CN115611613B - Sulfate microwave dielectric ceramic with low dielectric constant - Google Patents
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Abstract
The invention discloses a low dielectric constant sulfate microwave dielectric ceramic, which has the expression of xCaSO 4 ‑ySrSO 4 ‑zBaSO 4 Wherein 0.ltoreq.x.ltoreq.1, 0.ltoreq.y.ltoreq.1, 0.ltoreq.z.ltoreq.1, x+y+z=1. The microwave dielectric ceramic of the invention has low dielectric constant (epsilon) r =5.85 to 10.95) and a high Qf value (15,000 to 57,000 ghz) with an adjustable temperature coefficient of resonance frequency (τ f -98.8-101.6 ppm/°c). The invention provides a low epsilon r Sulfate microwave dielectric ceramics have low epsilon r High Qf and rare near zero or positive τ f Besides, the method has a series of advantages of low raw material cost, easy preparation, low sintering temperature, good cofiring with common metals and the like. The sulfate microwave dielectric ceramic provided by the invention can be used for components such as dielectric resonators, filters, antennas, substrates and the like, thereby meeting the higher requirements of high-end microwave communication, especially millimeter wave communication technology on the microwave dielectric ceramic.
Description
Technical Field
The invention relates to a microwave dielectric material applied to a communication system, in particular to sulfate microwave dielectric ceramic with low dielectric constant, high Qf value and adjustable resonant frequency temperature coefficient between positive and negative values.
Background
The low-dielectric-constant microwave dielectric ceramic is a key material in millimeter wave communication technology represented by 5G and future mobile communication, and the basic performance requirements are as follows: low dielectric constant epsilon r High Qf and small resonant frequency temperature coefficient tau f . In the case of a dielectric resonator, a filter, or the like having a high temperature stability, it is desirable to use |τ f The content is less than or equal to 10 ppm/DEG C; in the case of a dielectric antenna, a substrate, or the like having a relatively low temperature stability requirement, the temperature stability of the antenna can be relaxed f Is not limited. However, the three performance indicators are often mutually restricted and are concentrated to be represented by most single-phase low epsilon r τ of microwave dielectric ceramic f Is a relatively large negative value. For this purpose, it is generally necessary to introduce a high ε r Positive tau f Is formed into composite ceramic, τ f Decreasing, or even near zero. However, this approach would result in ε r Significantly elevated. Thus, development of a low ε r High Qf and smaller, in particular near zero τ f The single-phase microwave dielectric ceramic has important significance for the development of millimeter wave communication technology. In addition, has a low epsilon r Positive tau f The single-phase microwave dielectric ceramics of (2) are also very rare. And has a high epsilon r Positive tau f Compared to single phase materials with low epsilon r Negative τ f After the composite ceramic is formed by the material of (2), epsilon can be effectively inhibited r Thus, for developing low epsilon suitable for high-end microwave communication, especially millimeter wave communication technology r The microwave dielectric ceramic has important significance.
Disclosure of Invention
The object of the present invention is to provide a composition having a low epsilon r High Qf value and adjustable tau f Is a sulfate microwave dielectric ceramic. In particular, some of the components of the invention have a near zero or positive τ f This is at a single phase low ε r Microwave dielectric ceramics are rare and have important practical value.
The low epsilon of the present invention r The sulfate microwave dielectric ceramic expression is xCaSO 4 -ySrSO 4 -zBaSO 4 Wherein 0.ltoreq.x.ltoreq.1, 0.ltoreq.y.ltoreq.1, 0.ltoreq.z.ltoreq.1, x+y+z=1. The preferable components are as follows: 1. the expression is xCaSO 4 -ySrSO 4 Wherein 0.ltoreq.x<0.4，0.6<y is less than or equal to 1, x+y=1, with low ε r High Qf value and positive τ f The method comprises the steps of carrying out a first treatment on the surface of the 2. The expression is xCaSO 4 -ySrSO 4 Wherein x is more than or equal to 0.4 and less than or equal to 0.6,0.4, y is more than or equal to 0.6, and x+y=1, has low epsilon r High Qf value and near zero τ f The method comprises the steps of carrying out a first treatment on the surface of the 3. The expression is xCaSO 4 -zBaSO 4 Wherein 0.ltoreq.x.ltoreq.0.3, 0.7.ltoreq.z.ltoreq.1, x+z=1, has a low ε r High Qf value and near zero τ f The method comprises the steps of carrying out a first treatment on the surface of the 4. The expression is ySrSO 4 -zBaSO 4 Wherein y is 0.ltoreq. 0.45,0.55.ltoreq.z is 1, y+z=1, has a low ε r High Qf value and near zero τ f The method comprises the steps of carrying out a first treatment on the surface of the 5. The expression is ySrSO 4 -zBaSO 4 Wherein 0.45<y≤1，0≤z<0.55, y+z=1, withHas a low epsilon r High Qf value and positive τ f . 6. The expression is a (x 1 CaSO) 4 -y1SrSO 4 )-b(x2CaSO 4 -z2BaSO 4 ) Wherein 0.4.ltoreq.x1.ltoreq. 0.6,0.4.ltoreq.y1.ltoreq.0.6, x1+y1=1, 0.ltoreq.x2.ltoreq.0.3, 0.7.ltoreq.z2.ltoreq.1, x2+z2=1, 0<a<1，0<b<1, a+b=1, with low epsilon r High Qf value and near zero τ f . 7. The expression is a (x 1 CaSO) 4 -y1SrSO 4 )-b(y2SrSO 4 -z2BaSO 4 ) Wherein x1 is more than or equal to 0.4 and less than or equal to 0.6,0.4, y1 is more than or equal to 0.6, x1+y1=1, 0 is more than or equal to y2 is more than or equal to 0.45,0.55, z2 is more than or equal to 1, y2+z2=1, 0<a<1，0<b<1, a+b=1, with low epsilon r High Qf value and near zero τ f . 8. The expression is a (x 1 CaSO) 4 -z1BaSO 4 )-b(y2SrSO 4 -z2BaSO 4 ) Wherein 0.ltoreq.x1.ltoreq.0.3, 0.7.ltoreq.z1.ltoreq.1, x1+z1=1, 0.ltoreq.y2.ltoreq. 0.45,0.55.ltoreq.z2.ltoreq.1, y2+z2=1, 0<a<1，0<b<1, a+b=1, with low epsilon r High Qf value and near zero τ f . 9. The expression is a (x 1 CaSO) 4 -y1SrSO 4 )-b(y2SrSO 4 -z2BaSO 4 ) Wherein 0.ltoreq.x1<0.4，0.6<y1≤1，x1+y1＝1，0.45<y2≤1，0≤z2<0.55，y2+z2＝1，0<a<1，0<b<1, a+b=1, with low epsilon r High Qf value and positive τ f 。
The low dielectric constant sulfate microwave dielectric ceramic can be prepared by the following method.
First, caSO 4 、SrSO 4 、BaSO 4 The raw material powder is uniformly mixed by a wet ball milling method according to the proportion, and is pre-sintered at 400-700 ℃ after being dried, so as to obtain single-phase powder. And (3) performing secondary ball milling on the pre-sintered powder, adding a binder and granulating after drying, then forming under the uniaxial pressure of 30-200 MPa, and finally sintering in the atmosphere at 550-1050 ℃ to obtain the required microwave dielectric ceramic.
The low epsilon of the present invention r Sulfate microwave dielectric ceramic with dielectric constant of 5.85-10.95, qf value of 15,000-57,000 GHz and tau f Can be adjusted between positive and negative values. Tau provided by the invention f Near zero components can be used in resonatorsDevices, τ, having high temperature stability requirements, such as filters f Positive components can be used with tau f Low epsilon, typically a large negative value r Ceramic forming composite material, maintaining low epsilon while improving the temperature stability of the latter r All the components can be used for antennas, substrates and other devices with relatively low requirements on temperature stability. In addition, the invention provides a low epsilon r The sulfate microwave dielectric ceramic also has a series of advantages of low raw material cost, easy preparation, low sintering temperature, good cofiring with common metals and the like, so that the sulfate microwave dielectric ceramic has great practical value in industry.
Detailed Description
Tables 1 to 4 show several specific examples of the contents of the components constituting the present invention and their microwave dielectric properties. The preparation method is as described above.
TABLE 1 xCaSO 4 -ySrSO 4 Microwave dielectric properties of ceramics.
TABLE 2 xCaSO 4 -zBaSO 4 Microwave dielectric properties of ceramics.
TABLE 3 ySrSO 4 -zBaSO 4 Microwave dielectric properties of ceramics.
Table 4, a (x 1 CaSO) 4 -y1SrSO 4 )-b(x2CaSO 4 -z2BaSO 4 ) Microwave dielectric properties of ceramics.
TABLE 5 a (x 1 CaSO) 4 -y1SrSO 4 )-b(y2SrSO 4 -z2BaSO 4 ) Microwave dielectric properties of ceramics.
TABLE 6, a (x 1 CaSO) 4 -y1BaSO 4 )-b(y2SrSO 4 -z2BaSO 4 ) Microwave dielectric properties of ceramics.
As can be seen from tables 1 to 4, all of the xCaSOs 4 -ySrSO 4 -zBaSO 4 The ceramics all have a low epsilon r High Qf and smaller τ f Can be used as a dielectric antenna and a substrate in high-end microwave communication, in particular millimeter wave communication. While at the same time having a low epsilon r High Qf value, near zero or positive τ f Single-phase microwave dielectric ceramics are rare, with near zero τ f The material can be used for high-end microwave communication, especially for high-temperature stability components such as resonators, filters and the like in millimeter wave communication, and positive tau f The material can be used for preparing the composite material f Low epsilon, typically a large negative value r Ceramic forming composite material with low epsilon while keeping the latter low r And at the same time improve its temperature stability, thus τ can be reduced f Materials that are near zero or positive are preferred components. As shown in Table 1, xCaSO 4 -ySrSO 4 Epsilon of ceramic r And Qf monotonously decrease and increase with increasing x, τ f Then from positive value aloneThe modulation drops to a negative value. X is 0.ltoreq.x<At 0.4 τ f Is a larger positive value; and when x is more than or equal to 0.4 and less than or equal to 0.6, tau of the material f Near zero. As shown in Table 2, xCaSO 4 -zBaSO 4 Epsilon of ceramic r And Qf monotonously decreases and increases with increasing x, τ f Monotonically decreasing, and approaching zero when x is more than or equal to 0 and less than or equal to 0.3. As shown in Table 3, ySrSO 4 -zBaSO 4 Epsilon of ceramic r And Qf increases and decreases monotonically with y, τ f Monotonically increasing, and approaching zero when y is more than or equal to 0 and less than or equal to 0.45, and 0.45<y is a larger positive value when y is less than or equal to 1. In tables 1, 2 and 3, τ was also calculated f The near-zero component has near-zero tau after combination f Whereas τ in tables 1, 3 f Positive components also have positive τ after combination f The partial properties are shown in tables 4 to 7. Thus, τ f Near zero or positive values are the standard, and the preferable components are determined as follows: 1. the expression is xCaSO 4 -ySrSO 4 Wherein 0.ltoreq.x<0.4，0.6<y is less than or equal to 1, x+y=1, with low ε r High Qf value and positive τ f The method comprises the steps of carrying out a first treatment on the surface of the 2. The expression is xCaSO 4 -ySrSO 4 Wherein x is more than or equal to 0.4 and less than or equal to 0.6,0.4, y is more than or equal to 0.6, and x+y=1, has low epsilon r High Qf value and near zero τ f The method comprises the steps of carrying out a first treatment on the surface of the 3. The expression is xCaSO 4 -zBaSO 4 Wherein 0.ltoreq.x.ltoreq.0.3, 0.7.ltoreq.z.ltoreq.1, x+z=1, has a low ε r High Qf value and near zero τ f The method comprises the steps of carrying out a first treatment on the surface of the 4. The expression is ySrSO 4 -zBaSO 4 Wherein y is 0.ltoreq. 0.45,0.55.ltoreq.z is 1, y+z=1, has a low ε r High Qf value and near zero τ f The method comprises the steps of carrying out a first treatment on the surface of the 5. The expression is ySrSO 4 -zBaSO 4 Wherein 0.45<y≤1，0≤z<0.55, y+z=1, with low epsilon r High Qf value and positive τ f . 6. The expression is a (x 1 CaSO) 4 -y1SrSO 4 )-b(x2CaSO 4 -z2BaSO 4 ) Wherein 0.4.ltoreq.x1.ltoreq. 0.6,0.4.ltoreq.y1.ltoreq.0.6, x1+y1=1, 0.ltoreq.x2.ltoreq.0.3, 0.7.ltoreq.z2.ltoreq.1, x2+z2=1, 0<a<1，0<b<1, a+b=1, with low epsilon r High Qf value and near zero τ f . 7. The expression is a (x 1 CaSO) 4 -y1SrSO 4 )-b(y2SrSO 4 -z2BaSO 4 ) Wherein x1 is more than or equal to 0.4 and less than or equal to 0.6,0.4, y1 is more than or equal to 0.6, x1+y1=1, 0≤y2≤0.45，0.55≤z2≤1，y2+z2＝1，0<a<1，0<b<1, a+b=1, with low epsilon r High Qf value and near zero τ f . 8. The expression is a (x 1 CaSO) 4 -z1BaSO 4 )-b(y2SrSO 4 -z2BaSO 4 ) Wherein 0.ltoreq.x1.ltoreq.0.3, 0.7.ltoreq.z1.ltoreq.1, x1+z1=1, 0.ltoreq.y2.ltoreq. 0.45,0.55.ltoreq.z2.ltoreq.1, y2+z2=1, 0<a<1，0<b<1, a+b=1, with low epsilon r High Qf value and near zero τ f . 9. The expression is a (x 1 CaSO) 4 -y1SrSO 4 )-b(y2SrSO 4 -z2BaSO 4 ) Wherein 0.ltoreq.x1<0.4，0.6<y1≤1，x1+y1＝1，0.45<y2≤1，0≤z2<0.55，y2+z2＝1，0<a<1，0<b<1, a+b=1, with low epsilon r High Qf value and positive τ f 。
The microwave dielectric ceramic of the invention has low dielectric constant (epsilon) r =5.85 to 10.95) and a high Qf value (15,000 to 57,000 ghz) with an adjustable temperature coefficient of resonance frequency (τ f -98.8-101.6 ppm/°c). The sulfate microwave dielectric ceramic provided by the invention can be used for components such as dielectric resonators, filters, antennas, substrates and the like, thereby meeting the higher requirements of high-end microwave communication, especially millimeter wave communication technology on the microwave dielectric ceramic. Wherein τ f The near zero (within plus or minus 10 ppm/. Degree.C.) component can be used in resonator, filter, etc. components with high temperature stability requirement, τ f Positive components can be used with tau f Low epsilon, typically a large negative value r Ceramic forming composite material, maintaining low epsilon while improving the temperature stability of the latter r All the components can be used for components with relatively low requirements on temperature stability, such as antennas, substrates and the like. The invention provides a low epsilon r Sulfate microwave dielectric ceramics have low epsilon r High Qf and rare near zero or positive τ f Besides, the method has a series of advantages of low raw material cost, easy preparation, low sintering temperature, good cofiring with common metals and the like, so that the method has great practical value in industry.
Claims (10)
1. Sulfate ceramic as low dielectric constant microwave dielectricThe application of the ceramic is characterized in that: the sulfate ceramic expression is xCaSO 4 -ySrSO 4 -zBaSO 4 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 1, z is more than or equal to 0 and less than or equal to 1, and x+y+z=1; the method comprises the following steps: first, caSO 4 、SrSO 4 、BaSO 4 The raw material powder is uniformly mixed by a wet ball milling method according to the proportion, and is dried and then subjected to 400-700 o C, presintering to obtain single-phase powder; performing secondary ball milling on the pre-sintered powder, adding a binder and granulating after drying, then forming under the uniaxial pressure of 30-200 MPa, and finally at 550-1050 o C. Sintering in the atmosphere to obtain the required microwave dielectric ceramic.
2. The use of the sulfate ceramic according to claim 1 as a low dielectric constant microwave dielectric ceramic, characterized in that: the expression of the ceramic is xCaSO 4 -ySrSO 4 Wherein 0.ltoreq.x<0.4，0.6<y≤1，x+y=1。
3. The use of the sulfate ceramic according to claim 1 as a low dielectric constant microwave dielectric ceramic, characterized in that: the expression of the ceramic is xCaSO 4 -ySrSO 4 Wherein x is more than or equal to 0.4 and less than or equal to 0.6,0.4, y is more than or equal to 0.6, and x+y=1.
4. The use of the sulfate ceramic according to claim 1 as a low dielectric constant microwave dielectric ceramic, characterized in that: the expression of the ceramic is xCaSO 4 -zBaSO 4 Wherein 0.ltoreq.x.ltoreq.0.3, 0.7.ltoreq.z.ltoreq.1, and x+z=1.
5. The use of the sulfate ceramic according to claim 1 as a low dielectric constant microwave dielectric ceramic, characterized in that: the expression of the ceramic is ySrSO 4 -zBaSO 4 Wherein y is more than or equal to 0 and less than or equal to 0.45,0.55, z is more than or equal to 1, and y+z=1.
6. The use of the sulfate ceramic according to claim 1 as a low dielectric constant microwave dielectric ceramic, characterized in thatThe method comprises the following steps: the expression of the ceramic is ySrSO 4 -zBaSO 4 Wherein 0.45<y≤1，0≤z<0.55，y+z=1。
7. The use of the sulfate ceramic according to claim 1 as a low dielectric constant microwave dielectric ceramic, characterized in that: the expression of the ceramic is a (x 1 CaSO) 4 -y1SrSO 4 )-b(x2CaSO 4 -z2BaSO 4 ) Wherein 0.4.ltoreq.x1.ltoreq. 0.6,0.4.ltoreq.y1.ltoreq.0.6, x1+y1=1, 0.ltoreq.x2.ltoreq.0.3, 0.7.ltoreq.z2.ltoreq.1, x2+z2=1, 0<a<1，0<b<1，a+b=1。
8. The use of the sulfate ceramic according to claim 1 as a low dielectric constant microwave dielectric ceramic, characterized in that: the expression of the ceramic is a (x 1 CaSO) 4 -y1SrSO 4 )-b(y2SrSO 4 -z2BaSO 4 ) Wherein x1 is more than or equal to 0.4 and less than or equal to 0.6,0.4, y1 is more than or equal to 0.6, x1+y1=1, 0 is more than or equal to y2 is more than or equal to 0.45,0.55, z2 is more than or equal to 1, y2+z2=1, 0<a<1，0<b<1，a+b=1。
9. The use of the sulfate ceramic according to claim 1 as a low dielectric constant microwave dielectric ceramic, characterized in that: the expression of the ceramic is a (x 1 CaSO) 4 -z1BaSO 4 )-b(y2SrSO 4 -z2BaSO 4 ) Wherein 0.ltoreq.x1.ltoreq.0.3, 0.7.ltoreq.z1.ltoreq.1, x1+z1=1, 0.ltoreq.y2.ltoreq. 0.45,0.55.ltoreq.z2.ltoreq.1, y2+z2=1, 0<a<1，0<b<1，a+b=1。
10. The use of the sulfate ceramic according to claim 1 as a low dielectric constant microwave dielectric ceramic, characterized in that: the expression of the ceramic is a (x 1 CaSO) 4 -y1SrSO 4 )-b(y2SrSO 4 -z2BaSO 4 ) Wherein 0.ltoreq.x1<0.4，0.6<y1≤1，x1+y1=1，0.45<y2≤1，0≤z2<0.55，y2+z2=1，0<a<1，0<b<1，a+b=1。
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| CN106927792A (en) * | 2015-12-30 | 2017-07-07 | 上海晶材新材料科技有限公司 | The LTCC ceramic materials and preparation method of the nearly zero-temperature coefficient of low dielectric constant and low loss |
| CN109164303A (en) * | 2018-09-19 | 2019-01-08 | 东南大学 | Alternating temperature dielectric constant precision measurement apparatus and measurement method |
| CN111675530A (en) * | 2020-06-02 | 2020-09-18 | 浙江大学 | High-density and high-strength gypsum ceramic and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106927792A (en) * | 2015-12-30 | 2017-07-07 | 上海晶材新材料科技有限公司 | The LTCC ceramic materials and preparation method of the nearly zero-temperature coefficient of low dielectric constant and low loss |
| CN109164303A (en) * | 2018-09-19 | 2019-01-08 | 东南大学 | Alternating temperature dielectric constant precision measurement apparatus and measurement method |
| CN111675530A (en) * | 2020-06-02 | 2020-09-18 | 浙江大学 | High-density and high-strength gypsum ceramic and preparation method thereof |
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