CN1256296C - 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 PDFInfo
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- CN1256296C CN1256296C CN 200410018747 CN200410018747A CN1256296C CN 1256296 C CN1256296 C CN 1256296C CN 200410018747 CN200410018747 CN 200410018747 CN 200410018747 A CN200410018747 A CN 200410018747A CN 1256296 C CN1256296 C CN 1256296C
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- high frequency
- dielectric material
- ceramic dielectric
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Abstract
The present invention discloses a high frequency ceramic dielectric material of thermal stability and a preparation method thereof. The high frequency ceramic dielectric material is composed of components of the following proportion by weight: 40 to 45% of Ag2O3, 1.2 to 6.0% of Na2CO3, 36 to 39% of Nb2O5, 8 to 14% of Ta2O5, 1.5 to 3.5% of Bi2O3 and 1.0 to 4.0% of Sb2O5. A moderate temperature sintering technology is used for the preparation method of the high frequency ceramic dielectric material of thermal stability, and cost is effectively reduced at the time of saving energy. The high frequency ceramic dielectric material of thermal stability has the advantages of high dielectric constant and lower loss value.
Description
Technical field
The present invention relates to the dielectric substance field, in particular, relate to a kind of preparation method of high frequency heat stable ceramic medium material.
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 (1T) 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.A few days ago, 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 monooxide 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 the digitizing of electronics, high frequencyization, active network also towards the square I sentence development 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 higher owing to frequency in mobile communication, so that usefulness is COG (NPO), because the impedance of electrical condenser is 1/ (2 π fc), 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 preparation method of high frequency heat stable ceramic medium material in order to overcome the deficiencies in the prior art.
The preparation method of high frequency heat stable ceramic medium material of the present invention comprises the steps:
A) earlier with Ag
2O 38～43%, NbO
536～39%, Ta
2O
58～14%, NaCO
31.2～6.0%, mixed the back ball milling 220-260 minute;
B), form frit 800～1100 ℃ of Synthetic 2s 00～240 minute;
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.
High frequency heat stable ceramic dielectic of the present invention not only has higher dielectric constant (specific inductivity is greater than 500), and it is stable to have reduced sintering 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.
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.
In the present invention, insulation resistivity ρ
vVariation also with Na
+Content relevant.Work as Na
+Content hour, ρ
vGenerally all greater than 10
12Ω cm is with Na
+Content there is no very significantly relation.But work as Na
+When content is higher, ρ
vObviously descend.When x＞0.3, insulation resistivity pv＜10 of system
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 by suitably regulating the Nb/Ta ratio, the temperature coefficient of capacitance of ANT system is adjusted near 0ppm/ ℃, when Nb/Ta=2.5～6.5, 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 advantageous property is arranged also.Its specific inductivity is 49～52 (100MHz), and temperature coefficient of capacitance is about 0 ± 6ppm/ ℃.In addition, because Bi
2O
3Molten 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 that the ANT system loss increases.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, do not influence other dielectric characteristics simultaneously.
Embodiment 1:
Earlier with Ag
2O:42g, Nb
2O
539g, 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, the diameter 10mm of compressing tablet carries out compressing tablet, 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
539g, 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, carries 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
539g, 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, and ball milling 340 minutes adds the paraffin granulation of 6g then, every takes by weighing 0.5g and carries out compressing tablet, carries out sintering at last, and 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
539g, 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, and ball milling 360 minutes adds the paraffin granulation of 6g then, every takes by weighing 0.5g and carries out compressing tablet, carries out sintering at last, and 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
539g, 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, and ball milling 360 minutes adds the paraffin granulation of 6g then, every takes by weighing 0.5g and carries out compressing tablet, carries out sintering at last, and 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 110 minutes.
Claims (1)
1. 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%, NbO
536～39%, Ta
2O
58～14%, NaCO
31.2～6.0%, mixed the back ball milling 220-260 minute,
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.
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|---|---|---|---|
| CN 200410018747 CN1256296C (en) | 2004-03-16 | 2004-03-16 | High frequency ceramic dielectric material in thermal stability and preparaton method |
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|---|---|---|---|
| CN 200410018747 CN1256296C (en) | 2004-03-16 | 2004-03-16 | High frequency ceramic dielectric material in thermal stability and preparaton method |
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| Publication Number | Publication Date |
|---|---|
| CN1562867A CN1562867A (en) | 2005-01-12 |
| CN1256296C true CN1256296C (en) | 2006-05-17 |
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Families Citing this family (3)
| 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 |
| 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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