CN104030682B - A kind of without glass low-temperature sintering temperature stable type microwave dielectric ceramic materials and preparation method thereof - Google Patents
A kind of without glass low-temperature sintering temperature stable type microwave dielectric ceramic materials and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of without glass low-temperature sintering temperature stable type microwave dielectric ceramic materials and preparation method thereof.The chemical formula of this ceramic material is A1-3xBi2xMoO4, wherein A is Ca2+, Sr2+, Ba2+Or Pb2+；0.005≤x≤0.3.The ABO to have scheelite-type structure of its preparation method4Based on type molybdenio dielectric material, utilizing the method that valence state compensates, replace bivalent ions mode by trivalent bismuth ion and form A position deficiency solid solution, preparation method is simple, and sintering temperature is low.This ceramic material be a kind of need not add glass sintering aid just can sinter at low temperatures, the high performance microwave medium ceramic material that can be applicable to LTCC technology of temperature stabilization (temperature coefficient of resonance frequency is little), its dielectric constant is 8～45, most high-quality-factor is Q × f value=103750GHz, and minimum | TCF | value can reach 1.2ppm/ DEG C.
Description
Technical field
The invention belongs to technical field of electronic ceramic, relate to a kind of microwave dielectric ceramic materials and preparation method thereof, especially a kind of without glass low-temperature sintering temperature stable type microwave dielectric ceramic materials and preparation method thereof.
Background technology
Information technology develops rapidly in recent years, the demand in miniaturization, lightness, high reliability, high integration and low cost such as communication class electronic product, Military Electronics complete machine, and the microwave device based on microwave-medium ceramics is had higher requirement.Device volume can be effectively reduced with the multi-layer structure design based on LTCC (low-temperatureco-firedceramic, LTCC) technology, be the important technical realizing these demands.
LTCC technology is the integrated assembly technology of a kind of multi-crossed disciplines attracted people's attention, and relates to the wide spectrums such as circuit design, material science, microwave technology.It is the new material technology developed by Hughes Electronics the eighties in 20th century at first, utilizes low-temperature sintered ceramics material, the patterning according to design, by one-time sintering technology such as substrate, electronic component, electrode materials, substantially increases production efficiency.Compared with other component integration technology, LTCC technology has many advantages: the sintering temperature of LTCC technology is generally below 950 DEG C, it is possible to adopts the high conductivity metal such as gold, silver, copper as conducting medium, reduces technology difficulty and improve signaling rate；The dielectric constant of LTCC material can change within a large range, makes circuit design motility more；Temperature characterisitic is more outstanding, as having less thermal coefficient of expansion, less temperature coefficient of resonance frequency, is suitable for big electric current and high-temperature stability requirement；Reliability is higher, can be used for adverse circumstances；Thinner live width and distance between centers of tracks can be obtained, improve integrated level.
Microwave dielectric ceramic materials is as one of the critical material of LTCC technology, it should have low-loss (high Q × f value), nearly zero temperature coefficient of resonance frequency (temperature stabilization: TCF～0), sintering temperature and low (< 960 DEG C), can with the characteristic of Ag or Cu electrode matching co-firing.But, the microwave dielectric ceramic materials of the overwhelming majority does not have the temperature coefficient of resonance frequency of sintering temperature and low and nearly zero, being not suitable for the requirement of LTCC technology, it is meaningful that therefore R and D low-temperature sintering temperature-stabilized microwave medium ceramic material system just becomes very.
In sum, developing rapidly of microwave technology has promoted microwave device to miniaturization, integrated development.LTCC technology becomes Current electronic component integration, modular preferred manner with the electricity of its excellence, calorifics, mechanical property, is widely used in the fields such as aerospace industry, military affairs, radio communication, global positioning system, WLAN, automobile.Therefore, chemical composition and preparation technology is simple, sintering temperature is low, have temperature stability, microwave dielectric property excellent and can have broad application prospects with the novel microwave dielectric ceramic material that copper or silver electrode burn altogether.
Summary of the invention
It is an object of the invention to the shortcoming overcoming above-mentioned prior art, there is provided a kind of without glass low-temperature sintering temperature stable type microwave dielectric ceramic materials and preparation method thereof, this ceramic material be a kind of need not add glass sintering aid just can sinter at low temperatures, temperature coefficient of resonance frequency (TCF) close to zero, the high performance microwave medium ceramic material that can be applicable to LTCC technology.
It is an object of the invention to solve by the following technical programs:
A kind of without glass low-temperature sintering temperature stable type microwave dielectric ceramic materials, its chemical formula is: A1-3xBi2xMoO4, wherein A is Ca2+、Sr2+、Ba2+Or Pb2+；0.005≤x≤0.3.
Its dielectric constant is 8～45, Q × f value is 1880GHz～103750GHz, temperature coefficient of resonance frequency is-91ppm/ DEG C～+25ppm/ DEG C.
This is based on the A position deficiency solid solution of scheelite without glass low-temperature sintering temperature stable type microwave dielectric ceramic materials.
The preparation method of a kind of stable type microwave dielectric ceramic materials of sintering temperature without glass low-temperature, comprises the following steps:
1) by chemical formula A1-3xBi2xMoO4In the proportioning of each element weigh raw material Bi2O3And MoO3And CaCO3、SrCO3、BaCO3, one in PbO, wherein chemical formula A1-3xBi2xMoO4Middle A is Ca2+、Sr2+、Ba2+Or Pb2+, 0.005≤x≤0.3；
2) putting in ball grinder after being mixed by the raw material weighed, add ball milling solvent, the raw material after ball milling, to raw material mix homogeneously, is then taken out and dries, be pressed into block by wet ball grinding；
3) by the block of compacting 450～600 DEG C of pre-burnings, and it is incubated 4～6 hours, obtains sample agglomerate；
4) after being pulverized by sample agglomerate, ball milling is uniform, then drying, pelletize, obtains porcelain powder；
5) by porcelain powder pressing forming, sinter at 550～900 DEG C 2～6 hours and become porcelain, obtain without glass low-temperature sintering temperature stable type microwave dielectric ceramic materials.
Described step 2) in ball grinder be nylon tank, ball milling solvent is dehydrated alcohol.
Described step 2) in Ball-milling Time be 3～12 hours.
Described step 2) in drying temperature be 100～120 DEG C.
Described step 4) middle employing wet ball grinding, ball grinder is nylon tank, and ball milling solvent is dehydrated alcohol.
Described step 4) in Ball-milling Time be 4～12 hours.
Described step 4) in drying temperature be 100～120 DEG C.
Described step 4) in the powder body that obtains of pelletize sieve through 60 orders and 120 eye mesh screen bilayers, the part between two sieves is the porcelain powder of desired particle size.
Relative to prior art, the method have the advantages that
The stable type microwave dielectric ceramic materials of sintering temperature without glass low-temperature provided by the invention, its chemical formula is: A1-3xBi2xMoO4, wherein A is Ca2+、Sr2+、Ba2+Or Pb2+；0.005≤x≤0.3.This ceramic material be a kind of need not add glass sintering aid just can sinter at low temperatures, temperature coefficient of resonance frequency (TCF) close to zero, the high performance microwave medium ceramic material that can be applicable to LTCC technology, this ceramic material can be applicable to the needs of LTCC technology, expands its range of application.
The preparation method of the stable type microwave dielectric ceramic materials of sintering temperature without glass low-temperature provided by the invention, have employed the method for the most simple and effective solid state reaction sintering to prepare target product.First it is the formula choosing proper ratio, choose suitable initial oxide, oxide mix homogeneously is made by a ball milling, oxide is made to carry out preliminary reaction by presintering process, refine the particle size of reactant again through secondary ball milling, obtain required ceramics sample finally by sintering.The method raw material is easy to get, step is simple, easy to operate, sintering temperature is low.
The dielectric constant of the stable type microwave dielectric ceramic materials of sintering temperature without glass low-temperature that the present invention prepares with composition transfer between 8～45, Q × f Distribution value is at 1880GHz～103750GHz, temperature coefficient of resonance frequency is adjustable at-91ppm/ DEG C～+25ppm/ DEG C, and minimum | TCF | value can reach 1.2ppm/ DEG C.
Detailed description of the invention
Below present disclosure is described in further detail.
The stable type microwave dielectric ceramic materials of sintering temperature without glass low-temperature of the present invention is to have the ABO of scheelite-type structure4Based on type molybdenio dielectric material, utilizing the method that valence state compensates, replace bivalent ions mode by trivalent bismuth ion and form A position deficiency solid solution, its recipe formulation is: A1-3xBi2xMoO4, wherein A is Ca2+, Sr2+, Ba2+Or Pb2+；0.005≤x≤0.3.
The concrete preparation process of stable type microwave dielectric ceramic materials of sintering temperature without glass low-temperature of the present invention is as follows:
By formula formula A1-3xBi2xMoO4Preparation raw material CaCO3、SrCO3、BaCO3、PbO、Bi2O3、MoO3, wherein A is Ca2+, Sr2+, Ba2+, Pb2+One in ion, 0.005≤x≤0.3；
Ball milling 3～12 hours after the raw material of preparation is mixed, levigate post-drying, briquetting, then through 450～600 DEG C of pre-burnings, and it is incubated 4～6 hours, the block after pre-burning is carried out secondary ball milling, pelletize after levigate drying, sieve through 60 orders and 120 eye mesh screen bilayers, required porcelain can be obtained.Porcelain is compressing on demand, then sinter at 550～900 DEG C 2～6 hours and become porcelain, can obtain without glass low-temperature sintering temperature stable type microwave dielectric ceramic materials.
The present invention, from the relevant theory of morphology and Dielectric Physics, is compensated by ionic replacement and valence state and forms A position deficiency solid solution.Can under the premise not having any sintering aid, it is achieved low-temperature sintering (550～900 DEG C), and obtain the new function pottery that temperature coefficient of resonance frequency is nearly zero, microwave dielectric property is excellent.This kind of pottery can use as dielectric materials such as LTCC system (LTCC), radio frequency multilayer ceramic capacitor, resonator, wave filter, ceramic antenna, Medium Wave Guide loop, multi-chip module (MCM), bluetooth modules.Several embodiments of the present invention given below:
Embodiment 1
1) by analytically pure raw materials of Ca CO3、Bi2O3、MoO3By formula formula A1-3xBi2xMoO4Preparation, wherein A is Ca2+, x=0.005；
2) by the chemical raw material mixing after preparation, putting in nylon tank, add dehydrated alcohol, adopt wet ball grinding 4 hours, be sufficiently mixed uniformly, after taking-up, flash baking at 100 DEG C, is pressed into bulk；
3) block suppressed is through 600 DEG C of pre-burnings, and is incubated 4 hours, obtains sample agglomerate；
4) sample agglomerate is pulverized, put in nylon tank, add dehydrated alcohol, through the secondary wet process ball milling of 4 hours, be sufficiently mixed levigate after, pelletize after drying at 100 DEG C, the powder body after pelletize sieves through 60 orders and 120 eye mesh screen bilayers, and the part between two sieves is the porcelain powder of desired particle size；
5) porcelain powder is compressing (lamellar or column) on demand, sinter at 900 DEG C 2 hours and become porcelain, can obtain without glass low-temperature sintering temperature stable type microwave dielectric ceramic materials.
The performance of this ceramic material reaches following index:
900 DEG C of air sinter porcelain, the dielectric properties ε under microwave intor=9.3, Q × f value=99410GHz, the temperature coefficient of resonance frequency TCF under microwave～-52.8ppm/ DEG C (25～85 DEG C).
Embodiment 2
1) by analytically pure raw materials of Ca CO3、Bi2O3、MoO3By formula formula A1-3xBi2xMoO4Preparation, wherein A is Ca2+, x=0.015；
2) by the chemical raw material mixing after preparation, putting in nylon tank, add dehydrated alcohol, adopt wet ball grinding 4 hours, be sufficiently mixed uniformly, after taking-up, flash baking at 100 DEG C, is pressed into bulk；
3) block suppressed is through 600 DEG C of pre-burnings, and is incubated 4 hours, obtains sample agglomerate；
4) sample agglomerate is pulverized, put in nylon tank, add dehydrated alcohol, through the secondary wet process ball milling of 4 hours, be sufficiently mixed levigate after, pelletize after drying at 100 DEG C, the powder body after pelletize sieves through 60 orders and 120 eye mesh screen bilayers, and the part between two sieves is the porcelain powder of desired particle size；
5) porcelain powder is compressing (lamellar or column) on demand, sinter at 825 DEG C 2 hours and become porcelain, can obtain without glass low-temperature sintering temperature stable type microwave dielectric ceramic materials.
The performance of this ceramic material reaches following index:
825 DEG C of air sinter porcelain, the dielectric properties ε under microwave intor=10.5, Q × f value=103750GHz, the temperature coefficient of resonance frequency TCF under microwave～-51.8ppm/ DEG C (25～85 DEG C).
Embodiment 3:
1) by analytically pure raw materials of Ca CO3、Bi2O3、MoO3By formula formula A1-3xBi2xMoO4Preparation, wherein A is Ca2+, x=0.15；
2) by the chemical raw material mixing after preparation, putting in nylon tank, add dehydrated alcohol, adopt wet ball grinding 4 hours, be sufficiently mixed uniformly, after taking-up, flash baking at 100 DEG C, is pressed into bulk；
3) block suppressed is through 600 DEG C of pre-burnings, and is incubated 4 hours, obtains sample agglomerate；
4) sample agglomerate is pulverized, put in nylon tank, add dehydrated alcohol, through the secondary wet process ball milling of 4 hours, be sufficiently mixed levigate after, pelletize after drying at 100 DEG C, the powder body after pelletize sieves through 60 orders and 120 eye mesh screen bilayers, and the part between two sieves is the porcelain powder of desired particle size；
5) porcelain powder is compressing (lamellar or column) on demand, sinter at 700 DEG C 2 hours and become porcelain, can obtain without glass low-temperature sintering temperature stable type microwave dielectric ceramic materials.
The performance of this ceramic material reaches following index:
700 DEG C of air sinter porcelain, the dielectric properties ε under microwave intor=21.2, Q × f value=29290GHz, the temperature coefficient of resonance frequency TCF under microwave～-1.2ppm/ DEG C (25～85 DEG C).
Embodiment 4:
1) by analytically pure raw material SrCO3、Bi2O3、MoO3By formula formula A1-3xBi2xMoO4Preparation, wherein A is Sr2+, x=0.15；
2) by the chemical raw material mixing after preparation, putting in nylon tank, add dehydrated alcohol, adopt wet ball grinding 4 hours, be sufficiently mixed uniformly, after taking-up, flash baking at 100 DEG C, is pressed into bulk；
3) block suppressed is through 550 DEG C of pre-burnings, and is incubated 4 hours, obtains sample agglomerate；
4) sample agglomerate is pulverized, put in nylon tank, add dehydrated alcohol, through the secondary wet process ball milling of 4 hours, be sufficiently mixed levigate after, pelletize after drying at 100 DEG C, the powder body after pelletize sieves through 60 orders and 120 eye mesh screen bilayers, and the part between two sieves is the porcelain powder of desired particle size；
5) porcelain powder is compressing (lamellar or column) on demand, sinter at 700 DEG C 2 hours and become porcelain, can obtain without glass low-temperature sintering temperature stable type microwave dielectric ceramic materials.
The performance of this ceramic material reaches following index:
700 DEG C of air sinter porcelain, the dielectric properties ε under microwave intor=22, Q × f value=15000GHz, the temperature coefficient of resonance frequency TCF under microwave～-5ppm/ DEG C (25～85 DEG C).
Embodiment 5:
1) by analytically pure raw material BaCO3、Bi2O3、MoO3By formula formula A1-3xBi2xMoO4Preparation, wherein A is Ba2+, x=0.025；
2) by the chemical raw material mixing after preparation, putting in nylon tank, add dehydrated alcohol, adopt wet ball grinding 4 hours, be sufficiently mixed uniformly, after taking-up, flash baking at 100 DEG C, is pressed into bulk；
3) block suppressed is through 500 DEG C of pre-burnings, and is incubated 4 hours, obtains sample agglomerate；
4) sample agglomerate is pulverized, put in nylon tank, add dehydrated alcohol, through the secondary wet process ball milling of 4 hours, be sufficiently mixed levigate after, pelletize after drying at 100 DEG C, the powder body after pelletize sieves through 60 orders and 120 eye mesh screen bilayers, and the part between two sieves is the porcelain powder of desired particle size；
5) porcelain powder is compressing (lamellar or column) on demand, sinter at 650 DEG C 2 hours and become porcelain, can obtain without glass low-temperature sintering temperature stable type microwave dielectric ceramic materials.
The performance of this ceramic material reaches following index:
650 DEG C of air sinter porcelain, the dielectric properties ε under microwave intor=10.2, Q × f value=55620GHz, the temperature coefficient of resonance frequency TCF under microwave～-32.5ppm/ DEG C (25～85 DEG C).
Embodiment 6:
1) by analytically pure raw material BaCO3、Bi2O3、MoO3By formula formula A1-3xBi2xMoO4Preparation, wherein A is Ba2+, x=0.2；
2) by the chemical raw material mixing after preparation, putting in nylon tank, add dehydrated alcohol, adopt wet ball grinding 4 hours, be sufficiently mixed uniformly, after taking-up, flash baking at 100 DEG C, is pressed into bulk；
3) block suppressed is through 500 DEG C of pre-burnings, and is incubated 4 hours, obtains sample agglomerate；
4) sample agglomerate is pulverized, put in nylon tank, add dehydrated alcohol, through the secondary wet process ball milling of 4 hours, be sufficiently mixed levigate after, pelletize after drying at 100 DEG C, the powder body after pelletize sieves through 60 orders and 120 eye mesh screen bilayers, and the part between two sieves is the porcelain powder of desired particle size；
5) porcelain powder is compressing (lamellar or column) on demand, sinter at 625 DEG C 2 hours and become porcelain, can obtain without glass low-temperature sintering temperature stable type microwave dielectric ceramic materials.
The performance of this ceramic material reaches following index:
625 DEG C of air sinter porcelain, the dielectric properties ε under microwave intor=23, Q × f value=7070GHz, the temperature coefficient of resonance frequency TCF under microwave～+9.8ppm/ DEG C (25～85 DEG C).
Embodiment 7:
1) by analytically pure raw material BaCO3、Bi2O3、MoO3By formula formula A1-3xBi2xMoO4Preparation, wherein A is Ba2+, x=0.3；
2) by the chemical raw material mixing after preparation, putting in nylon tank, add dehydrated alcohol, adopt wet ball grinding 4 hours, be sufficiently mixed uniformly, after taking-up, flash baking at 100 DEG C, is pressed into bulk；
3) block suppressed is through 500 DEG C of pre-burnings, and is incubated 4 hours, obtains sample agglomerate；
4) sample agglomerate is pulverized, put in nylon tank, add dehydrated alcohol, through the secondary wet process ball milling of 4 hours, be sufficiently mixed levigate after, pelletize after drying at 100 DEG C, the powder body after pelletize sieves through 60 orders and 120 eye mesh screen bilayers, and the part between two sieves is the porcelain powder of desired particle size；
5) porcelain powder is compressing (lamellar or column) on demand, sinter at 625 DEG C 2 hours and become porcelain, can obtain without glass low-temperature sintering temperature stable type microwave dielectric ceramic materials.
The performance of this ceramic material reaches following index:
625 DEG C of air sinter porcelain, the dielectric properties ε under microwave intor=26.4, Q × f value=1880GHz, the temperature coefficient of resonance frequency TCF under microwave～-90.9ppm/ DEG C (25～85 DEG C).
Embodiment 8:
1) by analytically pure raw material PbO, Bi2O3、MoO3By formula formula A1-3xBi2xMoO4Preparation, wherein A is Pb2+, x=0.1；
2) by the chemical raw material mixing after preparation, putting in nylon tank, add dehydrated alcohol, adopt wet ball grinding 3 hours, be sufficiently mixed uniformly, after taking-up, flash baking at 100 DEG C, is pressed into bulk；
3) block suppressed is through 500 DEG C of pre-burnings, and is incubated 4 hours, obtains sample agglomerate；
4) sample agglomerate is pulverized, put in nylon tank, add dehydrated alcohol, through the secondary wet process ball milling of 4 hours, be sufficiently mixed levigate after, pelletize after drying at 100 DEG C, the powder body after pelletize sieves through 60 orders and 120 eye mesh screen bilayers, and the part between two sieves is the porcelain powder of desired particle size；
5) porcelain powder is compressing (lamellar or column) on demand, sinter at 600 DEG C 2 hours and become porcelain, can obtain without glass low-temperature sintering temperature stable type microwave dielectric ceramic materials.
The performance of this ceramic material reaches following index:
600 DEG C of air sinter porcelain, the dielectric properties ε under microwave intor=40, Q × f value=20000GHz, the temperature coefficient of resonance frequency TCF under microwave～-8ppm/ DEG C (25～85 DEG C).
Embodiment 9:
1) by analytically pure raw material PbO, Bi2O3、MoO3By formula formula A1-3xBi2xMoO4Preparation, wherein A is Pb2+, x=0.25；
2) by the chemical raw material mixing after preparation, putting in nylon tank, add dehydrated alcohol, adopt wet ball grinding 8 hours, be sufficiently mixed uniformly, after taking-up, flash baking at 120 DEG C, is pressed into bulk；
3) block suppressed is through 450 DEG C of pre-burnings, and is incubated 6 hours, obtains sample agglomerate；
4) sample agglomerate is pulverized, put in nylon tank, add dehydrated alcohol, through the secondary wet process ball milling of 12 hours, be sufficiently mixed levigate after, pelletize after drying at 120 DEG C, the powder body after pelletize sieves through 60 orders and 120 eye mesh screen bilayers, and the part between two sieves is the porcelain powder of desired particle size；
5) porcelain powder is compressing (lamellar or column) on demand, sinter at 550 DEG C 6 hours and become porcelain, can obtain without glass low-temperature sintering temperature stable type microwave dielectric ceramic materials.
Embodiment 10
1) by analytically pure raw material SrCO3、Bi2O3、MoO3By formula formula A1-3xBi2xMoO4Preparation, wherein A is Sr2+, x=0.05；
2) by the chemical raw material mixing after preparation, putting in nylon tank, add ethanol, adopt wet ball grinding 12 hours, be sufficiently mixed uniformly, after taking-up, flash baking at 110 DEG C, is pressed into bulk；
3) block suppressed is through 520 DEG C of pre-burnings, and is incubated 5 hours, obtains sample agglomerate；
4) sample agglomerate is pulverized, put in nylon tank, add ethanol, through the secondary wet process ball milling of 8 hours, be sufficiently mixed levigate after, at 110 DEG C dry after pelletize, powder body after pelletize sieves through 60 orders and 120 eye mesh screen bilayers, and the part between two sieves is the porcelain powder of desired particle size；
5) porcelain powder is compressing (lamellar or column) on demand, sinter at 750 DEG C 4 hours and become porcelain, can obtain without glass low-temperature sintering temperature stable type microwave dielectric ceramic materials.
The dielectric constant of the stable type microwave dielectric ceramic materials of sintering temperature without glass low-temperature that the present invention prepares with composition transfer between 8～45, Q × f Distribution value is at 1880GHz～103750GHz, temperature coefficient of resonance frequency is adjustable at-91ppm/ DEG C～+25ppm/ DEG C, and minimum | TCF | value can reach 1.2ppm/ DEG C.
It is pointed out that examples detailed above can also be enumerated many according to technical scheme, according to the substantial amounts of the results show of applicant, the scope that claims in the present invention are proposed, all can reach the purpose of the present invention.
Claims (7)
1. one kind without glass low-temperature sintering temperature stable type microwave dielectric ceramic materials, it is characterised in that this without glass low-temperature sintering temperature stable type microwave dielectric ceramic materials to have the ABO of scheelite-type structure4Based on type molybdenio dielectric material, utilizing the method that valence state compensates, replace bivalent ions mode by trivalent bismuth ion and form A position deficiency solid solution, its chemical formula is: A1-3xBi2xMoO4, wherein A is Ca2+、Sr2+、Ba2+Or Pb2+；0.005≤x≤0.3, and x ≠ 0.25；Its dielectric constant is 8～45, Q × f value is 1880GHz～103750GHz, temperature coefficient of resonance frequency is-91ppm/ DEG C～+25ppm/ DEG C.
2. the preparation method of the stable type microwave dielectric ceramic materials of sintering temperature without glass low-temperature described in claim 1, it is characterised in that comprise the following steps:
1) by chemical formula A1-3xBi2xMoO4In the proportioning of each element weigh raw material Bi2O3And MoO3And CaCO3、SrCO3、BaCO3, one in PbO, wherein chemical formula A1-3xBi2xMoO4Middle A is Ca2+、Sr2+、Ba2+Or Pb2+, 0.005≤x≤0.3, and x ≠ 0.25；
2) putting in ball grinder after being mixed by the raw material weighed, add ball milling solvent, then the raw material after ball milling is taken out and dries to raw material mix homogeneously, be pressed into block by wet ball grinding for 3～12 hours；
3) by the block of compacting 450～600 DEG C of pre-burnings, and it is incubated 4～6 hours, obtains sample agglomerate；
4) after being pulverized by sample agglomerate, ball milling is uniform, and Ball-milling Time is 4～12 hours, then drying, pelletize, obtains porcelain powder；
5) by porcelain powder pressing forming, sinter at 550～900 DEG C 2～6 hours and become porcelain, obtain without glass low-temperature sintering temperature stable type microwave dielectric ceramic materials.
3. the preparation method of the stable type microwave dielectric ceramic materials of sintering temperature without glass low-temperature according to claim 2, it is characterised in that: described step 2) in ball grinder be nylon tank, ball milling solvent is dehydrated alcohol.
4. the preparation method of the stable type microwave dielectric ceramic materials of sintering temperature without glass low-temperature according to claim 2, it is characterised in that: described step 2) in drying temperature be 100～120 DEG C.
5. the preparation method of the stable type microwave dielectric ceramic materials of sintering temperature without glass low-temperature according to claim 2, it is characterised in that: described step 4) middle employing wet ball grinding, ball grinder is nylon tank, and ball milling solvent is dehydrated alcohol.
6. the preparation method of the stable type microwave dielectric ceramic materials of sintering temperature without glass low-temperature according to claim 2, it is characterised in that: described step 4) in drying temperature be 100～120 DEG C.
7. the preparation method of the stable type microwave dielectric ceramic materials of sintering temperature without glass low-temperature according to claim 2, it is characterized in that: described step 4) in the powder body that obtains of pelletize sieve through 60 orders and 120 eye mesh screen bilayers, the part between two sieves is the porcelain powder of desired particle size.
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| CN101823879A (en) * | 2010-06-03 | 2010-09-08 | 西安交通大学 | Scheelite type molybdenum-based ultralow temperature-sintered microwave dielectric ceramic material and preparation method thereof |
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| Effect of substitution in the scheelite-like series, AxBa1_xBi2Mo4O16 (A = Ca, Sr, Pb);B. Muktha等;《Materials Research Bulletin》;20070130(第42期);2150－2155 * |
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