CN117142857A - Temperature-stable composite microwave dielectric ceramic and preparation method thereof - Google Patents
Temperature-stable composite microwave dielectric ceramic and preparation method thereof Download PDFInfo
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- CN117142857A CN117142857A CN202311197507.6A CN202311197507A CN117142857A CN 117142857 A CN117142857 A CN 117142857A CN 202311197507 A CN202311197507 A CN 202311197507A CN 117142857 A CN117142857 A CN 117142857A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 44
- 239000002131 composite material Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 229910010413 TiO 2 Inorganic materials 0.000 claims abstract description 16
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 238000000498 ball milling Methods 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 12
- 238000007873 sieving Methods 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 11
- 238000005245 sintering Methods 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 5
- IGSZZIUPCQHSQB-UHFFFAOYSA-N manganese tantalum Chemical compound [Mn][Ta] IGSZZIUPCQHSQB-UHFFFAOYSA-N 0.000 claims description 5
- 239000000463 material 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
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000011805 ball Substances 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 230000002194 synthesizing effect Effects 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 5
- 239000011787 zinc oxide Substances 0.000 description 4
- 238000004891 communication Methods 0.000 description 2
- 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
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012535 impurity Substances 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
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 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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- C04B35/495—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
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- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3232—Titanium oxides or titanates, e.g. rutile or anatase
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Abstract
The invention provides a temperature-stable composite microwave dielectric ceramic and a preparation method thereof, belonging to the technical field of electronic ceramics. The composition expression of the temperature stable composite microwave dielectric ceramic provided by the invention is ZnTi 0.95 Sc 0.05 Nb 2 O 8 ‑xTiO 2 Wherein x is TiO 2 The x is 0.12-0.14, which is the fraction of the total mass of the composite ceramic. The temperature-stable composite microwave dielectric ceramic provided by the invention has good temperature stability and higher dielectric constant.
Description
Technical Field
The invention relates to the technical field of electronic ceramics, in particular to a temperature-stable composite microwave dielectric ceramic and a preparation method thereof.
Background
In case of the arrival of the interconnecting age, higher requirements are put on the wireless communication technology and related passive devices. The temperature-stable microwave dielectric ceramic is used as a basic key material of passive devices, and is important for realizing a high-performance microwave dielectric resonator.
Temperature-stable microwave dielectric ceramics, i.e. dielectric ceramics having a resonant frequency temperature coefficient (τ) close to zero f ) The central resonant frequency of the device can be ensured not to be changed greatly along with the change of the ambient temperature. In practical applications, the temperature-stabilized microwave dielectric ceramic can reduce temperature variation and center frequency drift caused by thermal expansion of the device housing. For example, in the deployment of communication base stations, application scenes in different areas are complex and changeable, for example, the winter temperature in a part of high-latitude areas can be reduced to 40-50 ℃ below zero, and the summer temperature in certain africa areas can be 40-50 ℃ above zero, which requires that dielectric ceramics for preparing microwave passive devices have good temperature stability.
Disclosure of Invention
In view of the above, the invention aims to provide a temperature-stable composite microwave dielectric ceramic and a preparation method thereof.
In order to achieve the above object, the present invention provides the following technical solutions: a temperature stable composite microwave dielectric ceramic has a composition expression of ZnTi 0.95 Sc 0.05 Nb 2 O 8 -xTiO 2 Wherein x is 0.12 to 0.14, preferably 0.12, 0.13, 0.14.
The invention also provides a preparation method of the temperature-stable composite microwave dielectric ceramic, which comprises the following steps:
1) ZnO is put into 2 、TiO 2 、Sc 2 O 3 、Nb 2 O 5 ZnTi according to the chemical equation 0.95 Sc 0.05 Nb 2 O 8 Weighing required raw materials, mixing the weighed materials, ball milling, drying, crushing, sieving, pre-sintering, and primarily synthesizing the ZnTi of the manganese-tantalum ore structure 0.95 Sc 0.05 Nb 2 O 8 Dielectric ceramic powder;
2) Mixing the powder obtained in the step 1) with TiO 2 Mixing, adding polyvinyl alcohol, ball milling, drying, crushing, sieving, and pressing into cylindrical ceramic green body by using an electric tablet press;
3) And (3) sintering the ceramic green body obtained in the step (2) for 4-8 hours at 1120-1160 ℃ to obtain the temperature-stable composite microwave dielectric ceramic.
Preferably, the ball milling in the step 1) further comprises adding zirconia balls and deionized water or ethanol for ball milling; the ball milling rotating speed is 400 rpm, and the ball milling time is 5-8h.
Preferably, the drying temperature in the step 1) is 100 ℃; the sieving is a 40 mesh sieving.
Preferably, the pre-sintering temperature in the step 1) is 900-950 ℃, and the pre-sintering time is 5-8h.
Preferably, the polyvinyl alcohol of step 2) is added in an amount of ZnTi 0.95 Sc 0.05 Nb 2 O 8 And TiO 2 0.5% -2% of the total mass of the powder.
Preferably, the ball milling time in the step 2) is 10-12h.
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 composite microwave dielectric ceramic and a preparation method thereof, and the composition expression of the temperature-stable composite microwave dielectric ceramic is ZnTi 0.95 Sc 0.05 Nb 2 O 8 -xTiO 2 Wherein x is 0.12-0.14, the temperature stability of the temperature stable composite microwave dielectric ceramic provided by the invention is good, namely, the temperature coefficient of the resonant frequency is near zero, and the temperature stable composite microwave dielectric ceramic has higher dielectric constant.
Drawings
FIG. 1 shows ZnTi obtained in example 1 0.95 Sc 0.05 Nb 2 O 8 -0.13TiO 2 XRD diffractogram of microwave dielectric ceramic.
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) ZnO is put into 2 、TiO 2 、Sc 2 O 3 、Nb 2 O 5 ZnTi according to the chemical equation 0.95 Sc 0.05 Nb 2 O 8 Proportioning, wherein the powder material ratio is as follows: znO (zinc oxide) 2 1.1443g、TiO 2 1.0768g、Sc 2 O 3 0.0245g、Nb 2 O 5 3.7816g. Placing about 5g of powder into a polyester tank, adding 200ml of deionized water and 60g of zirconium balls, ball-milling for 6 hours by using a planetary ball mill, performing unidirectional operation at the rotating speed of 400 rpm, transferring the ball-milled slurry into a drying box, drying at 100 ℃, crushing, sieving with a 40-mesh sieve, placing the sieved powder into a sintering furnace, pre-sintering at 950 ℃, and preserving heat for 5 hours to obtain the ZnTi structure of the manganese-tantalum ore 0.95 Sc 0.05 Nb 2 O 8 Powder material;
2) Mixing the powder obtained in the step 1) with 0.7471g TiO 2 Mixing, adding polyvinyl alcohol, ball milling, drying, crushing, sieving, and pressing into cylindrical ceramic green body by using an electric tablet press; the method comprises the steps of carrying out a first treatment on the surface of the
3) Sintering the green body at 1140 ℃ and preserving heat for 6 hours to prepare ZnTi 0.95 Sc 0.05 Nb 2 O 8 -0.13TiO 2 Composite microwave dielectric ceramic.
The obtained ZnTi 0.95 Sc 0.05 Nb 2 O 8 -0.13TiO 2 As can be seen from FIG. 1, the phase composition of the composite microwave dielectric ceramic is typical complex phase ceramic through X-ray powder diffraction analysis, and the main phase is ZnTi with manganese-tantalum ore structure 0.95 Sc 0.05 Nb 2 O 8 Matching with standard card PDF 48-0323. The second phase is rutile TiO 2 In addition to this, the diffraction peaks of a small amount of impurity phase are contained. Description of ZnTi 0.95 Sc 0.05 Nb 2 O 8 And TiO 2 The composite ceramic is mainly composed of two phases of manganese-tantalum ore and rutileAnd (3) forming the finished product.
Example 2
As in example 1, the difference is that in step 2), znTi is reacted with 0.95 Sc 0.05 Nb 2 O 8 With TiO 2 According to ZnTi 0.95 Sc 0.05 Nb 2 O 8 -0.12TiO 2 Mixing is performed.
Example 3
As in example 1, the difference is that in step 2), znTi is reacted with 0.95 Sc 0.05 Nb 2 O 8 With TiO 2 According to ZnTi 0.95 Sc 0.05 Nb 2 O 8 -0.14TiO 2 Mixing is performed.
Comparative example 1
As in example 1, the difference is that in step 2), znTi is reacted with 0.95 Sc 0.05 Nb 2 O 8 With TiO 2 According to ZnTi 0.95 Sc 0.05 Nb 2 O 8 -0.10TiO 2 Mixing is performed.
Comparative example 2
As in example 1, the difference is that in step 2), znTi is reacted with 0.95 Sc 0.05 Nb 2 O 8 With TiO 2 According to ZnTi 0.95 Sc 0.05 Nb 2 O 8 -0.15TiO 2 Mixing is performed.
The microwave dielectric ceramics of examples 1-3 and comparative examples 1-2 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 1-3 and comparative examples 1-2
As can be seen from Table 1, the microwave dielectric ceramics of examples 1 to 3 of the present invention have more excellent temperature stability, i.e., a near-zero resonance frequency temperature coefficient, than the microwave dielectric ceramics of comparative examples 1 to 2. And has a high dielectric constant. Among them, the microwave dielectric composite properties of the microwave dielectric ceramic of example 1 were relatively optimal.
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 composite microwave dielectric ceramic and a preparation method thereof are characterized in that the composition expression is ZnTi 0.95 Sc 0.05 Nb 2 O 8 -xTiO 2 Wherein x is 0.12 to 0.14.
2. The temperature stable composite microwave dielectric ceramic of claim 1, wherein x is 0.12, 0.13 or 0.14 in the compositional expression.
3. The method for preparing the temperature-stable composite microwave dielectric ceramic according to any one of claims 1 to 2, comprising the steps of:
1) ZnO is put into 2 、TiO 2 、Sc 2 O 3 、Nb 2 O 5 ZnTi according to the chemical equation 0.95 Sc 0.05 Nb 2 O 8 Weighing required raw materials, mixing the weighed materials, ball milling, drying, crushing, sieving, pre-sintering, and primarily synthesizing the ZnTi of the manganese-tantalum ore structure 0.95 Sc 0.05 Nb 2 O 8 Dielectric ceramic powder;
2) Mixing the powder obtained in the step 1) with TiO 2 Mixing, adding polyvinyl alcohol, ball milling, drying, crushing, sieving, and pressing into cylindrical ceramic green body by using an electric tablet press;
3) Sintering the ceramic green body obtained in the step 2) for 4-8 hours at 1120-1160 ℃ to obtain the temperature-stable composite microwave dielectric ceramic.
4. The method of claim 3, wherein the ball milling of step 1) further comprises adding zirconia balls and deionized water or ethanol for ball milling; the ball milling rotating speed is 400 rpm, and the ball milling time is 5-8h.
5. The method of claim 3, wherein the drying temperature in step 1) is 100 ℃; the sieving is a 40 mesh sieving.
6. A method according to claim 3, wherein the pre-sintering temperature in step 1) is 900-950 ℃ and the pre-sintering time is 5-8 hours.
7. The method according to claim 3, wherein the polyvinyl alcohol in step 2) is added in an amount of ZnTi 0.95 Sc 0.05 Nb 2 O 8 And TiO 2 0.5% -2% of the total mass of the powder.
8. The method according to claim 3, wherein the ball milling time in step 2) is 10 to 12 hours.
9. A method of preparation according to claim 3 wherein step 2) the sieving is by a 80 mesh sieve.
10. A method of manufacturing according to claim 3, wherein the ceramic green body of step 2) has a diameter of 10mm and a thickness of 5mm.
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