CN103922739A - B-substituted BNT microwave dielectric ceramic material and preparation method - Google Patents

B-substituted BNT microwave dielectric ceramic material and preparation method Download PDF

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CN103922739A
CN103922739A CN201410092423.0A CN201410092423A CN103922739A CN 103922739 A CN103922739 A CN 103922739A CN 201410092423 A CN201410092423 A CN 201410092423A CN 103922739 A CN103922739 A CN 103922739A
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dielectric ceramic
microwave dielectric
metallic element
bnt
oxide compound
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CN103922739B (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 B-substituted BNT microwave dielectric ceramic material and its preparation method belong to the technical field of a functional material. The general chemical formula of the microwave dielectric ceramic material is Ba3.75Nd9.5Ti18-y(M,N)yO54, wherein y is less than or equal to 2.5 and greater than or equal to 0.6; the microwave dielectric ceramic material is prepared by steps of: burdening BaO, Nd2O3, TiO2, oxides of metallic elements M and N according to mole ratio of the general chemical formula, carrying out ball-milling, presintering and sintering; an oxide of the element M is Nb2O5; and an oxide of the element N is one or more compounds selected from Al2O3, MgO, ZnO, Co2O3 and NiO. According to the invention, simultaneous substitution of high and low valence elements is carried out in the B position of Ba6-3xNd8+2xTi18O54. The microwave dielectric ceramic material prepared by a one-step synthesis process has high dielectric constant, low loss characteristic and low frequency-temperature coefficient, can meet requirements in the microwave communication industry, and is especially suitable for manufacturing of RFID tags.

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 of making radio electronic label and preparation method thereof.
Background technology
In recent years, produce and promoted the development of REID (radio frequency identification, RFID) along with the development of mobile communication technology and technology of Internet of things and the cross coupled of the two.REID is one of core technology of 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 key foundation material of preparing radio electronic label, generally adopts specific inductivity to exceed 60 microwave dielectric ceramic materials making.Along with development and the application of micro-wave communication technology 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 important parameters that performance index are all microwave dielectric materials: under same condition, it is lower that microwave device adopts higher Q value material to make device loss, heating problem during effective solution device is integrated, can think that the Q value of microwave dielectric material is to weigh the important parameter of microwave material performance quality; Adopt the microwave dielectric material of larger specific inductivity to contribute to the miniaturization of microwave device; Meanwhile, the frequency-temperature coefficient going to zero is the whether stable important parameter of device performance.Therefore develop under microwave frequency and have high dielectric constant, the microwave dielectric ceramic materials of low-loss and the frequency-temperature coefficient that goes to zero has very large using value.
In current microwave-medium ceramics, study more material system and comprise microwave ceramics and the leaded pottery with complex perovskite structure various countries.Wherein composite perofskite has higher Q × f value, less frequency-temperature coefficient, but generally lower (being conventionally less than 60) of its specific inductivity 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 to 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) has hindered its application in batch production.This impels people to adopt various means regulating frequency temperature coefficient values, and current research is mixed and solved by two kinds of contrary potteries of temperature frequency coefficient on the one hand, adopts in addition various doping vario-properties or is replaced and reached the object of improving performance by A position.The compound specific inductivity that usually reduces system of two-phase, for example, Yu Shengquan adopts BaNd in " pottery is international " (Ceramic International, SCI) 2ti 4o 12and BaZn 2ti 4o 11compound, the ceramic Q × f value obtaining reaches 60000GHz, and temperature frequency coefficient is also close to zero, but specific inductivity 34 left and right; 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 replace 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 that adopts A position to replace in system is more, and has obtained the stupalith of various excellent performances, the higher specific inductivity of 90 left and right.
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 not good enough owing to replacing difficulty or modified effect.The people such as M.Mizuta were in the 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 54synthetic and the microwave-medium characteristic research of (α=1+y/36) sosoloid " (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 " U.S.'s pottery 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 reported the data that B position replaces; 1997, the people such as R.UBIC reported Ba in " investigation of materials journal " (Material Research Society) 6-3xnd 8+2xti 18o 54, when x=0.75, the specific inductivity of system approximately 89, Q × f > 10000GHz, 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, near higher x value (0.75) is still single tungsten copper ore deposit crystalline phase, and also relatively low (57～70ppm/ DEG C) of its frequency-temperature coefficient.Although up to the present, the research that B position replaces does not obtain gratifying practical microwave-medium ceramics, and these researchs have all confirmed at Ba 6-3xnd 8+2xti 18o 54in carry out B position and replace and there is feasibility.
Adoption of innovation of the present invention is to Ba 6-3xnd 8+2xti 18o 54the simultaneously-substituted research of the high low price element in middle B position, 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 have the microwave dielectric ceramic materials of lower frequency-temperature coefficient, to meet the application demand of micro-wave communication industry.
Summary of the invention
The mode that adoption of innovation B of the present invention position replaces, provide a kind of and there is high dielectric constant, compared with low-loss, approach zero frequency-temperature coefficient, 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, has tungsten copper ore deposit crystal phase structure, and its chemical general formula is Ba 3. 75nd 9.5ti 18-y(M, N) yo 54, wherein 0.6≤y≤2.5, M is metallic element Nb, N is one or more in metal element A l, Mg, Zn, Co, Ni; 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 mole proportioning of each element in described chemical general formula through batching, ball milling mix, at pre-burning and 1250～1350 DEG C, sintering is made at 1050～1150 DEG C; Its Q × f value reaches 6000～13000GHz, and relative permittivity is adjustable between 65～85, and temperature coefficient of resonance frequency is in ± 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 the oxide compound of metallic element N be according to chemical general formula Ba 3.75nd 9.5ti 18-y(M, N) yo 54in mole proportioning 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; The compound of step 1 is carried out to ball milling, obtain ball milling material;
Step 3: dry, sieve; 60 mesh sieves are dried and crossed to step 2 gained ball milling material and obtain dry powder;
Step 4: pre-burning; Dry step 3 gained powder is placed in to pre-burning under 1050～1150 DEG C of temperature condition and within 3～5 hours, obtains pre-burning powder;
Step 5: granulation, compression molding; Granulation after step 4 gained pre-burning powder is mixed with polyvinyl alcohol water solution, granulation size control, at 80～160 orders, is put into the dry-pressing formed green compact that obtain of forming mould by pellet;
Step 6: sintering; Step 5 gained green compact are placed in to 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: taking zirconia balls as ball-milling medium, according to compound: abrading-ball: the mass ratio of deionized water is 1:(3～5): (1～1.5) grinds the ball milling material that obtains mixing for 6～8 hours.
The starting material Main Function adopting in the present invention is as follows respectively: BaO, Nd 2o 3and TiO 2be mainly used to form principal crystalline phase, because the element of high price or low price replaces separately Ti 4+can produce valence state and not mate the problem that causes electric charge nonconservation, thereby 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 i.e. higher Q value of lower loss 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, and reaches the object of reduction system frequency-temperature coefficient, and specific inductivity and all higher Q × f values of adjustable maintenance simultaneously of frequency-temperature coefficient.
2. in formula of the present invention, do not contain Pb, the volatility such as Cd or heavy metal, be a kind of environment friendly microwave dielectric ceramic.
3. most formula sintering temperatures are all at pure BaO-Nd 2o 3-TiO 21350 DEG C of bases on be reduced to 1300 DEG C of left and right, there is certain power savings advantages.
4. adopt single synthesis technique, easily realize the stably manufactured of material.
5. in performance, realized larger lifting: prior art formula Q × f value generally in 5000～10000 left and right, and its temperature coefficient of resonance frequency is at+50～140ppm/ DEG C, can not meet the microwave device application requiring for RF identification, 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 in ± 10ppm/ DEG C, and stable performance, can meet the application demand of modern microwave device.
6. starting material are in liberal supply at home, cheap, make the cost degradation of high performance microwave pottery become possibility.
Brief description of the drawings
Fig. 1 is the XRD analysis result that B provided by the present invention position 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:
Press in table 1 mass percent and accurately weigh various raw materials, ball milling 6～8 hours in deionized water, 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 to carry out granulation, dry-pressing formed under 22Mpa pressure, obtaining diameter is 14.5mm, and the cylinder green compact that thickness is 7.8mm, at base substrate sintering 1.5～3 hours at 1250～1350 DEG C, obtain sintering block, technique and performance test results are in table 2.
The material composition of table 1 embodiment
Technique and microwave dielectric property that table 2 embodiment adopts

Claims (3)

1. B position replaces a BNT microwave dielectric ceramic materials, has tungsten copper ore deposit crystal phase structure, and its chemical general formula is Ba 3. 75nd 9.5ti 18-y(M, N) yo 54, wherein 0.6≤y≤2.5, M is metallic element Nb, N is one or more in metal element A l, Mg, Zn, Co, Ni; 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 mole proportioning of each element in described chemical general formula through batching, ball milling mix, at pre-burning and 1250～1350 DEG C, sintering is made at 1050～1150 DEG C; Its Q × f value reaches 6000～13000GHz, and relative permittivity is adjustable between 65～85, and temperature coefficient of resonance frequency is in ± 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 the oxide compound of metallic element N be according to chemical general formula Ba 3.75nd 9.5ti 18-y(M, N) yo 54in mole proportioning 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; The compound of step 1 is carried out to ball milling, obtain ball milling material;
Step 3: dry, sieve; 60 mesh sieves are dried and crossed to step 2 gained ball milling material and obtain dry powder;
Step 4: pre-burning; Dry step 3 gained powder is placed in to pre-burning under 1050～1150 DEG C of temperature condition and within 3～5 hours, obtains pre-burning powder;
Step 5: granulation, compression molding; Granulation after step 4 gained pre-burning powder is mixed with polyvinyl alcohol water solution, granulation size control, at 80～160 orders, is put into the dry-pressing formed green compact that obtain of forming mould by pellet;
Step 6: sintering; Step 5 gained green compact are placed in to 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 according to claim 2 position replaces the preparation method of BNT microwave dielectric ceramic materials, it is characterized in that, in step 2, concrete mechanical milling process is: taking zirconia balls as ball-milling medium, according to compound: abrading-ball: the mass ratio of deionized water is 1:(3～5): (1～1.5) grinds the ball milling material that obtains mixing for 6～8 hours.
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CN105837213A (en) * 2016-03-29 2016-08-10 电子科技大学 Microwave dielectric ceramic material doped with ReAlO3 and preparation method thereof.
CN111943673A (en) * 2020-07-03 2020-11-17 成都宏科电子科技有限公司 Low-temperature sintered BNT microwave dielectric material and preparation method thereof
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CN104261828A (en) * 2014-09-19 2015-01-07 天津大学 High-quality-factor neodymium-niobate microwave dielectric ceramic and preparation method thereof
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
CN104844194A (en) * 2015-04-13 2015-08-19 电子科技大学 A-B site simultaneously substituting microwave dielectric ceramic material and preparation method thereof
CN105016729A (en) * 2015-08-11 2015-11-04 电子科技大学 Ca-Nd-Ti microwave dielectric ceramic material 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
CN105272213A (en) * 2015-11-19 2016-01-27 电子科技大学 High-dielectric low-loss microwave dielectric ceramic material and preparation method thereof
CN105837213A (en) * 2016-03-29 2016-08-10 电子科技大学 Microwave dielectric ceramic material doped with ReAlO3 and preparation method thereof.
CN105837213B (en) * 2016-03-29 2019-03-29 电子科技大学 Add ReAlO3Microwave dielectric ceramic materials and preparation method thereof
CN111943673A (en) * 2020-07-03 2020-11-17 成都宏科电子科技有限公司 Low-temperature sintered BNT microwave dielectric material and preparation method thereof
CN113519906A (en) * 2021-08-25 2021-10-22 深圳麦克韦尔科技有限公司 Aerosol generating assembly and aerosol generating system
WO2023023987A1 (en) * 2021-08-25 2023-03-02 深圳麦克韦尔科技有限公司 Aerosol-generating assembly and aerosol-generating system
CN113519906B (en) * 2021-08-25 2023-09-12 深圳麦克韦尔科技有限公司 Aerosol generating assembly and aerosol generating system
EP4193855A4 (en) * 2021-08-25 2023-10-18 Shenzhen Smoore Technology Limited Aerosol-generating assembly and aerosol-generating system

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