CN115611613A - Low dielectric constant sulfate microwave dielectric ceramic - Google Patents

Low dielectric constant sulfate microwave dielectric ceramic Download PDF

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CN115611613A
CN115611613A CN202211287969.2A CN202211287969A CN115611613A CN 115611613 A CN115611613 A CN 115611613A CN 202211287969 A CN202211287969 A CN 202211287969A CN 115611613 A CN115611613 A CN 115611613A
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李雷
贾英强
罗炜坤
吴淑雅
陈湘明
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Zhejiang University ZJU
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Abstract

The invention discloses a low dielectric constant sulfate microwave dielectric ceramic, the expression of which 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, and z is more than or equal to 0 and less than or equal to 1, x + y + z =1. The microwave dielectric ceramic has low dielectric constant (epsilon) r = 5.85-10.95) and high Qf value (15,000-57,000GHz), while having an adjustable temperature coefficient of resonance frequency (tau) f = 98.8-101.6 ppm/° c). The invention provides a low epsilon r Sulfate microwave dielectric ceramic with low epsilon r High Qf values 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 property 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 higher requirements of high-end microwave communication, particularly millimeter wave communication technology on the microwave dielectric ceramic。

Description

Sulfate microwave dielectric ceramic with low dielectric constant
Technical Field
The invention relates to a microwave dielectric material applied to a communication system, in particular to a sulfate microwave dielectric ceramic which has low dielectric constant and high Qf value and can adjust the temperature coefficient of resonance frequency between the positive value and the negative value.
Background
The low dielectric constant microwave dielectric ceramic is a key material in the millimeter wave communication technology represented by 5G and future mobile communication, and the basic performance requirements of the low dielectric constant microwave dielectric ceramic are as follows: low dielectric constant epsilon r High Qf value and small temperature coefficient of resonance frequency tau f . Among them, in the case where a dielectric resonator, a filter, or the like has a high requirement for temperature stability, | τ is required f The absolute value is less than or equal to 10 ppm/DEG C; on the other hand, in the case of dielectric antenna, substrate, etc. with relatively low requirement for temperature stability, the width of τ can be relaxed f The requirements of (2). However, the above three performance indexes are often mutually restricted and are collectively reflected as the vast majority of single-phase low epsilon r Tau of microwave dielectric ceramic f Are more negative. For this purpose, it is generally necessary to introduce a material having a high epsilon r And positive tau f Forming a composite ceramic, and adding f Turn down to near zero. However, this method would result in ε r Is remarkably increased. Therefore, have been developed to have a low ε r High Qf value and small, in particular near zero tau f The single-phase microwave dielectric ceramic has important significance for the development of millimeter wave communication technology. In addition, has a low ε r And positive tau f The single-phase microwave dielectric ceramics are also rare. And has a high ε r And positive tau f Compared with single-phase materials having a low epsilon r And negative τ f After the material forms the composite ceramic, the epsilon can be effectively inhibited r Thus, it is desired to develop a low epsilon suitable for high-end microwave communication, particularly, millimeter wave communication technology r The microwave dielectric ceramic also has important significance.
Disclosure of Invention
It is an object of the present invention to provide a composition having a low epsilon r High Qf value and adjustable tau f The sulfate microwave dielectric ceramic. In particular, some of the components of the present invention have near zero or positive τ f This is at a single phase low ε r The microwave dielectric ceramic is rare and has important practical value.
Low epsilon of the invention r The expression of the sulfate microwave dielectric ceramic 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, x + y + z =1. The preferable components are as follows: 1. the expression is xCaSO 4 -ySrSO 4 Wherein 0 is less than or equal to x<0.4，0.6<y is less than or equal to 1,x + y =1, with low epsilon r High Qf value and positive τ f (ii) a 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, y is more than or equal to 0.4 and less than or equal to 0.6, x + y =1, and has low epsilon r High Qf value and near zero τ f (ii) a 3. The expression is xCaSO 4 -zBaSO 4 Wherein x is more than or equal to 0 and less than or equal to 0.3, z is more than or equal to 0.7 and less than or equal to 1, x + z =1, has low epsilon r High Qf value and near zero τ f (ii) a 4. The expression is ySrSO 4 -zBaSO 4 Wherein y is more than or equal to 0 and less than or equal to 0.45, z is more than or equal to 0.55 and less than or equal to 1, y + z =1, has low epsilon r High Qf value and near zero τ f (ii) a 5. The expression is ySrSO 4 -zBaSO 4 Wherein 0.45<y≤1，0≤z<0.55,y + z =1, with low ε 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 x1 is more than or equal to 0.4 and less than or equal to 0.6, y1 is more than or equal to 0.4 and less than or equal to 0.6, x1+ y1=1, x2 is more than or equal to 0.3, z2 is more than or equal to 0.7 and less than or equal to 1, and x2+ z2=1,0<a<1，0<b<1,a + b =1, having a 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, y1 is more than or equal to 0.4 and less than or equal to 0.6, x1+ y1=1, y2 is more than or equal to 0.45, z2 is more than or equal to 0.55 and less than or equal to 1, and 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 x1 is more than or equal to 0 and less than or equal to 0.3, z1 is more than or equal to 0.7 and less than or equal to 1, x1+ z1=1, y2 is more than or equal to 0 and less than or equal to 0.45, z2 is more than or equal to 0.55 and less than or equal to 1, and y2+ z2=1,0<a<1，0<b<1,a + b =1, having a 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 x1 is not less than 0<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, having a 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.
Firstly, 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 to obtain single-phase powder. And performing secondary ball milling on the pre-sintered powder, drying, adding a binder, granulating, molding under the uniaxial pressure of 30-200 MPa, and finally sintering at 550-1050 ℃ in the atmosphere to obtain the required microwave dielectric ceramic.
Low epsilon of the invention r The sulfate microwave dielectric ceramic has dielectric constant of 5.85-10.95, qf value of 15,000-57,000GHz, tau f And can be adjusted between positive and negative values. Tau provided by the invention f The near-zero component can be used for devices with higher requirements on temperature stability, such as resonators, filters and the like f Positive components may be used for the combination with tau f Low epsilon, which is generally a large negative value r Ceramics forming composites, maintaining a low epsilon while improving the temperature stability of the latter r All the components can be used for devices with relatively low requirements on temperature stability, such as antennas, substrates and the like. In addition, the invention provides low ε r The sulfate microwave dielectric ceramic also has a series of advantages of low raw material cost, easy preparation, low sintering temperature, good cofiring performance with common metals and the like, thereby having great practical value in industry.
Detailed Description
Tables 1 to 4 show several specific examples of the contents of the respective components constituting the present invention and their microwave dielectric properties. The preparation method is as described above.
TABLE 1 xCaSO 4 -ySrSO 4 The microwave dielectric properties of the ceramic.
Figure BDA0003900146020000021
Figure BDA0003900146020000031
TABLE 2 xCaSO 4 -zBaSO 4 The microwave dielectric properties of the ceramic.
Figure BDA0003900146020000032
TABLE 3 ySrSO 4 -zBaSO 4 The microwave dielectric properties of the ceramic.
Figure BDA0003900146020000033
Figure BDA0003900146020000041
TABLE 4, a (x 1 CaSO) 4 -y1SrSO 4 )-b(x2CaSO 4 -z2BaSO 4 ) The microwave dielectric properties of the ceramic.
Figure BDA0003900146020000042
TABLE 5, a (x 1 CaSO) 4 -y1SrSO 4 )-b(y2SrSO 4 -z2BaSO 4 ) The microwave dielectric properties of the ceramic.
Figure BDA0003900146020000043
Figure BDA0003900146020000051
TABLE 6 a (x 1 CaSO) 4 -y1BaSO 4 )-b(y2SrSO 4 -z2BaSO 4 ) The microwave dielectric properties of the ceramic.
Figure BDA0003900146020000052
As can be seen from tables 1 to 4, all of xCaSO 4 -ySrSO 4 -zBaSO 4 The ceramics all have a low epsilon r High Qf value and small τ f It can be used as medium antenna and substrate in high-end microwave communication, especially millimeter wave communication. While at the same time having a low epsilon r High Qf value and near zero or positive τ f Single-phase microwave dielectric ceramics are rare, in which near zero τ is f The material can be used for components and parts with high requirements on temperature stability, such as resonators, filters and the like in high-end microwave communication, particularly millimeter wave communication, and has positive tau f Materials are then available for use with tau f Low epsilon, which is generally a large negative value r Ceramic-forming composites, keeping the latter low epsilon r While improving its temperature stability, so that τ can be converted f Near zero or positive values of the material are preferred. xCaSO as shown in Table 1 4 -ySrSO 4 Epsilon of ceramics r And Qf monotonically decreases and increases with increasing x, τ f Monotonically decreases from a positive value to a negative value. X is more than or equal to 0<At 0.4, τ f A large positive value; and x is more than or equal to 0.4 and less than or equal to 0.6, the tau of the material f Near zero. xCaSO as shown in Table 2 4 -zBaSO 4 Of the ceramics r And Qf monotonically decreases and increases with increasing x, τ f The value is monotonously reduced, and the value is close to 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 Of the ceramics r And Qf monotonically increases and decreases with increasing y, τ f Then monotonously rises, y is more than or equal to 0 and less than or equal to 0.45, and is close to zero, 0.45<When y is less than or equal to 1, the value is a large positive value. In addition, τ in tables 1, 2 and 3 f The near-zero components have near-zero tau after combination f And in tables 1 and 3,. Tau f The positive component also has positive tau after combination f Some properties are shown in tables 4 to 7. Thus, at τ f The near zero or positive value is taken as a standard, and the preferable components are determined as follows: 1. the expression is xCaSO 4 -ySrSO 4 Wherein 0 is less than or equal to x<0.4，0.6<y is less than or equal to 1,x + y =1, with low epsilon r High Qf value and positive τ f (ii) a 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, y is more than or equal to 0.4 and less than or equal to 0.6, x + y =1, and has low epsilon r High Qf value and near zero τ f (ii) a 3. The expression is xCaSO 4 -zBaSO 4 Wherein x is more than or equal to 0 and less than or equal to 0.3, z is more than or equal to 0.7 and less than or equal to 1, x + z =1, has low epsilon r High Qf value and near zero τ f (ii) a 4. The expression is ySrSO 4 -zBaSO 4 Wherein y is more than or equal to 0 and less than or equal to 0.45, z is more than or equal to 0.55 and less than or equal to 1, y + z =1, has low epsilon r High Qf value and near zero τ f (ii) a 5. The expression is ySrSO 4 -zBaSO 4 Wherein 0.45<y≤1，0≤z<0.55,y + z =1, with low ε 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 x1 is more than or equal to 0.4 and less than or equal to 0.6, y1 is more than or equal to 0.4 and less than or equal to 0.6, x1+ y1=1, x2 is more than or equal to 0.3, z2 is more than or equal to 0.7 and less than or equal to 1, and x2+ z2=1,0<a<1，0<b<1,a + b =1, having a 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, y1 is more than or equal to 0.4 and less than or equal to 0.6, x1+ y1=1, y2 is more than or equal to 0.45, z2 is more than or equal to 0.55 and less than or equal to 1, and 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 x1 is more than or equal to 0 and less than or equal to 0.3, z1 is more than or equal to 0.7 and less than or equal to 1, x1+ z1=1, y2 is more than or equal to 0 and less than or equal to 0.45, z2 is more than or equal to 0.55 and less than or equal to 1, and y2+ z2=1,0<a<1，0<b<1,a + b =1, having a 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 x1 is not less than 0<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, having a low epsilon r High Qf value and positive τ f 。
The microwave dielectric ceramic has low dielectric constant (epsilon) r = 5.85-10.95) and a high Qf value (15,000-57,000ghz) with an adjustable resonant frequency temperature systemNumber (tau) 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, particularly millimeter wave communication technology on the microwave dielectric ceramic. Wherein, tau f The components with near zero (within plus or minus 10 ppm/DEG C) can be used for components with higher requirements on temperature stability, such as resonators, filters and the like, and tau f Positive components can be used in combination with tau f Low epsilon, which is generally a large negative value r Ceramics forming composites, maintaining a 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 ceramic with low epsilon r High Qf values 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 co-firing property with common metals and the like, thereby having great practical value in industry.

Claims (10)

1. The low dielectric constant sulfate microwave dielectric ceramic is characterized in that: the 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, and z is more than or equal to 0 and less than or equal to 1, x + y + z =1.
2. The low dielectric constant sulfate microwave dielectric ceramic of claim 1, wherein: the expression of the ceramic is xCaSO 4 -ySrSO 4 Wherein 0 is less than or equal to x<0.4，0.6<y≤1，x+y＝1。
3. The low dielectric constant sulfate microwave dielectric ceramic of claim 1, wherein: 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, y is more than or equal to 0.4 and less than or equal to 0.6, and x + y =1.
4. The low dielectric constant sulfate microwave dielectric ceramic of claim 1, wherein: watch of said ceramicsThe expression is xCaSO 4 -zBaSO 4 Wherein x is more than or equal to 0 and less than or equal to 0.3, z is more than or equal to 0.7 and less than or equal to 1, and x + z =1.
5. The low dielectric constant sulfate microwave dielectric ceramic of claim 1, wherein: 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, z is more than or equal to 0.55 and less than or equal to 1, y + z =1.
6. The low dielectric constant sulfate microwave dielectric ceramic of claim 1, wherein: the expression of the ceramic is ySrSO 4 -zBaSO 4 Wherein 0.45<y≤1，0≤z<0.55，y+z＝1。
7. The low dielectric constant sulfate microwave dielectric ceramic of claim 1, wherein: the expression of the ceramic is a (x 1 CaSO) 4 -y1SrSO 4 )-b(x2CaSO 4 -z2BaSO 4 ) Wherein x1 is more than or equal to 0.4 and less than or equal to 0.6, y1 is more than or equal to 0.4 and less than or equal to 0.6, x1+ y1=1, x2 is more than or equal to 0 and less than or equal to 0.3, z2 is more than or equal to 0.7 and less than or equal to 1, and x2+ z2=1,0<a<1，0<b<1，a+b＝1。
8. The low dielectric constant sulfate microwave dielectric ceramic of claim 1, wherein: 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, y1 is more than or equal to 0.4 and less than or equal to 0.6, x1+ y1=1, y2 is more than or equal to 0 and less than or equal to 0.45, z2 is more than or equal to 0.55 and less than or equal to 1, y2+ z2=1,0<a<1，0<b<1，a+b＝1。
9. The low dielectric constant sulfate microwave dielectric ceramic of claim 1, wherein: the expression of the ceramic is a (x 1 CaSO) 4 -z1BaSO 4 )-b(y2SrSO 4 -z2BaSO 4 ) Wherein x1 is more than or equal to 0 and less than or equal to 0.3, z1 is more than or equal to 0.7 and less than or equal to 1, x1+ z1=1, y2 is more than or equal to 0 and less than or equal to 0.45, z2 is more than or equal to 0.55 and less than or equal to 1, and y2+ z2=1,0<a<1，0<b<1，a+b＝1。
10. According to claim 1The low dielectric constant sulfate microwave dielectric ceramic is characterized in that: the expression of the ceramic is a (x 1 CaSO) 4 -y1SrSO 4 )-b(y2SrSO 4 -z2BaSO 4 ) Wherein x1 is not less than 0<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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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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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