CN100345795C - Coke green stone high frequency/microwave medium ceramic sintered by low temp. and preparation process thereof - Google Patents

Coke green stone high frequency/microwave medium ceramic sintered by low temp. and preparation process thereof Download PDF

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CN100345795C
CN100345795C CNB2005100963363A CN200510096336A CN100345795C CN 100345795 C CN100345795 C CN 100345795C CN B2005100963363 A CNB2005100963363 A CN B2005100963363A CN 200510096336 A CN200510096336 A CN 200510096336A CN 100345795 C CN100345795 C CN 100345795C
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high frequency
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CN1792999A (en
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汪宏
张美玲
姚熹
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Xian Jiaotong University
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Xian Jiaotong University
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Abstract

The present invention discloses coke green stone high frequency/microwave medium ceramic sintered by low temperature. On the basis of bismuthino high frequency medium ceramic, from the material science aspect, proper amount of ion is used for replacing bismuthino high frequency medium ceramic so as to form dielectric ceramic composite materials with the coke green stone used as main crystal phase. The expression of the microwave dielectric ceramic material sintered by low temperature is (Bi<3x>M<2-3x>)(Zn<x>Nb<2-x>)O<7>, wherein M is Zn<2+>, Ca<2+>, or Cd<2+> or Sr<2+>; x is equal or greater than 0.5 and is equal or lesser than 0.64. The low-loss high dielectric high frequency/microwave medium ceramic sintered by low temperature of the present invention has the characteristics of high dielectric constant (epsilon=70 to 150), small medium loss (tandelta<6x10<-4>), wide temperature coefficient coverage area of dielectric constant (alpha<epsilon>=-300 ppm/DEGC-+60 ppm/DEGC), low sintering temperature (900 DEG C to 1020 DEG C), large insulation resistance (rhov>=10<13>omega. cm), favorable microwave performance (Qf=1000 to 6000), low frequency temperature coefficient (tauf=-50-80) and simple technology; the temperature coefficient of dielectric constant can be regulated within the range of-55 to 125 DEG C according to the raw materials.

Description

A kind of low-temperature sintering coke green stone high frequency/microwave medium ceramic and preparation thereof
Technical field
The invention belongs to electronic ceramics and manufacturing field thereof, relate to a kind of low-temperature sintering coke green stone high frequency/microwave medium ceramic material and preparation thereof, and this material application on microwave devices such as ceramic antenna.
Background technology
Aspect mobile communication, its development one improves the carrier information capacity towards more high frequency band expansion, another side has also proposed portable requirement to facility communication system, and it is integrated that machine system moves towards, in the hope of obtaining small volume, light weight, high reliability, product cheaply.In the integrated process of microwave circuit, the appearance of metal wave-guide and microwave tube makes microwave circuit obtain to a certain degree integrated and miniaturization, but a used traditionally heavy fat person's metal resonator cavity makes microstrip circuit integratedly becomes a difficulty, with microwave-medium ceramics (microwave dielectric ceramics, MWDC) make resonator an outlet but is provided for this reason, microwave-medium ceramics has high-k (10＜ε r＜90), low-loss (tan δ＜3 * 10-4), the little (10＜τ of frequency-temperature coefficient f＜characteristics such as 10ppm) therefore have been widely used in the making of microwave device.
The microwave dielectric material system of having developed so far is a lot, and several important commercial systems can be summarized as follows:
BaO-TiO 2System: this is that the raw material cost is low, is the microwave-medium system that obtains practice the earliest.Wherein two of Bao Dao microwave property excellence is BaTi mutually 4O 9(BT4, under the 4.5GHz, ε r=38, Q＞13K, τ f=14ppm) and Ba 2Ti 9O 20(B2T9, under the 4.5GHz, ε r=39, Q＞12K, τ f=4ppm), discovered afterwards that this system was all available in whole microwave region by regulating the B2T9/BT4 two-phase proportion.Insufficient is that the BT4 frequency-temperature coefficient is bigger than normal, and B2T9 requires harshness to preparation technology.
BaO-Ln 2O 3-TiO 2System: this is to be the more sufficient individual system of research in the microwave-medium, and wherein Ln is a rare earth element, can be Nd, Sm, La etc.With this is the basis, forms by mixing and changing, and can obtain the different material system of a series of electric properties.
When Ln=Nd, system has excellent temperature stability, and specific inductivity is higher relatively, but complex structure mainly exists ternary phase and binary phase composite, and the Q value is not high yet.By adding PbO, Bi 2O 3Can improve ε greatly rAnd Q, reduce sintering temperature simultaneously.During Ln=Sm, the system specific inductivity descends to some extent, but the Q value raises to some extent, and temperature factor is little in addition, is a kind of excellent material therefore.By a small amount of adding Sr, can linearly promote specific inductivity, the simultaneous temperature coefficient will increase.The system of Ln=La has high DIELECTRIC CONSTANT r＞100, but temperature factor is very big negative value, so research is undertaken by doping, and tc compensation does not destroy its high-k simultaneously and high Q characteristic becomes the research focus.
Ba (B ' 1/3B " 2/3) O 3System: this individual system has complex perovskite structure, has high Q value at high microwave frequency band, therefore is the used main dielectric materials in high frequency field such as satellite communications.Wherein main says, B '=Zn, Mg, B "=Ta, Nb.When B position ion was more or less the same, B position ion was arranged unordered, is cubic; When B position ionic radius and electric charge went far mutually, B position ion was made ordered arrangement, is transformed into orderly tripartite crystal formation.By using Mn, W, Sn, Co displacement B position ion can improve material at the Q of high microwave frequency band value and attemperation coefficient.
(Zr x, Sn 1-x) TiO 4System: this based material specific inductivity hangs down usually＜40, but the Q value is high, is used for microwave frequency band.When the x=0.8 left and right sides, under the 2GHz, ε r=38, Q=15K, frequency-temperature coefficient are 0.The ZST weak point is the sintering temperature height, in the time of the agent of annex solution phase sintering, reduces the Q value easily.
Various microwave devices based on dielectric resonator, be convenient to miniaturization and microwave is integrated, be used widely in practice, but along with mobile communication striding forward to higher frequency, depend merely on the minimizing of tank circuit and can not satisfy the requirement of further microminiaturization of mobile communication terminal and portability, and new outlet has been opened up in passive integrated appearance for this reason.Bi 2O 3-ZnO-Nb 2O 5The base pottery is the not leaded low temperature sintered high frequency capacitor material of a class, and its sintering temperature is low, the specific inductivity height, and temperature factor can be adjusted, and dielectric loss is little, therefore the miniaturization of very suitable chip multilayer element and integrated.But its microwave dielectric property of report is unexcellent.
Summary of the invention
At defective that exists in the above-mentioned background technology or deficiency, the object of the present invention is to provide a kind of high-performance high-frequency of agglomerating at low temperatures/microwave dielectric stupalith.
First purpose of the present invention provides a kind of low-temperature sintering coke green stone high frequency/microwave medium ceramic, the relative permittivity behind this ceramic post sintering between 70～150, low dielectric loss (tan δ＜3 * 10 -4), big insulation resistance (ρ v〉=10 13Ω cm), good microwave property (Qf=1000～6000), low frequency-temperature coefficient (τ f=-50～-80), the adjustable (α of temperature factor ε=-300ppm/ ℃～+ 60ppm/ ℃), except these performances, it can (900 ℃～1020 ℃) carry out sintering under low relatively temperature.Sintering and the dielectric ceramic press cake that forms, the multilayer ceramic base material that forms by this dielectric ceramic press cake, the laminated ceramic electronic components of ceramic electron element with excellent high frequency performance.
Second purpose of the present invention provides the preparation method of above-mentioned low-temperature sintering coke green stone high frequency/microwave medium ceramic.
The present invention is on the basis of bismuthino high-frequency dielectric ceramic, and from the angle of Materials science, what form by an amount of ionic replacement is the dielectric ceramic composite system of principal crystalline phase with Jiao Lvshi.By the existing low-temperature sintering dielectric ceramics Bi of the method improvement of ionic replacement 2O 3-ZnO-Nb 2O 5Material system, widen its sintering range, temperature coefficient of permittivity is changed less than 60ppm/ ℃ in-55 ℃～125 ℃ scope, and further reduce sintering temperature (minimum can sinter porcelain into), make it to adapt to the needs of high-performance and low-cost scale operation at 900 ℃.
To achieve these goals, technical scheme of the present invention is, a kind of low-temperature sintering coke green stone high frequency/microwave medium ceramic is characterized in that, this low temperature sintered high frequency dielectric ceramic material structure expression is: (Bi 3xM 2-3x) (Zn xNb 2-x) O 7, wherein, M is Zn 2+, or Ca 2+, or Cd 2+, or Sr 2+0.56≤x≤0.64.
Realize the preparation method of above-mentioned low-temperature sintering coke green stone high frequency/microwave medium ceramic, this method adopts solid reaction process, it is characterized in that, carries out with processing parameter according to the following steps:
1) with analytical pure raw material Bi 2O 3, ZnO, Nb 2O 5, CaCO 3, CdO, SrCO 3By prescription general formula (Bi 3xM 2-3x) (Zn xNb 2-x) O 7Preparation, wherein, M is Zn 2+, or Ca 2+, or Cd 2+, or Sr 2+0.56≤x≤0.64;
2) the chemical feedstocks thorough mixing after will preparing, and through ball milling levigate after, cross 70～120 mesh sieves;
3) chemical feedstocks after sieving is through 750～850 ℃ of pre-burnings, and insulation 2h～3h, obtains burning piece;
4) will burn piece and pulverize and to reproduce grain after levigate and cross 120 mesh sieves, can obtain required porcelain;
5) porcelain is made finished product as required after, sinter porcelain at 900 ℃～1020 ℃, can obtain that low-temperature sintering is low decreases high Jie's high frequency/microwave medium ceramic.
Low-temperature sintering coke green stone high frequency/microwave medium ceramic of the present invention has following characteristics: specific inductivity height (ε=70～150), little (tan δ＜3 * 10 of dielectric loss -4), the wide (α of temperature coefficient of permittivity coverage ε=-300ppm/ ℃～+ 60ppm/ ℃), sintering temperature low (900 ℃～1020 ℃), the big (ρ of insulation resistance v〉=10 13Ω cm), microwave property good (Qf=1000～6000), the low (τ of frequency-temperature coefficient f=-50～-80), technology is simple.And temperature coefficient of permittivity can be formed adjusting according to material in-55 ℃～125 ℃ scope.
Description of drawings
Fig. 1 is HFSS emulation and the actual resonator ceramic antenna S that records 11Graphic representation.
The present invention is further illustrated below in conjunction with specific embodiment that the contriver provides.
Embodiment
According to technical scheme of the present invention, the structure expression of low-temperature sintering coke green stone high frequency/microwave medium ceramic of the present invention is: (Bi 3xM 2-3x) (Zn xNb 2-x) O 7, wherein, M=Zn 2+, Ca 2+, Cd 2+, Sr 2+0.56≤x≤0.64.
Preparation technology of the present invention is, with chemical feedstocks Bi 2O 3, ZnO, Nb 2O 5, CaCO 3, CdO, SrCO 3, by prescription general formula (Bi 3xM 2-3x) (Zn xNb 2-x) O 7Preparation, wherein M=Zn 2+, Ca 2+, Cd 2+, Sr 2+, 0.56≤x≤0.64; After preparation back thorough mixing ball milling is levigate, cross 70～120 mesh sieves,, and be incubated 2～3 hours and obtain burning piece through 750 ℃～850 ℃ pre-burnings, will burn piece pulverize the back levigate reproduce grain 120 mesh sieves, can obtain required porcelain.After making finished product as required, sinter porcelain into, can obtain the low-temperature sintering coke green stone high frequency/microwave medium ceramic at 900 ℃～1020 ℃.
Low-temperature sintering coke green stone high frequency/microwave medium ceramic of the present invention is owing to comprised Bi 2O 3, ZnO, Nb 2O 5Deng composition, make that this media ceramic matrix material of sintering becomes possibility at low temperatures.
The present invention is relevant with dielectric medium theoretical according to the green stone crystal chemistry of Jiao principle, and the method that adopts ionic replacement is to existing Bi 2O 3-ZnO-Nb 2O 5The base pottery improves.Use positively charged ion Ca 2+, Cd 2+, Sr 2+Part replaces Bi 2O 3-ZnO-Nb 2O 5In Zn 2+, Bi before and after research summary goes out to replace 2O 3-ZnO-Nb 2O 5The rule relation that base ceramic pyrochlore structure and dielectric properties change designs and develops out on this basis that crystalline structure and phase composite are simple, temperature coefficient of permittivity is stablized and the Bi of seriation 2O 3-ZnO-Nb 2O 5Base high-performance low-temperature sintered ceramics material, can be used as laminated ceramic capacitor, direct current with exchange middle and high pressure laminated ceramic capacitor, radio-frequency capacitor, microwave dielectric resonator, LTCC system (LTCC), microwave filter, the dielectric material of micro-wave coupler and ceramic antenna etc. uses.
Be the embodiment that the contriver provides below.
Embodiment 1:
With chemical feedstocks Bi 2O 3, ZnO, Nb 2O 5By filling a prescription: (Bi 3xZn 2-3x) (Zn xNb 2-x) O 7, wherein, x=0.64 after preparation back thorough mixing ball milling is levigate, crosses 70～120 mesh sieves, through 700 ℃～800 ℃ pre-burnings, and is incubated 2～3 hours and obtains burning piece, will burn piece pulverize the back levigate reproduce grain 120 mesh sieves, can obtain required porcelain.After porcelain made finished product as required, sinter porcelain into, can obtain the low-temperature sintering coke green stone high frequency/microwave medium ceramic at 940 ℃～1040 ℃.
The performance of this group stupalith reaches following index:
Temperature coefficient of permittivity α ε=248ppm/ ℃ (1MHz), DIELECTRIC CONSTANT=84 (1MHz), dielectric loss tan δ＜6 * 10 -4(1MHz), insulation resistivity ρ v〉=10 14Ω cm, and the good ε of microwave property=75 (3～5GHz), Qf=1667.
Embodiment 2:
With chemical feedstocks Bi 2O 3, ZnO, Nb 2O 5, CaCO 3By filling a prescription: (Bi 3xCa 2-3x) (Zn xNb 2-x) O 7, wherein, x=0.56 after preparation back thorough mixing ball milling is levigate, crosses 70～120 mesh sieves, through 700 ℃～800 ℃ pre-burnings, and is incubated 2～3 hours and obtains burning piece, will burn piece pulverize the back levigate reproduce grain 120 mesh sieves, can obtain required porcelain.After porcelain made finished product as required, sinter porcelain into, can obtain the low-temperature sintering coke green stone high frequency/microwave medium ceramic at 900 ℃～980 ℃.
The performance of this group stupalith reaches following index:
Temperature coefficient of permittivity α ε=214ppm/ ℃ (1MHz), DIELECTRIC CONSTANT=80 (1MHz), dielectric loss tan δ＜6 * 10 -4(1MHz), insulation resistivity ρ v〉=10 14Ω cm, and the good ε of microwave property=76 (3～5GHz), Qf=5076, frequency-temperature coefficient τ f=-82.
Embodiment 3:
With chemical feedstocks Bi 2O 3, ZnO, Nb 2O 5, CdO is by filling a prescription: (Bi 3xCd 2-3x) (Zn xNb 2-x) O 7, wherein, x=0.64 after preparation back thorough mixing ball milling is levigate, crosses 70～120 mesh sieves, through 700 ℃～800 ℃ pre-burnings, and is incubated 2～3 hours and obtains burning piece, will burn piece pulverize the back levigate reproduce grain 120 mesh sieves, can obtain required porcelain.After porcelain made finished product as required, sinter porcelain into, can obtain the low-temperature sintering coke green stone high frequency/microwave medium ceramic at 940 ℃～1020 ℃.
The performance of this group stupalith reaches following index:
Temperature coefficient of permittivity α ε=336ppm/ ℃ (1MHz), DIELECTRIC CONSTANT=90 (1MHz), dielectric loss tan δ＜6 * 10 -4(1MHz), insulation resistivity ρ v〉=10 12Ω cm, and the good ε of microwave property=76 (3～5GHz), Qf=704, frequency-temperature coefficient τ f=-77.
Embodiment 4:
With chemical feedstocks Bi 2O 3, ZnO, Nb 2O 5, SrCO 3By filling a prescription: (Bi 3xSr 2-3x) (Zn xNb 2-x) O 7, wherein, x=0.64 after preparation back thorough mixing ball milling is levigate, crosses 70～120 mesh sieves, through 700 ℃～800 ℃ pre-burnings, and is incubated 2～3 hours and obtains burning piece, will burn piece pulverize the back levigate reproduce grain 120 mesh sieves, can obtain required porcelain.After porcelain made finished product as required, sinter porcelain into, can obtain the low-temperature sintering coke green stone high frequency/microwave medium ceramic at 880 ℃～920 ℃.
The performance of this group stupalith reaches following index:
Temperature coefficient of permittivity α ε=272ppm/ ℃ (1MHz), DIELECTRIC CONSTANT=88 (1MHz), dielectric loss tan δ＜6 * 10 -4(1MHz), insulation resistivity ρ v〉=10 13Ω cm, and the good ε of microwave property=76 (3～5GHz), Qf=1125, frequency-temperature coefficient τ 1=-65.
Embodiment 5:
Adopt and press embodiment 2 agglomerating low-temperature sintering coke green stone high frequency/microwave medium ceramics, design and made the prototype resonator ceramic antenna, it is of a size of radius a=5.01mm, height h=9.12mm, and Fig. 1 is HFSS emulation and the actual resonator ceramic antenna S that records 11Graphic representation.As can see from Figure 1, be 2.74GHz (curve 1 among the figure) with the resonant frequency of HFSS emulation, the actual resonant frequency that records is 2.91GHz (curve 2 among the figure), both basically identicals, its error is 5.8%.The 10dB impedance bandwidth of antenna is 40MHz (1.37%).
It is pointed out that according to technical scheme of the present invention, the foregoing description can also be enumerated many, do not enumerate one by one at this, prove according to applicant's lot of experiment results,, all can implement the present invention and reach the good technical effect in the given scope of technical scheme of the present invention.

Claims (2)

1. a low-temperature sintering coke green stone high frequency/microwave medium ceramic is characterized in that, the DIELECTRIC CONSTANT of this low temperature sintered high frequency dielectric ceramic material=70～150, dielectric loss tan δ＜3 * 10 -4, temperature coefficient of permittivity α ε=-300ppm/ ℃～+ 60ppm/ ℃, 900 ℃～1020 ℃ of sintering temperatures, insulation resistance ρ v〉=10 13Ω cm, microwave property Qf=1000～6000, frequency-temperature coefficient τ f=-50～-80;
Its structure expression is: (Bi 3xM 2-3x) (Zn xNb 2-x) O 7, wherein, M is Zn 2+, or Ca 2+, or Cd 2+, or Sr 2+0.56≤x≤0.64.
2. realize the preparation method of the low-temperature sintering coke green stone high frequency/microwave medium ceramic of claim 1, this method adopts solid reaction process, it is characterized in that, carries out with processing parameter according to the following steps:
1) with analytical pure raw material Bi 2O 3, ZnO, Nb 2O 5, CaCO 3, CdO, SrCO 3By prescription general formula (Bi 3xM 2-3x) (Zn xNb 2-x) O 7Preparation, wherein, M is Zn 2+, or Ca 2+, or Cd 2+, or Sr 2+0.56≤x≤0.64;
2) the chemical feedstocks thorough mixing after will preparing, and through ball milling levigate after, cross 70 orders～120 mesh sieves;
3) chemical feedstocks after sieving is through 750～850 ℃ of pre-burnings, and insulation 2h～3h, obtains burning piece;
4) will burn piece and pulverize and to reproduce grain after levigate and cross 120 mesh sieves, can obtain required porcelain;
5) porcelain is made finished product as required after, sinter porcelain at 900 ℃～1020 ℃, can obtain that low-temperature sintering is low decreases high Jie's high frequency/microwave medium ceramic.
CNB2005100963363A 2005-11-10 2005-11-10 Coke green stone high frequency/microwave medium ceramic sintered by low temp. and preparation process thereof Expired - Fee Related CN100345795C (en)

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