CN107640970B - The AgNb of low frequency low-dielectric loss is co-doped with titania-based dielectric ceramic material and preparation method thereof - Google Patents
The AgNb of low frequency low-dielectric loss is co-doped with titania-based dielectric ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of AgNb of low frequency low-dielectric loss to be co-doped with titania-based dielectric ceramic material and preparation method thereof, and the general formula of the ceramic material is (Ag1/4Nb3/4)xTi1‑xO2, wherein x indicates that molar fraction, the value of x are 0.005~0.01.The preparation method of ceramic material of the present invention is simple, reproducible, high yield rate, by introducing metal element A g in the mono- titanium dioxide base ceramic material mixed of Nb, makes ceramic material in frequency 40~106There is high dielectric constant (> 10 within the scope of Hz4), low-dielectric loss (< 0.09), especially significantly reduce ceramic material low-frequency dielectric loss, 40~103Dielectric loss remains at 0.06 hereinafter, have excellent frequency and temperature stability simultaneously in Hz frequency range, is maintained between -10%~10%, meets the parameter request of ceramic capacitor, has huge application value.
Description
Technical field
The invention belongs to technical field of ceramic material, and in particular to a kind of high dielectric constant, the titanium dioxide of low-dielectric loss
Titanium-based dielectric ceramic material and preparation method thereof.
Background technique
The information age electron industry of high speed development brings the new situation with rapid changepl. never-ending changes and improvements, and microelectronics industry has no at present
Query has become one of maximum industry in the whole world, and capacitor as the main element in high volume used in electronic equipment it
One, mobile phone, computer, household electrical appliances, the automobile either used in our daily lifes, or in industrial instruments, agricultural, state
Anti- department even aerospace field, all plays very important role.
Dielectric material is as important functional material, by extensively should be many in capacitor, memory, microelectronic component etc.
Field.As manufacturing process continues to develop, the characteristic size of integrated circuit constantly reduces, electronic component it is integrated, small-sized
Change, high speed has become the important research topic in one, present information field.Common dielectric material strontium barium titanate system, zirconium titanium
Lead plumbate system etc. is mostly ferroelectric material, since in Curie temperature ferroelectricity-paraelectric phase transition can occur for ferroelectric material, so that ferroelectric material
Dielectric constant with temperature variation it is obvious, so as to cause device temperature stability be deteriorated, limit its application range.For lead
Sill, since system contains lead element, and lead element is a kind of disagreeableness metallic element of environment.Therefore, a kind of nothing is researched and developed
Lead and have high dielectric constant, low-dielectric loss, the good dielectric material of frequency stability of temperature extremely urgent.
Since titania-based ceramics have relatively high dielectric constant in simple compounds, research is caused
The extensive concern of person.In recent years, it whether singly mixes or titanium dioxide base ceramic material that two pentavalents, three pentavalents are co-doped with is ground
Study carefully layer and go out not group, but most of material cannot meet the requirement of high dielectric constant, low-dielectric loss simultaneously, especially single doping
Titanium dioxide base ceramic material.Such as the titania-based ceramics that niobium list is mixed have relatively high dielectric constant (> 104),
But the dielectric loss of its low frequency is larger (> 1), is not able to satisfy the requirement of low-dielectric loss.
Summary of the invention
Technical problem to be solved by the present invention lies in provide one kind to have high dielectric constant, low-dielectric loss (especially
Low frequency low-dielectric loss), frequency stability of temperature AgNb that is good, practical, being readily produced be co-doped with titania-based dielectric
Ceramic material, and a kind of preparation method is provided for the ceramic material.
The general formula for solving ceramic material used by above-mentioned technical problem is (Ag1/4Nb3/4)xTi1-xO2, wherein x indicates to rub
That score, the value of x are 0.005~0.01.
Above-mentioned AgNb be co-doped with titania-based dielectric ceramic material the preparation method is as follows:
1, according to (Ag1/4Nb3/4)xTi1-XO2Stoichiometry weigh respectively purity be 99.5% or more raw material A g2O、
Nb2O5And TiO2, it is sufficiently mixed ball milling 16~24 hours, it is 12~24 hours dry at 80~100 DEG C, obtain raw mixture.
2, by raw mixture 1000~1200 DEG C pre-burning 2~4 hours, obtain pre-burning powder.
3, it by pre-burning powder after secondary ball milling, granulation, tabletting, dumping, is sintered 5~10 hours, obtains at 1400~1450 DEG C
Titania-based dielectric ceramic material is co-doped with to AgNb.
In above-mentioned steps 2, preferably by raw mixture 1100 DEG C pre-burning 3 hours.
It is small in 1450 DEG C of sintering 10 preferably by pre-burning powder after secondary ball milling, granulation, tabletting, dumping in above-mentioned steps 3
When.
The present invention makes ceramic material simultaneous by introducing metal element A g in the mono- titanium dioxide base ceramic material mixed of Nb
In the case where having high dielectric constant, the low-frequency dielectric loss of ceramic material is significantly reduced, 40~103It is situated between in Hz frequency range
Electrical loss remains at 0.06 hereinafter, have excellent frequency and temperature stability simultaneously, be maintained at -10%~10Z% it
Between.
The preparation method of ceramic material of the present invention is simple, reproducible, high yield rate, it is practical, be readily produced.
Detailed description of the invention
Fig. 1 is the XRD diagram of the ceramic material of Examples 1 to 2 preparation.
Fig. 2 is the dielectric constant of the ceramic material of Examples 1 to 6 preparation with the variation relation figure of test frequency.
Fig. 3 is the dielectric loss of the ceramic material of Examples 1 to 6 preparation with the variation relation figure of test frequency.
Fig. 4 is the dielectric constant of ceramic material prepared by embodiment 1 with test temperature variation and temperature stability relational graph.
Fig. 5 is the dielectric constant of ceramic material prepared by embodiment 2 with test temperature variation and temperature stability relational graph.
Specific embodiment
The present invention is described in more detail with reference to the accompanying drawings and examples, but protection scope of the present invention is not limited only to
These embodiments.
Embodiment 1
1, according to (Ag1/4Nb3/4)0.005Ti0.995O2Stoichiometry weigh raw material A g respectively2O (purity 99.7%)
0.0361g、Nb2O5(purity 99.99%) 0.1237g, TiO2(purity 99.5%) 19.8401g, and be fitted into nylon tank, with zirconium
Ball is abrading-ball, dehydrated alcohol is ball-milling medium, and the mass ratio of dehydrated alcohol and raw mixture is 1:1.2, with ball mill 401
Revs/min ball milling 24 hours, separating zirconium ball was 24 hours dry at 80 DEG C by raw mixture, with mortar grinder 30 minutes, obtained
To raw mixture.
2, raw mixture is placed in alumina crucible, covers, is warming up to 1100 DEG C with 3 DEG C/min of heating rate
Heat preservation 3 hours, cooled to room temperature is come out of the stove, and with mortar grinder 5 minutes, obtains pre-burning powder.
3, pre-burning powder is fitted into nylon tank, is ball-milling medium, dehydrated alcohol and pre-burning by abrading-ball, dehydrated alcohol of zirconium ball
The mass ratio of powder is 1:1.2, is sufficiently mixed ball milling 20 hours, separating zirconium ball, by pre-burning powder dry 24 hours at 80 DEG C, with grinding
Alms bowl grinding, obtains the pre-burning powder of secondary ball milling；The polyvinyl alcohol water solution that mass fraction is 5%, polyethylene is added thereto again
The additional amount of alcohol solution is 50% of the pre-burning silty amount after secondary ball milling, is granulated, and crosses 120 meshes, spherical powder is made, will
Spherical powder is put into the stainless steel mould that diameter is 11.5mm, is compressed into thickness under the pressure of 6MPa with powder compressing machine
Degree is the cylindric blank of 1.5mm；Cylindric blank is placed on zirconium oxide plate, zirconium oxide plate is placed in aluminium oxide porcelain boat
In, 500 DEG C first were warming up to 380 minutes in Muffle furnace, 2 hours are kept the temperature, with furnace cooled to room temperature, then in tube furnace
Middle elder generation was warming up to 1000 DEG C with 100 minutes, then was warming up to 1450 DEG C with 2 DEG C/min of heating rate, 10 hours was kept the temperature, with furnace
Cooled to room temperature, the AgNb for obtaining low frequency low-dielectric loss are co-doped with titania-based dielectric ceramic material.
Embodiment 2
In the present embodiment, according to (Ag1/4Nb3/4)0.01Ti0.99O2Stoichiometry weigh raw material A g respectively2O (99.7%)
0.0719g、Nb2O5(99.99%) 0.2468g, TiO2(99.5%) 19.6813g, other steps are same as Example 1, obtain
The AgNb of low frequency low-dielectric loss is co-doped with titania-based dielectric ceramic material.
Embodiment 3
In the present embodiment, 1000 DEG C first were warming up to 100 minutes in tube furnace, then with 2 DEG C/min of heating rate liter
Temperature keeps the temperature 10 hours, other steps are same as Example 1, and the AgNb for obtaining low frequency low-dielectric loss is co-doped with dioxy to 1410 DEG C
Change titanium-based dielectric ceramic material.
Embodiment 4
In the present embodiment, 1000 DEG C first were warming up to 100 minutes in tube furnace, then with 2 DEG C/min of heating rate liter
Temperature keeps the temperature 10 hours, other steps are same as Example 2, and the AgNb for obtaining low frequency low-dielectric loss is co-doped with dioxy to 1410 DEG C
Change titanium-based dielectric ceramic material.
Embodiment 5
In the present embodiment, 1000 DEG C first were warming up to 100 minutes in tube furnace, then with 2 DEG C/min of heating rate liter
Temperature keeps the temperature 5 hours, other steps are same as Example 1, and the AgNb for obtaining low frequency low-dielectric loss is co-doped with titanium dioxide to 1450 DEG C
Titanium-based dielectric ceramic material.
Embodiment 6
In the present embodiment, 1000 DEG C first were warming up to 100 minutes in tube furnace, then with 2 DEG C/min of heating rate liter
Temperature keeps the temperature 5 hours, other steps are same as Example 2, and the AgNb for obtaining low frequency low-dielectric loss is co-doped with titanium dioxide to 1450 DEG C
Titanium-based dielectric ceramic material.
Ceramic material prepared by above-described embodiment 1 and 2 is respectively adopted D/max-2200X type x ray diffractometer x and (is managed by Japan
Company production) carry out XRD test, the result is shown in Figure 1.As seen from Figure 1, the ceramic material of Examples 1 and 2 preparation is pure class
Perovskite structure, no second phase generate.
The ceramic material surfaces of Examples 1 to 6 preparation are successively polished to 0.5 with 320 mesh, 800 mesh, 1500 mesh sand paper~
0.6mm is thick, then in the silver paste that ceramic upper and lower surface coating thickness is 0.01~0.03mm, is placed in 840 DEG C of heat preservations in resistance furnace
30 minutes.Using Agilient4294A type precise impedance analyzer and E4980A type LCR tester respectively to the dielectricity of ceramics
It can be carried out test, as a result see Fig. 2~5.By Fig. 2 and 3 as it can be seen that when 1kHz, opposite Jie of the ceramic material of Examples 1 to 6 preparation
Electric constant is followed successively by 9409,17252,9345,17150,9259,16234, dielectric loss is followed successively by 0.036,0.044,0.057,
0.060,0.043,0.059, and frequency is 40~103Dielectric loss within the scope of Hz remains at 0.06 or less.It can by Fig. 4
See, the dielectric constant of ceramic material prepared by embodiment 1 in different frequency within the scope of -55~150 DEG C generally concentrates on 9000
Left and right, rate of temperature change are -1.5%~7%.As seen from Figure 5, embodiment 2 prepare ceramic material in different frequency -55~
Dielectric constant within the scope of 150 DEG C is concentrated mainly between 14000~16000, and rate of temperature change is -8.6%~10%.By
This as it can be seen that ceramic material of the invention has a high dielectric constant, low-dielectric loss, and temperature stability remain at-
Between 10%~10%, meet the application requirement of material.
Claims (3)
1. a kind of AgNb of low frequency low-dielectric loss is co-doped with titania-based dielectric ceramic material, it is characterised in that: the ceramics material
The general formula of material is (Ag1/4Nb3/4)xTi1-xO2, wherein the value of x is 0.005~0.01；The ceramic material is prepared by the following method
It obtains:
(1) according to (Ag1/4Nb3/4)xTi1-xO2Stoichiometry weigh respectively purity be 99.5% or more raw material A g2O、Nb2O5With
TiO2, it is sufficiently mixed ball milling 16~24 hours, it is 12~24 hours dry at 80~100 DEG C, obtain raw mixture；
(2) by raw mixture 1000~1200 DEG C pre-burning 2~4 hours, obtain pre-burning powder；
(3) it by pre-burning powder after secondary ball milling, granulation, tabletting, dumping, is sintered 5~10 hours, obtains at 1400~1450 DEG C
The AgNb of low frequency low-dielectric loss is co-doped with titania-based dielectric ceramic material.
2. the AgNb of low frequency low-dielectric loss according to claim 1 is co-doped with titania-based dielectric ceramic material, special
Sign is: in step (2), by raw mixture 1100 DEG C pre-burning 3 hours.
3. the AgNb of low frequency low-dielectric loss according to claim 1 is co-doped with titania-based dielectric ceramic material, special
Sign is: in step (3), by pre-burning powder after secondary ball milling, granulation, tabletting, dumping, being sintered 10 hours at 1450 DEG C.
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| CN109133914B (en) * | 2018-11-23 | 2021-07-06 | 陕西师范大学 | Titanium dioxide-based ceramic material with high thermal stability and preparation method thereof |
| CN111205085B (en) * | 2020-02-03 | 2021-07-27 | 河南理工大学 | Preparation method of titanium dioxide-based ceramic with ultrahigh dielectric constant and low dielectric loss |
| CN113788673A (en) * | 2021-09-29 | 2021-12-14 | 陕西师范大学 | Titanium dioxide-based ceramic material with medium-low frequency, ultralow dielectric loss and high dielectric constant and preparation method thereof |
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