CN115947600B - Li-Mg-Mo-based single-phase ultralow-temperature ceramic material and preparation method thereof - Google Patents
Li-Mg-Mo-based single-phase ultralow-temperature ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of functional ceramic materials, and in particular relates to a Li-Mg-Mo-based single-phase ultralow-temperature ceramic material and a preparation method thereof, wherein the molecular formula of the Li-Mg-Mo-based single-phase ultralow-temperature ceramic material is Li 2 Mg 2‑x Na 2x Mo 3 O 12 The material has ultra-low sintering temperature and high Q multiplied by f value, and can be used as a substrate material of microwave and terahertz polarization selector. The invention adopts a solid phase reaction method to realize Na + For Li 2 Mg 2 Mo 3 O 12 Middle Mg 2+ Is subjected to pure phase substitution to obtain excellent microwave dielectric properties (. Epsilon.) r ＝7.9,Q×f＝43844GHz,τ f = -48.3ppm/°c) and terahertz transmission performance (epsilon) r 1 ＝7.4,tanσ 1 ＝0.0158,T coefficient =0.598). Ag paste and Li with good chemical compatibility 2 Mg 1.94 Na 0.12 Mo 3 O 12 The ceramic material is respectively designed with a circular polarization selection device and a linear polarization selection device at 9.7GHz and 0.45THz, and the normalized polarization selection difference of the microwave device and the terahertz device is respectively 0.876 and 0.523. The invention well solves the problems of dielectric ceramics and ULTCC technology in microwave and terahertz applications.
Description
Technical Field
The invention belongs to the technical field of functional ceramic materials, and in particular relates to a Li-Mg-Mo-based single-phase ultralow-temperature ceramic material and a preparation method thereof, wherein the molecular formula of the Li-Mg-Mo-based single-phase ultralow-temperature ceramic material is Li 2 Mg 2-x Na 2x Mo 3 O 12 The material has ultra-low sintering temperature and high Q multiplied by f value, and can be used as a substrate material of microwave and terahertz polarization selector.
Background
In communication systems in the microwave and terahertz frequency bands, polarization selection devices are typically used as radomes for 5G/6G base stations. Conventional antennas typically have a fixed polarization mode (including circular polarization CP, linear polarization LP, and elliptical polarization EP) that otherwise fails to meet the requirements for a prescribed polarization in the operating environment, which greatly facilitates the development of polarization selection devices. High efficiency, high frequency, multi-band, and low delay have become current pursuit indicators. Based on these index considerations, ceramic materials having excellent dielectric properties in both the microwave and terahertz frequency bands show great potential. Its excellent microwave dielectric properties and terahertz transmission properties mean that there is an opportunity to achieve the 5G/6G polarization selection requirement from the substrate perspective.
Ceramic processes are classified into ultra low temperature co-fired ceramics (ULTCC), low temperature co-fired ceramics (LTCC) and high temperature co-fired ceramics (HTCC). Wherein ULTCC @ is<650 ℃ has the advantages of low energy consumption, short processing time, high integration level with semiconductors and metals, and the like. Common ultra-low temperature ceramic systems are vanadate, borate, tellurate, molybdate and glass composite ceramics. Li with sintering temperature of 650 DEG C 2 Mg 2 Mo 3 O 12 Ceramics, though, are notable for microwave dielectric properties, terahertz transmission properties, ultra-low temperature sintering, toxicity, and the like. However, ULTCC polarization selection device pair Li applied to microwave and terahertz frequency bands 2 Mg 2 Mo 3 O 12 The sintering temperature and dielectric properties of ceramic materials are more demanding, and thus further reductions in sintering temperature and improvements in dielectric properties are required.
Experiments find Na + The substitution has good effects of reducing sintering temperature and improving dielectric property, but due to Na + The prior art cannot obtain pure phase ceramic substrate materials due to the high activity of the material. The mixed phase tends to deteriorate the dielectric property of the ceramic and affect the sintering temperature, so that the application range of the material is greatly limited.
Disclosure of Invention
Aiming at the problems or the shortcomings, the invention provides a Li-Mg-Mo-based single-phase ultralow-temperature ceramic material and a preparation method thereof. In Li 2 Mg 2 Mo 3 O 12 Na is realized in the ceramic system + For Mg 2+ The pure phase substitution of the material maintains excellent microwave dielectric property and terahertz transmission property at the ultra-low sintering temperature, and can be used as a substrate material of a microwave and terahertz frequency band ULTCC polarization selection device.
Li-Mg-Mo based single-phase ultralow-temperature ceramic material with molecular formula of Li 2 Mg 2-x Na 2x Mo 3 O 12 X is more than or equal to 0.03 and less than or equal to 0.12; the solid phase method is adopted to presintere the raw materials of each element component at 550-590 ℃, and then sinter and sinter the raw materials at 600-650 ℃ after compression molding.
Further, the x=0.09, the presintering is carried out at 560 ℃ and the sintering is carried out at 625 ℃; corresponding to the obtained Li 2 Mg 0.91 Na 0.18 Mo 3 O 12 The microwave dielectric properties of the ultralow-temperature ceramic material are as follows: epsilon r ＝7.9,Q×f＝43844GHz,τ f -48.3ppm/°c; the terahertz transmission performance is as follows: epsilon r 1 ＝7.4,tanσ 1 ＝0.0158,T coefficient ＝0.598。
The preparation method of the Li-Mg-Mo-based single-phase ultralow-temperature ceramic material comprises the following steps:
step 1, according to the molecular formula Li 2 Mg 2-x Na 2x Mo 3 O 12 (0.03.ltoreq.x.ltoreq.0.12) Li is weighed using the stoichiometric ratio 2 CO 3 、Na 2 CO 3 、MoO 3 And MgO raw material, the purity of the raw material is more than 98 percent.
And 2, ball-milling and uniformly mixing the raw materials weighed in the step 1 in an organic solvent, and then drying.
Step 3, calcining the drying material obtained in the step 2 for 2-3 hours at 550-590 ℃ to obtain a presintered material, wherein the heating and cooling rates are set to be 1-3 ℃/min;
and step 4, putting the presintered material obtained in the step 3 into an organic solvent again, performing secondary ball milling and mixing uniformly, and then drying.
And 5, granulating the drying material obtained in the step 4 and 10-13 wt% of binder (polyvinyl alcohol) to obtain green granules.
And 6, pressing and forming the green body granules obtained in the step 5 under the pressure of 10-15 MPa to obtain a green body, wherein the pressure maintaining time is 60-120 s.
Step 7, sintering the green body obtained in the step 6 at 600-650 ℃ to obtain Li 2 Mg 0.91 Na 0.18 Mo 3 O 12 The ultralow temperature ceramic material has heat preservation time of 2-4 hr.
Further, the drying temperature in the step 2 and the step 4 is lower than 100 ℃.
Furthermore, the Li-Mg-Mo-based single-phase ultralow-temperature ceramic material is used as a ceramic substrate material to be applied to ULTCC polarization selection devices in microwave and terahertz frequency bands.
In conclusion, the invention is characterized in Li 2 Mg 2 Mo 3 O 12 On the basis of good dielectric properties of ceramics, the ceramic is prepared by Na + For Mg 2+ The pure phase substitution of the ceramic improves the microwave dielectric property and terahertz transmission property of the ceramic. Wherein, the optimal microwave dielectric properties are: epsilon r ＝7.9,Q×f＝43844GHz,τ f -48.3ppm/°c. The optimal terahertz transmission performance is as follows: epsilon r 1 ＝7.4,tanσ 1 ＝0.0158,T coefficient =0.598. Can be used as a substrate material of a ULTCC polarization selection device in microwave and terahertz frequency bands simultaneously.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is Li in examples 1 to 5 2 Mg 2-x Na 2x Mo 3 O 12 XRD pattern of the ceramic material;
FIG. 3 is Li in examples 1 to 5 2 Mg 2-x Na 2x Mo 3 O 12 SEM images of ceramic materials;
FIG. 4 is Li in examples 1 to 5 2 Mg 2-x Na 2x Mo 3 O 12 Microwave dielectric properties of ceramic materials;
FIG. 5 is Li in examples 1 to 5 2 Mg 2-x Na 2x Mo 3 O 12 Terahertz transmission performance of the ceramic material;
FIG. 6 is Li in example 4 2 Mg 1.91 Na 0.18 Mo 3 O 12 SEM image of ceramic and Ag paste after cofiring;
FIG. 7 is a demonstration of the circular polarization selection function of example 4 at 9.7 GHz;
fig. 8 is a demonstration of the linear polarization selection function at 0.45THz for example 4.
Detailed Description
The invention is described in further detail below with reference to the drawings and examples.
Example 1:
(1) The solid phase reaction method comprises preparing Li material according to the following raw material composition 2 Mg 2 Mo 3 O 12 。
Table 1: example 1 formulation table (Unit: mol)
| Li 2 CO 3 | Na 2 CO 3 | MoO 3 | MgO |
| 1 | 0 | 3 | 2 |
(2) Raw materials are weighed according to the formula proportion of the table 1, and the raw materials are subjected to ball milling, drying, presintering, granulating, tabletting and sintering in sequence to obtain the ceramic material. Wherein the concentration of the polyvinyl alcohol adhesive is 12wt%, the drying temperature is 80 ℃, the presintering temperature is 560 ℃, the presintering time is 2h, the molding pressure is 10MPa, the pressure maintaining time is 60s, the sintering temperature is 600 ℃,625 ℃, 650 ℃, the heating rate and the cooling rate are 2 ℃/min, the heat preservation time is 3h, and the temperature is naturally cooled after 500 ℃.
Example 2:
(1) The solid phase reaction method comprises preparing Li material according to the following raw material composition 2 Mg 1.97 Na 0.06 Mo 3 O 12 。
Table 1: example 1 formulation table (Unit: mol)
| Li 2 CO 3 | Na 2 CO 3 | MoO 3 | MgO |
| 1 | 0.03 | 3 | 1.97 |
(2) Raw materials are weighed according to the formula proportion of the table 1, and the raw materials are subjected to ball milling, drying, presintering, granulating, tabletting and sintering in sequence to obtain the ceramic material. Wherein the concentration of the polyvinyl alcohol adhesive is 12wt%, the drying temperature is 80 ℃, the presintering temperature is 560 ℃, the presintering time is 2h, the molding pressure is 10MPa, the pressure maintaining time is 60s, the sintering temperature is 600 ℃,625 ℃, 650 ℃, the heating rate and the cooling rate are 2 ℃/min, the heat preservation time is 3h, and the temperature is naturally cooled after 500 ℃.
Example 3:
(1) The solid phase reaction method comprises preparing Li material according to the following raw material composition 2 Mg 1.94 Na 0.12 Mo 3 O 12 。
Table 1: example 1 formulation table (Unit: mol)
| Li 2 CO 3 | Na 2 CO 3 | MoO 3 | MgO |
| 1 | 0.06 | 3 | 1.94 |
(2) Raw materials are weighed according to the formula proportion of the table 1, and the raw materials are subjected to ball milling, drying, presintering, granulating, tabletting and sintering in sequence to obtain the ceramic material. Wherein the concentration of the polyvinyl alcohol adhesive is 12wt%, the drying temperature is 80 ℃, the presintering temperature is 560 ℃, the presintering time is 2h, the molding pressure is 10MPa, the pressure maintaining time is 60s, the sintering temperature is 600 ℃,625 ℃, 650 ℃, the heating rate and the cooling rate are 2 ℃/min, the heat preservation time is 3h, and the temperature is naturally cooled after 500 ℃.
Example 4:
(1) The solid phase reaction method comprises preparing Li material according to the following raw material composition 2 Mg 1.91 Na 0.18 Mo 3 O 12 。
Table 1: example 1 formulation table (Unit: mol)
| Li 2 CO 3 | Na 2 CO 3 | MoO 3 | MgO |
| 1 | 0.09 | 3 | 1.91 |
(2) Raw materials are weighed according to the formula proportion of the table 1, and the raw materials are subjected to ball milling, drying, presintering, granulating, tabletting and sintering in sequence to obtain the ceramic material. Wherein the concentration of the polyvinyl alcohol adhesive is 12wt%, the drying temperature is 80 ℃, the presintering temperature is 560 ℃, the presintering time is 2h, the molding pressure is 10MPa, the pressure maintaining time is 60s, the sintering temperature is 600 ℃,625 ℃, 650 ℃, the heating rate and the cooling rate are 2 ℃/min, the heat preservation time is 3h, and the temperature is naturally cooled after 500 ℃.
Example 5:
(1) The solid phase reaction method comprises preparing Li material according to the following raw material composition 2 Mg 1.88 Na 0.24 Mo 3 O 12 。
Table 1: example 1 formulation table (Unit: mol)
| Li 2 CO 3 | Na 2 CO 3 | MoO 3 | MgO |
| 1 | 0.24 | 3 | 1.88 |
(2) Raw materials are weighed according to the formula proportion of the table 1, and the raw materials are subjected to ball milling, drying, presintering, granulating, tabletting and sintering in sequence to obtain the ceramic material. Wherein the concentration of the polyvinyl alcohol adhesive is 12wt%, the drying temperature is 80 ℃, the presintering temperature is 560 ℃, the presintering time is 2h, the molding pressure is 10MPa, the pressure maintaining time is 60s, the sintering temperature is 600 ℃,625 ℃, 650 ℃, the heating rate and the cooling rate are 2 ℃/min, the heat preservation time is 3h, and the temperature is naturally cooled after 500 ℃.
The materials prepared in the above 5 examples were tested and the results obtained are shown in fig. 2 to 5. XRD and SEM test results for examples 1-5 are shown in FIGS. 2 and 3, respectively, and it can be seen that Na + Substituted Li 2 Mg 2 Mo 3 O 12 Mg of (B) 2+ No second phase appeared and Na + Substitution is beneficial to the growth of rod-shaped grains.
The ceramic materials prepared in examples 1 to 5 were subjected to a microwave dielectric property test, and the test results are shown in fig. 4. Optimum microwave dielectric properties are ε r =7.9, q×f= 43844GHz and τ f -48.3ppm/°c. The ceramic materials prepared in examples 1 to 5 were subjected to terahertz transmission performance testThe results are shown in FIG. 5. The optimal terahertz transmission performance is epsilon r 1 ＝7.4,tanσ 1 =0.0158 and T coefficient ＝0.598。
Li obtained in example 4 2 Mg 1.91 Na 0.18 Mo 3 O 12 After co-firing with Ag paste, the ceramic material did not show any chemical reaction, had good chemical compatibility, and the XRD and SEM of the interface were shown in fig. 6. Li of example 4 2 Mg 1.91 Na 0.18 Mo 3 O 12 The ceramic material is used as a substrate to respectively design a circular polarization selection device and a linear polarization selection device at 9.7GHz and 0.45THz, and the structure and simulation results are shown in fig. 7 and 8. The normalized polarization selection differences for the microwave device and the terahertz device were found to be 0.876 and 0.523, respectively.
As can be seen from the above examples, the present invention is embodied in Li 2 Mg 2 Mo 3 O 12 On the basis of ceramics, through Na + For Mg 2+ The pure phase substitution of the ceramic improves the microwave dielectric property and the terahertz transmission property of the ceramic, and well solves the problems of the dielectric ceramic and ULTCC technology in the application of the microwave and terahertz fields.
Claims (6)
1. A Li-Mg-Mo based single-phase ultralow temperature ceramic material is characterized in that: molecular formula is Li 2 Mg x2- Na x2 Mo 3 O 12 ，0.03≤xLess than or equal to 0.12; the solid phase method is adopted to presintere the raw materials of the element components at 550-590 ℃, and then sinter the raw materials at 600-650 ℃ after compression molding.
2. The Li-Mg-Mo based single-phase ultra-low temperature ceramic material according to claim 1, wherein:
taking outx=0.09, and pre-sintered at 560 ℃,625 ℃; corresponding to the obtained Li 2 Mg 1.91 Na .018 Mo 3 O 12 The microwave dielectric properties of the ultralow-temperature ceramic material are as follows:ε r = 7.9, Q×f = 43844 GHz, τ f -48.3ppm/°c; terahertz waveThe transmission performance is as follows:ε r 1 = 7.4,tanσ 1 = 0.0158, T coefficient = 0.598。
3. the method for preparing the Li-Mg-Mo based single-phase ultralow temperature ceramic material according to claim 1, comprising the steps of:
step 1, according to the molecular formula Li 2 Mg x2- Na x2 Mo 3 O 12 Weighing Li using stoichiometric ratio 2 CO 3 、Na 2 CO 3 、MoO 3 And MgO raw material, the content of which is 0.03 to less than or equal toxThe purity of the raw materials is less than or equal to 0.12, and the purity of the raw materials is more than 98 percent;
step 2, ball-milling and uniformly mixing the raw materials weighed in the step 1 in an organic solvent, and then drying;
step 3, calcining the drying material obtained in the step 2 at 550-590 ℃ for 2-3 hours to obtain a presintered material, wherein the heating and cooling rates are set to be 1-3 ℃/min;
step 4, putting the presintered material obtained in the step 3 into an organic solvent again, performing secondary ball milling and mixing uniformly, and then drying;
step 5, granulating the drying material obtained in the step 4 and 10-13 wt% of adhesive to obtain green granules;
step 6, pressing and forming the green granules obtained in the step 5 under the pressure of 10-15 MPa to obtain a green body, and maintaining the pressure for 60-120 s;
step 7, sintering the green body obtained in the step 6 at 600-650 ℃ to obtain Li 2 Mg x2- Na x2 Mo 3 O 12 The ultralow-temperature ceramic material has the heat preservation time of 2-4 hours.
4. The method for preparing the Li-Mg-Mo based single-phase ultralow temperature ceramic material according to claim 3, wherein: the drying temperature in the step 2 and the step 4 is lower than 100 ℃.
5. The method for preparing the Li-Mg-Mo based single-phase ultralow temperature ceramic material according to claim 3, wherein: the adhesive in the step 5 is polyvinyl alcohol.
6. The use of a Li-Mg-Mo based single-phase ultra-low temperature ceramic material according to claim 1, characterized in that: the material is used as a ceramic substrate material of a ULTCC polarization selection device in microwave and terahertz frequency bands.
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