CN104692795B - A kind of ultra-low loss magnesium titanate lithium microwave dielectric ceramic materials and preparation method thereof - Google Patents
A kind of ultra-low loss magnesium titanate lithium microwave dielectric ceramic materials and preparation method thereof Download PDFInfo
- Publication number
- CN104692795B CN104692795B CN201510066787.6A CN201510066787A CN104692795B CN 104692795 B CN104692795 B CN 104692795B CN 201510066787 A CN201510066787 A CN 201510066787A CN 104692795 B CN104692795 B CN 104692795B
- Authority
- CN
- China
- Prior art keywords
- microwave
- ceramic materials
- ultra
- dielectric ceramic
- magnesium titanate
- 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.)
- Active
Links
Landscapes
- Compositions Of Oxide Ceramics (AREA)
- Inorganic Insulating Materials (AREA)
Abstract
The invention discloses a kind of ultra-low loss magnesium titanate lithium microwave dielectric ceramic materials and preparation method thereof, the chemical composition of the ceramic material is Li2Mg3TiO6, its dielectric loss is that 0.000037~0.000048, Q × f is 123000~152000GHz, and dielectric constant is 14.5~15.5, and temperature coefficient of resonance frequency is 42~36ppm/ DEG C, is prepared from using high-temperature solid phase reaction method.Microwave dielectric ceramic materials preparation method of the present invention is simple, it is raw materials used abundant, with low cost, be conducive to industrialized production, obtained microwave-medium ceramics performance is stable, it can be used as the manufacture material of electronic circuit substrate, dielectric resonator, wave filter, high frequency satellite microwave device substrate and microstrip line, there is important application prospect and economic worth on electronic circuit, microwave mobile communication, satellite communication, radar system field.
Description
Technical field
The invention belongs to electronic information material and its device arts, and in particular to a kind of ultra-low loss magnesium titanate lithium is micro-
Ripple medium ceramic material and preparation method thereof.
Background technology
Microwave-medium ceramics refer to be applied to complete as dielectric material in microwave frequency band (300MHz~300GHz) circuit
The ceramic material of one or more functions.Ideal microwave media ceramic has suitable dielectric constant (εr), high quality factor (Q
× f) (low-dielectric loss) and the temperature coefficient of resonance frequency (τ that goes to zerof).The resonator that is made of microwave-medium ceramics, filter
The components such as ripple device, Microwave integrated circuit substrate, in the modern communication technologys such as mobile communication, WLAN, military communication
It is widely applied.In addition, with the continuous improvement of communication equipment running frequency, system loss and caloric value increase therewith,
The stability of a system is gradually deteriorated.The great number of issues brought to overcome frequency to widen, needs exploitation high q-factor and low, middle ε badlyr(10≤εr
≤ 25) and nearly zero τfThe microwave dielectric material of value.Low εrThe coupling interaction loss between material and electrode can be reduced, and improved
Signal transmission rate, low-dielectric loss is conducive to improving the alternative of device operating frequencies, nearly zero τfIt is favorably improved device
Frequency temperature stability characteristic (quality).
Traditional low εrCeramics are mainly made up of glass-ceramic (devitrified glass), glass+ceramics (multiphase ceramic) etc..
Although glass ceramic material can be sintered at a lower temperature, due to the introducing of a large amount of low-melting glass materials, material is added
Dielectric loss, it is difficult to use in high frequency.It is new low the need for developing for adaptation electronic component to high frequency, high speed direction
Dielectric constant (εr<15), high q-factor microwave dielectric ceramic materials are increasingly paid attention to by domestic and international material scholar.Report in recent years
The typical low ε in roadr, high q-factor (low-dielectric loss) material system mainly includes：M2SiO4(M=Mg, Zn) base, Al2O3Base, A4B2O9
(A=Co, Mg；B=Nb, Ta) and spinel structure M2TiO4(M=Cu, Zn, Ni etc.) base microwave dielectric ceramics.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of new have ultra-low loss and excellent microwave to be situated between
Magnesium titanate lithium microwave dielectric ceramic materials of electrical property and preparation method thereof.
Solving the technical scheme that is used of above-mentioned technical problem is：The ultra-low loss magnesium titanate lithium microwave dielectric ceramic materials
Chemical composition be Li2Mg3TiO6, its dielectric loss is that 0.000037~0.000048, Q × f is 123000~152000GHz,
Dielectric constant is 14.5~15.5, and temperature coefficient of resonance frequency is -42~-36ppm/ DEG C.
The preparation method of above-mentioned ultra-low loss magnesium titanate lithium microwave dielectric ceramic materials is made up of following step：
1st, batch mixing
According to Li2Mg3TiO6Stoichiometric proportion weigh material purity be more than 99.9% Li2CO3Powder, MgO powder, TiO2
Powder, raw material and zirconia ball, absolute ethyl alcohol are fitted into ball grinder for 1: 2: 2 in mass ratio, ball milling 6~10 is sufficiently mixed small
When, 80~100 DEG C of dryings.
2nd, pre-burning
By the dried mixture of step 1 in 1000~1200 DEG C of pre-burnings 2~6 hours, pre-burning powder is prepared into.
3rd, rerolling
Pre-burning powder and zirconia ball, absolute ethyl alcohol are fitted into ball grinder for 1: 2: 2 in mass ratio, ball milling 6 is sufficiently mixed
~10 hours, 80~100 DEG C of dryings.
4th, granulate, be molded
Mass fraction is added into the dried pre-burning powder of step 3 to granulate for 5% polyvinyl alcohol water solution, excessively 80~
120 mesh sieves, then it is pressed into cylindrical green body with powder compressing machine.
5th, sinter
The cylindrical green body that step 4 is obtained is sintered 2~10 hours at 1260~1340 DEG C, obtains ultra-low loss magnesium titanate
Lithium microwave dielectric ceramic materials.
In above-mentioned steps 2, preferably by the dried mixture of step 1 in 1000 DEG C of pre-burnings 4 hours.
In above-mentioned steps 5, the cylindrical green body for preferably obtaining step 4 is sintered 6 hours at 1280 DEG C.
Microwave dielectric ceramic materials preparation method of the present invention is simple, raw materials used abundant, with low cost, is conducive to industrialization
Production, obtained microwave-medium ceramics have ultra-low loss and excellent microwave dielectric property, can as electronic circuit substrate,
Dielectric resonator, wave filter, the manufacture material of high frequency satellite microwave device substrate and microstrip line are used, in electronic circuit, microwave
Mobile communication, satellite communication, there is important application prospect and economic worth on radar system field.
Brief description of the drawings
Fig. 1 is the X-ray diffractogram of ultra-low loss magnesium titanate lithium microwave dielectric ceramic materials prepared by embodiment 1~6.
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, batch mixing
According to Li2Mg3TiO6Stoichiometric proportion, weigh material purity be more than 99.9% Li2CO3Powder 3.268g, MgO powder
5.243g、TiO2Powder 3.462g, raw material and zirconia ball, absolute ethyl alcohol is fitted into ball grinder for 1: 2: 2 in mass ratio, 360
Rev/min it is sufficiently mixed ball milling 8 hours, 80~100 DEG C of dryings 12 hours.
2nd, pre-burning
The dried mixture of step 1 is placed in alumina crucible, 1000 are warming up to 2 DEG C/min of heating rate
DEG C, constant temperature pre-burning 4 hours is prepared into pre-burning powder.
3rd, rerolling
Pre-burning powder and zirconia ball, absolute ethyl alcohol are fitted into ball grinder for 1: 2: 2 in mass ratio, ball milling 8 is sufficiently mixed
Hour, 80~100 DEG C of dryings 12 hours.
4th, granulate, be molded
The mass fraction of its quality 5% is added into the dried pre-burning powder of step 3 to make for 5% polyvinyl alcohol water solution
Grain, crosses 120 mesh sieves, then the circle that a diameter of 11.5mm, thickness are 5.5mm is compressed into powder compressing machine under 4MPa pressure
Cylindricality green compact.
5th, sinter
The cylindrical green body that step 4 is obtained is sintered 6 hours at 1280 DEG C, obtains ultra-low loss magnesium titanate lithium microwave-medium
Ceramic material.
Embodiment 2
In the step 5 of embodiment 1, cylindrical green body is sintered 6 hours at 1260 DEG C, other steps and the phase of embodiment 1
Together, ultra-low loss magnesium titanate lithium microwave dielectric ceramic materials are obtained.
Embodiment 3
In the step 5 of embodiment 1, cylindrical green body is sintered 6 hours at 1300 DEG C, other steps and the phase of embodiment 1
Together, ultra-low loss magnesium titanate lithium microwave dielectric ceramic materials are obtained.
Embodiment 4
In the step 5 of embodiment 1, cylindrical green body is sintered 6 hours at 1340 DEG C, other steps and the phase of embodiment 1
Together, ultra-low loss magnesium titanate lithium microwave dielectric ceramic materials are obtained.
Embodiment 5
In the step 5 of embodiment 1, cylindrical green body is sintered 2 hours at 1280 DEG C, other steps and the phase of embodiment 1
Together, ultra-low loss magnesium titanate lithium microwave dielectric ceramic materials are obtained.
Embodiment 6
In the step 5 of embodiment 1, cylindrical green body is sintered 10 hours at 1280 DEG C, other steps and the phase of embodiment 1
Together, ultra-low loss magnesium titanate lithium microwave dielectric ceramic materials are obtained.
The ultra-low loss metatitanic acid prepared using RagukuD/Max2550 types (Japan) X-ray diffractometer to embodiment 1~6
Magnesium lithium microwave dielectric ceramic materials are characterized, and as a result see Fig. 1.As seen from Figure 1, the microwave-medium ceramics that prepared by embodiment 1~6
Material is respectively provided with single Li2Mg3TiO6Phase structure.
Ceramic material grinding and polishing post-processing that inventor prepares embodiment 1~6 is into a diameter of 9~10mm, high 5mm
Cylinder, coordinates high-low temperature incubator test ceramic microwave dielectric properties with vector network analyzer, closed chamber the resonance method, the results are shown in Table 1.
The dielectric properties and sintering characteristic of the microwave dielectric ceramic materials of the present invention of table 1
From table 1, magnesium titanate lithium microwave dielectric ceramic materials prepared by embodiment 1~6 are respectively provided with ultralow loss, Q
× f between 123000~152000GHz, dielectric constant between 14.5~15.5, temperature coefficient of resonance frequency -42~-
Between 36ppm/ DEG C, its sintering range wide (1260~1340 DEG C) and performance are stable, are a kind of new to have ultralow damage
The microwave dielectric ceramic materials of consumption and excellent microwave dielectric property.
Claims (3)
1. a kind of ultra-low loss magnesium titanate lithium microwave dielectric ceramic materials, it is characterised in that：The chemical composition of the ceramic material is
Li2Mg3TiO6, its dielectric loss is that 0.000037~0.000048, Q × f is 123000~152000GHz, and dielectric constant is
14.5~15.5, temperature coefficient of resonance frequency is -42~-36ppm/ DEG C；It is prepared by following methods：
(1) batch mixing
According to Li2Mg3TiO6Stoichiometric proportion weigh material purity be more than 99.9% Li2CO3Powder, MgO powder, TiO2Powder, will
Raw material is fitted into ball grinder for 1: 2: 2 in mass ratio with zirconia ball, absolute ethyl alcohol, is sufficiently mixed ball milling 6~10 hours, 80~
100 DEG C of dryings；
(2) pre-burning
By step (1) dried mixture in 1000~1200 DEG C of pre-burnings 2~6 hours, pre-burning powder is prepared into；
(3) rerolling
Pre-burning powder and zirconia ball, absolute ethyl alcohol are fitted into ball grinder for 1: 2: 2 in mass ratio, ball milling 6~10 is sufficiently mixed
Hour, 80~100 DEG C of dryings；
(4) granulate, be molded
Mass fraction is added into the dried pre-burning powder of step (3) to granulate for 5% polyvinyl alcohol water solution, crosses 80~120
Mesh sieve, then it is pressed into cylindrical green body with powder compressing machine；
(5) sinter
The cylindrical green body that step (4) is obtained is sintered 2~10 hours at 1260~1340 DEG C, obtains ultra-low loss magnesium titanate lithium
Microwave dielectric ceramic materials.
2. ultra-low loss magnesium titanate lithium microwave dielectric ceramic materials according to claim 1, it is characterised in that：The step
(2) in, by step (1) dried mixture in 1000 DEG C of pre-burnings 4 hours.
3. ultra-low loss magnesium titanate lithium microwave dielectric ceramic materials according to claim 1, it is characterised in that：The step
(5) in, the cylindrical green body that step (4) is obtained is sintered 6 hours at 1280 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510066787.6A CN104692795B (en) | 2015-02-09 | 2015-02-09 | A kind of ultra-low loss magnesium titanate lithium microwave dielectric ceramic materials and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510066787.6A CN104692795B (en) | 2015-02-09 | 2015-02-09 | A kind of ultra-low loss magnesium titanate lithium microwave dielectric ceramic materials and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104692795A CN104692795A (en) | 2015-06-10 |
| CN104692795B true CN104692795B (en) | 2017-07-11 |
Family
ID=53340398
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510066787.6A Active CN104692795B (en) | 2015-02-09 | 2015-02-09 | A kind of ultra-low loss magnesium titanate lithium microwave dielectric ceramic materials and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104692795B (en) |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106083034A (en) * | 2016-06-13 | 2016-11-09 | 天津大学 | A kind of low-loss lithium magnesium titanium series microwave dielectric ceramic |
| CN106518051B (en) * | 2016-11-06 | 2019-07-23 | 桂林理工大学 | A kind of temperature-stabilized microwave medium ceramic material and preparation method thereof |
| CN107236544B (en) * | 2017-08-03 | 2019-04-09 | 广东工业大学 | A kind of red illuminating material and preparation method thereof |
| CN107352998B (en) * | 2017-09-04 | 2021-03-09 | 济南大学 | Ultralow-loss lithium-magnesium-titanium-based microwave dielectric ceramic and preparation method thereof |
| CN108314444A (en) * | 2018-03-12 | 2018-07-24 | 天津大学 | A kind of high q-factor rock salt class microwave dielectric material |
| CN110407576A (en) * | 2018-04-28 | 2019-11-05 | 中国科学院上海硅酸盐研究所 | A kind of low dielectric microwave media ceramic and preparation method thereof |
| CN109437887A (en) * | 2018-11-08 | 2019-03-08 | 天津大学 | A kind of anion substitution low temperature sintering lithium magnesium titanium series microwave dielectric ceramic |
| CN110218086A (en) * | 2019-05-08 | 2019-09-10 | 天津大学 | A kind of lithium-based ceramic material of microwave-medium substrate low dielectric constant and high Q value |
| CN111217603A (en) * | 2020-02-07 | 2020-06-02 | 天津大学 | high-Q-value low-temperature sintered lithium-magnesium-titanium dielectric material and preparation method thereof |
| CN114874005B (en) * | 2022-06-10 | 2023-01-13 | 安徽理工大学 | Temperature-stable magnesium titanate base microwave medium composite ceramic and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104058748A (en) * | 2014-06-30 | 2014-09-24 | 桂林理工大学 | Microwave dielectric ceramic LiMg2V3O10 allowing low-temperature sintering and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101786875B (en) * | 2010-01-02 | 2012-10-03 | 桂林理工大学 | Microwave medium ceramic material with low-temperature sintering spinel structure and preparation method thereof |
| CN102320825B (en) * | 2011-08-16 | 2013-04-10 | 广西新未来信息产业股份有限公司 | Low-temperature sintered microwave dielectric ceramic and sintering method thereof |
-
2015
- 2015-02-09 CN CN201510066787.6A patent/CN104692795B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104058748A (en) * | 2014-06-30 | 2014-09-24 | 桂林理工大学 | Microwave dielectric ceramic LiMg2V3O10 allowing low-temperature sintering and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104692795A (en) | 2015-06-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104692795B (en) | A kind of ultra-low loss magnesium titanate lithium microwave dielectric ceramic materials and preparation method thereof | |
| CN101260001A (en) | High-Q microwave dielectric ceramic material and preparing method thereof | |
| CN108249902B (en) | Silicate-based low-dielectric microwave dielectric ceramic and preparation method thereof | |
| CN108358632B (en) | Ultralow-temperature sintered high-Q x f-value microwave dielectric material and preparation method thereof | |
| CN102153343A (en) | Method for preparing high Q-value magnesium titanate base microwave medium ceramics by adopting reactive sintering method | |
| US11629102B2 (en) | Li3Mg2SbO6-based microwave dielectric ceramic material easy to sinter and with high q value, and preparation method therefor | |
| CN104671773B (en) | A kind of low dielectric constant microwave dielectric ceramic material and preparation method thereof | |
| CN110092655B (en) | Barium samarium-titanium series low-loss microwave dielectric ceramic and preparation method thereof | |
| CN102531571B (en) | High-Q-value medium-dielectric-constant microwave dielectric ceramic and preparation method thereof | |
| CN105036741A (en) | Microwave dielectric ceramic material high in quality factor and preparation method thereof | |
| CN103351155B (en) | Low temperature sintering silica based composite ceramic and preparation method thereof | |
| CN108358633A (en) | A kind of low-temperature sintering Ca5Mn4-xMgxV6O24Microwave dielectric material and preparation method thereof | |
| CN104710175B (en) | A kind of low-k magnesium zirconate lithium microwave dielectric ceramic materials and preparation method thereof | |
| CN103833351B (en) | Microwave dielectric ceramic and preparation method thereof | |
| CN109251028A (en) | A kind of low high Q lithium magnesium niobium series microwave dielectric ceramic and preparation method thereof that is situated between | |
| CN105060878A (en) | Microwave dielectric ceramic with low dielectric constant and high quality factor and preparation method thereof | |
| CN102093053A (en) | New microwave medium ceramic material prepared through middle-temperature sintering | |
| CN102491744A (en) | Low-loss microwave dielectric ceramic and preparation method thereof | |
| CN104692792B (en) | Low-temperature sintering temperature-stable stannate microwave dielectric ceramic materials | |
| CN102219515A (en) | Novel medium temperature sintered microwave dielectric ceramic material | |
| CN104987071A (en) | Low-temperature sintered microwave dielectric ceramic material with middle permittivity | |
| CN104944937A (en) | ZnAl2O4/Li4Ti5O12 microwave dielectric ceramic material and preparation method thereof | |
| CN109231982A (en) | A kind of preparation method of magnesium titanate base microwave medium ceramics | |
| CN104030685A (en) | High-Q-value microwave dielectric ceramic and preparation method thereof | |
| CN104876568B (en) | Vanadio temperature-stable ultralow temperature-sintered microwave dielectric ceramic material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |