CN103922739B - A kind of B position replaces BNT microwave dielectric ceramic materials and preparation method thereof - Google Patents

A kind of B position replaces BNT microwave dielectric ceramic materials and preparation method thereof Download PDF

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CN103922739B
CN103922739B CN201410092423.0A CN201410092423A CN103922739B CN 103922739 B CN103922739 B CN 103922739B CN 201410092423 A CN201410092423 A CN 201410092423A CN 103922739 B CN103922739 B CN 103922739B
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oxide compound
dielectric ceramic
ceramic materials
microwave dielectric
metallic element
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CN103922739A (en
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唐斌
陈鹤拓
袁颖
钟朝位
张树人
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University of Electronic Science and Technology of China
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Abstract

A kind of B position replaces BNT microwave dielectric ceramic materials and preparation method thereof, belongs to technical field of function materials.The chemical general formula of microwave dielectric ceramic materials is Ba 3.75nd 9.5ti 18-y(M, N) yo 54, wherein 0.6≤y≤2.5; By BaO, Nd 2o 3, TiO 2, metallic element M, N oxide compound make through batching, ball milling, pre-burning and sintering by the mol ratio of chemical general formula; Wherein the oxide compound of element M is Nb 2o 5, the oxide compound of element N is Al 2o 3, MgO, ZnO, Co 2o 3, one or more in NiO.The present invention is to Ba 6-3xnd 8+2xti 18o 54middle B position is carried out high low price element and is replaced simultaneously, the microwave dielectric ceramic materials obtained through single sintering technique has higher specific inductivity, lower loss characteristic and lower frequency-temperature coefficient, the demand of micro-wave communication industry can be met, be especially applicable to making radio electronic label.

Description

A kind of B position replaces BNT microwave dielectric ceramic materials and preparation method thereof
Technical field
The invention belongs to technical field of function materials, relate to microwave dielectric ceramic materials and preparation method thereof, be especially applicable to microwave dielectric ceramic materials making radio electronic label and preparation method thereof.
Background technology
In recent years, along with the development of mobile communication technology and technology of Internet of things and the cross coupled of the two produce and promoted the development of REID (radio frequency identification, RFID).One of REID core technology being thing network sensing layer; REID is also a kind of wireless communication technology, is made up of read write line, antenna and electronic tag, and at electronic tag, antenna and read write line all need to use microwave-medium ceramics.Microwave-medium ceramics is the core base material preparing radio electronic label, and the general microwave dielectric ceramic materials of specific inductivity more than 60 that adopt makes.Along with development and the application of microwave communication techniques and Internet of Things, the succinct and cost degradation of high frequency, high stability, preparation technology has become the important requirement of radio electronic label manufacture and production.Along with the development of Internet of Things, the requirement of microwave dielectric ceramic materials is also improved increasingly: higher specific inductivity, lower frequency-temperature coefficient, lower lossy microwave.These three performance index are all important parameters of microwave dielectric material: under same condition, microwave device adopts higher Q value material making devices loss lower, heating problem during effective solution device is integrated, can think that the Q value of microwave dielectric material weighs the important parameter of microwave material performance quality; The microwave dielectric material of larger specific inductivity is adopted to contribute to the miniaturization of microwave device; Meanwhile, the frequency-temperature coefficient gone to zero is the whether stable important parameter of device performance.Therefore develop under microwave frequency and there is high dielectric constant, low-loss and the microwave dielectric ceramic materials of the frequency-temperature coefficient gone to zero has very large using value.
In current microwave-medium ceramics, various countries study more material system and comprise the microwave ceramics and leaded pottery with complex perovskite structure.Wherein composite perofskite has higher Q × f value, less frequency-temperature coefficient, but its specific inductivity general lower (being usually less than 60), be unsuitable for the use in RF identification.Leaded ceramic high temperature is volatile and by toxicity, now less use.In practical application, more is adopt the BaO-Nd with tungsten copper ore deposit structure 2o 3-TiO 2system pottery, cost is relatively cheap, and firing temperature is wider, has become one of most widely used microwave dielectric ceramic materials, can be used for making dielectric filter, laminated ceramic capacitor and dielectric resonator etc.
Although Ba 6-3xnd 8+2xti 18o 54system pottery has higher specific inductivity, excellent Q × f value, but frequency-temperature coefficient excessive (60 ~ 140ppm/ DEG C), hinders its application in batch production.This impels people to adopt various means regulating frequency temperature coefficient value, and current research by the pottery mixing solution that two kinds of temperature frequency coefficient are contrary, is adopted various doping vario-property in addition or replaced the object reaching and improve performance by A position on the one hand.Two-phase compound usually reduces the specific inductivity of system, and such as, Yu Shengquan adopts BaNd in " pottery is international " (Ceramic International, SCI) 2ti 4o 12and BaZn 2ti 4o 11compound, the ceramic Q × f value obtained reaches 60000GHz, and temperature frequency coefficient is also close to zero, but specific inductivity about 34; Zhu Jianhua is at " European ceramic association proceedings " (Journal of the European Ceramic Society, SCI) Ba 4.2nd 9.2ti 18o 54in system, doping is as LnAlO 3, successfully reduce temperature frequency coefficient, but its mechanism indefinite; Belous adopts Ca to carry out replacement preparation (Ba to Ba position 1-yca y) 6- xnd 8+2xti 18o 54pottery, is successfully adjusted to zero by frequency-temperature coefficient.Various countries researchist is at BaO-Nd 2o 3-TiO 2the research work adopting A position to replace in system is more, and obtains the stupalith of various excellent performance, the higher specific inductivity of about 90.
Both at home and abroad to Ba 6-3xnd 8+2xti 18o 54the research that system pottery B position replaces is less, and generally speaking trace it to its cause is owing to replacing difficulty or modified effect is not good enough.The people such as M.Mizuta were in document " eka-tungsten copper mine (Ba in " Japanese Applied Physics journal " (Japanese Journal of Applied Physics) in 1996 6- 3xsm 8+2x) Ti 18-yal yo 54the synthesis of (α=1+y/36) sosoloid and microwave-medium characteristic research " (Formation of tungsten bronze-type (Ba 6-3xsm 8+2x) ɑti 18-yal yo 54(α=1+y/36) solid solutions and microwave dielectric properties) report adopt in adopt Al 3+replace Ti 4+, along with Al 2o 3increasing of content, specific inductivity successively decreases, and Q × f value increases progressively, and temperature frequency coefficient is more negative; 2002, the document " Ba of the people such as Chen in " American Ceramics proceedings " (Journal of the American Ceramic Society) 6-3xsm 8+2xti 18o 54middle A, B position replaces ceramic performance research jointly " (A-and B Site Cosubstituted Ba 6-3xsm 8+2xti 18o 54microwave Dielectric Ceramics) in report B position replace data; 1997, the people such as R.UBIC are report Ba in " investigation of materials journal " (Material Research Society) 6-3xnd 8+2xti 18o 54, during x=0.75, specific inductivity about 89, Q × f > 10000GHz of system, frequency-temperature coefficient is near 60ppm/ DEG C simultaneously.2007, the article " Ba of the people such as L.Zhang in " European ceramic proceedings " (Journal of the European ceramic society) 6-3xnd 8+2xti 18o 54form the research of the x upper limit in the sosoloid of new tungsten copper ore deposit " (Upper limit of x in Ba 6-3xnd 8+2xti 18o 54new tungsten bronze solid solution) report, higher x value (near 0.75) is still single tungsten copper ore deposit crystalline phase, and its frequency-temperature coefficient is also relatively low (57 ~ 70ppm/ DEG C).Although up to the present, the research that B position replaces does not obtain gratifying practical microwave-medium ceramics, and these researchs all confirm at Ba 6-3xnd 8+2xti 18o 54in carry out B position replace there is feasibility.
The present invention innovates and adopts Ba 6-3xnd 8+2xti 18o 54the simultaneously-substituted research of middle B position high low price element, and it is simple to obtain a kind of technique by this mode exploitation, material cost is low, specific inductivity is higher, low loss characteristic, and the microwave dielectric ceramic materials having lower frequency-temperature coefficient, to meet the application demand of micro-wave communication industry.
Summary of the invention
The present invention innovates the mode adopting B position to replace, and provides a kind of and has high dielectric constant, compared with low-loss, frequency-temperature coefficient close to zero, and production technique BNT microwave dielectric ceramic materials simple, with low cost and preparation method thereof.
For achieving the above object, the technical solution used in the present invention is:
A kind of B position replaces BNT microwave dielectric ceramic materials, and have tungsten copper ore deposit crystal phase structure, its chemical general formula is Ba 3. 75nd 9.5ti 18-y(M, N) yo 54, wherein 0.6≤y≤2.5, M to be metallic element Nb, N be in metal element A l, Mg, Zn, Co, Ni one or more; Described B position replaces BNT microwave dielectric ceramic materials by BaO, Nd 2o 3, TiO 2, the oxide compound of metallic element M and the oxide compound of metallic element N according to the mol ratio of element each in described chemical general formula through batching, ball milling mixing, sinter at pre-burning and 1250 ~ 1350 DEG C at 1050 ~ 1150 DEG C and make; Its Q × f value reaches 6000 ~ 13000GHz, and relative permittivity is adjustable between 65 ~ 85, and temperature coefficient of resonance frequency is within ± 10ppm/ DEG C; The oxide compound of wherein said metallic element M is Nb 2o 5, the oxide compound of described metallic element N is Al 2o 3, MgO, ZnO, Co 2o 3, one or more in NiO.
Above-mentioned B position replaces the preparation method of BNT microwave dielectric ceramic materials, comprises the following steps:
Step 1: batching; Adopt BaO, Nd 2o 3, TiO 2, the oxide compound of metallic element M and metallic element N oxide compound according to chemical general formula Ba 3.75nd 9.5ti 18-y(M, N) yo 54in the mol ratio of each element prepare burden; Wherein 0.6≤y≤2.5, the oxide compound of described metallic element M is Nb 2o 5, the oxide compound of described metallic element N is Al 2o 3, MgO, ZnO, Co 2o 3, one or more in NiO.
Step 2: ball milling; By step 1 compound carry out ball milling, obtain ball milling material;
Step 3: dry, sieve; Step 2 gained ball milling material is dried and crossed 60 mesh sieves and obtains dry powder;
Step 4: pre-burning; Under dry for step 3 gained powder is placed in 1050 ~ 1150 DEG C of temperature condition, pre-burning obtains pre-burning powder in 3 ~ 5 hours;
Step 5: granulation, compression molding; Granulation after step 4 gained pre-burning powder is mixed with polyvinyl alcohol water solution, pellet, at 80 ~ 160 orders, is put into that forming mould is dry-pressing formed obtains green compact by granulation size control;
Step 6: sintering; Step 5 gained green compact are placed in 1250 ~ 1350 DEG C of temperature condition sintering 1.5 ~ 3 hours, obtain final B position and replace BNT microwave dielectric ceramic materials.
In step 2, concrete mechanical milling process is: be ball-milling medium with zirconia balls, according to compound: abrading-ball: the mass ratio of deionized water is 1:(3 ~ 5): (1 ~ 1.5) carries out the ball milling material that grinding obtains mixing for 6 ~ 8 hours.
The starting material Main Function adopted in the present invention is as follows respectively: BaO, Nd 2o 3and TiO 2be mainly used to form principal crystalline phase, because high price or element at a low price replace Ti separately 4+valence state can be produced and do not mate the problem causing electric charge nonconservation, thus adopt aluminum oxide (Al at a low price simultaneously 2o 3), magnesium oxide (MgO), zinc oxide (ZnO), nickel oxide (NiO), cobalt sesquioxide (Co 2o 3) in the Niobium Pentxoxide (Nb of one or several and high price 2o 5) replace Ti 4+position, realizes reduction system frequency-temperature coefficient, promotes the object of ceramic Q value.
Microwave dielectric ceramic materials provided by the invention, has the Q value that lower loss is namely higher after testing, higher specific inductivity and nearly zero temperature coefficient of resonance frequency.
Compared with prior art, the present invention has following characteristics:
1. the present invention adopts at Ba 6-3xnd 8+2xti 18o 54the high low price element in middle enforcement B position replaces Ti position simultaneously, is different from traditional A position and replaces, reach the object of reduction system frequency-temperature coefficient, and specific inductivity and frequency-temperature coefficient are all adjustable keeps higher Q × f value simultaneously.
2. not containing volatility or the heavy metals such as Pb, Cd in formula of the present invention, is a kind of environment friendly microwave dielectric ceramic.
3. most formula sintering temperature is all at pure BaO-Nd 2o 3-TiO 21350 DEG C of bases on be reduced to about 1300 DEG C, there is certain power savings advantages.
4. adopt single synthesis technique, easily realize the stably manufactured of material.
5. performance achieves larger lifting: prior art formula Q × f value is general about 5000 ~ 10000, and its temperature coefficient of resonance frequency is at+50 ~ 140ppm/ DEG C, the microwave device application requiring for RF identification can not be met, microwave dielectric ceramic materials Q × f value provided by the invention between 6000 ~ 13000GHz, relative permittivity ε rbetween 65 ~ 85, and temperature coefficient of resonance frequency is all within ± 10ppm/ DEG C, and stable performance, the application demand of modern microwave device can be met.
6. starting material are in liberal supply at home, cheap, make the cost degradation of high performance microwave pottery become possibility.
Accompanying drawing explanation
Fig. 1 is the XRD analysis result that B position provided by the present invention replaces BNT microwave dielectric ceramic materials.
Fig. 2 is microwave ceramic dielectric material scanning electron microscope sem figure prepared by the present invention.
Embodiment
Specific embodiment
The first step:
By the various raw material of mass percent precise in table 1, in deionized water ball milling 6 ~ 8 hours, then drying, sieve after 1050 ~ 1150 DEG C of pre-burnings 5 ~ 8 hours.
Second step:
Take the Ba after pre-burning 3.75nd 9.5ti 18-y(M, N) yo 54powder, adds polyvinyl alcohol water solution and carries out granulation, dry-pressing formed under 22Mpa pressure, obtaining diameter is 14.5mm, and thickness is the cylinder green compact of 7.8mm, sinters 1.5 ~ 3 hours at base substrate at 1250 ~ 1350 DEG C, obtain sintering block, technique and performance test results are in table 2.
The material composition of table 1 embodiment
The technique that table 2 embodiment adopts and microwave dielectric property

Claims (3)

1. B position replaces a BNT microwave dielectric ceramic materials, and have tungsten bronze(s) ore deposit crystal phase structure, its chemical general formula is Ba 3.75nd 9.5ti 18-y(M, N) yo 54, wherein 0.6≤y≤2.5, M to be metallic element Nb, N be in metal element A l, Mg, Zn, Co, Ni one or more; Described B position replaces BNT microwave dielectric ceramic materials by BaO, Nd 2o 3, TiO 2, the oxide compound of metallic element M and the oxide compound of metallic element N according to the mol ratio of element each in described chemical general formula through batching, ball milling mixing, sinter at pre-burning and 1250 ~ 1350 DEG C at 1050 ~ 1150 DEG C and make; Its Q × f value reaches 6000 ~ 13000GHz, and relative permittivity is adjustable between 65 ~ 85, and temperature coefficient of resonance frequency is within ± 10ppm/ DEG C; The oxide compound of wherein said metallic element M is Nb 2o 5, the oxide compound of described metallic element N is Al 2o 3, MgO, ZnO, Co 2o 3, one or more in NiO.
2. B position replaces a preparation method for BNT microwave dielectric ceramic materials, comprises the following steps:
Step 1: batching; Adopt BaO, Nd 2o 3, TiO 2, the oxide compound of metallic element M and metallic element N oxide compound according to chemical general formula Ba 3.75nd 9.5ti 18-y(M, N) yo 54in the mol ratio of each element prepare burden; Wherein 0.6≤y≤2.5, the oxide compound of described metallic element M is Nb 2o 5, the oxide compound of described metallic element N is Al 2o 3, MgO, ZnO, Co 2o 3, one or more in NiO;
Step 2: ball milling; By step 1 compound carry out ball milling, obtain ball milling material;
Step 3: dry, sieve; Step 2 gained ball milling material is dried and crossed 60 mesh sieves and obtains dry powder;
Step 4: pre-burning; Under dry for step 3 gained powder is placed in 1050 ~ 1150 DEG C of temperature condition, pre-burning obtains pre-burning powder in 3 ~ 5 hours;
Step 5: granulation, compression molding; Granulation after step 4 gained pre-burning powder is mixed with polyvinyl alcohol water solution, pellet, at 80 ~ 160 orders, is put into that forming mould is dry-pressing formed obtains green compact by granulation size control;
Step 6: sintering; Step 5 gained green compact are placed in 1250 ~ 1350 DEG C of temperature condition sintering 1.5 ~ 3 hours, obtain final B position and replace BNT microwave dielectric ceramic materials.
3. B position according to claim 2 replaces the preparation method of BNT microwave dielectric ceramic materials, it is characterized in that, in step 2, concrete mechanical milling process is: be ball-milling medium with zirconia balls, according to compound: abrading-ball: the mass ratio of deionized water is 1:(3 ~ 5): (1 ~ 1.5) carries out the ball milling material that grinding obtains mixing for 6 ~ 8 hours.
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CN104844194B (en) * 2015-04-13 2017-07-11 电子科技大学 AB simultaneously-substituted microwave dielectric ceramic materials and preparation method thereof
CN105016729B (en) * 2015-08-11 2018-04-13 电子科技大学 Ca Nd Ti microwave dielectric ceramic materials and preparation method thereof
CN105272213B (en) * 2015-11-19 2018-05-15 电子科技大学 Low damage microwave dielectric ceramic materials of height Jie and preparation method thereof
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