CN111635230B - High-quality-factor strontium cerate microwave dielectric ceramic material and preparation method thereof - Google Patents
High-quality-factor strontium cerate microwave dielectric ceramic material and preparation method thereof Download PDFInfo
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 18
- XMHIUKTWLZUKEX-UHFFFAOYSA-N hexacosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCC(O)=O XMHIUKTWLZUKEX-UHFFFAOYSA-N 0.000 title claims abstract description 12
- 229910052712 strontium Inorganic materials 0.000 title claims abstract description 12
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 238000005245 sintering Methods 0.000 claims abstract description 25
- 239000000919 ceramic Substances 0.000 claims abstract description 23
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 19
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 17
- 239000002131 composite material Substances 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 7
- 238000000498 ball milling Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 9
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 8
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 7
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- 239000011812 mixed powder Substances 0.000 claims description 5
- 239000012752 auxiliary agent Substances 0.000 claims description 4
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical compound [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 claims description 4
- 229910000018 strontium carbonate Inorganic materials 0.000 claims description 4
- 230000008595 infiltration Effects 0.000 claims description 3
- 238000001764 infiltration Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 1
- 239000013078 crystal Substances 0.000 abstract description 5
- 230000002159 abnormal effect Effects 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 239000000758 substrate Substances 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 5
- 238000004891 communication Methods 0.000 description 2
- 238000000748 compression moulding Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract
The invention relates to the field of material science, and aims to provide a strontium cerate microwave dielectric ceramic material with a high quality factor and a preparation method thereof. Is prepared from the ceramic base material Sr2CeO4Middle doped composite assistant Li2CO3‑Bi2O3Reducing the sintering temperature to 875-1100 ℃; the chemical expression of the dielectric ceramic material is as follows: (100-a) wt% Sr2CeO4+a wt％Li2CO3‑Bi2O3(ii) a Wherein 0 < a < 4, Li2CO3:Bi2O3The mass ratio of (a) to (b) is 0.25 to 4. The invention is realized by reducing Sr2CeO4The sintering temperature of the ceramic avoids the abnormal growth of ceramic crystal grains, and keeps the stability of the ceramic crystal structure and excellent microwave dielectric property. The invention has simple preparation process, low cost and good repeatability, is suitable for large-scale production, and has wide application prospect in the fields of microwave components such as filters, antennas, dielectric substrates and the like.
Description
Technical Field
The invention belongs to the field of material science, and particularly relates to a high-quality-factor microwave dielectric ceramic material and a preparation method thereof.
Background
In recent years, with the rapid development of technologies such as 5G mobile communication, satellite communication, wireless networks, Bluetooth and the like, microwave devices are developing in the direction of miniaturization, high frequency and light weight, and higher requirements are put forward on microwave dielectric ceramic materials, namely the dielectric constant serialization is carried out so as to meet the requirements of different communication frequency bands; the higher the Q multiplied by f value is, the better the quality factor Q multiplied by f value is, so as to reduce the loss of the device; the lower the sintering temperature, the better the sintering temperature, the microstructure control and energy saving are facilitated; frequency ofThe temperature coefficient is controllable and adjustable. Strontium cerate Sr2CeO4Has extremely high quality factor and moderate dielectric constant, and attracts wide attention. But has the disadvantages that the strontium cerate system has high sintering temperature (1400 ℃), and the crystal phase structure is unstable, thereby limiting the practical application of the strontium cerate system.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects of the existing material system and technology and providing a high-quality-factor microwave dielectric ceramic material with low sintering temperature and stable crystalline phase structure and a preparation method thereof.
In order to solve the technical problem, the solution provided by the invention is as follows:
the high-quality factor strontium cerate microwave dielectric ceramic material is prepared by doping a composite auxiliary agent in a ceramic base material to reduce the sintering temperature to 875-1100 ℃; wherein the chemical formula of the ceramic base material is Sr2CeO4The chemical formula of the composite auxiliary agent is Li2CO3-Bi2O3(ii) a The chemical expression of the dielectric ceramic material is as follows:
(100-a)wt％Sr2CeO4+a wt％Li2CO3-Bi2O3
wherein 0 < a < 4, Li2CO3:Bi2O3The mass ratio of (a) to (b) is 0.25 to 4.
The invention further provides a preparation method of the dielectric ceramic material, which comprises the following steps:
(1) according to SrCO3:CeO2The raw material SrCO is weighed according to the molar ratio of 2:13And CeO2Powder is subjected to ball milling and mixing for 4 hours; pre-burning for 4h at 1150 ℃, and performing secondary ball milling to obtain Sr2CeO4A ceramic base material;
(2) according to Sr2CeO4With Li2CO3-Bi2O3A, Li in a mass ratio of (100-a)2CO3-Bi2O3Li in (1)2CO3And Bi2O3Taking raw material Li with the mass ratio of x to y being 0.25-42CO3And Bi2O3Powder; sr is2CeO4Ceramic base material, Li2CO3And Bi2O3Ball milling and mixing the powder, and then drying;
(3) adding the mixed powder prepared in the step (2) into a polyvinyl alcohol solution, and uniformly mixing; pressing under the pressure of 120MPa to prepare a cylindrical blank;
(4) and (4) sintering the blank obtained in the step (3) for 4 hours at the temperature of 875-.
In the invention, in the step (1), the ball milling and mixing are carried out under the condition of ethanol infiltration.
In the invention, in the step (3), the mass fraction of the polyvinyl alcohol solution is 15%, and the mass percentage of the mixed powder in the polyvinyl alcohol solution is 8%.
Compared with the prior art, the invention has the beneficial effects that:
1. in the microwave dielectric ceramic of the invention, strontium cerate Sr has high Q multiplied by f value2CeO4Is a ceramic base material, by doping with Li2CO3-Bi2O3Composite assistants of Li in sintering process2CO3And Bi2O3Liquid phase is generated, ceramic particles are infiltrated, the sintering mass transfer process is promoted, and the Sr is obviously reduced2CeO4The sintering temperature of the ceramic. Pure Sr2CeO4The sintering temperature range is 1300-1400 ℃; the invention is based on the addition of Li2CO3-Bi2O3The sintering temperature range is reduced to 875-1100 ℃.
2. The invention is realized by reducing Sr2CeO4The sintering temperature of the ceramic avoids the abnormal growth of ceramic crystal grains, and keeps the stability of the ceramic crystal structure and excellent microwave dielectric property. The dielectric constant of the microwave dielectric ceramic material is 13.5-14.5, the Q multiplied by f value is 69000-.
3. The invention has simple preparation process, low cost and good repeatability, is suitable for large-scale production, and has wide application prospect in the fields of microwave components such as filters, antennas, dielectric substrates and the like.
Detailed Description
The following examples are presented to enable those skilled in the art to more fully understand the present invention and are not intended to limit the invention in any way.
Examples
1. According to molar ratio SrCO3:CeO2Weighing SrCO as raw material 2:13And CeO2Ball milling and mixing materials for 4 hours under the condition of ethanol infiltration; baking, pre-sintering at 1150 deg.C for 4 hr to obtain Sr2CeO4And (5) standby.
2. According to the total mass ratio of Sr2CeO4:Li2CO3-Bi2O3A starting materials were prepared with different Li2CO3-Bi2O3Ingredients the chemical formula of the total ingredients can be written as:
P0.5-1 99.5wt％Sr2CeO4-0.4wt％Bi2O3-0.1wt％Li2CO3；(a＝0.5,x:y＝4)
P0.5-2 99.5wt％Sr2CeO4-0.3wt％Bi2O3-0.2wt％Li2CO3；(a＝0.5,x:y＝1.5)
P0.5-3 99.5wt％Sr2CeO4-0.2wt％Bi2O3-0.3wt％Li2CO3；(a＝0.5,x:y＝0.67)
P0.5-4 99.5wt％Sr2CeO4-0.1wt％Bi2O3-0.4wt％Li2CO3；(a＝0.5,x:y＝0.25)
P1-1 99wt％Sr2CeO4-0.8wt％Bi2O3-0.2wt％Li2CO3；(a＝1,x:y＝4)
P1-2 99wt％Sr2CeO4-0.6wt％Bi2O3-0.4wt％Li2CO3；(a＝1,x:y＝1.5)
P1-3 99wt％Sr2CeO4-0.4wt％Bi2O3-0.6wt％Li2CO3；(a＝1,x:y＝0.67)
P1-4 99wt％Sr2CeO4-0.2wt％Bi2O3-0.8wt％Li2CO3；(a＝1,x:y＝0.25)
P4-1 96wt％Sr2CeO4-3.2wt％Bi2O3-0.8wt％Li2CO3；(a＝4,x:y＝4)
P4-2 96wt％Sr2CeO4-2.4wt％Bi2O3-1.6wt％Li2CO3；(a＝4,x:y＝1.5)
P4-3 96wt％Sr2CeO4-1.6wt％Bi2O3-2.4wt％Li2CO3；(a＝4,x:y＝0.67)
P4-4 96wt％Sr2CeO4-0.8wt％Bi2O3-3.2wt％Li2CO3；(a＝4,x:y＝0.25)
3. adding the prepared P0.5-P4 mixed powder into 15% polyvinyl alcohol solution by mass percent according to the mass percent of 8 wt%, uniformly mixing, and performing compression molding under the pressure of 120MPa to prepare a cylindrical blank.
4. And sintering the blank at 875-1100 ℃ for 4h to obtain the strontium cerate microwave dielectric ceramic with high quality factor.
Comparative example
According to SrCO3:CeO2The raw material SrCO is weighed according to the molar ratio of 2:13And CeO2Ball-milling the powder, mixing for 4h, presintering at 1150 ℃ for 4h to obtain pure Sr2CeO4Powder material; pure Sr2CeO4Adding the powder into 15% polyvinyl alcohol solution by mass percent according to the mass percentage of 8 wt%, uniformly mixing, and performing compression molding under the pressure of 120MPa to prepare a cylindrical blank; sintering the blank at 1300 plus 1400 ℃ for 4h to obtain pure Sr2CeO4Microwave dielectric ceramics.
Performance testing
Aiming at pure Sr without addition2CeO4And the product of the invention is used for microwave dielectric property test.
The test instrument is AgilentThe test conditions of the dielectric constant and the Qxf value of the E5071C network analyzer are 25 ℃, 9-10GHz and the test temperature range of the frequency temperature coefficient is 25-80 ℃. Pure Sr without addition2CeO4And the microwave dielectric properties of the product of the invention are shown in tables 1 and 2, respectively.
TABLE 1 pure Sr2CeO4Microwave dielectric properties at different sintering temperatures
TABLE 2 microwave dielectric Properties of P0.5-P4 groups at different sintering temperatures
As can be seen from the data in tables 1 and 2, the vector Sr2CeO4In which a composite assistant Li is added2CO3-Bi2O3After that, the sintering temperature of the ceramic is obviously reduced. When a is 1 and the sintering temperature of the P1-1 group is 1075 ℃, the maximum Q multiplied by f value of the material is more than 100,000 GHz; with Li in the composite assistant2CO3The content is gradually increased, the temperature is further reduced, and the ceramics of the P1-3 group and the P1-4 group can be sintered at the temperature below 950 ℃ and have excellent Q x f value which is more than 65,000 GHz. Therefore, the sintering temperature of the system can be reduced to the temperature range of co-sintering with Ag by doping, so that the practicability is greatly enhanced and the application range of the material is expanded.
Claims (2)
1. A high quality factor strontium cerate microwave dielectric ceramic material is characterized in that a ceramic base material is doped with a composite auxiliary agent to reduce the sintering temperature to 1075 ℃; wherein the chemical formula of the ceramic base material is Sr2CeO4 The chemical formula of the composite auxiliary agent is Li2CO3 - Bi2O3(ii) a In the dielectric ceramic material, Sr2CeO4 ∶Li2CO3∶Bi2O3The mass ratio of the components is 99 to0.8∶0.2；
The dielectric ceramic material is prepared by the following method:
(1) according to SrCO3∶CeO2The raw material SrCO is weighed according to the molar ratio = 2:13And CeO2Powder is mixed by ball milling for 4 hours under the condition of ethanol infiltration; pre-burning for 4h at 1150 ℃, and performing secondary ball milling to obtain Sr2CeO4A ceramic base material;
(2) according to Sr2CeO4 ∶Li2CO3∶Bi2O3Taking raw material Li with the mass ratio of 99: 0.8: 0.22CO3 And Bi2O3Powder; sr is2CeO4Ceramic base material, Li2CO3 And Bi2O3Ball milling and mixing the powder, and then drying;
(3) adding the mixed powder prepared in the step (2) into a polyvinyl alcohol solution with the mass fraction of 15%, wherein the mixed powder accounts for 8% of the mass of the polyvinyl alcohol solution; after being uniformly mixed, the mixture is pressed under the pressure of 120MPa to prepare a cylindrical blank;
(4) and (4) sintering the blank obtained in the step (3) for 4 hours at 1075 ℃ to obtain the strontium cerate microwave dielectric ceramic material with high quality factor.
2. The high-quality-factor strontium cerate microwave dielectric ceramic material as claimed in claim 1, wherein the high-quality factor of the dielectric ceramic material is characterized in that the dielectric ceramic material has a dielectric constant of 14.367, a quality factor of 102023 GHz, and a temperature coefficient of frequency of-69.63 ppm/° C.
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