CN102775144A - BCZN microwave ceramic medium material and preparation method thereof - Google Patents

BCZN microwave ceramic medium material and preparation method thereof Download PDF

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CN102775144A
CN102775144A CN201210248673XA CN201210248673A CN102775144A CN 102775144 A CN102775144 A CN 102775144A CN 201210248673X A CN201210248673X A CN 201210248673XA CN 201210248673 A CN201210248673 A CN 201210248673A CN 102775144 A CN102775144 A CN 102775144A
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唐斌
张晓�
杨成韬
周晓华
钟朝位
张树人
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University of Electronic Science and Technology of China
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Abstract

The invention discloses a microwave ceramic medium material and a preparation method thereof, belonging to the technical field of electronic materials. The microwave ceramic medium material comprises a crystalline phase structure and a doping agent, wherein the principal crystalline phase is BCZN(BaCo1/3Nb2/3O3-BaZn1/3Nb2/3O3), and the secondary crystalline phase is Ba5Nb4O9 and is generated by following a B: bite and B:: bite atom non-stoichiometric ratio and raw material doping. The principal crystalline phase comprises the following raw materials including BaCO3, Co2O3, ZnO and Nb2O5; and a doping agent comprises Al203 and Ta2O5 which account for 0.1-1.50 percent of crystalline phase structural mass, or comprises CeO2 or Y2O3 which accounts for 0.0-0.5 percent of the crystalline phase structural mass. Due to the adoption of the traditional solid phase sintering method, the microwave ceramic medium material has the characteristics of simpleness, easy control, environment friendliness and low cost; and the obtained microwave ceramic medium material has a high Q*f value (-76500GHz), a medium dielectric constant (35+/1) and a frequency temperature coefficient (0+/-10) close to 0, is suitable for making a microwave device medium material, and can meet the manufacturing requirement of a microwave device.

Description

A kind of BCZN microwave ceramic dielectric material and preparation method thereof
Technical field
The invention belongs to electronic information function material and device technology field, be specifically related to that a kind of specific inductivity is moderate, quality factor are higher, frequency-temperature coefficient is near BCZN microwave ceramic dielectric material of zero and preparation method thereof.
Background technology
Microwave dielectric material is widely used in the communications fields such as TV, radar in the microwave epoch that the communication technology has got into removableization, facilitation, miniaturized with characteristics such as its low-loss, high-k, small frequency temperature coefficients.The file of " planning outline is revitalized in the electronics and information industry adjustment " proposes the importance of the media ceramic of the seriation of development specific inductivity, microwave dielectric property excellence.It is the primary study developing direction of microwave-medium ceramics that high-k, hi-q, frequency-temperature coefficient hang down near zero and sintering temperature.
Microwave dielectric material mainly can be divided into BaO-TiO by material system 2, BaO-Ln 2O 3-TiO 2, (Zr, Sn) TiO 4And A (B ' 1/3B " 2/3O 3) be four types, AB ' wherein 1/3B " 2/3O 3The research of system is the most extensive, AB ' 1/3B " 2/3O 3BCZN (BaCo in the system 1/3Nb 2/3O 3-BaZn 1/3Nb 2/3O 3) system since Q * f value higher, τ fAdjustable and Nb 2O 5Advantage such as relative low price, sintering temperature are lower and receiving much concern.BZN: ε r=41, τ f≈ 30ppm/ ℃; BCN: ε r=32, τ f≈-12ppm/ ℃, its ε rAnd τ fAll adjustable, forefathers are in the research process to this system microwave-medium ceramics, and its main purpose is to keep its high specific inductivity and high quality factor, and adjustment τ fApproach zero.1977, people such as Kawashima reported the meliority of BZN as the low-loss microwave dielectric material; 1987, Cheol-Woo Ahn etc. did concrete research to structure, the performance of BCN and xBZN-(1-x) BCN system, points out that microwave property is best when x=0.7: ε r=34.5, Q * f=97000GHz, τ f=0ppm/ ℃, but should research need annealing under 20 ℃/min annealing conditions, condition is harsh; Paik etc. find that in the research of BMN the Mg ionic departs from meeting and promotes the degree of order of BMN and the increase of density, improve microwave property, thereby have promoted the research of domestic and international BCZN system A position, B position atom non-stoichiometric; 2005, F.Azough etc. discovered the 0.4wt%CeO that mixes among the 0.7BZN-0.3BCN 2Can reach the excellent properties of Q * f=84000GHz, but because ball milling can not be applied to actual production for up to 36 hours, forming pressure up to restriction such as 100MPa; 2006, G.A.Ravi and co-worker thereof found at Ca 0.7Ti 0.7La 0.3Al 0.3O 3A spot of Al mixes in the ceramic systems 2O 3Can promote the growth of crystal grain and reduce the space, this method can be applicable in the BCZN system pottery equally.
Summary of the invention
The purpose of this invention is to provide that a kind of specific inductivity is moderate, quality factor are higher, near frequency-temperature coefficient continuous adjustable and BCZN microwave ceramic dielectric material that can intermediate sintering temperature and preparation method thereof zero.
Technical scheme of the present invention is following:
A kind of BCZN microwave ceramic dielectric material comprises crystal phase structure and doping agent; Principal crystalline phase is Ba (Co in the said crystal phase structure 1/3Nb 2/3) O 3-Ba (Zn 1/3Nb 2/3) O 3, with the secondary crystalline phase Ba of trace 5Nb 4O 15Said doping agent comprises 0.1% ~ 1.50% the Al that is equivalent to crystal phase structure quality summation 2O 3And Ta 2O 5
In the above-mentioned BCZN microwave ceramic dielectric material, said Al 2O 3Doping be equivalent to 0.03% ~ 0.5% of crystal phase structure quality summation; Said Ta 2O 5Doping be to be equivalent to 0.07% ~ 1.0% of crystal phase structure quality summation.
In the above-mentioned BCZN microwave ceramic dielectric material, said doping agent also comprises 0.0% ~ 0.5% the CeO that is equivalent to crystal phase structure quality summation 2Or Y 2O 3
It is compound with the BCN ceramic phase with negative frequency temperature factor that the present invention will have the BZN pottery of positive frequency temperature factor; Their two opposite frequency-temperature coefficients are cancelled out each other; And through nonstoichiometry doping way when; Sintering temperature is reduced, the more important thing is that the microwave dielectric property of two kinds of crystalline phases is all very excellent, the microwave dielectric property of the pottery after making has had assurance.In the BCZN microwave ceramic dielectric material, suitable B ' position atom disappearance or the B " microwave property that can improve pottery more than needed.Mix mainly is in order to improve the Q * f value of pottery.The addition of C eO 2, Y 2O 3The doping of rare earth oxide can promote the ceramic crystalline grain growth and increase the degree of order of crystalline structure, thereby improve Q * f value; A spot of Al 2O 3Can promote the grain growing and the intercrystalline space of minimizing of pottery; The Ta of trace 2O 5Doping can significantly improve the Q * f value of BCZN pottery.The sintering temperature of this microwave-medium ceramics is at 1340 ℃～1420 ℃, DIELECTRIC CONSTANTS r=35.0 ± 1, Q * f value reaches as high as 76469GHz, frequency-temperature coefficient τ fAdjustable continuously near 0.
The preparation method of above-mentioned BCZN microwave ceramic dielectric material, as shown in Figure 1, may further comprise the steps:
Step 1: get the raw materials ready.
Select BaCO 3, Co 2O 3, ZnO, Nb 2O 5Be synthetic Ba (Co 1/3Nb 2/3) O 3-Ba (Zn 1/3Nb 2/3) O 3The raw material of principal crystalline phase, the mol ratio between control Ba, Co, Zn and the Nb is Ba:Co:Zn:Nb=3: (0.6+x): (0.4+y): (2+z), wherein-0.041≤x≤0 ,-0.048≤y≤0 ,-0.024≤z≤0.012, the purity of each component raw material is more preferably greater than 99%.Select Al 2O 3And Ta 2O 5As doped raw material and above-mentioned four kinds of raw materials mix batching, Al 2O 3And Ta 2O 5The quality of doped raw material and be Ba (Co 1/3Nb 2/3) O 3-Ba (Zn 1/3Nb 2/3) O 3Principal crystalline phase and Ba 5Nb 4O 150.1% ~ 1.50% of secondary crystalline phase quality summation, wherein said Al 2O 3Doping for being equivalent to Ba (Co 1/3Nb 2/3) O 3-Ba (Zn 1/3Nb 2/3) O 3Principal crystalline phase and Ba 5Nb 4O 150.03% ~ 0.5% of secondary crystalline phase quality summation; Said Ta 2O 5Doping for being equivalent to Ba (Co 1/3Nb 2/3) O 3-Ba (Zn 1/3Nb 2/3) O 3Principal crystalline phase and Ba 5Nb 4O 150.07% ~ 1.0% of secondary crystalline phase quality summation.Doped raw material also can contain simultaneously and be equivalent to Ba (Co 1/3Nb 2/3) O 3-Ba (Zn 1/3Nb 2/3) O 3Principal crystalline phase and Ba 5Nb 4O 150.0% ~ 0.5% CeO of secondary crystalline phase quality summation 2Or Y 2O 3
Step 2: ball milling.
Principal crystalline phase raw material and doped raw material that step 1 is got ready are mixed in nylon ball grinder; With the zirconium ball is that abrading-ball, deionized water are as ball-milling medium; According to material: ball: water=1:5:0.8 weight ratio, ball milling 4 hours, with ball milling material in 100 ℃ of oven dry and cross 40 mesh sieves down.
Step 3: pre-burning.
To dry material pre-burning 5 hours under 1150 ℃ ~ 1200 ℃ temperature condition, obtain the pre-burning material.
Step 4: granulation, moulding.
The pre-burning material is added Z 150PH (PVA) granulation be equivalent to pre-burning material quality 5 ~ 9%, and press down at 20MPa and to process green compact.
Step 5: sintering.
With step 4 gained green compact, sintering is 20 hours under 1340 ℃ ~ 1420 ℃ temperature condition, obtains final BCZN microwave ceramic dielectric material.
The microwave device ceramic medium material of the present invention's preparation has lower loss, moderate specific inductivity and good workability through detecting.Its preparation technology and traditional production process process are basic identical, and it is single to obtain crystalline phase, the microwave device ceramic medium material with lower sintering temperature and higher quality factor that compact structure and processing characteristics are good.It is as shown in Figure 1 with the XRD diffraction approach BCZN principal crystalline phase powder sample have been carried out material phase analysis; With scanning electron microscope sem final microwave device ceramic medium material is observed as shown in Figure 2ly, can be found out that microwave device ceramic medium material surfacing provided by the invention is fine and close, when mixing experiment, the second small phase Ba occurs 5Nb 4O 15
Compared with prior art, the present invention has following characteristics:
1, " the non-stoichiometric research and the doping vario-property research of position atom combine, and obtain the microwave-medium ceramics of excellent performance for B ' position, B;
2, BCN and BZN needn't prepare respectively, have adopted the single synthesis technique, realize the stably manufactured of material easily;
3, not containing volatility or heavy metal substances such as Pb, Cd in the prescription of the present invention, is a kind of environment friendly microwave dielectric ceramic;
4, sintering temperature is minimum can have certain power savings advantages to 1340 ℃;
5, starting material are sufficient, cheap at home, make the cost degradation of high performance microwave communication components and parts material in the modern communication technology become possibility.
Description of drawings
Fig. 1 is a schematic flow sheet of the present invention.
Fig. 2 is the XRD analysis result of BCZN microwave ceramic dielectric material provided by the present invention.
Fig. 3 is the microwave device ceramic medium material scanning electron microscope sem figure that the present invention prepares.
Embodiment
Embodiment 1 ~ 4
The practical implementation step that makes these embodiment microwave-medium ceramics is following:
(1) selects BaCO 3, Co 2O 3, ZnO, Nb 2O 5, Al 2O 3And Ta 2O 5Be raw material, the mol ratio between control Ba, Co, Zn and the Nb is Ba:Co:Zn:Nb=3: (0.6-0.041): (0.4-0.048): (2+0.012), and Al 2O 3And Ta 2O 5Total doping ratio be respectively Ba (Co 1/3Nb 2/3) O 3-Ba (Zn 1/3Nb 2/3) O 3Principal crystalline phase and Ba 5Nb 4O 15Secondary crystalline phase quality summation 0.125%, 0.250t, 0.500%, 1.000%.Al wherein 2O 3Doping ratio be respectively Ba (Co 1/3Nb 2/3) O 3-Ba (Zn 1/3Nb 2/3) O 3Principal crystalline phase and Ba 5Nb 4O 150.034%, 0.068%, 0.136%, 0.272% of secondary crystalline phase quality summation; Ta 2O 5Doping ratio be respectively Ba (Co 1/3Nb 2/3) O 3-Ba (Zn 1/3Nb 2/3) O 3Principal crystalline phase and Ba 5Nb 4O 150.091%, 0.182%, 0.364%, 0.728% of secondary crystalline phase quality summation.Concrete prescription is seen table 1;
Table 1 embodiment 1 ~ 4 concrete one-tenth is grouped into
Figure BDA00001902162600041
(2) in each starting material of the accurate weighing of ratio in the table 1, ball milling 4 hours.Material after the oven dry was crossed behind 40 mesh sieves under 1150 ℃ of temperature condition pre-burning 5 hours, obtained the pre-burning material.Add PVA solution and carry out granulation, dry-pressing formed under 20MPa pressure, base substrate 1340 ℃ of following sintering 20 hours, is made microwave-medium ceramics;
(3) according to Hakki-Coleman dielectric resonance method, with the dielectric properties under network analyzer (Agilent Technologies E5071C) the specimen high frequency.Frequency-temperature coefficient is by formula
Figure BDA00001902162600042
Calculate gained, wherein t 1=25 ℃, t 2=80 ℃, f T1And f T2It is resonant frequency at these two temperature spots.Test result is as shown in table 2.
Table 2 embodiment 1 ~ 4 microwave dielectric property
Figure BDA00001902162600051
Embodiment 5 ~ 9
These embodiment discuss B " non-stoichiometric of position Nb atom, and doped with Al simultaneously 2O 3And Ta 2O 5Improve grain morphology and microwave property, the practical implementation step that makes these embodiment microwave-medium ceramics is following:
(1) selects BaCO 3, Co 2O 3, ZnO, Nb 2O 5, Al 2O 3And Ta 2O 5Be raw material, the mol ratio between control Ba, Co, Zn and the Nb is Ba:Co:Zn:Nb=3: (0.6-0.041): (0.4-0.048): (2+z), and wherein-0.024≤z≤0.006, Al 2O 3And Ta 2O 5Doping be respectively Ba (Co 1/3Nb 2/3) O 3-Ba (Zn 1/3Nb 2/3) O 3Principal crystalline phase and Ba 5Nb 4O 150.068%, 0.182% of secondary crystalline phase quality summation, concrete prescription is seen table 3;
Table 3 embodiment 5 ~ 9 concrete one-tenth are grouped into
(2) in each starting material of the accurate weighing of ratio in the table 3, ball milling 4 hours.Material after the oven dry was crossed behind 40 mesh sieves under 1150 ℃ of temperature condition pre-burning 5 hours, obtained the pre-burning material.Add PVA solution and carry out granulation, dry-pressing formed under 20MPa pressure, base substrate 1340 ℃ of following sintering 20 hours, is made microwave-medium ceramics;
(3) according to Hakki – Coleman dielectric resonance method, with the dielectric properties under network analyzer (Agilent Technologies E5071C) the specimen high frequency.Frequency-temperature coefficient is by formula Calculate gained, wherein t 1=25 ℃, t 2=80 ℃, f T1And f T2It is resonant frequency at these two temperature spots.Test result is as shown in table 4.
Table 4 embodiment 5 ~ 9 microwave dielectric properties
Figure BDA00001902162600062
Embodiment 10 ~ 11
The practical implementation step that makes these embodiment microwave-medium ceramics is following:
(1) selects BaCO 3, Co 2O 3, ZnO, Nb 2O 5 doRaw material, the mol ratio between control Ba, Co, Zn and the Nb is Ba:Co:Zn:Nb=3:0.6:0.4:2, simultaneously doped with Al 2O 3And Ta 2O 5, doping is respectively Ba (Co 1/3Nb 2/3) O 3-Ba (Zn 1/3Nb 2/3) O 3Principal crystalline phase and Ba 5Nb 4O 150.068%, 0.182% of secondary crystalline phase quality summation, and doping Ba (Co 1/3Nb 2/3) O 3-Ba (Zn 1/3Nb 2/3) O 3Principal crystalline phase and Ba 5Nb 4O 150.40% CeO of secondary crystalline phase quality summation 2Perhaps 0.46%Y 2O 3, concrete prescription sees table 5 for details;
(2) in each starting material of the accurate weighing of ratio in the table 5, ball milling 4 hours.Material after the oven dry was crossed behind 40 mesh sieves under 1200 ℃ of temperature condition pre-burning 5 hours, obtained the pre-burning material.Add PVA solution and carry out granulation, dry-pressing formed under 20MPa pressure, base substrate 1420 ℃ of following sintering 20 hours, is made microwave-medium ceramics; Test performance is as shown in table 6.
The present invention is not limited to above-mentioned 11 specific embodiments; Can find out that through above embodiment embodiment 2,9; 10 have all obtained excellent microwave property; Through carrying out the B ' position and the B of BZCN system simultaneously " position atom non-stoichiometric, the adjustment of doping vario-property two aspects, and suitably adjust preparation technology and parameter, thus the microwave-medium ceramics that obtains new excellent performance is feasible fully.
Table 5 embodiment 10 ~ 11 concrete one-tenth are grouped into
Figure BDA00001902162600071
Table 6 embodiment 10 ~ 11 microwave dielectric properties

Claims (6)

1. a BCZN microwave ceramic dielectric material comprises crystal phase structure and doping agent; Principal crystalline phase is Ba (Co in the said crystal phase structure 1/3Nb 2/3) O 3-Ba (Zn 1/3Nb 2/3) O 3, with the secondary crystalline phase Ba of trace 5Nb 4O 15Said doping agent comprises 0.1% ~ 1.50% the Al that is equivalent to crystal phase structure quality summation 2O 3And Ta 2O 5
2. BCZN microwave ceramic dielectric material according to claim 1 is characterized in that, said Al 2O 3Doping be equivalent to 0.03% ~ 0.5% of crystal phase structure quality summation; Said Ta 2O 5Doping be to be equivalent to 0.07% ~ 1.0% of crystal phase structure quality summation.
3. BCZN microwave ceramic dielectric material according to claim 1 is characterized in that, said doping agent also comprises 0.0% ~ 0.5% the CeO that is equivalent to crystal phase structure quality summation 2Or Y 2O 3
4. the preparation method of a BCZN microwave ceramic dielectric material may further comprise the steps:
Step 1: get the raw materials ready;
Select BaCO 3, Co 2O 3, ZnO, Nb 2O 5Be synthetic Ba (Co 1/3Nb 2/3) O 3-Ba (Zn 1/3Nb 2/3) O 3The raw material of principal crystalline phase, the mol ratio between control Ba, Co, Zn and the Nb is Ba:Co:Zn:Nb=3: (0.6+x): (0.4+y): (2+z), wherein-0.041≤x≤0 ,-0.048≤y≤0 ,-0.024≤z≤0.012; Select Al 2O 3And Ta 2O 5As doped raw material and above-mentioned four kinds of raw materials mix batching, Al 2O 3And Ta 2O 5The quality of doped raw material and be Ba (Co 1/3Nb 2/3) O 3-Ba (Zn 1/3Nb 2/3) O 3Principal crystalline phase and Ba 5Nb 4O 150.1% ~ 1.50% of secondary crystalline phase quality summation;
Step 2: ball milling;
Principal crystalline phase raw material and doped raw material that step 1 is got ready are mixed in nylon ball grinder; With the zirconium ball is that abrading-ball, deionized water are as ball-milling medium; According to material: ball: water=1:5:0.8 weight ratio, ball milling 4 hours, with ball milling material in 100 ℃ of oven dry and cross 40 mesh sieves down;
Step 3: pre-burning;
To dry material pre-burning 5 hours under 1150 ℃ ~ 1200 ℃ temperature condition, obtain the pre-burning material;
Step 4: granulation, moulding.
The pre-burning material is added the Z 150PH granulation be equivalent to pre-burning material quality 5% ~ 9%, and press down at 20MPa and to process green compact;
Step 5: sintering;
With step 4 gained green compact, sintering is 20 hours under 1340 ℃～1420 ℃ temperature condition, obtains final BCZN microwave ceramic dielectric material.
5. the preparation method of BCZN microwave ceramic dielectric material according to claim 4 is characterized in that, in the material that mixes: said Al 2O 3Doping for being equivalent to Ba (Co 1/3Nb 2/3) O 3-Ba (Zn 1/3Nb 2/3) O 3Principal crystalline phase and Ba 5Nb 4O 150.03% ~ 0.5% of secondary crystalline phase quality summation; Said Ta 2O 5Doping for being equivalent to Ba (Co 1/3Nb 2/3) O 3-Ba (Zn 1/3Nb 2/3) O 3Principal crystalline phase and Ba 5Nb 4O 150.07% ~ 1.0% of secondary crystalline phase quality summation.
6. according to the preparation method of claim 4 or 5 described BCZN microwave ceramic dielectric materials, it is characterized in that doped raw material contains simultaneously and is equivalent to Ba (Co 1/3Nb 2/3) O 3-Ba (Zn 1/3Nb 2/3) O 3Principal crystalline phase and Ba 5Nb 4O 150.0% ~ 0.5% CeO of secondary crystalline phase quality summation 2Or Y 2O 3
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CN110183228A (en) * 2019-06-06 2019-08-30 桂林理工大学 A kind of positive and negative adjustable two-phase composite microwave medium ceramic material of temperature coefficient of resonance frequency and preparation method thereof
CN114349504A (en) * 2022-01-07 2022-04-15 湖南省美程陶瓷科技有限公司 Doped perovskite relay electronic ceramic material and preparation method thereof

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CN102992762A (en) * 2012-11-16 2013-03-27 武汉凡谷电子技术股份有限公司 Barium-cobalt-zinc-niobium based microwave dielectric ceramics and preparation method thereof
CN107586131A (en) * 2017-09-06 2018-01-16 天津大学 A kind of near-zero resonance frequency temperature coefficient microwave-medium ceramics and preparation method thereof
CN110183228A (en) * 2019-06-06 2019-08-30 桂林理工大学 A kind of positive and negative adjustable two-phase composite microwave medium ceramic material of temperature coefficient of resonance frequency and preparation method thereof
CN114349504A (en) * 2022-01-07 2022-04-15 湖南省美程陶瓷科技有限公司 Doped perovskite relay electronic ceramic material and preparation method thereof
CN114349504B (en) * 2022-01-07 2022-12-23 湖南省美程陶瓷科技有限公司 Doped perovskite relay electronic ceramic material and preparation method thereof

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