CN1562867A - High frequency ceramic dielectric material in thermal stability and preparaton method - Google Patents

High frequency ceramic dielectric material in thermal stability and preparaton method Download PDF

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CN1562867A
CN1562867A CN 200410018747 CN200410018747A CN1562867A CN 1562867 A CN1562867 A CN 1562867A CN 200410018747 CN200410018747 CN 200410018747 CN 200410018747 A CN200410018747 A CN 200410018747A CN 1562867 A CN1562867 A CN 1562867A
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minutes
high frequency
warming
ball milling
sintering
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CN1256296C (en
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李玲霞
吴霞宛
陈长庆
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Tianjin University
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Tianjin University
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Abstract

The weight percentage ratio of each compound is (wt%): Ag2O3 40-45, Na2CO3 1.2-6.0, Nb2O5 36-39, Ta2O5 8-14, Bi2O3 1.5-3.5, Sb2O5 1.0-4.0. In this invention. prepn. method of high frequency heat stability ceramics medium material is mesotherm firing technology.

Description

High frequency heat stable ceramic medium material and preparation method thereof
Technical field
The present invention relates to the dielectric substance field, in particular, relate to a kind of high frequency heat stable ceramic medium material and preparation method thereof.
Background technology
Because the 20th century a series of great discovery and the development in Solid State Electronics field promoted the flourish of electronics and information industry.The development course of modern information industry (IT) shows that fully advancing by leaps and bounds of information technology have benefited from the develop rapidly of semiconducter device unicircuit and various new components.
The inoganic solids person in electronics is commonly referred to as " Solid State Electronics ", and the history of its research and application has had more than 100 year.At present, silicon microelectronics and compound semiconductor are its main bodys.Research and application at aspects such as metal, alloy and insulating material are also quite extensive.Wherein the invention of metal-oxide compound-semiconductor field effect transistor (MOS-FET) device is an incident with milestone significance on microelectronics and solid-state electronic techniques history.It is the basic circuit form of present super large-scale integration.Yet the research in inoganic solids field is not idle, the still not enough exploitation of instructing room temperature superconductive of the research of Superconductor Physics above-mentioned aspect, the research of nanometer mesoscopic physics also just begins, energy band engineering also is the research emphasis of Solid State Electronics, and the gate of semiconductor material with wide forbidden band and device is opened.In addition, especially electron ceramic material technical study and exploitation have also obtained great achievement to electronic material.Wherein, the development pole the earth of MLC and high frequency and even microwave-medium ceramics technology has promoted the new component development of Communication Technique.
The traditional ceramics electrical condenser generally adopts thermally-stabilised pottery of I type and II type high-dielectric coefficient pottery as medium.According to the regulation of international standards such as IEC, its test frequency is respectively 1MHz and 1KHz, is called the high and low frequency ceramic capacitor.Capacitor lead wire length at the wiring board plug-in mounting is about 2-3mm, the about 600～1000PF of rated capacitance specification in early days.The use frequency range of electrical condenser is far below natural resonance frequency on the one hand.On the other hand for the range of frequency that is higher than 1MHz, all multifactor influences that the dissipation factor of electrical condenser is subjected to that dielectric polarization, lead-in wire and electrode negative effect and electricity are led etc. and sharply increasing, promptly tg δ raises.The shortcoming of conventional high frequency ceramic capacitor aspect high frequency that Here it is, and make it to be subjected to great limitation in the application of high-frequency band.Along with the rise of SMT technology, the MLC chip develops into chip multilayer ceramic capacitor (MLC) and directly is mounted on printed circuit board (PCB) (PCB), has greatly improved the high frequency characteristics of circuit and functional module.For example colour TV, video recorder tuner are the functional modules of early realizing the complete chip type of element, and the high frequency characteristics of chip capacitor is had higher requirements.After this radio pager, mobile telephone also need the sheet capacitor that uses high frequency performance good.
Along with digitizing, high frequencyization, the active network of electronics also develops towards the direction of miniaturization, multifunction, (Electromagnetic Interference, harm EMI) the more and more electromagnetic environment of ambassador's finite space more worsens electromagnetic interference.Utilizing electrical condenser to suppress electromagnetic interference is the most frequently used, the simplest method.This electric capacity is called shunt capacitance (bypass) device or decoupling capacitor (decoupling) device, it can effectively high frequency noise be switched to " ".Be used in electrical condenser among the EMI at present and can be divided into two types of X7R and COG (NPO).Wherein X7R is used in the low-frequency channel, and in mobile communication because frequency is higher, so that usefulness is COG (NPO), because the impedance of electrical condenser is 1/ (2 π f c), so electrical capacity is big more, anti-high-frequency electromagnetic effects of jamming is just good more.Therefore for to make the continuous miniaturization of complete machine need have the system of ultra-high dielectric coefficient, also can effectively improve the anti-high-frequency electromagnetic interference performance of complete machine simultaneously.
Summary of the invention
The objective of the invention is provides a kind of high frequency heat stable ceramic medium material and preparation method thereof in order to overcome the deficiencies in the prior art.
High frequency heat stable ceramic medium material of the present invention is achieved by following technical proposals, comprises following each component by weight percentage:
Ag 2O 3： 40～45％；
Na 2CO 3： 1.2～6.0％；
Nb 2O 5： 36～39％；
Ta 2O 5： 8～14％
Bi 2O 3： 1.5～3.5％；
Sb 2O 5： 1.0～4.0％。
Each component concentration of the best of high frequency heat stable ceramic medium material of the present invention is:
Ag 2O 3： 39～41％；
Na 2CO 3： 3.5～5.0％；
Nb 2O 5： 37～38％；
Ta 2O 5： 10～12％；
Bi 2O 3： 2.0～3.0％；
Sb 2O 5： 2.0～3.0％。
Can also in described said components, add MnCO by weight percentage as required 3: 1.2～4.5%.
The preparation method of high frequency heat stable ceramic medium material of the present invention comprises the steps:
(1) earlier with Ag 2O38～43%, Nb 2O 536～39%, Ta 2O 58～14%, NaCO 31.2～6.0%, mixed the back ball milling 220～260 minutes,
(2) 800～1100 ℃ of Synthetic 2s 00～240 minute, form frit,
(3) with Bi 2O 31.0 Sb～4.0%, 2O 51.0 MnCO～4.0%, 31.2～4.5%, add in the above-mentioned frit, ball milling 320～380 minutes,
(4) add the tamanori granulation of 6-7wt% then, every takes by weighing 0.45～0.55g and carries out compressing tablet,
(5) carry out sintering at last: its sintering schedule is: be warming up to 550 ℃ through 200～240 minutes, after be warming up to 1050～1160 ℃ through 50～70 minutes again, and be incubated 100～120 minutes.
From Fig. 1, can observe the temperature coefficient of capacity of material system of the present invention and Na +Content there is no tangible relation.Temperature coefficient of capacity is more satisfactory when y=0.2, i.e. α cWithin 0 ± 30ppm/ ℃ scope.
As can be seen from Figure 2, when x＜0.1 along with Na +The increase of content, the loss of ANNT system descends gradually, reaches minimum value when x=0.1.The specific inductivity of ANNT system is along with Na when x＞0.1 +The increase of content increases on the contrary.
Send out in the material system insulation resistivity ρ in the present invention vVariation also with Na +Content relevant.Work as Na +Content hour, ρ vGenerally all greater than i0 12Ω cm is with Na +Content there is no very significantly relation.But work as Na +When content is higher, ρ vObviously descend.The insulation resistivity ρ of system when x＞0.3 v＜10 9Ω cm.This is because in the ANNT system, its sintering temperature is along with Na +The increase of content and increasing, and, when sintering temperature is too high, can cause the decomposition aggravation of ANNT system as the research of front, can form many holes on the surface of system, there is silver-colored simple substance separating out simultaneously.This macroscopic defective in surface will inevitably cause reducing of system insulating resistance rate, and loss simultaneously also increases accordingly.Therefore, for the insulation resistivity that makes the ANNT system reaches requirement, Na +Content unsuitable too many, must be less than 0.1mol or between 0.01mol～0.1mol.
In the native system, Nb/Ta ratio is fairly obvious with the variation of temperature influence to the electrical capacity of ANT system, along with Nb 5+The increase of content, the temperature coefficient of capacitance of ANT system moves to positive dirction, these characteristics help us and research and develop thermostability media ceramic system, promptly, the temperature coefficient of capacitance of ANT system can be adjusted near 0ppm/ ℃, when Nb/Ta=2.5～6.5 by suitably regulating the Nb/Ta ratio, the loss of system is less, specific inductivity reaches 512, and the temperature coefficient of capacitance of system is in 0 ± 30ppm/ ℃ of scope, dielectric loss tg δ＜5 * 10 -4(1MHz), thus obtained NPO high frequency heat stable type system.
Bi 2O 3Compound through being usually used in preparing radio ceramics, as Bi 4Ti 3O 12It is a kind of ferroelectric material with laminated perovskite structure.Its room temperature dielectric constant is 110, temperature coefficient of capacitance is+and 650ppm/ ℃.BiNbO 4As microwave-medium ceramics good character is arranged also.Its specific inductivity is 49-52 (100MHz), and temperature coefficient of capacitance is about 0 ± 6ppm/ ℃.In addition, because Bi 2O 3Fusing point very low, can reduce the sintering temperature of ceramic system, improve the sintering character of system.
In native system, because there is relaxation polarization in B position ion, thereby the dielectric properties of system under high frequency are produced certain influence, show as the ANT system loss and increase.And loss is one of key index of measurement system quality in frequency applications.An amount of Bi 2O 3, Sb 2O 5Doping can effectively reduce the dielectric loss of ANT system, does not influence other dielectric characteristics simultaneously.
As seen by above-mentioned, superelevation Jie's heat stable dielectric material of new generation of the present invention not only has higher dielectric constant (specific inductivity is greater than 500), and has reduced sintering temperature effectively, can be in mesophilic range sintering.Also can reduce the cost of electrical condenser during with material preparation laminated ceramic capacitor of the present invention greatly.
Description of drawings
Fig. 1 is Na +The relation of content and power system capacity temperature factor,
Fig. 2 is Na +Content to the influence of system loss of the present invention.
Embodiment
Below in conjunction with embodiment the present invention is described further.
Embodiment 1:
Earlier with Ag 2O:42g, Nb 2O 5: 39g, Ta 2O 5: 14g, NaCO 3: 2.5g, mixed the back ball milling 220 minutes, 800 ℃ of Synthetic 2s 00 minute, form frit, with Bi 2O 3: 1.5g, Sb 2O 5: 1g, MnCO 3: 1.2g, add in the above-mentioned frit, ball milling 320 minutes, the powder after the ball milling oven dry is a khaki color.The paraffin granulation that adds 6g then, every takes by weighing the pressure of 0.45g when compressing tablet is 6Mpa, and the diameter 10mm of compressing tablet carries out compressing tablet, and carry out sintering at last: its sintering schedule is: be warming up to 550 ℃ through 200 minutes, after be warming up to 1050 ℃ through 50 minutes again, and be incubated 100 minutes.
Embodiment 2:
Earlier with Ag 2O:42g, Nb 2O 5: 39g, Ta 2O 5: 14g, NaCO 3: 2.5g, mixed the back ball milling 260 minutes, 1100 ℃ of Synthetic 2s 40 minutes, form frit, with Bi 2O 3: 1.5g, Sb 2O 5: 1g, MnCO 3: 3.5g adds in the above-mentioned frit ball milling 380 minutes, the polyvinyl alcohol granulation that adds 7g then, every takes by weighing 0.55g and carries out compressing tablet, and carry out sintering at last: its sintering schedule is: be warming up to 550 ℃ through 240 minutes, after be warming up to 1160 ℃ through 70 minutes again, and be incubated 120 minutes.
Embodiment 3:
Earlier with Ag 2O:42g, Nb 2O 5: 39g, Ta 2O 5: 14g, NaCO 3: 2.5g, mixed the back ball milling 240 minutes, 900 ℃ of Synthetic 2s 20 minutes, form frit, with Bi 2O 3: 1.5g, Sb 2O 5: 1g, MnCO 3: 4.5g adds in the above-mentioned frit ball milling 340 minutes, the paraffin granulation that adds 6g then, every takes by weighing 0.5g and carries out compressing tablet, and carry out sintering at last: its sintering schedule is: be warming up to 550 ℃ through 220 minutes, after be warming up to 1060 ℃ through 60 minutes again, and be incubated 110 minutes.
Embodiment 4:
Earlier with Ag 2O:42g, Nb 2O 5: 39g, Ta 2O 5: 14g, NaCO 3: 2.5g, mixed the back ball milling 240 minutes, 1000 ℃ of Synthetic 2s 30 minutes, form frit, with Bi 2O 3: 1.5g, Sb 2O 5: 1g, MnCO 3: 2.5g adds in the above-mentioned frit ball milling 360 minutes, the polyvinyl alcohol granulation that adds 6g then, every takes by weighing 0.5g and carries out compressing tablet, and carry out sintering at last: its sintering schedule is: be warming up to 550 ℃ through 230 minutes, after be warming up to 1060 ℃ through 60 minutes again, and be incubated 110 minutes.
Embodiment 5:
Earlier with Ag 2O:42g, Nb 2O 5: 39g, Ta 2O 5: 14g, NaCO 3: 2.5g, mixed the back ball milling 240 minutes, 950 ℃ of Synthetic 2s 40 minutes, form frit, with Bi 2O 3: 1.5g, Sb 2O 5: 1g, MnCO 3: 1.2g adds in the above-mentioned frit ball milling 360 minutes, the paraffin granulation that adds 6g then, every takes by weighing 0.5g and carries out compressing tablet, and carry out sintering at last: its sintering schedule is: be warming up to 550 ℃ through 240 minutes, after be warming up to 1060 ℃ through 60 minutes again, and be incubated 120 minutes.

Claims (4)

1. a high frequency heat stable ceramic medium material is characterized in that, comprises following each component by weight percentage:
Ag 2O 3： 40～45％；
Na 2CO 3： 1.2～6.0％；
Nb 2O 5： 36～39％；
Ta 2O 5： 8～14％；
Bi 2O 3： 1.5～3.5％；
Sb 2O 5： 1.0～4.0％。
2. high frequency heat stable ceramic medium material according to claim 1 is characterized in that, comprises following each component by weight percentage:
Ag 2O 3： 39～41％；
Na 2CO 3： 3.5～5.0％；
Nb 2O 5： 37～38％；
Ta 2O 5： 10～12％；
Bi 2O 3： 2.0～3.0％；
Sb 2O 5： 2.0～3.0％。
3. the high-frequency dielectric material with high-k according to claim 1 is characterized in that, adds MnCO in described component by weight percentage 3: 1.0～5.0%.
4. the preparation method of a high frequency heat stable ceramic medium material is characterized in that, comprises the steps:
A) earlier with Ag 2O 38～43%, Nb 2O 536～39%, Ta 2O 58～14%, NaCO 31.2～6.0%, mixed the back ball milling 220～260 minutes,
B) 800～1100 ℃ of Synthetic 2s 00～240 minute, form frit,
C) with Bi 2O 31.0 Sb～4.0%, 2O 51.0 MnCO～4.0%, 31.0～5.0%, add in the above-mentioned frit, ball milling 320～380 minutes,
D) add the tamanori granulation of 6-7wt% then, every takes by weighing 0.45～0.55g and carries out compressing tablet,
E) carry out sintering at last: its sintering schedule is: be warming up to 550 ℃ through 200～240 minutes, after be warming up to 1050～1160 ℃ through 50～70 minutes again, and be incubated 100～120 minutes.
CN 200410018747 2004-03-16 2004-03-16 High frequency ceramic dielectric material in thermal stability and preparaton method Expired - Fee Related CN1256296C (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN110105065A (en) * 2019-05-13 2019-08-09 太原师范学院 A kind of temperature-stable ceramic medium material and preparation method thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN110105065A (en) * 2019-05-13 2019-08-09 太原师范学院 A kind of temperature-stable ceramic medium material and preparation method thereof
CN110105065B (en) * 2019-05-13 2021-12-17 太原师范学院 Temperature-stable ceramic dielectric material and preparation method thereof

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