CN114874010A - Microwave ceramic material DyVO 4 And method for preparing the same - Google Patents

Microwave ceramic material DyVO 4 And method for preparing the same Download PDF

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CN114874010A
CN114874010A CN202210437166.4A CN202210437166A CN114874010A CN 114874010 A CN114874010 A CN 114874010A CN 202210437166 A CN202210437166 A CN 202210437166A CN 114874010 A CN114874010 A CN 114874010A
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李波
陈丽
杨瑞佳
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University of Electronic Science and Technology of China
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Abstract

The invention belongs to the field of electronic ceramics and manufacture thereof, and particularly provides a microwave ceramic material DyVO 4 And a method for preparing the same. The chemical formula of the microwave dielectric material provided by the invention is DyVO 4 DyVO with microstructure of tetragonal zircon structure 4 Crystalline phase, with excellent microwave dielectric properties: a dielectric constant of 11.1 to 11.7, a Qxf value of 21000 to 25000GHz, and a temperature coefficient of resonance frequency of-23 to-19 ppm/DEG C. In addition, the microwave dielectric material has low production cost and simple preparation process, is beneficial to industrial production, and can be widely applied to microwave resonators, filters and the likeAnd (5) manufacturing a device.

Description

Microwave ceramic material DyVO 4 And method for preparing the same
Technical Field
The invention belongs to the field of electronic ceramics and manufacture thereof, and relates to a microwave ceramic material DyVO 4 And a method for preparing the same.
Background
With the advent of the fifth generation mobile communication technology, the problems of high threshold voltage, low signal path mobility, etc. caused by high dielectric constant devices have become more prominent. In order to meet the requirement of high-speed signal transmission capability, the search for microwave dielectric ceramics with low dielectric constant has great significance and value. The vanadate ceramic has lowSintering temperature and excellent microwave dielectric properties are receiving increasing attention. "Preparation, Crystal Structure and Microwave digital Properties of ray-Earth Vanadates ReVO 4 (Re ═ Nd, Sm) "reported herein is NdVO 4 、SmVO 4 The sintering temperature is 1160 ℃, and the microwave dielectric property is as follows: epsilon r ＝11～12、Q×f＝35000～38000GHz、τ f -44.3p to-48.4 ppm/° c. However, the high temperature coefficients of the resonant frequencies of these two materials can deteriorate the stability of the microwave device, and it is necessary to develop a microwave ceramic material with a temperature coefficient of the resonant frequency close to zero.
Based on the background, the invention provides a microwave ceramic material DyVO 4 And a method for preparing the same.
Disclosure of Invention
The invention aims to provide a microwave dielectric material DyVO 4 And a method for preparing the same.
In order to achieve the purpose, the technical scheme implemented by the invention is as follows:
a microwave ceramic material, characterized in that: the chemical formula of the microwave ceramic material is as follows: DyVO 4 。
Further, the microwave ceramic material is DyVO of tetragonal system 4 A crystalline phase.
Further, the preparation method of the microwave ceramic material is characterized by comprising the following steps:
by Dy 2 O 3 、V 2 O 5 Is prepared from DyVO 4 The molar ratio of (A) to (B) is mixed;
(2) taking deionized water and zirconium balls as ball milling media, putting the raw materials into a ball milling tank for ball milling for 5-8 hours, and putting the mixture into an oven for drying after primary ball milling;
(3) sieving the dried material, and presintering at 650-750 ℃ for 3-4 hours to obtain a main crystal phase DyVO 4 The pre-sintering material of (1);
(4) taking deionized water and zirconium balls as ball milling media, putting the pre-sintered material into a ball milling tank for ball milling for 5-8 hours, and putting the mixture into an oven for drying after secondary ball milling;
(5) mixing the dried material with a polyvinyl alcohol solution, granulating, and pressing under the pressure of 10-20 MPa to prepare a green body;
(6) and sintering the green body at 1050-1200 ℃ for 5-6 hours to obtain the microwave ceramic material.
The invention has the beneficial effects that:
the invention provides a microwave ceramic material DyVO 4 Is single crystal phase DyVO 4 The material is a crystal structure square zircon structure, and has a better resonant frequency temperature coefficient due to large Dy-O bond energy in a microstructure, so that the stability of the device in working is improved;
the invention provides a microwave ceramic material DyVO 4 The microwave dielectric property is excellent at a sintering temperature of 1050-1200 ℃: a dielectric constant of 11.1 to 11.7, a Qxf value of 21000 to 25000GHz, and a temperature coefficient of resonance frequency of-23 to-19 ppm/DEG C. The microwave ceramic material has simple preparation process and low production cost, is beneficial to realizing industrial production, and can be widely applied to the manufacture of microwave devices such as resonators, filters and the like.
Drawings
FIG. 1 is DyVO (DyVO) which is a microwave ceramic material prepared in example 3 4 XRD pattern at sintering temperature 1150 ℃.
FIG. 2 is the microwave ceramic material DyVO prepared in example 3 4 SEM image at a sintering temperature of 1150 ℃.
Detailed description of the preferred embodiments
The present invention will be described in further detail with reference to the drawings and examples.
The invention provides 4 embodiments totally, the formula and sintering temperature of the microwave ceramic material provided by each embodiment are as follows: DyVO 4 Wherein the sintering temperature is 1050 ℃, 1100 ℃, 1150 ℃ and 1200 ℃; the microwave ceramic material is prepared by the following method:
by Dy 2 O 3 、V 2 O 5 Is prepared from DyVO 4 The molar ratio of (A) to (B) is mixed;
taking deionized water and zirconium balls as ball milling media, putting the raw materials into a ball milling tank for ball milling for 5-8 hours, and putting the mixture into an oven for drying after primary ball milling;
sieving the dried material, and presintering at 650-750 ℃ for 3-4 hours to obtain a main crystal phase DyVO 4 The pre-sintering material of (1);
taking deionized water and zirconium balls as ball milling media, putting the pre-sintered material into a ball milling tank for ball milling for 5-8 hours, and putting the mixture into an oven for drying after secondary ball milling;
mixing the dried material with a polyvinyl alcohol solution, granulating, and pressing under the pressure of 10-20 MPa to prepare a green body;
and sintering the green body at 1050-1200 ℃ for 5-6 hours to obtain the microwave ceramic material.
The specific process parameters and microwave dielectric properties of the above 4 examples are shown in the following table:
Figure BDA0003600588920000021
Figure BDA0003600588920000031
as can be seen from the above table, the microwave ceramic material DyVO provided by the invention 4 The microwave dielectric material has excellent microwave dielectric property at a sintering temperature of 1050-1200 ℃: a dielectric constant of 11.1 to 11.7, a Qxf value of 21000 to 25000GHz, and a temperature coefficient of resonance frequency of-23 to-19 ppm/DEG C. In addition, DyVO, a microwave ceramic material, prepared in example 3 4 As shown in FIGS. 1 and 2, the characteristic peaks of the XRD diffraction pattern have high matching degree with PDF #86-0997 standard card, indicating that the prepared ceramic is DyVO with single crystal phase 4 From the SEM results, it was found that the ceramic had a dense and uniform microstructure, a large relative density, and a small porosity, thereby obtaining a low dielectric loss.
While the invention has been described with reference to specific embodiments, any feature disclosed in this specification may be replaced by alternative features serving the same, equivalent or similar purpose, unless expressly stated otherwise; all of the disclosed features, or all of the method or process steps, may be combined in any combination, except mutually exclusive features and/or steps.

Claims (3)

1. The microwave ceramic material is characterized by having a chemical formula of DyVO 4 。
2. The microwave ceramic material of claim 1 wherein said microwave ceramic material is DyVO of tetragonal zircon structure 4 A crystalline phase.
3. A process for the preparation of a microwave ceramic material according to claim 1, comprising the steps of:
(1) by Dy 2 O 3 、V 2 O 5 Is prepared from DyVO 4 The molar ratio of (A) to (B) is mixed;
(2) taking deionized water and zirconium balls as ball milling media, putting the raw materials into a ball milling tank for ball milling for 5-8 hours, and putting the mixture into an oven for drying after primary ball milling;
(3) sieving the dried material, and presintering at 650-750 ℃ for 3-4 hours to obtain a main crystal phase DyVO 4 The pre-sintering material of (1);
(4) taking deionized water and zirconium balls as ball milling media, putting the pre-sintered material into a ball milling tank for ball milling for 5-8 hours, and putting the mixture into an oven for drying after secondary ball milling;
(5) mixing the dried material with a polyvinyl alcohol solution, granulating, and pressing under the pressure of 10-20 MPa to prepare a green body;
(6) and sintering the green body at 1050-1200 ℃ for 5-6 hours to obtain the microwave ceramic material.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115353387A (en) * 2022-08-17 2022-11-18 电子科技大学 Microwave dielectric material ErVO 4 And method for preparing the same
CN115353388A (en) * 2022-09-19 2022-11-18 电子科技大学 Microwave ceramic material PrVO 4 And method for preparing the same
CN115403377A (en) * 2022-08-31 2022-11-29 电子科技大学 Microwave dielectric material HoVO 4 And method for preparing the same

Citations (4)

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Publication number Priority date Publication date Assignee Title
JPH038760A (en) * 1989-06-06 1991-01-16 Matsushita Electric Ind Co Ltd Production of voltage-dependent nonlinear resistor porcelain composition and varistor
CN104193336A (en) * 2014-08-29 2014-12-10 桂林电子科技大学 Low-sintering-temperature microwave dielectric ceramic material and preparation method thereof
CN111646796A (en) * 2020-05-19 2020-09-11 电子科技大学 Low-temperature sintered low-dielectric microwave ceramic material Sr2VxO7And method for preparing the same
CN113582690A (en) * 2021-07-09 2021-11-02 电子科技大学 Ultralow temperature sintered microwave dielectric material Zn2V2O7And method for preparing the same

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH038760A (en) * 1989-06-06 1991-01-16 Matsushita Electric Ind Co Ltd Production of voltage-dependent nonlinear resistor porcelain composition and varistor
CN104193336A (en) * 2014-08-29 2014-12-10 桂林电子科技大学 Low-sintering-temperature microwave dielectric ceramic material and preparation method thereof
CN111646796A (en) * 2020-05-19 2020-09-11 电子科技大学 Low-temperature sintered low-dielectric microwave ceramic material Sr2VxO7And method for preparing the same
CN113582690A (en) * 2021-07-09 2021-11-02 电子科技大学 Ultralow temperature sintered microwave dielectric material Zn2V2O7And method for preparing the same

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
WEI LI, ET AL: "Preparation, Crystal Structure and Microwave Dielectric Properties of Rare-Earth Vanadates: ReVO4 (Re＝Nd, Sm)", 《JOURNAL OF ELECTRONIC MATERIALS》 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115353387A (en) * 2022-08-17 2022-11-18 电子科技大学 Microwave dielectric material ErVO 4 And method for preparing the same
CN115353387B (en) * 2022-08-17 2023-10-03 电子科技大学 Microwave dielectric material ErVO 4 And a method for preparing the same
CN115403377A (en) * 2022-08-31 2022-11-29 电子科技大学 Microwave dielectric material HoVO 4 And method for preparing the same
CN115403377B (en) * 2022-08-31 2023-10-03 电子科技大学 Microwave dielectric material HoVO 4 And a method for preparing the same
CN115353388A (en) * 2022-09-19 2022-11-18 电子科技大学 Microwave ceramic material PrVO 4 And method for preparing the same

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