparing composite powder: according to molar ratio [2x 1 x 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 and SiO with the purity of more than 99.5 percent2、SrCO3、CaCO3、TiO2Ball milling the powder in a high-speed ball mill, fully mixing, drying, grinding, and presintering at high temperature to obtain (Zn)2SiO4)0.95-(Sr0.2Ca0.8TiO3)0.05And (3) composite powder, wherein 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 Ta, a rare metal oxide, was added to the composite powder2O5And performing secondary ball milling in a high-speed ball mill, adding a bonding agent accounting for 8 percent of the weight of the composite powder, and granulating to obtain the ceramic powder. The composition of the ceramic powder is (Zn)2SiO4)0.95-(Sr0.2Ca0.8TiO3)0.05+0.2wt％Ta2O5. The binder is polyvinyl alcohol (PVA).
(3) Blank preparation: adding a release agent accounting for 3 percent of the weight of the composite powder into the ceramic powder, then sieving the mixture by a 80-mesh sieve, and pressing the mixture on a press to form a cylindrical ceramic green body. 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 ceramic blank formed by pressing at high temperature into ceramic 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 ceramicrIs 8.0, temperature coefficient of resonance frequency taufIs-15 ppm/DEG C, and the Qf value is 40000 GHz.
Example 13
The specific steps of this example are as follows:
(1) preparing composite powder: according to molar ratio [2X 0.5X 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 and SiO with the purity of more than 99.5 percent2、SrCO3、CaCO3、TiO2Ball-milling the powder in a high-speed ball mill, fully mixing, drying, grinding, and presintering at high temperature to obtain [ (Zn)0.5Mg0.5)2SiO4]0.86-(Sr0.05Ca0.95TiO3)0.14And (3) composite powder, wherein 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 Ta, a rare metal oxide, was added to the composite powder2O5And performing secondary ball milling in a high-speed ball mill, adding a bonding agent accounting for 8 percent of the weight of the composite powder, and granulating to obtain the ceramic powder. The composition of the ceramic powder is [ (Zn)0.5Mg0.5)2SiO4]0.86-(Sr0.05Ca0.95TiO3)0.14+0.1wt％Ta2O5. The binder is polyvinyl alcohol (PVA).
(3) Blank preparation: adding a release agent accounting for 3 percent of the weight of the composite powder into the ceramic powder, then sieving the mixture by a 80-mesh sieve, and pressing the mixture on a press to form a cylindrical ceramic green body. 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 ceramic blank formed by pressing at high temperature into ceramic 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 ceramicrIs 8.5, temperature coefficient of resonance frequency taufIs +0.5 ppm/DEG C, and the Qf value is 38500 GHz.
Example 14
The specific steps of this example are as follows:
(1) preparing composite powder: in mole ratioRatio [2x 0.5 x 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 and SiO with the purity of more than 99.5 percent2、SrCO3、CaCO3、TiO2Ball-milling the powder in a high-speed ball mill, fully mixing, drying, grinding, and presintering at high temperature to obtain [ (Zn)0.5Mg0.5)2SiO4]0.86-(Sr0.05Ca0.95TiO3)0.14And (3) composite powder, wherein 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 a rare metal oxide Nb is added to the composite powder2O5And 0.1 wt% of rare metal oxide CeO2And performing secondary ball milling in a high-speed ball mill, adding a bonding agent accounting for 8 percent of the weight of the composite powder, and granulating to obtain the ceramic powder. The composition of the ceramic powder is [ (Zn)0.5Mg0.5)2SiO4]0.86-(Sr0.05Ca0.95TiO3)0.14+0.1wt％Nb2O5+0.1wt％CeO2. The binder is polyvinyl alcohol (PVA).
(3) Blank preparation: adding a release agent accounting for 3 percent of the weight of the composite powder into the ceramic powder, then sieving the mixture by a 80-mesh sieve, and pressing the mixture on a press to form a cylindrical ceramic green body. 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 ceramic blank formed by pressing at high temperature into ceramic 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 ceramicrIs 8.5, temperature coefficient of resonance frequency taufIs +0.5 ppm/DEG C, and the Qf value is 38000 GHz.
Table 1 shows the composition, sintering temperature, dielectric constant ε of a microwave dielectric ceramic according to several embodiments of the present inventionrTemperature coefficient of resonance frequency τfQf value, composition, sintering temperature and dielectric constant epsilon of the conventional microwave dielectric ceramicrTemperature coefficient of resonance frequency τfAnd Qf value.
TABLE 1
Figure BDA0002956266460000131
Figure BDA0002956266460000141
As can be seen from Table 1, compared with the existing microwave dielectric ceramic, the microwave dielectric ceramic of the invention can be prepared at a lower sintering temperature, the sintering window is larger, namely the stability of the microwave dielectric ceramic is good when the performance fluctuates with the sintering temperature, the Qf value is higher, better microwave dielectric performance can be obtained, and the dielectric constant epsilon isrIs 8.0 to 9.0, and has a temperature coefficient of resonance frequency of τfIs-15- +20 ppm/DEG C, Qf value is 35000-40000 GHz, and resonant frequency temperature coefficient taufCan be adjusted according to requirements, and the temperature coefficient tau of the resonant frequencyfThe adjustable range is wide.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (7)

1. A low-dielectric-constant microwave dielectric ceramic is characterized by comprising the following components in parts by weight:
titanate silicate composite 100 parts
0.1-0.3 parts of rare metal oxide;
the titanate silicate complex is [ (Zn)xMg1-x)2SiO4]z-(SryCa1-yTiO3)1-z(ii) a Said rarityThe metal oxide being CeO2、Nb2O5And/or Ta2O5；
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, and z is more than or equal to 0.75 and less than or equal to 0.95.
2. The microwave dielectric ceramic of claim 1, wherein the dielectric constant is 8.0 to 9.0, the temperature coefficient of resonance frequency is-15 to +20ppm/° C, and the Qf value is 35000 to 40000 GHz.
3. The method for preparing a low dielectric constant microwave dielectric ceramic according to claim 1, comprising the steps of:
preparing composite powder: in molar ratio of [2xz ]]：[2z-2xz]：[z]：[y-yz]：[1-y-z+yz]：[1-z]Respectively weighing ZnO, MgO and SiO with the purity of more than 99.5 percent2、SrCO3、CaCO3、TiO2Ball milling, mixing, stoving, grinding and high temperature pre-sintering to obtain [ (Zn)xMg1-x)2SiO4]z-(SryCa1-yTiO3)1-zComposite powder;
preparing ceramic powder: adding 0.1-0.3% by weight of rare metal oxide into the composite powder, performing secondary ball milling, adding a binder, and granulating to obtain ceramic powder;
blank preparation: adding a release agent into the ceramic powder, sieving, and pressing into a ceramic green body on a pressing machine;
sintering and forming: sintering the ceramic blank formed by pressing at high temperature into ceramic to obtain the ceramic;
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, and z is more than or equal to 0.75 and less than or equal to 0.95; the rare metal oxide is CeO2、Nb2O5And/or Ta2O5。
4. The preparation method according to claim 3, wherein the binder is polyvinyl alcohol, and the addition amount of the polyvinyl alcohol is 5-10% of the weight of the composite powder.
5. The preparation method according to claim 3, wherein 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.
6. The preparation method according to claim 3, wherein the pre-sintering temperature is 800-900 ℃ and the pre-sintering time is 1.8-2.5 hours.
7. The preparation method according to claim 3, wherein the high-temperature sintering temperature is 1050-1100 ℃ and the sintering time is 4-5 hours.
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CN113321496A (en) * 2021-07-01 2021-08-31 宜宾红星电子有限公司 Composite microwave dielectric ceramic material and preparation method thereof
CN115536376A (en) * 2022-09-14 2022-12-30 西北工业大学 Preparation method of low-dielectric low-loss zinc magnesium silicate system microwave dielectric ceramic
CN116143508A (en) * 2022-12-20 2023-05-23 无锡鑫圣慧龙纳米陶瓷技术有限公司 Low-dielectric-constant high-temperature stable microwave dielectric ceramic and preparation method thereof

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