CN117447196A - Temperature-stable millimeter wave dielectric ceramic and preparation method thereof - Google Patents
Temperature-stable millimeter wave dielectric ceramic and preparation method thereof Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 238000000498 ball milling Methods 0.000 claims description 17
- 238000005245 sintering Methods 0.000 claims description 13
- 238000007873 sieving Methods 0.000 claims description 12
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 9
- 229910017493 Nd 2 O 3 Inorganic materials 0.000 claims description 9
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 9
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 5
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052721 tungsten Inorganic materials 0.000 claims description 4
- 239000010937 tungsten Substances 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 230000002194 synthesizing effect Effects 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 230000000052 comparative effect Effects 0.000 description 4
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910000906 Bronze Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000010974 bronze Substances 0.000 description 1
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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Abstract
The invention provides a temperature-stable millimeter wave dielectric ceramic and a preparation method thereof, belonging to the technical field of electronic ceramics. The composition expression of the temperature stable millimeter wave dielectric ceramic provided by the invention is Ba 4 Nd 9.33‑x Sm x Ti 17.5‑y Hf 0.5 Al y O 54 Wherein x is 0 to 3 and y is 0.5 to 2. The temperature-stable millimeter wave dielectric ceramic provided by the invention has good temperature stability, and simultaneously has adjustable dielectric constant and higher Qf value, and can be matched with the application requirements of passive devices such as a multi-band millimeter wave dielectric resonator, a dielectric metamaterial and the like.
Description
Technical Field
The invention relates to the technical field of electronic ceramics, in particular to a temperature-stable millimeter wave dielectric ceramic and a preparation method thereof.
Background
With the continuous development of 5G millimeter wave technology, the application of multiple scenes under "everything interconnection" puts more stringent requirements (high reliability, high performance, low power consumption, etc.) on the development of contemporary passive devices, and the corresponding millimeter wave dielectric ceramic should have good temperature stability, and simultaneously have a suitable dielectric constant (the dielectric constant is too large to cause signal delay) and lower dielectric loss (the device integration is high, and the power consumption is large to cause the performance deterioration thereof).
In the field of wireless communications, the temperature coefficient of resonant frequency (τ f ) The method is a key index for measuring the temperature stability of passive devices such as a dielectric resonator, a dielectric metamaterial and the like, and the value near zero means that the passive devices have good frequency selection characteristics in a wider temperature area range; meanwhile, the dielectric constant of the ceramic is closely related to the size of the device, and the coverage frequency range of the current 5G millimeter wave technology is wide (24.25 GHz-52.6 GHz), so that a corresponding dielectric constant system is required to match the device requirement of a specific frequency, and the power consumption is kept low. Therefore, in order to cope with the complex application scene and the functional requirement of the 5G millimeter wave, the high-performance temperature-stable millimeter wave dielectric ceramic is a key material necessary for facing the scene.
Disclosure of Invention
In view of the above, the invention aims to provide a temperature-stable millimeter wave dielectric ceramic and a preparation method thereof, and the temperature-stable millimeter wave dielectric ceramic provided by the invention has good temperature stability, adjustable dielectric constant and higher Qf value, and can be matched with application requirements of passive devices such as a multi-band millimeter wave dielectric resonator, a dielectric metamaterial and the like.
In order to achieve the above object and related objects, the present invention provides a temperature-stable millimeter wave dielectric ceramic having a composition expressed by Ba 4 Nd 9.33-x Sm x Ti 17.5-y Hf 0.5 Al y O 54 Wherein x is 0 to 3 and y is 0.5 to 2, preferably after which x is 0, 1, 2 or 3 and y is 0.5, 1, 1.5 or 2.
The invention also provides a preparation method of the temperature-stable millimeter wave dielectric ceramic, which comprises the following steps:
1) BaCO is carried out 3 、Sm 2 O 3 、Nd 2 O 3 、TiO 2 、Al 2 O 3 、Hf 2 O 3 According to the chemical equation Ba 4 Nd 9.33-x Sm x Ti 17.5- y Hf 0.5 Al y O 54 Weighing required raw materials, mixing the weighed materials, ball milling, drying, crushing, sieving, pre-sintering, and primarily synthesizing the single-phase tungsten bronze structure Ba 4 Nd 9.33-x Sm x Ti 17.5-y Hf 0.5 Al y O 54 Dielectric ceramic powder;
2) Adding the medium ceramic powder obtained in the step 1) into polyvinyl alcohol Ding Quanzhi, performing ball milling, drying, crushing, sieving, and pressing into a cylindrical ceramic green body by using an automatic tablet press;
3) Sintering the ceramic green body obtained in the step 2) for 4-8 hours at 1280-1350 ℃ to obtain a temperature-stable millimeter wave dielectric ceramic sample.
Preferably, the ball milling in the step 1) further comprises adding zirconia balls and absolute ethyl alcohol for ball milling; the ball milling rotating speed is 400 rpm, and the ball milling time is 4-10h.
Preferably, the drying temperature in the step 1) is 80 ℃; the sieving is that a 40-mesh sieve is firstly adopted, and then an 80-mesh sieve is adopted.
Preferably, the pre-sintering temperature in the step 1) is 1150-1200 ℃, and the pre-sintering time is 4-8h.
Preferably, the adding amount of the polyvinyl alcohol Ding Quanzhi in the step 2) is 0.8-1.5% of the mass of the powder.
Preferably, the ball milling time in the step 2) is 10-14h.
Preferably, the sieving in step 2) is through an 80 mesh sieve.
Preferably, the ceramic green body of step 2) has a diameter of 10mm and a thickness of 5mm.
The beneficial technical effects are as follows:
the invention provides a temperature-stable millimeter wave dielectric ceramic and a preparation method thereof, the composition expression of the temperature-stable millimeter wave dielectric ceramic is Ba 4 Nd 9.33-x Sm x Ti 17.5-y Hf 0.5 Al y O 54 Wherein x is 0-3, y is 0.5-2, the temperature stability of the millimeter wave dielectric ceramic provided by the invention is good, and the ceramic has adjustable dielectric constant and higher Qf value, and can be matched with a multi-band millimeter wave dielectricPassive device application requirements such as resonators, dielectric metamaterials and the like.
Drawings
FIG. 1 shows the Ba obtained in example 1 4 Nd 7.33 Sm 2 Ti 16 Hf 0.5 Al 1.5 O 54 XRD diffractogram of microwave dielectric ceramic.
FIG. 2 shows the Ba obtained in example 1 4 Nd 7.33 Sm 2 Ti 16 Hf 0.5 Al 1.5 O 54 SEM pictures of microwave dielectric ceramics.
Detailed Description
For a better understanding of the present invention, the following examples are further illustrated, but are not limited to the following examples.
Example 1
1) BaCO is carried out 3 、Sm 2 O 3 、Nd 2 O 3 、TiO 2 、Al 2 O 3 、Hf 2 O 3 Stoichiometric Ba 4 Nd 7.33 Sm 2 Ti 16 Hf 0.5 Al 1.5 O 54 And (5) batching. Placing about 10g of powder into a polyester tank, adding 200ml of absolute ethyl alcohol and 150g of zirconium balls, ball-milling for 6 hours by using a planetary ball mill, performing unidirectional operation at the rotation speed of 400 rpm, transferring the ball-milled slurry into a drying oven, drying at 80 ℃, crushing, sieving with a 40-mesh sieve, sieving with a 80-mesh sieve, placing the sieved powder into a sintering furnace, pre-sintering at 1185 ℃, and preserving heat for 4 hours;
2) Adding 1wt% of polyvinyl alcohol Ding Quanzhi into the pre-sintered powder in the step 1, mixing, putting into a ball milling tank, adding zirconia balls and absolute ethyl alcohol, ball milling for 12 hours, drying, crushing, sieving with an 80-mesh sieve, and pressing into a cylindrical ceramic green body by an automatic tablet press under the pressure of 2 MPa;
3) Sintering the ceramic green body at 1300 ℃, and preserving heat for 6 hours to prepare Ba 4 Nd 7.33 Sm 2 Ti 16 Hf 0.5 Al 1.5 O 54 Temperature stable millimeter wave dielectric ceramic.
The obtained Ba 4 Nd 7.33 Sm 2 Ti 16 Hf 0.5 Al 1.5 O 54 As can be seen from FIG. 1, the phase composition of the ceramic is a typical tungsten bronze structure which is matched with the standard card PDF#89-4356 through X-ray powder diffraction analysis, and other redundant diffraction peaks are not found, so that the phase composition of other oxides is unchanged due to the introduction. As can be seen from fig. 1, the resulting sample exhibited rod-shaped grains, conforming to the crystalline characteristics of the tungsten bronze structured ceramic.
Example 2
As in example 1, the difference is that BaCO 3 、Sm 2 O 3 、Nd 2 O 3 、TiO 2 、Al 2 O 3 、Hf 2 O 3 Stoichiometric Ba 4 Nd 6.33 Sm 3 Ti 16.5 Hf 0.5 AlO 54 And (5) batching.
Example 3
As in example 1, the difference is that BaCO 3 、Sm 2 O 3 、Nd 2 O 3 、TiO 2 、Al 2 O 3 、Hf 2 O 3 Stoichiometric Ba 4 Nd 8.33 SmTi 15.5 Hf 0.5 Al 2 O 54 And (5) batching.
Example 4
As in example 1, the difference is that BaCO 3 、Sm 2 O 3 、Nd 2 O 3 、TiO 2 、Al 2 O 3 、Hf 2 O 3 Stoichiometric Ba 4 Nd 6.33 Sm 3 Ti 17 Hf 0.5 Al 0.5 O 54 And (5) batching.
Comparative example 1
As in example 1, the difference is that BaCO 3 、Sm 2 O 3 、Nd 2 O 3 、TiO 2 、Al 2 O 3 、Hf 2 O 3 Stoichiometric Ba 4 Nd 7.33 Sm 2 Ti 16 Hf 0.5 Al 1.5 O 54 Batching is carried out, and the sintering temperature is 1280 ℃.
As in example 1, the difference is that BaCO 3 、Sm 2 O 3 、Nd 2 O 3 、TiO 2 、Al 2 O 3 、Hf 2 O 3 Stoichiometric Ba 4 Nd 7.33 Sm 2 Ti 16 Hf 0.5 Al 1.5 O 54 The ingredients were dosed at a sintering temperature of 1330 ℃.
As in example 1, the difference is that BaCO 3 、Sm 2 O 3 、Nd 2 O 3 、TiO 2 、Al 2 O 3 、Hf 2 O 3 Stoichiometric Ba 4 Nd 7.33 Sm 2 Ti 16 Hf 0.5 Al 1.5 O 54 Proportioning and sintering at 1350 deg.C.
The microwave dielectric ceramics of examples 1 to 4 and comparative examples 1 to 3 were tested for microwave dielectric properties by a network analyzer, and the test results are shown in table 1.
TABLE 1 microwave dielectric Properties of examples 1-5 and comparative examples 1-3
As can be seen from Table 1, the millimeter wave dielectric ceramics of examples 1 to 4 of the present invention have more excellent overall dielectric properties than the millimeter wave dielectric ceramics of comparative examples 1 to 3. Among them, the millimeter wave dielectric ceramic of example 1 is the best in comprehensive dielectric properties.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (10)
1. A temperature stable millimeter wave dielectric ceramic is characterized in that the composition expression is Ba 4 Nd 9.33-x Sm x Ti 17.5- y Hf 0.5 Al y O 54 Wherein x is 0 to 3 and y is 0.5 to 2.
2. The temperature-stabilized millimeter wave dielectric ceramic of claim 1, wherein in said composition expression, x is 0, 1, 2 or 3 and y is 0.5, 1, 1.5 or 2.
3. The method for preparing the temperature-stable millimeter wave dielectric ceramic according to any one of claims 1 to 2, comprising the following steps:
1) BaCO is carried out 3 、Sm 2 O 3 、Nd 2 O 3 、TiO 2 、Al 2 O 3 、Hf 2 O 3 According to the chemical equation Ba 4 Nd 9.33-x Sm x Ti 17.5- y Hf 0.5 Al y O 54 Weighing required raw materials, mixing the weighed materials, ball milling, drying, crushing, sieving, presintering, and primarily synthesizing the single-phase tungsten bronze structure Ba 4 Nd 9.33-x Sm x Ti 17.5-y Hf 0.5 Al y O 54 Dielectric ceramic powder;
2) Adding the medium ceramic powder obtained in the step 1) into polyvinyl alcohol Ding Quanzhi, performing ball milling, drying, crushing, sieving, and pressing into a cylindrical ceramic green body by using an automatic tablet press;
3) Sintering the ceramic green body obtained in the step 2) for 4-8 hours at 1280-1350 ℃ to obtain a temperature-stable millimeter wave dielectric ceramic sample.
4. The method for preparing temperature-stable millimeter wave dielectric ceramic according to claim 3, wherein the ball milling in step 1) further comprises adding zirconia balls and absolute ethyl alcohol for ball milling; the ball milling rotating speed is 400 rpm, and the ball milling time is 4-10h.
5. The method for preparing a temperature-stable millimeter wave dielectric ceramic according to claim 3, wherein the drying temperature in step 1) is 80 ℃; the sieving is that a 40-mesh sieve is firstly adopted, and then an 80-mesh sieve is adopted.
6. The method for preparing a temperature-stabilized millimeter wave dielectric ceramic according to claim 3, wherein the pre-sintering temperature in step 1) is 1150-1200 ℃ and the pre-sintering time is 4-8h.
7. The method for preparing temperature-stable millimeter wave dielectric ceramic according to claim 3, wherein the adding amount of the polyvinyl alcohol Ding Quanzhi in the step 2) is 0.8-1.5% of the mass of the powder.
8. The method for preparing temperature-stable millimeter wave dielectric ceramic according to claim 3, wherein the ball milling time in the step 2) is 10-14h.
9. The method for preparing a temperature-stabilized millimeter wave dielectric ceramic according to claim 3, wherein the sieving in the step 2) is 80 mesh sieving.
10. The method for preparing a temperature-stable millimeter wave dielectric ceramic according to claim 3, wherein the ceramic green body in step 2) has a diameter of 10mm and a thickness of 5mm.
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