CN101823880B - Phenacite type molybdenum-based and tungsten-based ultralow temperature sintered microwave dielectric ceramic materials and preparation method thereof - Google Patents

Phenacite type molybdenum-based and tungsten-based ultralow temperature sintered microwave dielectric ceramic materials and preparation method thereof Download PDF

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CN101823880B
CN101823880B CN2010101920277A CN201010192027A CN101823880B CN 101823880 B CN101823880 B CN 101823880B CN 2010101920277 A CN2010101920277 A CN 2010101920277A CN 201010192027 A CN201010192027 A CN 201010192027A CN 101823880 B CN101823880 B CN 101823880B
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ceramic materials
tungsten
microwave dielectric
phenacite
preparation
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CN101823880A (en
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周迪
汪宏
姚熹
庞利霞
吴新光
郭靖
张高群
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Xian Jiaotong University
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Abstract

The invention discloses a phenacite type molybdenum-based and tungsten-based ultralow temperature sintered microwave dielectric ceramic materials and a preparation method thereof. Based on a structural formula of A2BO4, a low-valent Li+1 ion is selected to occupy the position A, and high-valent Mo6+ and W6+ compound cations are selected to occupy the position B; and a series of ceramic materials, which can be sintered in the ultralow temperature range of between 540 and 640 DEG C and have low microwave dielectric constant (epsilon r is more than or equal to 5.3 and less than or equal to 5.5), adjustable resonant frequency temperature coefficient (TCF is more than or equal to 133ppm per DEG C below zero and less than or equal to 149 ppm per DEG C below zero and low microwave dielectric loss (high quality factor Qf value, wherein Qf is more than or equal to 37,000GHz and less than or equal to 63,400 GHz), are obtained by the traditional solid-phase reaction sintering method. The structural expression of the ceramic materials is Li2(Mo1-xWx)O4, wherein x is more than 0.0 and less than 1.0.

Description

A kind of Phenacite type molybdenum-based and tungsten-based ultralow temperature sintered microwave dielectric ceramic materials and preparation method thereof
Technical field
The invention belongs to electronic ceramics and preparation field thereof, particularly a kind of Phenacite type molybdenum-based and tungsten-based ultralow temperature sintered microwave dielectric ceramic materials of agglomerating and preparation thereof under very low temperature.
Background technology
Microwave-medium ceramics is a kind of new function stupalith that grows up nearly decades; It is the critical material of making microwave-medium wave filter resonator; In recent years rapidly to the very active development of its research; Its impellent mainly comes from the demand of commercial radio communication high speed development, like cellular mobile telecommunication system, TV receiving system, direct loudspeaker system and satellite communication system etc.Microwave-medium ceramics has premium propertiess such as specific inductivity wider distribution, low microwave loss, frequency-temperature coefficient be little; Be fit to make resonator oscillator wave filter and frequency discriminator in the equipment such as various microwave devices and mobile telephone, can satisfy microwave circuit miniaturized, integrated, high reliability and requirement cheaply.Along with the development of mobile communication cause, the research of microwave-medium ceramics receives people's attention day by day.
LTCC LTCC (Low Temperature Co-fired Ceramics) technology has become one of major technique of electronic-component moduleization with its excellent electricity, machinery, calorifics and operational characteristic.What as its name suggests, the LTCC technology referred to is exactly with the technology of ceramic green agglomerating together with electrode.According to the difference of material, the specific inductivity of LTCC material can in very large range change, and has increased the handiness of circuit layout.Applied microwave-medium ceramics has lower dielectric loss than resin material used in the PCB printed substrate in the LTCC technology, has very good high frequency characteristics.So after the metal electrode with high conductivity burnt altogether, integral module also can keep very low loss.In addition, compare with organism such as resin materials, stupalith has lower thermal expansivity, has further improved the safety of components and parts wrapping processs.Rely on above-described various advantages, the LTCC technology becomes the prefered method of high frequency substrate and integrated device application just gradually.Medium ceramic substrate is widely used in thin film circuit, large-scale integrated circuit, high-power hybrid integrated circuit in the electronic industry or the like now.Use still is traditional Al the most widely 2O 3Pottery, its specific inductivity are 9, and dielectric loss is below 0.0001, and thermal conductivity that it is good and temperature stability also are as the indispensable characteristic of ceramic substrate material.
Since last century the seventies; The research of microwave-medium ceramics system development, is added up according to document if do not consider this index of sintering temperature near 40 years; Hundreds of kind system has at least been arranged till now, and the up to ten thousand kinds of potteries with good microwave dielectric property are developed.But most of microwave-medium ceramics all has higher sintering temperature (>=1000 oC).In recent ten years, a kind of more efficiently research approach more and more receives people's attention, i.e. searching itself have low fever's temperature (<900 oC) material system, this type of material system generally is referred to as low fever's ceramic systems.
In sum; Along with being widely used in high-frequency multilayer, microwave-medium ceramics burns fields such as electrical condenser, medium substrate and the ultra material of medium altogether; LTCC Technology is with its superiority of not replacing; Become the mainstream technology of microwave device preparation, further promote all kinds of microwave devices to miniaturized, integrated, development in pluralism.In order to satisfy the production needs of LTCC Technology, research and development have low-loss under certain distributed scope specific inductivity, the microwave frequency band (Qf>5000GHz), resonant frequency temperature profile stable, can become current research focus and difficult point gradually with the novel microwave dielectric pottery of respective electrode material sintering coupling.When taking into account each item performance index, that the novel material of being researched and developed should possess is cheap, do not contain or contain less characteristics such as poisonous element, to satisfy the requirement of environmental protection Sustainable development.
Summary of the invention
The objective of the invention is to overcome the deficiency of above-mentioned prior art material, a kind of Phenacite type molybdenum-based and tungsten-based ultralow temperature sintered microwave dielectric ceramic materials and preparation method thereof be provided, this stupalith be a kind of need not add any sintering agent just can be 540 oC ~ 660 oThe C agglomerating can be applicable to the high-performance Phenacite type molybdenum-based and tungsten-based ultralow temperature sintered microwave dielectric stupalith of LTCC, and its minimum sintering temperature is low to moderate 540 oC.
First purpose of the present invention provides a kind of Phenacite type molybdenum-based and tungsten-based ultralow temperature sintered microwave dielectric ceramic materials, and the relative permittivity behind its sintering is 5.3 ~ 5.5, low low-frequency dielectric loss (tan δ<3 * 10 -4, 1MHz), good microwave property (37,000 GHz≤Qf≤63,400 GHz), temperature coefficient of resonance frequency is adjustable (133 ppm/ oC≤TCF≤-149 ppm/ oC), its principal feature is can be under lower sintering temperature (540 in addition oC ~ 640 oC) carry out sintering, chemical constitution and preparation technology are simple, and thing is mutually single.
Second purpose of the present invention provides the preparation method of the Phenacite type molybdenum-based and tungsten-based microwave dielectric ceramic materials of above-mentioned sintered at ultra low temperature.
The present invention has adopted the most simple and effective solid state reaction agglomerating method to realize the foregoing invention purpose.It at first is the prescription of choosing proper ratio; Choose suitable initial oxide and suitable substituent (carbonate); Make oxide compound mix through a ball milling; Make oxide compound carry out preliminary reaction through the presintering process, through the particle size of secondary ball milling refinement reactant, obtain needed ceramics sample through sintering process at last again.Through a kind of so simple effective preparation method, the specific inductivity of the ceramics sample that obtains changes between 5.3 ~ 5.5 with composition, and Qf is distributed in 37,000 GHz ~ 63,400 GHz, temperature coefficient of resonance frequency at TCF at-133 ppm/ oC ~-149 ppm/ oAdjustable between the C, sintering temperature 540 oC ~ 640 oC makes it to be applicable to the needs of LTCC technology to enlarge its range of application.
Technical scheme of the present invention is achieved in that
A kind of Phenacite type molybdenum-based and tungsten-based ultralow temperature sintered microwave dielectric ceramic materials, this stupalith structure expression is: Li 2(Mo 1-xW x) O 4, in the formula 0.0<x<1.0.
The micro-wave dielectric constant ε of said stupalith r=5.3 ~ 5.5, temperature coefficient of resonance frequency TCF=-133 ~-149 ppm/ oC, hi-q Qf=37000 ~ 63400 GHz, sintering temperature are 540 oC ~ 640 oDielectric loss is under C, the 1MHz low frequency: tan δ<3 * 10 -4
The preparation method of described Phenacite type molybdenum-based and tungsten-based ultralow temperature sintered microwave dielectric ceramic materials, carry out according to the following steps:
1) with chemical feedstocks MoO 3, WO 3And Li 2CO 3By prescription general formula Li 2(Mo 1-xW x) O 4Preparation is in the formula 0.0<x<1.0;
2) with the step 1) batch mixes, ball milling 5 ~ 8 hours is 100 oC ~ 200 oC is oven dry down, is pressed into block body behind 200 orders that sieve;
3) with step 2) blocks through 500 oC ~ 800 oThe C pre-burning, and be incubated 4 ~ 6 hours, obtain sample and burn piece;
4) sample is burnt piece and pulverize, and through 5 ~ 6 hours secondary ball milling, 100 oC ~ 200 oC is oven dry, granulation down, and granulation obtains the porcelain powder after 60 orders and 120 eye mesh screen bilayers sieve;
5) with the porcelain powder pressing forming, 540 oC ~ 640 oSintering became porcelain in 2 ~ 4 hours under the C, obtained Phenacite type molybdenum-based and tungsten-based ultralow temperature sintered microwave dielectric ceramic materials.
The molybdenum-based and tungsten-based microwave dielectric ceramic materials of sintered at ultra low temperature of the present invention has following characteristics: relative permittivity low (5.3 ~ 5.5), little (the tan δ of dielectric loss under the low frequency<3 * 10 -4, 1MHz), microwave property good (37,000 GHz≤Qf≤63,400 GHz), sintering temperature is low by (540 oC ~ 640 oC), adjustable (133 ppm/ of temperature coefficient of resonance frequency oC≤TCF≤-149 ppm/ oC), chemical constitution and preparation technology are simple.
Embodiment
Do further explain in the face of content of the present invention down.
The formulation of Phenacite type molybdenum-based and tungsten-based ultralow temperature sintered microwave dielectric ceramic materials of the present invention is: Li 2(Mo 1-xW x) O 4, in the formula 0.0<x<1.0.
The concrete preparation process of the molybdenum-based and tungsten-based microwave dielectric ceramic materials of sintered at ultra low temperature of the present invention is: with chemical feedstocks MoO 3, WO 3And Li 2CO 3By prescription general formula Li 2(Mo 1-xW x) O 4Preparation is in the formula 0.0<x<1.0.
Thorough mixing ball milling 5 hours is dried after levigate, is sieved, briquetting, then through 500 oThe C pre-burning, and be incubated 4 hours, the block after the pre-burning is carried out secondary ball milling, granulation after the levigate oven dry is sieved through 60 orders and 120 eye mesh screen bilayers, can obtain required porcelain.With porcelain compression moulding on demand, then 540 oC ~ 640 oSintering became porcelain in 2 hours under the C, can obtain the molybdenum-based and tungsten-based microwave dielectric ceramic materials of sintered at ultra low temperature.
Phenacite type molybdenum-based and tungsten-based its principal feature of ultramicrowave medium ceramic material of sintered at ultra low temperature of the present invention is with low melting point oxide MoO 3And Li 2O makes that as pivot this medium ceramic material of sintering becomes possibility at low temperatures.The present invention is relevant with dielectric medium theoretical according to the crystal chemistry principle, with A 2BO 4This typical Phenacite type consists of the basis, uses Li + 1Ion occupies the A position, uses the Mo of high valence state 6+And W 6+The ionic combined ionic occupies the B position, under the prerequisite of not adding any sintering aid, and can be in low-down TR (540 oC ~ 640 oC) interior sintering goes out new function pottery fine and close and that good microwave dielectric property is arranged, and this type pottery can be used as radio frequency laminated ceramic capacitor, chip microwave dielectric resonator or wave filter, LTCC system (LTCC), ceramic substrate, the use of mcm dielectric materials such as (MCM).
Embodiment 1:
Raw material MoO with purity assay 3, WO 3And Li 2CO 3By prescription general formula Li 2(Mo 0.99W 0.01) O 4Preparation.Preparation back thorough mixing ball milling 4 hours is dried then, is sieved, briquetting, through 500 oC pre-burning 4 hours was carried out secondary ball milling 5 hours after then the bulk sample after the pre-burning being pulverized again, and levigate oven dry back granulation is sieved through 60 orders and 120 eye mesh screen bilayers, can obtain required porcelain.With porcelain compression moulding on demand (sheet or column), then 540 oC ~ 640 oSintering became porcelain in 2 hours under the C air, can obtain Phenacite type molybdenum-based and tungsten-based ultralow temperature sintered microwave dielectric ceramic materials.
The performance of this group stupalith reaches following index:
540 oC ~ 640 oSinter porcelain in the C air, the dielectric properties ε under the microwave r=5.3 (13.1GHz), quality factor q=2,800, Qf=37, the temperature coefficient of resonance frequency TCF=-133ppm/ under 000 GHz, microwave oC (25 oC ~ 85 oC).
Embodiment 2:
Raw material MoO with purity assay 3, WO 3And Li 2CO 3By prescription general formula Li 2(Mo 0.5W 0.5) O 4Preparation.Preparation back thorough mixing ball milling 4 hours is dried then, is sieved, briquetting, through 500 oC pre-burning 4 hours was carried out secondary ball milling 5 hours after then the bulk sample after the pre-burning being pulverized again, and levigate oven dry back granulation is sieved through 60 orders and 120 eye mesh screen bilayers, can obtain required porcelain.With porcelain compression moulding on demand (sheet or column), then 540 oC ~ 640 oSintering became porcelain in 2 hours under the C air, can obtain Phenacite type molybdenum-based and tungsten-based ultralow temperature sintered microwave dielectric ceramic materials.
The performance of this group stupalith reaches following index:
540 oC ~ 640 oSinter porcelain in the C air, the dielectric properties ε under the microwave r=5.4 (14.2GHz), quality factor q=3,500, Qf=49, the temperature coefficient of resonance frequency TCF=-139ppm/ under 700 GHz, microwave oC (25 oC ~ 85 oC).
Embodiment 3:
Raw material MoO with purity assay 3, WO 3And Li 2CO 3By prescription general formula Li 2(Mo 0.01W 0.99) O 4Preparation.Preparation back thorough mixing ball milling 4 hours is dried then, is sieved, briquetting, through 500 oC pre-burning 4 hours was carried out secondary ball milling 5 hours after then the bulk sample after the pre-burning being pulverized again, and levigate oven dry back granulation is sieved through 60 orders and 120 eye mesh screen bilayers, can obtain required porcelain.With porcelain compression moulding on demand (sheet or column), then 540 oC ~ 640 oSintering became porcelain in 2 hours under the C air, can obtain Phenacite type molybdenum-based and tungsten-based ultralow temperature sintered microwave dielectric ceramic materials.
The performance of this group stupalith reaches following index:
540 oC ~ 640 oSinter porcelain in the C air, the dielectric properties ε under the microwave r=5.5 (15.7GHz), quality factor q=4,300, Qf=63, the temperature coefficient of resonance frequency TCF=-149ppm/ under 400 GHz, microwave oC (25 oC ~ 85 oC).
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. Phenacite type molybdenum-based and tungsten-based ultralow temperature sintered microwave dielectric ceramic materials, it is characterized in that: this stupalith structure expression is: Li 2(Mo 1-xW x) O 4, 0.0＜x in the formula＜1.0.
2. realize the preparation method of the described Phenacite type molybdenum-based and tungsten-based ultralow temperature sintered microwave dielectric ceramic materials of claim 1, it is characterized in that, carry out according to the following steps:
1) with chemical feedstocks MoO 3, WO 3And Li 2CO 3By prescription general formula Li 2(Mo 1-xW x) O 4Preparation, 0.0＜x in the formula＜1.0;
2) with the step 1) batch mixes, ball milling 5～8 hours 100 ℃～200 ℃ oven dry down, is pressed into block body behind 200 orders that sieve;
3) with step 2) blocks through 500 ℃～800 ℃ pre-burnings, and be incubated 4～6 hours, obtain sample and burn piece;
4) sample is burnt piece and pulverize, and through 5～6 hours secondary ball milling, 100 ℃～200 ℃ oven dry, granulations down, granulation obtained the porcelain powder after 60 orders and 120 eye mesh screen bilayers sieve;
5) with the porcelain powder pressing forming, became porcelain in 2～4 hours at 540 ℃～640 ℃ following sintering, obtain Phenacite type molybdenum-based and tungsten-based ultralow temperature sintered microwave dielectric ceramic materials.
CN2010101920277A 2010-06-04 2010-06-04 Phenacite type molybdenum-based and tungsten-based ultralow temperature sintered microwave dielectric ceramic materials and preparation method thereof Expired - Fee Related CN101823880B (en)

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