CN1792998A - Low-loss high frequency medium ceramic and preparation process thereof - Google Patents

Low-loss high frequency medium ceramic and preparation process thereof Download PDF

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Publication number
CN1792998A
CN1792998A CN 200510016200 CN200510016200A CN1792998A CN 1792998 A CN1792998 A CN 1792998A CN 200510016200 CN200510016200 CN 200510016200 CN 200510016200 A CN200510016200 A CN 200510016200A CN 1792998 A CN1792998 A CN 1792998A
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low
ceramic
frequency medium
preparation
loss high
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CN100378026C (en
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李玲霞
孙晓东
明翠
王大鹏
王洪儒
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Tianjin University
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Tianjin University
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Abstract

The invention discloses a low consumption high frequency medium ceramics and the manufacturing method. The mol percentage of the material is Ag<SUB>2</SUB>O 40-50%, Nb<SUB>2</SUB>O<SUB>5</SUB> 10-40%, Ta<SUB>2</SUB>O<SUB>5</SUB> 10-40%, and the weight percentage of MnO<SUB>2</SUB> 1-3%. It adopts pre-compounding precursor method. The invention is the critical material to make high frequency medium components.

Description

Low-loss high-frequency medium ceramic and prepare method
Technical field
The invention relates to the composition is ceramic composition of feature and preparation method thereof, or rather, is about low-loss high-frequency medium ceramic and preparation method thereof.
Background technology
In modern communication, the high-frequency dielectric components and parts are one of key elements that influence communication quality, and the high-frequency dielectric porcelain is the critical material of preparation high frequency dielectric device.Therefore the preparation of high frequency material plays a part very important to the development of communications industry.As everyone knows, the preparation of material and performance thereof are very responsive to technology.Same material gets with different prepared, and its performance may greatly differ from each other.Therefore reasonably preparation technology is extremely important to the dielectric properties that improve dielectric material.
For the high-frequency dielectric material, preparation technology is very complicated, different systems, different purposes, and processing requirement also has very big difference.Rationally good technology can further improve the performance of dielectric material.For the high-frequency dielectric ceramic system, its good high frequency characteristics is the basis that the high frequency components and parts are made.
Ag (Nb yTa 1-y) O 3(being abbreviated as ANT) system is a kind of novel high-frequency dielectric system, and relevant research is quite few, the ε height (ε＞400) that has in ANT system in the last few years just, tg δ＜18 * 10 -4Characteristic caused people's attention gradually.With some researchers headed by A.Kania etc. the ANT system some preliminary study have been carried out.But its dielectric properties are unsatisfactory, when loss tg δ＜10 * 10 -4The time, the temperature coefficient of capacitance of system is bigger negative value α ε=-500～-100ppm/ ℃.
People such as A.Kania and G.E.Kugal respectively at 1986 and 1987 to AgNbO 3And AgTaO 3System furthers investigate.The ANT medium ceramic material has two kinds of preparation methods: first method is with Ag 2O, Nb 2O 5And Ta 2O 5According to testing the proportioning uniform mixing and under specified temp, carrying out the synthetic ANT system of solid state reaction.Second method is earlier with Nb 2O 5And Ta 2O 5Be pre-mixed evenly according to the experiment proportioning, prepare presoma 1200 ℃ of left and right sides pre-burnings.And then with Ag 2O adds the presoma uniform mixing in proportion, is fired into the ANT media ceramic at last." adjustable microwave medium A g (Ta, Nb) O that people such as F.Zimmermann delivered at Journal ofEuropean Ceramic Society in 2004 3Research " in mention Ag (Nb, Ta) O of its preparation 3The specific inductivity of system is 310, and temperature factor is adjustable.
The ANT system is easy to decompose in sintering process, influences the electrical property of system, with Nb in the system 5+/ Ta 5+=1 is example, and the decomposition reaction of system is:
This decomposition will cause the rapid increase of system loss, and therefore restraining this decomposition is the key that this porcelain system of preparation reduces the wastage.
Summary of the invention
The objective of the invention is to overcome deficiency of the prior art, a kind of low-loss high-frequency medium ceramic and preparation method thereof is provided.
The present invention is achieved by the following technical programs.
Low-loss high-frequency medium ceramic of the present invention, its raw material and molar percentage are Ag 2O 40-50%, Nb 2O 510-40%, Ta 2O 510-40%; Add MnO 2Weight percent is 1-3%.
The preparation method of low-loss high-frequency medium ceramic of the present invention, concrete steps are as follows:
1. with Nb 2O 5, Ta 2O 510-40% and 10-40% batching in molar ratio respectively, materials: deionized water: the ratio of abrading-ball=1: 1: 1.5 adds ball grinder, ball milling 4-6h; After the discharging in 110 ℃ of oven dry; Be fired into frit in 1000-1200 ℃;
2. adding mol ratio in frit is the Ag of 40-50% 20, materials: deionized water: the ratio of abrading-ball=1: 1: 1.5 adds ball grinder, ball milling 6-12h; Make ceramic powder in 800-900 ℃ of oven dry again;
3. adding weight percent in ceramic powder is the MnO of 1-3% 2, 4-6h is in 110 ℃ of oven dry.
4. the paraffin that adds weight percent and be 7-9% is pressed into Ф 10mm as the tamanori granulation, and thickness is the disc green compact of 1-1.5mm, be warming up to 550 ℃ through 3.5h and carry out de-waxing, be warming up to 1050 ℃ of-1150 ℃ of calcinings through 2h again, insulation 4-8h makes ceramic sample;
5. gained sample upper and lower surface is applied the silver slurry, prepare electrode through 800 ℃ of-840 ℃ of burning infiltrations;
6. make high-frequency dielectric ceramic behind welding lead, the test analysis.
The 1. synthetic in advance precursor of described step is (Nb xTa 1-x) 2O 5, X=0.2-0.8 wherein.
Described step mixture 2. reacts under oxidizing atmosphere and generates Ag (Nb xTa 1-x) O 3, X=0.2-0.8 wherein.
Described step calcining temperature 4. is 1050 ℃.
The invention has the beneficial effects as follows provides a kind of constant low-loss high frequency medium ceramic, and has improved the dielectric properties of system, and a kind of method that adopts the precursor legal system to be equipped with low-loss high-frequency medium ceramic is provided simultaneously.
Embodiment
Below in conjunction with embodiment the present invention is further described, but is not limited to embodiment.The present invention is with analytical pure Nb 2O 5, Ta 2O 5Be raw material, adopt pre-synthetic precursor method, prepare (Nb earlier xTa 1-x) 2O 5, wherein X=0.2-0.8 adds a certain proportion of analytical pure Ag again in precursor 2O allows mixture react under oxidizing atmosphere and generates Ag (Nb xTa 1-x) O 3, wherein X=0.2-0.8 adds MnO more by a certain percentage 2
In the solid state reaction, a small amount of non-reactant of adding or may be present in impurities in raw materials regular meeting reaction is produced some special effects.These materials are exactly so-called mineralizer.They in reaction not with reactant or resultant react with, but affect some link of reaction in a different manner with program.Mechanism about mineralizer is complicated various, can be different fully because of the difference of reaction system.But can think that mineralizer is to participate in some way in the solid state reaction process to go.Mineralizer role in reaction process roughly can be divided into: the generating rate that 1. influences nucleus.2. influence crystallization rate and lattice mechanism.3. reduce the system eutectic point, improve property of liquid phase.In this experiment in order to improve the sintering character of system, through experimental selection MnO 2Be mineralizer, in order to improve the performance of system.Specific embodiment is as follows.
Embodiment 1:
Take by weighing 12g Nb 2O 5, 12g Ta 2O 5, mixing and ball milling 4h, 110 ℃ of oven dry are fired into frit in 1200 ℃ again in loft drier.Take by weighing 16g Ag 2O adds in the above-mentioned frit, ball milling 6h, and the oven dry back makes powder in 800 ℃.In above-mentioned powder, add 0.4g MnO again 2, mixing and ball milling 4h, oven dry.Add 7% paraffin again, granulation, being pressed into diameter is that 10mm, thickness are the circular green compact of 1mm.In the high temperature resistance case, rise to 550 ℃ and carry out de-waxing, be warming up to 1150 ℃ through 2h again, insulation 4h through 3.5h.Gained sample upper and lower surface is applied the silver slurry, prepare electrode through 800 ℃ of burning infiltrations; Make high-frequency dielectric ceramic behind welding lead, the test analysis.
Embodiment 2:
Take by weighing 12g Nb 2O 5, 12g Ta 2O 5Mixing and ball milling 4h, 110 ℃ of oven dry are fired into frit in 1100 ℃ again in loft drier.Take by weighing 16g Ag 2O adds in the above-mentioned frit, and ball milling 8h oven dry back makes powder in 850 ℃.In above-mentioned powder, add 0.8g MnO again 2, mixing and ball milling 4h, oven dry.Add 7% paraffin, granulation, being pressed into diameter is that 10mm, thickness are the circular green compact of 1mm.In the high temperature resistance case, rise to 550 ℃ and carry out de-waxing, be warming up to 1130 ℃ through 2h again, insulation 4h through 3.5h.Gained sample upper and lower surface is applied the silver slurry, prepare electrode through 820 ℃ of burning infiltrations; Make high-frequency dielectric ceramic behind welding lead, the test analysis.
Embodiment 3:
Take by weighing 10g Nb 2O 5, 16g Ta 2O 5, mixing and ball milling 5h, 110 ℃ of oven dry are fired into frit in 1000 ℃ again in loft drier.Take by weighing 14g Ag 2O adds in the above-mentioned frit, and ball milling 10h oven dry back makes powder in 900 ℃.In above-mentioned powder, add 1g MnO again 2, mixing and ball milling 5h, oven dry.Add 8% paraffin, granulation, being pressed into diameter is that 10mm, thickness are the circular green compact of 1.5mm, rises to 550 ℃ through 3.5h and carry out de-waxing in the high temperature resistance case, is warming up to 1100 ℃ through 2h again, insulation 6h.Gained sample upper and lower surface is applied the silver slurry, prepare electrode through 800 ℃ of burning infiltrations; Make high-frequency dielectric ceramic behind welding lead, the test analysis.
Embodiment 4:
Take by weighing 10g Nb 2O 5, 16g Ta 2O 5, mixing and ball milling 6h, 110 ℃ of oven dry are fired into frit in 1000 ℃ again in loft drier.Take by weighing 14g Ag 2O adds in the above-mentioned frit, and ball milling 12h oven dry back makes powder in 900 ℃.In above-mentioned powder, add 1.2g MnO again 2, mixing and ball milling 6h, oven dry.Add 9% paraffin, granulation, being pressed into diameter is that 10mm, thickness are the circular green compact of 1mm, rises to 550 ℃ through 3.5h and carry out de-waxing in the high temperature resistance case, is warming up to 1050 ℃ through 2h again, insulation 8h.Gained sample upper and lower surface is applied the silver slurry, prepare electrode through 840 ℃ of burning infiltrations; Make high-frequency dielectric ceramic behind welding lead, the test analysis.
Detection method of the present invention is as follows:
One, the detection of the specific inductivity of disc medium
Utilize the electrical capacity C of HP4278A electric capacity instrument measure sample, according to the specific inductivity of formula (2-1) calculation sample.
&epsiv; = 14.4 &times; C &times; d D 2 - - - ( 2 - 1 )
Wherein: C is the electrical capacity of sample, and unit is pF.
D is the diameter of sample, and unit is cm.
D is the thickness of sample, and unit is cm.
Two, the calculating of the test of sample temperature characteristic and temperature factor
Utilize WAYNE KEER Multi Bridge 6425 testing tools and the high cold cycle incubator of GZ-ESPEC MC-710P to cooperatively interact, measure the electrical capacity of sample under the differing temps, finish the test of sample temperature characteristic.The temperature coefficient of capacity of material calculates according to following formula:
&alpha; c = 1 C 0 &CenterDot; C 1 - C 0 T 1 - T 0 &times; 10 6 (ppm/℃) (2-2)
Wherein: T 0-room temperature (25 ℃)
T 1-probe temperature (85 ℃)
C 0-sample is at T 0The time electrical capacity (PF)
C 1-sample is T in temperature 1The time electrical capacity (PF)
Three, the calculating of the measurement of sample insulation resistance and material bodies resistivity
Utilize the insulation resistance of ZC36 type ultra-high resistance tester measure sample, utilize following formula to calculate the body resistivity ρ of material v:
&rho; v = R i &times; &pi; &times; D 2 4 d ( &Omega; &CenterDot; cm ) - - - ( 2 - 3 )
Wherein: R iThe insulation resistance of-sample (Ω)
The diameter of D-sample (cm)
D-sample thickness (cm)
Four, the measurement of sample dielectric loss
Utilize the dielectric loss tg δ (1MHz) of HP4278A electric capacity instrument measure sample.
The detected result of the embodiment of the invention and the reduced parameter of prior art see table 1 for details.
Table 1
Numbering Loss tangent tg δ (* 10 -4) (1MHz) DIELECTRIC CONSTANT (1MHz) Temperature coefficient of capacitance α c(ppm/℃) Insulation resistivity ρ v(Ω·cm)
Embodiment 1 6.6 430 89 ＞10 12
Embodiment 2 6.0 455 25 ＞10 12
Embodiment 3 6.6 420 -21 ＞10 12
Embodiment 4 7.0 412 -80.3 ＞10 12
Prior art 18 300-400 -500-300 ＞10 11
The present invention is described by preferred embodiment, and person skilled obviously can realize the present invention to the suitably change and combination of the techniques described herein scheme under the situation that does not break away from content of the present invention, spirit and scope.The replacement that all are similar and change apparent to those skilled in the artly, they are regarded as being included among spirit of the present invention, scope and the content.

Claims (5)

1. a low-loss high-frequency medium ceramic is characterized in that, its raw material and molar percentage are Ag 2O 40-50%, Nb 2O 510-40%, Ta 2O 510-40%; Add MnO 2Weight percent is 1-3%.
2. the preparation method of the low-loss high-frequency medium ceramic of claim 1 is characterized in that, it is as follows to have step:
1. with Nb 2O 5, Ta 2O 510-40% and 10-40% batching in molar ratio respectively, materials: deionized water: the ratio of abrading-ball=1: 1: 1.5 adds ball grinder, ball milling 4-6h; After the discharging in 110 ℃ of oven dry; Be fired into frit in 1000-1200 ℃ again;
2. adding mol ratio in frit is the Ag of 40-50% 2O, materials: deionized water: the ratio of abrading-ball=1: 1: 1.5 adds ball grinder, ball milling 6-12h; Make ceramic powder in 800-900 ℃ of oven dry again;
3. adding weight percent in ceramic powder is the MnO of 1-3% 2, ball milling 4-6h is in 110 ℃ of oven dry.
4. the paraffin that adds weight percent and be 7-9% is pressed into Φ 10mm as the tamanori granulation, and thickness is the disc green compact of 1-1.5mm, be warming up to 550 ℃ through 3.5h and carry out de-waxing, be warming up to 1050 ℃ of-1150 ℃ of calcinings through 2h again, insulation 4-8h makes ceramic sample;
5. gained sample upper and lower surface is applied the silver slurry, prepare electrode through 800 ℃ of-840 ℃ of burning infiltrations;
6. make high-frequency dielectric ceramic behind welding lead, the test analysis.
3. the preparation method of low-loss high-frequency medium ceramic according to claim 2 is characterized in that, the 1. synthetic in advance precursor of described step is (Nb xTa 1-x) 2O 5, X=0.2-0.8 wherein.
4. the preparation method of low-loss high-frequency medium ceramic according to claim 2 is characterized in that, described step mixture 2. reacts under oxidizing atmosphere and generates Ag (Nb xTa 1-x) O 3, X=0.2-0.8 wherein.
5. the preparation method of low-loss high-frequency medium ceramic according to claim 2 is characterized in that, described step calcining temperature 4. is 1050 ℃.
CNB2005100162007A 2005-11-21 2005-11-21 Low-loss high frequency medium ceramic and preparation process thereof Expired - Fee Related CN100378026C (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100456393C (en) * 2006-12-04 2009-01-28 天津大学 High-dielectric constant microwave dielectric ceramic and producing method thereof
CN101343179B (en) * 2008-08-15 2011-03-23 天津大学 Low-loss high-frequency medium ceramic and preparation thereof
CN101265096B (en) * 2008-04-25 2011-03-23 天津大学 High frequency medium ceramic with ultrahigh dielectric constant

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2727693B2 (en) * 1989-10-20 1998-03-11 松下電器産業株式会社 Voltage-dependent nonlinear resistor porcelain composition and method for manufacturing varistor
CN1143836C (en) * 2001-01-22 2004-03-31 兰招武 High-frequency high-permittivity microwave medium ceramics and its production method
KR100455218B1 (en) * 2001-12-27 2004-11-06 주식회사 에스세라 Piezoelectric ceramic composition and piezoelectric device using the same
CN1193377C (en) * 2003-06-16 2005-03-16 浙江大学 Microwave medium ceramics with high dielectric constant

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100456393C (en) * 2006-12-04 2009-01-28 天津大学 High-dielectric constant microwave dielectric ceramic and producing method thereof
CN101265096B (en) * 2008-04-25 2011-03-23 天津大学 High frequency medium ceramic with ultrahigh dielectric constant
CN101343179B (en) * 2008-08-15 2011-03-23 天津大学 Low-loss high-frequency medium ceramic and preparation thereof

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