Nb-based composite microwave dielectric ceramic material and preparation method thereof

A microwave dielectric ceramic and niobium-based technology, which is applied in the field of niobium-based microwave dielectric ceramic materials and their preparation, can solve the problems of large absolute value, insignificant change of frequency temperature coefficient, and inability to meet the application needs of microwave devices, thereby reducing the preparation cost. , the effect of abundant reserves and high Q×f value

Inactive Publication Date: 2017-06-30
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Researchers changed niobite ZnNb 2 o 6 The molar ratio of zinc-site ions in the middle, found that Zn 3 Nb 2 o 8 It still has a niobite structure, but its quality factor becomes higher (Q×f~83300GHz), and the frequency temperature coefficient changes to a negative direction (τ f ~-71ppm / ℃); Recently, we reported in the journal "Journal of Materials Science: Materials in Electronics" that (Zn 0.95 Ni 0.05 ) 3 Nb 2 o 8 Ceramics, the crystal structure of ceramics has not changed, and the microwave dielectric properties at a temperature of 1160 ° C: ε r ~21.81, Q×f~123558GHz, τ f ~-78.45ppm / ℃, it can be seen that the quality factor of the system has further improved significantly, but the frequency temperature coefficient does not change significantly, and the absolute value is still relatively large, which cannot meet the application needs of microwave devices

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024]Analytical pure (purity ≥ 99%) ZnO, NiO, TiO 2 and Nb 2 o 5 As a raw material, according to (1-x)(Zn 0.95 Ni 0.05 ) 3 Nb 2 o 8 -xNi 0.5 Ti 0.5 NbO 4 (wherein x is mole fraction, and x=0.5) the stoichiometric ratio carries out batching.

[0025] Concrete preparation steps are as follows:

[0026] (1) will analyze pure ZnO, NiO, and Nb 2 o 5 As a raw material (purity ≥ 99%), the ingredients are weighed in a molar ratio of 2.85:0.15:1, and then the weighed ZnO, NiO, and Nb 2 o 5 Put it into a nylon ball mill tank, the volume ratio of raw materials, ball milling medium, and deionized water is 1:1:1, use a planetary ball mill for ball milling, the ball mill speed is 400 rpm, ball mill on the ball mill for 12 hours, and then grind at 100°C Drying under the bottom, passed through 80 mesh sieve, and pre-fired to make (Zn 0.95 Ni 0.05 ) 3 Nb 2 o 8 , the calcining temperature is 1100℃, and the calcining time is 3h. 0.95 Ni 0.05 ) 3 Nb 2 o 8 Pre-fired powder...

Embodiment 2

[0033] Analytical pure (purity ≥ 99%) ZnO, NiO, TiO 2 and Nb 2 o 5 As a raw material, according to (1-x)(Zn 0.95 Ni 0.05 ) 3 Nb 2 o 8 -xNi 0.5 Ti 0.5 NbO 4 (wherein x is the mole fraction, and x=0.55) the stoichiometric ratio carries out batching.

[0034] Concrete preparation steps are as follows:

[0035] (1) will analyze pure ZnO, NiO, and Nb 2 o 5 As a raw material (purity ≥ 99%), weigh the ingredients in a molar ratio of 2.85:0.15:1, and weigh ZnO, NiO, and Nb 2 o 5 Put it into a nylon ball mill tank, the volume ratio of raw materials, ball milling medium, and deionized water is 1:1:1, use a planetary ball mill for ball milling, the ball mill speed is 400 rpm, ball mill on the ball mill for 12 hours, and then grind at 100°C Drying under the bottom, passed through 80 mesh sieve, and pre-fired to make (Zn 0.95 Ni 0.05 ) 3 Nb 2 o 8 , the calcining temperature is 1100℃, and the calcining time is 3h. 0.95 Ni 0.05 ) 3 Nb 2 o 8 Pre-fired powder;

[0036]...

Embodiment 3

[0042] Analytical pure (purity ≥ 99%) ZnO, NiO, TiO 2 and Nb 2 o 5 As a raw material, according to (1-x)(Zn 0.95 Ni 0.05 ) 3 Nb 2 o 8 -xNi 0.5 Ti 0.5 NbO 4 (wherein x is mole fraction, and x=0.6) stoichiometric ratio carries out batching.

[0043] Concrete preparation steps are as follows:

[0044] (1) will analyze pure ZnO, NiO, and Nb 2 o 5 As a raw material (purity ≥ 99%), weigh the ingredients in a molar ratio of 2.85:0.15:1, and weigh ZnO, NiO, and Nb 2 o 5 Put it into a nylon ball mill tank, the volume ratio of raw materials, ball milling medium, and deionized water is 1:1:1, use a planetary ball mill for ball milling, the ball mill speed is 400 rpm, ball mill on the ball mill for 12 hours, and then grind at 100°C Drying under the bottom, passed through 80 mesh sieve, and pre-fired to make (Zn 0.95 Ni 0.05 ) 3 Nb 2 o 8 , the calcining temperature is 1100℃, and the calcining time is 3h. 0.95 Ni 0.05 ) 3 Nb 2 o 8 Pre-fired powder;

[0045] (2) Anal...

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Abstract

The invention discloses Nb-based composite microwave dielectric ceramic. The constituting expression of the Nb-based composite microwave dielectric ceramic is (1-x)(Zn0.95Ni0.05)3Nb2O(8-x)Ni0.5Ti0.5NbO4, wherein x is larger than or equal to 0.5 and smaller than or equal to 0.7. The Nb-based composite microwave dielectric ceramic is prepared through steps as follows: ZnO, NiO and Nb2O5 in a mole ratio being 2.85:0.15:1 are blended firstly and subjected to ball milling, drying, sieving, pre-sintering, secondary ball milling, drying and sieving, and pre-sintered powder of (Zn0.95Ni0.05)3Nb2O8 is obtained; NiO, TiO2 and Nb2O5 in a mole ratio being 1:1:1 are blended, and pre-sintered powder of Ni0.5Ti0.5NbO4 is prepared with the same method; the pre-sintered powder of (Zn0.95Ni0.05)3Nb2O8 and the pre-sintered powder of Ni0.5Ti0.5NbO4 are blended in a stoichiometric ratio and subjected to compression moulding, and a green body is obtained; the green body is sintered at the temperature of 1,140-1,180 DEG C, and the Nb-based composite microwave dielectric ceramic is prepared. The dielectric constant epsilon r of the ceramic is 32.8-44.1, a Q*f value of a quality factor is 37,500 GHz-57,600 GHz, temperature coefficient tau f of resonant frequency is (-25.6) ppm/DEG C-(+6.7) ppm/DEG C, and the Nb-based composite microwave dielectric ceramic has important industrial application value.

Description

technical field [0001] The invention belongs to a ceramic composition characterized by components, in particular to a niobium-based microwave dielectric ceramic material with two-phase composite and nearly zero resonance frequency temperature coefficient and a preparation method thereof. Background technique [0002] With the rapid development of microwave communication technology, higher and higher requirements are put forward for the performance of microwave devices. Microwave dielectric ceramics are the key components of microwave devices. A series of microwave dielectric ceramic materials with different dielectric constants have been developed to meet different purposes. Among them, dielectric ceramics with a dielectric constant between 20 and 50 are mainly used for communication. Satellites, navigation antennas and military radars and other fields. Such microwave dielectric ceramic materials should generally meet the following requirements: (1) Serialized dielectric co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/495C04B35/622C04B35/626
CPCC04B35/495C04B35/622C04B35/6261C04B35/62645C04B2235/3232C04B2235/3279C04B2235/3284
Inventor 李玲霞吕笑松罗伟嘉
Owner TIANJIN UNIV
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