CN102424578A - Preparation method for BaO-Li2O-Nb2O5-Sb2O5 microwave dielectric ceramics material - Google Patents

Preparation method for BaO-Li2O-Nb2O5-Sb2O5 microwave dielectric ceramics material Download PDF

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Publication number
CN102424578A
CN102424578A CN2011102593830A CN201110259383A CN102424578A CN 102424578 A CN102424578 A CN 102424578A CN 2011102593830 A CN2011102593830 A CN 2011102593830A CN 201110259383 A CN201110259383 A CN 201110259383A CN 102424578 A CN102424578 A CN 102424578A
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hours
microwave
microwave dielectric
powder
alcohol
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刘晓斌
周焕福
陈秀丽
王一良
方亮
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Guilin University of Technology
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Guilin University of Technology
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Abstract

The present invention discloses a BaO-Li2O-Nb2O5-Sb2O5 microwave dielectric ceramics material and a preparation method thereof. According to the method, BaCO3, Li2CO3, Nb2O5 and Sb2O5 are firstly prepared into main powder according to a molecular formula Ba4LiNb3-xSbxO12, wherein the purities of the BaCO3, the Li2CO3, the Nb2O5 and the Sb2O5 are more than 99%, x is more than or equal to 0.25 and less than or equal to 3; then treatments of pelletizing, tableting, and sintering are performed to obtain the microwave dielectric material. The microwave dielectric material prepared by the method of the present invention has characteristics of excellent microwave performance, high dielectric constant (epsilonr), high Q*f value, and small harmonic frequency temperature coefficient, and can be adopted for microwave device manufacture, wherein the microwave devices comprise resonators, microwave antennas, filters and the like.

Description

BaO-Li 2O-Nb 2O 5-Sb 2O 5The preparation method of microwave dielectric ceramic materials
Technical field
The invention belongs to electronic ceramics and manufacturing field thereof, relate to a kind of preparation method of high-performance temperature-stable microwave dielectric ceramic materials.
Background technology
Microwave-medium ceramics is meant and is applied in microwave frequency band (mainly being UHF, the SHF frequency range) circuit as dielectric material and accomplishes the pottery of one or more functions.Microwave dielectric ceramic materials with high-k, low-loss, low resonant frequency temperature factor can be used for making components and parts such as dielectric resonator, wave filter, polyrod antenna and chip capacitor; Be widely used in communication, radar, navigation, electronic countermeasure, Global Positioning System fields such as (GPS), become the key foundation material of modern communication technology.
From early 1980s microwave dielectric resonator practicability realize to break through since, researched and developed out multiple practicability microwave dielectric ceramic materials, thus the development that has promoted modern communication technology greatly with popularize.Yet, must develop specific inductivity seriation, high, nearly zero the microwave-medium ceramics of frequency-temperature coefficient of quality factor for the fast development of satisfying mobile communication requirement to microwave-medium ceramics.
Summary of the invention
The present invention provides a kind of have low-loss, high-k, the BaO-Li of temperature-stable 2O-Nb 2O 5-Sb 2O 5The preparation method of microwave dielectric ceramic materials.
The chemical constitution formula of the microwave dielectric ceramic materials that the present invention relates to is: Ba 4LiNb 3-xSb xO 12, wherein: 0.25≤x≤3.
Preparing method's concrete steps of microwave dielectric ceramic materials are:
1) at first with the BaCO of purity>=99% 3, Li 2CO 3, Nb 2O 5And Sb 2O 5By molecular formula Ba 4LiNb 3-xSb xO 12Be mixed with main powder, wherein: 0.25≤x≤3;
The main powder that 2) will prepare then mixes, and according to main powder: alcohol: the weight ratio of zirconium ball is to add alcohol and zirconium ball at 1: 1: 2, adopts wet milling process mixing 4 hours; Take out the back 140 ℃ of oven dry down; Sieve with 80 purpose screen clothes, be pressed into bulk after sieving, the block main powder that will suppress with the temperature rise rate of 5 ℃/min then rises to 1200 ℃ and insulation 4 hours under this temperature by room temperature; Process the burning piece, promptly synthetic principal crystalline phase;
3) will burn piece pulverize powder, according to powder: alcohol: the weight ratio of zirconium ball is to add alcohol and zirconium ball at 1: 1: 2, puts into nylon jar ball milling 4 hours; Taking-up is dried under 140 ℃ of temperature, and being pressed into diameter after the granulation is 12mm, and thickness is the small column of 6mm; Temperature rise rate with 2 ℃/min rises to 550 ℃ of binder removals 4 hours; Furnace cooling 1350 ℃～1450 ℃ following sintering 4 hours, can obtain BaO-Li then 2O-Nb 2O 5-Sb 2O 5High-performance temperature-stable microwave dielectric ceramic materials.
The microwave-medium ceramics of the present invention's preparation, its microwave property is excellent: specific inductivity (ε r) and (τ f) temperature coefficient of resonance frequency is adjustable, Q * f value is high; Can be used for the manufacturing of microwave devices such as resonator, microwave antenna, wave filter.
Embodiment
Embodiment 1:
1) at first with BaCO 3, Li 2CO 3, Nb 2O 5And Sb 2O 5By molecular formula Ba 4LiNb 2.75Sb 0.25O 12Be mixed with main powder;
The main powder that 2) will prepare then mixes; According to main powder: alcohol: the weight ratio of zirconium ball is to add alcohol and zirconium ball at 1: 1: 2, adopts wet milling process to mix 4 hours, and dry down at 140 ℃ levigate back; Sieve with 80 purpose screen clothes; Be pressed into bulk after sieving, the block raw material that will suppress with the temperature rise rate of 5 ℃/min then rises to 1200 ℃ and insulation 4 hours under this temperature by room temperature, processes the burning piece;
3) with the above-mentioned burning piece of processing pulverize powder, according to powder: alcohol: the weight ratio of zirconium ball is to add alcohol and zirconium ball at 1: 1: 2, puts into nylon jar ball milling and takes out after 4 hours; Put into baker 140 ℃ of oven dry down; Being pressed into diameter after the granulation is 12mm, and thickness is the small column of 6mm, rises to 550 ℃ of binder removals 4 hours with the temperature rise rate of 2 ℃/min; Obtain porcelain behind the furnace cooling, again porcelain can be obtained microwave dielectric ceramic materials in 4 hours at 1350 ℃ of following sintering.The microwave property of this material is: ε r=34.8, Q * f=46500GHz, τ f=52.5ppm/ ℃.
Embodiment 2:
1) at first with BaCO 3, Li 2CO 3, Nb 2O 5And Sb 2O 5By molecular formula Ba 4LiNb 2.5Sb 0.5O 12Be mixed with main powder;
The main powder that 2) will prepare then mixes; According to main powder: alcohol: the weight ratio of zirconium ball is to add alcohol and zirconium ball at 1: 1: 2, adopts wet milling process to mix 4 hours, and dry down at 140 ℃ levigate back; Sieve with 80 purpose screen clothes; Be pressed into bulk after sieving, the block raw material that will suppress with the temperature rise rate of 5 ℃/min then rises to 1200 ℃ and insulation 4 hours under this temperature by room temperature, processes the burning piece;
3) with the above-mentioned burning piece of processing pulverize powder, according to powder: alcohol: the weight ratio of zirconium ball is to add alcohol and zirconium ball at 1: 1: 2, puts into nylon jar ball milling and takes out after 4 hours; Put into baker 140 ℃ of oven dry down; Being pressed into diameter after the granulation is 12mm, and thickness is the small column of 6mm, rises to 550 ℃ of binder removals 4 hours with the temperature rise rate of 2 ℃/min; Obtain porcelain behind the furnace cooling, again porcelain can be obtained microwave dielectric ceramic materials in 4 hours at 1375 ℃ of following sintering.The microwave property of this material is: ε r=27.1, Q * f=50300GHz, τ f=27.2ppm/ ℃.
Embodiment 3:
1) at first with BaCO 3, Li 2CO 3, Nb 2O 5And Sb 2O 5By molecular formula Ba 4LiNb 2.25Sb 0.75O 12Be mixed with main powder;
The main powder that 2) will prepare then mixes; According to main powder: alcohol: the weight ratio of zirconium ball is to add alcohol and zirconium ball at 1: 1: 2, adopts wet milling process to mix 4 hours, and dry down at 140 ℃ levigate back; Sieve with 80 purpose screen clothes; Be pressed into bulk after sieving, the block raw material that will suppress with the temperature rise rate of 5 ℃/min then rises to 1200 ℃ and insulation 4 hours under this temperature by room temperature, processes the burning piece;
3) with the above-mentioned burning piece of processing pulverize powder, according to powder: alcohol: the weight ratio of zirconium ball is to add alcohol and zirconium ball at 1: 1: 2, puts into nylon jar ball milling and takes out after 4 hours; Put into baker 140 ℃ of oven dry down; Being pressed into diameter after the granulation is 12mm, and thickness is the small column of 6mm, rises to 550 ℃ of binder removals 4 hours with the temperature rise rate of 2 ℃/min; Obtain porcelain behind the furnace cooling, again porcelain can be obtained microwave dielectric ceramic materials in 4 hours at 1400 ℃ of following sintering.The microwave property of this material is: ε r=26.3, Q * f=73150GHz, τ f=14.7ppm/ ℃.
Embodiment 4:
1) at first with BaCO 3, Li 2CO 3, Nb 2O 5And Sb 2O 5By molecular formula Ba 4LiNb 2SbO 12Be mixed with main powder;
The main powder that 2) will prepare then mixes; According to main powder: alcohol: the weight ratio of zirconium ball is to add alcohol and zirconium ball at 1: 1: 2, adopts wet milling process to mix 4 hours, and dry down at 140 ℃ levigate back; Sieve with 80 purpose screen clothes; Be pressed into bulk after sieving, the block raw material that will suppress with the temperature rise rate of 5 ℃/min then rises to 1200 ℃ and insulation 4 hours under this temperature by room temperature, processes the burning piece;
3) with the above-mentioned burning piece of processing pulverize powder, according to powder: alcohol: the weight ratio of zirconium ball is to add alcohol and zirconium ball at 1: 1: 2, puts into nylon jar ball milling and takes out after 4 hours; Put into baker 140 ℃ of oven dry down; Being pressed into diameter after the granulation is 12mm, and thickness is the small column of 6mm, rises to 550 ℃ of binder removals 4 hours with the temperature rise rate of 2 ℃/min; Obtain porcelain behind the furnace cooling, again porcelain can be obtained microwave dielectric ceramic materials in 4 hours at 1425 ℃ of following sintering.The microwave property of this material is: ε r=24.6, Q * f=52100GHz, τ f=0ppm/ ℃.
Embodiment 5:
1) at first with BaCO 3, Li 2CO 3, Nb 2O 5And Sb 2O 5By molecular formula Ba 4LiNb 1.75Sb 1.25O 12Be mixed with main powder;
The main powder that 2) will prepare then mixes; According to main powder: alcohol: the weight ratio of zirconium ball is to add alcohol and zirconium ball at 1: 1: 2, adopts wet milling process to mix 4 hours, and dry down at 140 ℃ levigate back; Sieve with 80 purpose screen clothes; Be pressed into bulk after sieving, the block raw material that will suppress with the temperature rise rate of 5 ℃/min then rises to 1200 ℃ and insulation 4 hours under this temperature by room temperature, processes the burning piece;
3) with the above-mentioned burning piece of processing pulverize powder, according to powder: alcohol: the weight ratio of zirconium ball is to add alcohol and zirconium ball at 1: 1: 2, puts into nylon jar ball milling and takes out after 4 hours; Put into baker 140 ℃ of oven dry down; Being pressed into diameter after the granulation is 12mm, and thickness is the small column of 6mm, rises to 550 ℃ of binder removals 4 hours with the temperature rise rate of 2 ℃/min; Obtain porcelain behind the furnace cooling, again porcelain can be obtained microwave dielectric ceramic materials in 4 hours at 1425 ℃ of following sintering.The microwave property of this material is: ε r=2 3.4, Q * f=32500GHz, τ f=-12.8ppm/ ℃.
Embodiment 6:
1) at first with BaCO 3, Li 2CO 3, Nb 2O 5And Sb 2O 5By molecular formula Ba 4LiNbSb 2O 12Be mixed with main powder;
The main powder that 2) will prepare then mixes; According to main powder: alcohol: the weight ratio of zirconium ball is to add alcohol and zirconium ball at 1: 1: 2, adopts wet milling process to mix 4 hours, and dry down at 140 ℃ levigate back; Sieve with 80 purpose screen clothes; Be pressed into bulk after sieving, the block raw material that will suppress with the temperature rise rate of 5 ℃/min then rises to 1200 ℃ and insulation 4 hours under this temperature by room temperature, processes the burning piece;
3) with the above-mentioned burning piece of processing pulverize powder, according to powder: alcohol: the weight ratio of zirconium ball is to add alcohol and zirconium ball at 1: 1: 2, puts into nylon jar ball milling and takes out after 4 hours; Put into baker 140 ℃ of oven dry down; Being pressed into diameter after the granulation is 12mm, and thickness is the small column of 6mm, rises to 550 ℃ of binder removals 4 hours with the temperature rise rate of 2 ℃/min; Obtain porcelain behind the furnace cooling, again porcelain can be obtained microwave dielectric ceramic materials in 4 hours at 1450 ℃ of following sintering.The microwave property of this material is: ε r=21.5, Q * f=27000GHz, τ f=-24ppm/ ℃.
Embodiment 7:
1) at first with BaCO 3, Li 2CO 3, Nb 2O 5And Sb 2O 5By molecular formula Ba 4LiSb 3O 12Be mixed with main powder;
The main powder that 2) will prepare then mixes; According to main powder: alcohol: the weight ratio of zirconium ball is to add alcohol and zirconium ball at 1: 1: 2, adopts wet milling process to mix 4 hours, and dry down at 140 ℃ levigate back; Sieve with 80 purpose screen clothes; Be pressed into bulk after sieving, the block raw material that will suppress with the temperature rise rate of 5 ℃/min then rises to 1200 ℃ and insulation 4 hours under this temperature by room temperature, processes the burning piece;
3) with the above-mentioned burning piece of processing pulverize powder, according to powder: alcohol: the weight ratio of zirconium ball is to add alcohol and zirconium ball at 1: 1: 2, puts into nylon jar ball milling and takes out after 4 hours; Put into baker 140 ℃ of oven dry down; Being pressed into diameter after the granulation is 12mm, and thickness is the small column of 6mm, rises to 550 ℃ of binder removals 4 hours with the temperature rise rate of 2 ℃/min; Obtain porcelain behind the furnace cooling, again porcelain can be obtained microwave dielectric ceramic materials in 4 hours at 1450 ℃ of following sintering.The microwave property of this material is: ε r=20.3, Q * f=26100GHz, τ f=-30ppm/ ℃.
It is pointed out that according to technical scheme of the present invention, the foregoing description can also be enumerated many, prove,, all can reach the object of the invention in the scope that claims of the present invention proposed according to applicant's lot of experiment results.

Claims (2)

1. a microwave dielectric ceramic materials is characterized in that the chemical constitution formula of microwave dielectric ceramic materials is: Ba 4LiNb 3-xSb xO 12, wherein: 0.25≤x≤3.
2. according to the preparation method of the said microwave dielectric ceramic materials of claim 1, it is characterized in that concrete steps are:
1) at first with the BaCO of purity>=99% 3, Li 2CO 3, Nb 2O 5And Sb 2O 5By molecular formula Ba 4LiNb 3-xSb xO 12Be mixed with main powder, wherein: 0.25≤x≤3;
The main powder that 2) will prepare then mixes, and according to main powder: alcohol: the weight ratio of zirconium ball is to add alcohol and zirconium ball at 1: 1: 2, adopts wet milling process mixing 4 hours; Take out the back 140 ℃ of oven dry down; Sieve with 80 purpose screen clothes, be pressed into bulk after sieving, the block main powder that will suppress with the temperature rise rate of 5 ℃/min then rises to 1200 ℃ and insulation 4 hours under this temperature by room temperature; Process the burning piece, promptly synthetic principal crystalline phase;
3) will burn piece pulverize powder, according to powder: alcohol: the weight ratio of zirconium ball is to add alcohol and zirconium ball at 1: 1: 2, puts into nylon jar ball milling 4 hours; Taking-up is dried under 140 ℃ of temperature, and being pressed into diameter after the granulation is 12mm, and thickness is the small column of 6mm; Rose under 550 ℃ of conditions binder removal 4 hours with the temperature rise rate of 2 ℃/min; Furnace cooling 1350 ℃～1450 ℃ following sintering 4 hours, can obtain microwave dielectric ceramic materials then.
CN2011102593830A 2011-09-03 2011-09-03 Preparation method for BaO-Li2O-Nb2O5-Sb2O5 microwave dielectric ceramics material Pending CN102424578A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105174917A (en) * 2015-09-20 2015-12-23 桂林理工大学 Ultra-low dielectric constant microwave dielectric ceramic Li3La2Sb5O17 and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN1793004A (en) * 2006-01-05 2006-06-28 武汉理工大学 Low temp. sintering niobate microwave dielectric ceramic and preparation process thereof
CN101863658A (en) * 2010-06-17 2010-10-20 西北工业大学 Preparation method of barium-strontium titanate ceramic

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1793004A (en) * 2006-01-05 2006-06-28 武汉理工大学 Low temp. sintering niobate microwave dielectric ceramic and preparation process thereof
CN101863658A (en) * 2010-06-17 2010-10-20 西北工业大学 Preparation method of barium-strontium titanate ceramic

Non-Patent Citations (1)

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Title
张冲: "微波介质陶瓷Ba5Nb4O15的低温烧结和MCT凝胶注模成型的工艺研究", 《中国优秀硕士学位论文全文数据库（工程科技I辑）》, no. 8, 15 August 2009 (2009-08-15) *

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105174917A (en) * 2015-09-20 2015-12-23 桂林理工大学 Ultra-low dielectric constant microwave dielectric ceramic Li3La2Sb5O17 and preparation method thereof

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Application publication date: 20120425