Low-temperature-sintered temperature-stable composite microwave dielectric ceramic and preparation method thereof

Abstract

The invention relates to a low-temperature-sintered temperature-stable composite microwave dielectric ceramic and a preparation method thereof. The composite microwave dielectric ceramic comprises the following components: a low-temperature-sintered microwave dielectric ceramic material with a negative resonant frequency temperature coefficient and a low-temperature-sintered microwave dielectric ceramic material with a positive resonant frequency temperature coefficient. According to the invention, the low-temperature-sintered microwave dielectric ceramic material with a negative resonant frequency temperature coefficient or the low-temperature-sintered microwave dielectric ceramic material with the positive resonant frequency temperature coefficient is used as a main material, a low-temperature-sintered microwave dielectric ceramic material with the same structure and an opposite resonant frequency temperature coefficient is added as an adjusting material through a two-phase compounding method, and compounding is conducted to form a multiphase ceramic material or a solid solution so as to obtain a low-temperature-sintered microwave dielectric ceramic material having a nearly-zero resonance frequency temperature coefficient. The problems that existing microwave dielectric ceramic is high in sintering temperature, and the temperature coefficient of resonance frequency changes greatly along with temperature are solved. The microwave dielectric ceramic material has a wide application scope in the LTCC low-temperature-sintered microwave dielectric ceramic materials.

Description

technical field

[0001] The invention belongs to the field of electronic components, specifically, to the field of microwave electronic components, and more specifically, to the field of ceramic materials for microwave electronic components. Background technique

[0002] Microwave dielectric ceramics (MWDC) refer to ceramic materials that are used as dielectric materials in microwave frequency (300MHz-300GHz) circuits and perform one or more functions. In microwave electronic components, microwave dielectric ceramics are the key materials for making microwave resonators and filters. frequency, with a near-zero resonant frequency temperature coefficient to ensure the stability of the device. At present, although the widely used microwave dielectric ceramic materials meet the requirements of some electronic components in terms of performance, with the continuous upgrading of modern electronic information technology (such as 5G technology), the upgrading and popularization of v...

Examples

Embodiment 1

[0030] Embodiment 1: x=0.2

[0031] Preparation:

[0032] 1) Li with a purity ≥ 99.9% 2 CO 3 , NiO, Bi 2 o 3 and MoO 3 as raw material, according to Li 2 / 3 Ni 2 / 3 MoO 4 , (Li 1 / 2 Bi 1 / 2 )MoO 4 Stoichiometric ratio preparation and weighing, using absolute ethanol and agate balls as the ball milling medium, ball milling at a speed of 300r / min for 4-6 hours, drying at 80°C, and then heating at a rate of 2°C / min-5°C / min Li 2 / 3 Ni 2 / 3 MoO 4 , (Li 1 / 2 Bi 1 / 2 )MoO 4 ceramic powder.

[0033] 2) The ceramic powder synthesized by step 1) pre-fired in proportion to (1-x)Li 2 / 3 Ni 2 / 3 MoO 4 -x(Li 1 / 2 Bi 1 / 2 ) MoO 4 The ingredients get {(Li 1.6 / 3 Bi 0.2 / 2 )(Li 0.2 / 2 Ni 1.6 / 3 )}MoO 4 Composite ceramic powder; use absolute ethanol and agate balls as the ball milling medium to mill the prepared composite ceramic powder in a high-speed ball mill with a speed of 250r / min to 350r / min for 8h to 12h and mix evenly; bake at 80°C Dry, grind into powder and sieve, add p...

Embodiment 2

[0037] Embodiment 2: x=0.3

[0038] Preparation:

[0039] 1) Li with a purity ≥ 99.9% 2 CO 3 , NiO, Bi 2 o 3 and MoO 3 as raw material, according to Li 2 / 3 Ni 2 / 3 MoO 4 , (Li 1 / 2 Bi 1 / 2 ) MoO 4 Stoichiometric ratio preparation and weighing, using absolute ethanol and agate balls as the ball milling medium, ball milling at a speed of 300r / min for 4h~6h after mixing, drying at 80°C, and then heating at a rate of 2°C / min~5°C / min Li 2 / 3 Ni 2 / 3 MoO 4 , (Li 1 / 2 Bi 1 / 2 ) MoO 4 ceramic powder.

[0040] 2) The ceramic powder synthesized by step 1) pre-fired in proportion to (1-x) Li 2 / 3 Ni 2 / 3 MoO 4 -x(Li 1 / 2 Bi 1 / 2 ) MoO 4 The ingredients get {(Li 1.4 / 3 Bi 0.3 / 2 )(Li 0.3 / 2 Ni 1.4 / 3 )}MoO 4 Composite ceramic powder; use absolute ethanol and agate balls as the ball milling medium to mill the prepared composite ceramic powder in a high-speed ball mill with a speed of 250r / min to 350r / min for 8h to 12h and mix evenly; at a temperature of 80°C Drying, grindin...

Embodiment 3

[0044] Embodiment 3: x=0.4

[0045] Preparation:

[0046] 1) Li with a purity ≥ 99.9% 2 CO 3 , NiO, Bi 2 o 3 and MoO 3 For raw materials, press Li 2 / 3 Ni 2 / 3 MoO 4 , (Li 1 / 2 Bi 1 / 2 ) MoO 4 The stoichiometric ratio of the chemical formula is prepared and weighed, with anhydrous ethanol and agate balls as the ball milling medium, ball milled at a speed of 300r / min for 4h to 6h, then dried at 80°C, and then dried at 2°C / min to 5°C / min The heating rate is kept at 500°C-600°C for 2-4 hours to obtain Li 2 / 3 Ni 2 / 3 MoO 4 , (Li 1 / 2 Bi 1 / 2 ) MoO 4 ceramic powder.

[0047] 2) The ceramic powder synthesized by step 1) pre-fired in proportion to (1-x)Li 2 / 3 Ni 2 / 3 MoO 4 -x(Li 1 / 2 Bi 1 / 2 ) MoO 4 Mixing ingredients to obtain composite ceramic powder; use absolute ethanol and agate balls as the ball milling medium for the prepared composite ceramic powder, and ball mill it in a high-speed ball mill with a speed of 250r / min to 350r / min for 8 to 12 hours to mix evenly;...

technical field

[0001] The invention belongs to the field of electronic components, specifically, to the field of microwave electronic components, and more specifically, to the field of ceramic materials for microwave electronic components. Background technique

[0002] Microwave dielectric ceramics (MWDC) refer to ceramic materials that are used as dielectric materials in microwave frequency (300MHz-300GHz) circuits and perform one or more functions. In microwave electronic components, microwave dielectric ceramics are the key materials for making microwave resonators and filters. frequency, with a near-zero resonant frequency temperature coefficient to ensure the stability of the device. At present, although the widely used microwave dielectric ceramic materials meet the requirements of some electronic components in terms of performance, with the continuous upgrading of modern electronic information technology (such as 5G technology), the upgrading and popularization of v...

Examples

Embodiment 1

[0030] Embodiment 1: x=0.2

[0031] Preparation:

[0032] 1) Li with a purity ≥ 99.9% 2 CO 3 , NiO, Bi 2 o 3 and MoO 3 as raw material, according to Li 2 / 3 Ni 2 / 3 MoO 4 , (Li 1 / 2 Bi 1 / 2 )MoO 4 Stoichiometric ratio preparation and weighing, using absolute ethanol and agate balls as the ball milling medium, ball milling at a speed of 300r / min for 4-6 hours, drying at 80°C, and then heating at a rate of 2°C / min-5°C / min Li 2 / 3 Ni 2 / 3 MoO 4 , (Li 1 / 2 Bi 1 / 2 )MoO 4 ceramic powder.

[0033] 2) The ceramic powder synthesized by step 1) pre-fired in proportion to (1-x)Li 2 / 3 Ni 2 / 3 MoO 4 -x(Li 1 / 2 Bi 1 / 2 ) MoO 4 The ingredients get {(Li 1.6 / 3 Bi 0.2 / 2 )(Li 0.2 / 2 Ni 1.6 / 3 )}MoO 4 Composite ceramic powder; use absolute ethanol and agate balls as the ball milling medium to mill the prepared composite ceramic powder in a high-speed ball mill with a speed of 250r / min to 350r / min for 8h to 12h and mix evenly; bake at 80°C Dry, grind into powder and sieve, add p...

Embodiment 2

[0037] Embodiment 2: x=0.3

[0038] Preparation:

[0039] 1) Li with a purity ≥ 99.9% 2 CO 3 , NiO, Bi 2 o 3 and MoO 3 as raw material, according to Li 2 / 3 Ni 2 / 3 MoO 4 , (Li 1 / 2 Bi 1 / 2 ) MoO 4 Stoichiometric ratio preparation and weighing, using absolute ethanol and agate balls as the ball milling medium, ball milling at a speed of 300r / min for 4h~6h after mixing, drying at 80°C, and then heating at a rate of 2°C / min~5°C / min Li 2 / 3 Ni 2 / 3 MoO 4 , (Li 1 / 2 Bi 1 / 2 ) MoO 4 ceramic powder.

[0040] 2) The ceramic powder synthesized by step 1) pre-fired in proportion to (1-x) Li 2 / 3 Ni 2 / 3 MoO 4 -x(Li 1 / 2 Bi 1 / 2 ) MoO 4 The ingredients get {(Li 1.4 / 3 Bi 0.3 / 2 )(Li 0.3 / 2 Ni 1.4 / 3 )}MoO 4 Composite ceramic powder; use absolute ethanol and agate balls as the ball milling medium to mill the prepared composite ceramic powder in a high-speed ball mill with a speed of 250r / min to 350r / min for 8h to 12h and mix evenly; at a temperature of 80°C Drying, grindin...

Embodiment 3

[0044] Embodiment 3: x=0.4

[0045] Preparation:

[0046] 1) Li with a purity ≥ 99.9% 2 CO 3 , NiO, Bi 2 o 3 and MoO 3 For raw materials, press Li 2 / 3 Ni 2 / 3 MoO 4 , (Li 1 / 2 Bi 1 / 2 ) MoO 4 The stoichiometric ratio of the chemical formula is prepared and weighed, with anhydrous ethanol and agate balls as the ball milling medium, ball milled at a speed of 300r / min for 4h to 6h, then dried at 80°C, and then dried at 2°C / min to 5°C / min The heating rate is kept at 500°C-600°C for 2-4 hours to obtain Li 2 / 3 Ni 2 / 3 MoO 4 , (Li 1 / 2 Bi 1 / 2 ) MoO 4 ceramic powder.

[0047] 2) The ceramic powder synthesized by step 1) pre-fired in proportion to (1-x)Li 2 / 3 Ni 2 / 3 MoO 4 -x(Li 1 / 2 Bi 1 / 2 ) MoO 4 Mixing ingredients to obtain composite ceramic powder; use absolute ethanol and agate balls as the ball milling medium for the prepared composite ceramic powder, and ball mill it in a high-speed ball mill with a speed of 250r / min to 350r / min for 8 to 12 hours to mix evenly;...

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