CN115947600A - 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 particularly relates to a Li-Mg-Mo based single-phase ultralow-temperature ceramic material and a preparation method thereof, wherein the molecular formula is Li 2 Mg 2‑x Na 2x Mo 3 O 12 The material has ultralow sintering temperature and high Q multiplied by f value, and can be used as a substrate material of microwave and terahertz polarization selectors at the same time. The invention adopts a solid-phase reaction method to realize Na + For Li 2 Mg 2 Mo 3 O 12 Medium Mg 2+ To obtain excellent microwave dielectric properties (epsilon) r ＝7.9,Q×f＝43844GHz,τ f = 48.3 ppm/deg.c) and terahertz transmission performance (e) r 1 ＝7.4,tanσ 1 ＝0.0158,T coefficient = 0.598). By using Ag paste and Li with good chemical compatibility 2 Mg 1.94 Na 0.12 Mo 3 O 12 The ceramic material is respectively at 9.7GHz and 0.4 GHzPolarization selection devices for circular polarization and linear polarization are designed under 5THz, and the normalized polarization selection difference of the microwave device and the terahertz device is 0.876 and 0.523 respectively. The invention well solves the problems of dielectric ceramics and ULTCC technology in microwave and terahertz application.
Description
Technical Field
The invention belongs to the technical field of functional ceramic materials, and particularly relates to a Li-Mg-Mo based single-phase ultralow-temperature ceramic material and a preparation method thereof, wherein the molecular formula is Li 2 Mg 2-x Na 2x Mo 3 O 12 The material has ultralow sintering temperature and high Q multiplied by f value, and can be used as a substrate material of microwave and terahertz polarization selectors at the same time.
Background
In communication systems of microwave and terahertz frequency bands, a polarization selection device is generally used as a radome of a 5G/6G base station. Conventional antennas typically have fixed polarization modes (including circularly polarized CP, linearly polarized LP, and elliptically polarized EP) that otherwise do not meet the polarization requirements specified 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 pursuits. Based on the consideration of the indexes, the ceramic material with excellent dielectric property at the same time in the microwave and terahertz frequency bands shows huge potential. The excellent microwave dielectric property and terahertz transmission property mean that the polarization selection requirement of 5G/6G can be realized from the substrate angle.
Ceramic processes are classified into ultra low temperature co-fired ceramic (ULTCC), low temperature co-fired ceramic (LTCC), and high temperature co-fired ceramic (HTCC). Wherein, ULTCC: (A), (B)<650 ℃ has the advantages of low energy consumption, short processing time, high integration degree with semiconductors and metals, and the like. Common ultralow temperature ceramic systems include vanadate, borate, tellurate, molybdate and glass composite ceramics. Li with sintering temperature of exactly 650 DEG C 2 Mg 2 Mo 3 O 12 The ceramic has remarkable advantages in the aspects of microwave dielectric property, terahertz transmission property, ultralow temperature sintering, toxicity and the like. However, applicationsULTCC polarization selection device pair Li in microwave and terahertz frequency bands 2 Mg 2 Mo 3 O 12 The sintering temperature and dielectric properties of ceramic materials are more demanding, so that further reduction of the sintering temperature and improvement of the dielectric properties are required.
Found in experiments to be Na + The substitution has good effects on reducing sintering temperature and improving dielectric property, but because of Na + Due to high activity of the material, pure-phase ceramic substrate materials cannot be obtained in the prior art. The mixed phase often deteriorates the dielectric property of the ceramic and affects the sintering temperature, thus greatly limiting the application range of the material.
Disclosure of Invention
Aiming at the problems or the defects, 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 Realizes Na in a ceramic system + For Mg 2+ The dielectric material can be used as a substrate material of a microwave and terahertz frequency band ULTCC polarization selection device at the same time.
A Li-Mg-Mo based single-phase ultralow temperature ceramic material with a 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 raw materials of each element component are presintered at 550-590 ℃ by a solid phase method, pressed and molded, and then sintered and sintered at 600-650 ℃.
Further, the x =0.09, presintering at 560 ℃ and sintering at 625 ℃; corresponding to the obtained Li 2 Mg 0.91 Na 0.18 Mo 3 O 12 The microwave dielectric property of the ultralow temperature ceramic material is 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, preparation of Li according to molecular formula 2 Mg 2-x Na 2x Mo 3 O 12 (x is not less than 0.03 and not more than 0.12) weighing Li in a 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%.
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 dried material obtained in the step 2 at the temperature of 550-590 ℃ for 2-3 h to obtain a pre-sintered material, wherein the heating and cooling rates are set to be 1-3 ℃/min;
and 4, putting the pre-sintered material obtained in the step 3 into the organic solvent again, performing secondary ball milling, uniformly mixing, and drying.
And 5, granulating the dried material obtained in the step 4 and 10-13 wt% of adhesive (polyvinyl alcohol) to obtain green pellets.
And 6, pressing the green body granules obtained in the step 5 under the pressure of 10-15 MPa to obtain a green body, and keeping 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 0.91 Na 0.18 Mo 3 O 12 The ultra-low temperature ceramic material has the heat preservation time of 2-4 h.
Further, the drying temperature in the step 2 and the drying temperature in the step 4 are both 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 summary, the present invention is described in Li 2 Mg 2 Mo 3 O 12 On the basis of good dielectric property of the ceramic, na is added + For Mg 2+ The pure phase substitution improves the microwave dielectric property and terahertz transmission property of the ceramic. Wherein, the optimal microwave dielectric property is as follows: 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 ULTCC polarization selection in microwave and terahertz frequency bands simultaneouslyThe substrate material of the device is selected.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 shows Li in examples 1 to 5 2 Mg 2-x Na 2x Mo 3 O 12 XRD pattern of ceramic material;
FIG. 3 shows Li in examples 1 to 5 2 Mg 2-x Na 2x Mo 3 O 12 SEM pictures of ceramic materials;
FIG. 4 shows Li in examples 1 to 5 2 Mg 2-x Na 2x Mo 3 O 12 The microwave dielectric properties of the ceramic material;
FIG. 5 shows 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 picture after ceramic and Ag thick liquid are fired together;
FIG. 7 is a demonstration of the circular polarization selection function at 9.7GHz in example 4;
figure 8 is a linear polarization selection functional demonstration at 0.45THz for example 4.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples.
Example 1:
(1) The solid-phase reaction method disposes the material Li 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) Weighing the raw materials according to the formula proportion of the formula shown in the table 1, and sequentially performing ball milling, drying, presintering, granulating, tabletting and sintering on the raw materials 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 ℃ and 650 ℃, the heating rate and the cooling rate are both 2 ℃/min, the heat preservation time is 3h, and the temperature is cooled to 500 ℃ and then is naturally cooled.
Example 2:
(1) The solid-phase reaction method disposes the material Li 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) Weighing the raw materials according to the formula proportion of the formula shown in the table 1, and sequentially performing ball milling, drying, presintering, granulating, tabletting and sintering on the raw materials 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 ℃ and 650 ℃, the heating rate and the cooling rate are both 2 ℃/min, the heat preservation time is 3h, and the temperature is cooled to 500 ℃ and then is naturally cooled.
Example 3:
(1) The solid-phase reaction method is to prepare the material Li 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) Weighing the raw materials according to the formula proportion of the formula shown in the table 1, and sequentially performing ball milling, drying, presintering, granulating, tabletting and sintering on the raw materials 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 ℃ and 650 ℃, the heating rate and the cooling rate are both 2 ℃/min, the heat preservation time is 3h, and the temperature is cooled to 500 ℃ and then is naturally cooled.
Example 4:
(1) The solid-phase reaction method is to prepare the material Li 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) Weighing raw materials according to the formula proportion of the formula shown in the table 1, and sequentially performing ball milling, drying, presintering, granulating, tabletting and sintering on the raw materials 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 ℃ and 650 ℃, the heating rate and the cooling rate are both 2 ℃/min, the heat preservation time is 3h, and the temperature is cooled to 500 ℃ and then is naturally cooled.
Example 5:
(1) The solid-phase reaction method disposes the material Li 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) Weighing the raw materials according to the formula proportion of the formula shown in the table 1, and sequentially performing ball milling, drying, presintering, granulating, tabletting and sintering on the raw materials 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 ℃ and 650 ℃, the heating rate and the cooling rate are both 2 ℃/min, the heat preservation time is 3h, and the temperature is cooled to 500 ℃ and then is naturally cooled.
The materials prepared in the above 5 examples were tested and the results are shown in fig. 2 to 5. The XRD and SEM test results for examples 1-5 are shown in FIG. 2 and FIG. 3, respectively, and it can be seen that Na + Substituted Li 2 Mg 2 Mo 3 O 12 Mg in (1) 2+ No second phase and Na + The substitution favors the growth of rod-like grains.
The ceramic materials prepared in examples 1 to 5 were subjected to microwave dielectric property test, and the test results are shown in FIG. 4. The optimal dielectric property of the microwave is epsilon r =7.9, q × f =43844GHz and τ f = 48.3 ppm/DEG C. The ceramic materials prepared in examples 1 to 5 were subjected to a terahertz transmission performance test, and the test 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。
Using Li obtained in example 4 2 Mg 1.91 Na 0.18 Mo 3 O 12 After the ceramic material is co-fired with the Ag paste, no chemical reaction is found, and the ceramic material has good chemical compatibility, and the XRD and the SEM of an interface are shown in figure 6. Using Li of example 4 2 Mg 1.91 Na 0.18 Mo 3 O 12 The ceramic material as the substrate is provided with polarization selection devices with circular polarization and linear polarization at 9.7GHz and 0.45THz respectively, and the structure and simulation results are shown in fig. 7 and fig. 8. The normalized polarization selection difference of the visible microwave device and the terahertz device is 0.876 and 0.523 respectively.
As can be seen from the above examples, the present invention is in Li 2 Mg 2 Mo 3 O 12 On the basis of ceramics, by Na + For Mg 2+ The pure phase substitution improves the microwave dielectric property and terahertz transmission property of the ceramic, and well solves the problems of the application of the dielectric ceramic and ULTCC technology in the microwave and terahertz fields.
Claims (6)
1. Li-Mg-Mo based single phase ultra low temperature ceramic material characterized by: molecular formula is 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 raw materials of each element component are presintered at 550-590 ℃ by a solid phase method, pressed and molded, and then sintered and sintered at 600-650 ℃.
2. The Li-Mg-Mo based single phase ultra low temperature ceramic material of claim 1 wherein:
the x =0.09, presintering at 560 ℃ and sintering at 625 ℃; corresponding to the obtained Li 2 Mg 0.91 Na 0.18 Mo 3 O 12 The microwave dielectric property of the ultralow temperature ceramic material is 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。
3. The method for preparing the Li-Mg-Mo based single phase ultra low temperature ceramic material of claim 1, comprising the steps of:
step 1, preparation of Li according to molecular formula 2 Mg 2-x Na 2x Mo 3 O 12 Weighing Li using stoichiometric ratio 2 CO 3 、Na 2 CO 3 、MoO 3 And MgO raw material, wherein x is more than or equal to 0.03 and less than or equal to 0.12, and the purities of the raw materials are all 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 dried material obtained in the step 2 at the temperature of 550-590 ℃ for 2-3 h to obtain a pre-sintered material, wherein the heating and cooling rates are set to be 1-3 ℃/min;
step 4, putting the pre-sintered material obtained in the step 3 into the organic solvent again, performing secondary ball milling and uniformly mixing, and then drying;
step 5, granulating the dried material obtained in the step 4 and 10-13 wt% of adhesive to obtain green pellets;
step 6, pressing and forming the green body particles obtained in the step 5 under the pressure of 10-15 MPa to obtain a green body, and keeping 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 0.91 Na 0.18 Mo 3 O 12 The ultra-low temperature ceramic material has the heat preservation time of 2-4 h.
4. The method for preparing the Li-Mg-Mo based single phase ultra low temperature ceramic material of claim 1, wherein: the drying temperature in the step 2 and the drying temperature in the step 4 are both lower than 100 ℃.
5. The method for preparing a Li-Mg-Mo based single phase ultra low temperature ceramic material according to claim 1, wherein: the adhesive in the step 5 is polyvinyl alcohol.
6. The use of the Li-Mg-Mo based single phase ultra low temperature ceramic material of claim 1 wherein: the material is used as a ceramic substrate material of an ULTCC polarization selection device in microwave and terahertz frequency bands.
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