CN107640970A - 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
- Publication number
- CN107640970A CN107640970A CN201711021284.2A CN201711021284A CN107640970A CN 107640970 A CN107640970 A CN 107640970A CN 201711021284 A CN201711021284 A CN 201711021284A CN 107640970 A CN107640970 A CN 107640970A
- Authority
- CN
- China
- Prior art keywords
- ceramic material
- low
- dielectric loss
- doped
- agnb
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Inorganic Insulating Materials (AREA)
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 formula of the ceramic material is (Ag1/4Nb3/4)xTi1‑xO2, wherein x expression molar fractions, x value is 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 materials mixed of Nb, makes ceramic material in frequency be 40~106There is high-k (＞ 10 in the range of Hz4), low-dielectric loss (＜ 0.09), especially significantly reduce ceramic material low-frequency dielectric loss, 40~103Dielectric loss remains at less than 0.06 in Hz frequency ranges, while has excellent frequency and temperature stability, 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-k, the titanium dioxide of low-dielectric loss
Titanium-based dielectric ceramic material and preparation method thereof.
Background technology
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.Conventional dielectric material strontium barium titanate system, zirconium titanium
Lead plumbate system etc. is mostly ferroelectric material, because in Curie temperature ferroelectricity-paraelectric phase transition can occur for ferroelectric material so that ferroelectric material
Dielectric constant with temperature change it is obvious, so as to cause the temperature stability of device to be deteriorated, limit its application.For lead
Sill, because 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 extremely urgent with the good dielectric material of high-k, low-dielectric loss, frequency stability of temperature.
Because titania-based ceramics have of a relatively high dielectric constant in simple compounds, therefore cause research
The extensive concern of person.In recent years, whether singly mix, or two pentavalents, the three pentavalents titanium dioxide base ceramic materials that are co-doped with is ground
Study carefully layer and go out not group, but most of material can not meet the requirement of high-k, low-dielectric loss simultaneously, especially single doping
Titanium dioxide base ceramic material.Such as the titania-based ceramics that niobium list is mixed have of a relatively high dielectric constant (＞ 104),
But the dielectric loss of its low frequency is larger (＞ 1), it is impossible to meets the requirement of low-dielectric loss.
The content of the invention
The technical problems to be solved by the invention are that providing one kind has high-k, low-dielectric loss (particularly
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 provide a kind of preparation method for the ceramic material.
The formula of ceramic material is (Ag used by solution above-mentioned technical problem1/4Nb3/4)xTi1-xO2, wherein x represent rub
That fraction, x value is 0.005~0.01.
The preparation method that above-mentioned AgNb is co-doped with titania-based dielectric ceramic material is as follows：
1st, according to (Ag1/4Nb3/4)xTi1-XO2Stoichiometry weigh respectively purity be more than 99.5% raw material A g2O、
Nb2O5And TiO2, it is sufficiently mixed ball milling 16~24 hours, is dried 12~24 hours at 80~100 DEG C, obtain raw mixture.
2nd, raw mixture is obtained into pre-burning powder in 1000~1200 DEG C of pre-burnings 2~4 hours.
3rd, by pre-burning powder after secondary ball milling, granulation, tabletting, dumping, sinter 5~10 hours, obtain 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 in 1100 DEG C of pre-burnings 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 materials mixed of Nb
In the case of having high-k, the low-frequency dielectric loss of ceramic material is significantly reduced, 40~103It is situated between in Hz frequency ranges
Electrical loss remains at less than 0.06, while has excellent frequency and temperature stability, 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.
Brief description of the drawings
Fig. 1 is the XRD of ceramic material prepared by embodiment 1~2.
Fig. 2 is the dielectric constant of ceramic material prepared by embodiment 1~6 with the variation relation figure of test frequency.
Fig. 3 is the dielectric loss of ceramic material prepared by embodiment 1~6 with the variation relation figure of test frequency.
Fig. 4 is the dielectric constant of ceramic material prepared by embodiment 1 with test temperature change and temperature stability graph of a relation.
Fig. 5 is the dielectric constant of ceramic material prepared by embodiment 2 with test temperature change and temperature stability graph of a relation.
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
1st, 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, absolute ethyl alcohol is ball-milling medium, and the mass ratio of absolute ethyl alcohol and raw mixture is 1:1.2, with ball mill 401
Rev/min ball milling 24 hours, separating zirconium ball, raw mixture is dried 24 hours at 80 DEG C, with mortar grinder 30 minutes, obtained
To raw mixture.
2nd, raw mixture is placed in alumina crucible, is capped, 1100 DEG C are warming up to 3 DEG C/min of heating rate
Insulation 3 hours, naturally cools to room temperature, comes out of the stove, and with mortar grinder 5 minutes, obtains pre-burning powder.
3rd, pre-burning powder is fitted into nylon tank, is ball-milling medium, absolute ethyl alcohol and pre-burning by abrading-ball, absolute ethyl alcohol of zirconium ball
The mass ratio of powder is 1:1.2, it is sufficiently mixed ball milling 20 hours, separating zirconium ball, pre-burning powder is dried 24 hours at 80 DEG C, with grinding
Alms bowl is ground, and obtains the pre-burning powder of secondary ball milling；Add the polyvinyl alcohol water solution that mass fraction is 5%, polyethylene thereto again
The addition of alcohol solution is 50% of the pre-burning silty amount after secondary ball milling, is granulated, and crosses 120 mesh sieves, spherical powder is made, will
Spherical powder is put into a diameter of 11.5mm stainless steel mould, and thickness is compressed under 6MPa pressure with powder compressing machine
Spend the cylindric blank for 1.5mm；Cylindric blank is placed on zirconium oxide flat board, zirconium oxide flat board is placed in aluminum oxide porcelain boat
In, 500 DEG C first were warming up to 380 minutes in Muffle furnace, 2 hours is incubated, room temperature is naturally cooled to stove, 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 incubated, with stove
Room temperature is naturally cooled to, the AgNb for obtaining low frequency low-dielectric loss is 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 is incubated 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 is incubated 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 is incubated 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 is incubated 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 types x ray diffractometer x and (managed by Japan
Company produces) XRD tests are carried out, as a result see Fig. 1.As seen from Figure 1, the ceramic material that prepared by Examples 1 and 2 is pure class
Perovskite structure, generated without the second phase.
Ceramic material surfaces prepared by embodiment 1~6 are polished to 0.5 with 320 mesh, 800 mesh, 1500 mesh sand paper successively~
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 insulations in resistance furnace
30 minutes.Using Agilient4294A type precise impedance analyzers and E4980A type LCR testers respectively to the dielectricity of ceramics
It can be tested, as a result see Fig. 2~5.During from Fig. 2 and 3,1kHz, relative Jie of ceramic material prepared by embodiment 1~6
Electric constant is followed successively by 9409,17252,9345,17150,9259,16234, dielectric loss is followed successively by 0.036,0.044,0.057,
0.060th, 0.043,0.059, and frequency is 40~103Dielectric loss in the range of Hz remains at less than 0.06.Can by Fig. 4
See, the dielectric constant of ceramic material prepared by embodiment 1 in different frequency in the range 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 in the range of 150 DEG C is concentrated mainly between 14000~16000, and its rate of temperature change is -8.6%~10%.By
This is visible, and ceramic material of the invention has high-k, a low-dielectric loss, and temperature stability remain at-
Between 10%~10%, meet the application requirement of material.
Claims (4)
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 ceramic material
The formula of material is (Ag1/4Nb3/4)xTi1-xO2, wherein x value is 0.005~0.01.
2. a kind of AgNb of the low frequency low-dielectric loss described in claim 1 is co-doped with the preparation of titania-based dielectric ceramic material
Method, it is characterised in that it is made up of following step：
(1) according to (Ag1/4Nb3/4)xTi1-xO2Stoichiometry weigh respectively purity be more than 99.5% raw material A g2O、Nb2O5
And TiO2, it is sufficiently mixed ball milling 16~24 hours, is dried 12~24 hours at 80~100 DEG C, obtain raw mixture；
(2) raw mixture is obtained into pre-burning powder in 1000~1200 DEG C of pre-burnings 2~4 hours；
(3) by pre-burning powder after secondary ball milling, granulation, tabletting, dumping, sinter 5~10 hours, obtain low at 1400~1450 DEG C
The AgNb of frequency low-dielectric loss is co-doped with titania-based dielectric ceramic material.
3. the AgNb of low frequency low-dielectric loss according to claim 2 is co-doped with the preparation of titania-based dielectric ceramic material
Method, it is characterised in that：In step (2), by raw mixture in 1100 DEG C of pre-burnings 3 hours.
4. the AgNb of low frequency low-dielectric loss according to claim 2 is co-doped with the preparation of titania-based dielectric ceramic material
Method, it is characterised in that：In step (3), by pre-burning powder after secondary ball milling, granulation, tabletting, dumping, in 1450 DEG C of sintering
10 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711021284.2A CN107640970B (en) | 2017-10-26 | 2017-10-26 | The AgNb of low frequency low-dielectric loss is co-doped with titania-based dielectric ceramic material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711021284.2A CN107640970B (en) | 2017-10-26 | 2017-10-26 | The AgNb of low frequency low-dielectric loss is co-doped with titania-based dielectric ceramic material and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107640970A true CN107640970A (en) | 2018-01-30 |
| CN107640970B CN107640970B (en) | 2019-12-03 |
Family
ID=61124965
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711021284.2A Active CN107640970B (en) | 2017-10-26 | 2017-10-26 | The AgNb of low frequency low-dielectric loss is co-doped with titania-based dielectric ceramic material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107640970B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109133914A (en) * | 2018-11-23 | 2019-01-04 | 陕西师范大学 | A kind of titanium dioxide base ceramic material of high thermal stability and preparation method thereof |
| WO2019206321A1 (en) * | 2018-04-27 | 2019-10-31 | The Hong Kong Polytechnic University | Multilayer and flexible capacitors with metal-ion doped tio2 colossal permittivity material/polymer composites |
| CN111205085A (en) * | 2020-02-03 | 2020-05-29 | 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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6078494A (en) * | 1997-08-28 | 2000-06-20 | U.S. Philips Corporation | Multilayer capacitor comprising barium-titanate doped with silver and rare earth metal |
| CN101186496A (en) * | 2007-11-27 | 2008-05-28 | 西安交通大学 | Low-temperature sintering Ti-base microwave medium ceramic material and preparation thereof |
| CN104478431A (en) * | 2014-11-26 | 2015-04-01 | 四川大学 | Ion modified titanium dioxide ceramic material with high dielectric constant and preparation method thereof |
-
2017
- 2017-10-26 CN CN201711021284.2A patent/CN107640970B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6078494A (en) * | 1997-08-28 | 2000-06-20 | U.S. Philips Corporation | Multilayer capacitor comprising barium-titanate doped with silver and rare earth metal |
| CN101186496A (en) * | 2007-11-27 | 2008-05-28 | 西安交通大学 | Low-temperature sintering Ti-base microwave medium ceramic material and preparation thereof |
| CN104478431A (en) * | 2014-11-26 | 2015-04-01 | 四川大学 | Ion modified titanium dioxide ceramic material with high dielectric constant and preparation method thereof |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019206321A1 (en) * | 2018-04-27 | 2019-10-31 | The Hong Kong Polytechnic University | Multilayer and flexible capacitors with metal-ion doped tio2 colossal permittivity material/polymer composites |
| CN109133914A (en) * | 2018-11-23 | 2019-01-04 | 陕西师范大学 | A kind of titanium dioxide base ceramic material of high thermal stability and preparation method thereof |
| 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 |
| CN111205085A (en) * | 2020-02-03 | 2020-05-29 | 河南理工大学 | Preparation method of titanium dioxide-based ceramic with ultrahigh dielectric constant and low dielectric loss |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107640970B (en) | 2019-12-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107640970B (en) | The AgNb of low frequency low-dielectric loss is co-doped with titania-based dielectric ceramic material and preparation method thereof | |
| CN105732020B (en) | A kind of preparation method of giant dielectric, low-loss titanium dioxide base composite ceramic | |
| CN106892659A (en) | A kind of anti-reduction huge dielectric constant medium material for multilayer ceramic capacitors | |
| CN110015894B (en) | Sodium bismuth titanate-based ceramic with high dielectric stability at high temperature and preparation method and application thereof | |
| CN106747410A (en) | The bias titania-based composite dielectric ceramic material of stable type giant dielectric low-loss | |
| CN103214238A (en) | Preparation method of barium strontium titanate dielectric temperature stable ceramic capacitor material | |
| CN108610042A (en) | Dielectric material and preparation method thereof with the high insulation characterisitic of huge dielectric constant | |
| CN109231985A (en) | A kind of preparation method of low-loss X8R type dielectric substance | |
| CN104058741A (en) | Medium ceramic with stable ultra-wide temperature and preparation method thereof | |
| CN108218423A (en) | A kind of X8R types ceramic capacitor dielectric material and preparation method thereof | |
| CN106278261A (en) | A kind of low-temperature sintering low-loss high frequency medium ceramic material and preparation method thereof | |
| CN106187189B (en) | A kind of energy storage microwave dielectric ceramic materials and preparation method thereof | |
| CN109231983A (en) | A kind of preparation method of the barium zirconate titanate-based ceramics of bilayer | |
| CN104310986A (en) | High dielectric constant stable-temperature ceramic capacitor dielectric material | |
| CN107746271A (en) | The AgTa of low frequency low-dielectric loss is co-doped with titania-based dielectric ceramic material and preparation method thereof | |
| CN112851347A (en) | Low-temperature sintered low-loss oxyfluoride microwave dielectric ceramic and preparation method thereof | |
| CN110357618B (en) | Low-temperature sintering temperature-stable zirconate microwave dielectric ceramic material and preparation method thereof | |
| CN107226696A (en) | X7R types BaTiO3Based capacitor ceramic material and preparation method thereof | |
| CN103864416A (en) | Method for preparing barium titanate ceramic capacitor medium at low sintering temperature | |
| CN109626999B (en) | Negative temperature coefficient ceramic dielectric material and preparation method thereof | |
| CN108727013B (en) | Ceramic dielectric material with ultralow dielectric loss and high dielectric constant and preparation method thereof | |
| CN107473743A (en) | A kind of lead base high-K capacitor dielectric material and preparation method thereof | |
| CN109133914A (en) | A kind of titanium dioxide base ceramic material of high thermal stability and preparation method thereof | |
| CN104725036B (en) | A kind of barium-strontium titanate-based energy storage ceramic of high temperature low loss and preparation method thereof | |
| CN110963796B (en) | Giant dielectric constant low-loss X8R type ceramic capacitor material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |