CN108395234A - Sintered at ultra low temperature, ultralow dielectric microwave dielectric material and preparation method thereof - Google Patents
Sintered at ultra low temperature, ultralow dielectric microwave dielectric material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of sintered at ultra low temperature, ultralow dielectric microwave dielectric material and preparation method thereof.By LiAlB2O5Molecular formula dispensing mixes 4h using wet grinding, then dries, is sieved, briquetting, rises to 600 DEG C of 4 h of heat preservation by room temperature, LiAlB is made2O5Pre-burning block, is added absolute ethyl alcohol and zirconium ball, 4 h of ball milling, and LiAlB is made in drying2O5Powder；By CaTiO3Molecular formula dispensing mixes 4h using wet grinding, then dries, is sieved, briquetting, rises to 1100 DEG C of heat preservation 4h by room temperature, CaTiO is made3Pre-burning block, adds absolute ethyl alcohol and zirconium ball, ball milling 4h, and CaTiO is made in drying3Two kinds of powders are pressed LiAlB by powder2O5‑xCaTiO3Weighing batch mixing is carried out, ball milling 4h is dried, and is granulated, and small column, dumping are pressed into, and sintering obtains sintered at ultra low temperature, ultralow dielectric microwave dielectric material.
Description
Technical field
The invention belongs to electronic ceramics and its manufacturing field, more particularly to a kind of sintered at ultra low temperature, ultralow dielectric are micro-
Wave dielectric material and preparation method thereof.The microwave dielectric material can be used in the medium substrate used in microwave frequency, antenna and
The microwave devices such as resonator.
Background technology
Microwave dielectric material refers to being applied to microwave frequency band（300MHz~300GHz）It is used as medium in circuit and completes one kind
Or the ceramics of multiple functions, mainly for the preparation of microwave devices such as resonator, filter, diectric antenna, medium wave circuits.
In recent years, as microwave mobile communication technology constantly develops to cost effective and digitlization direction, component module is wanted
Ask also more and more urgent.LTCC Technology（LTCC, Low Temperature Co-fired Ceramics）It is excellent with its
Different electricity, machinery, calorifics and operational characteristic, has become one of major technique of electronic-component module.LTCC technology is wanted
Ask microwave dielectric material with excellent microwave dielectric property（HighQ×fValue, moderate dielectric constant, nearly zeroτ f Value）
While also to have low sintering temperature and with the good chemical compatibility of electrodes in base metal such as silver.Most of commercial at present
Microwave dielectric material although there is excellent microwave dielectric property, its sintering temperature is higher（≥1100℃）.High burning
Junction temperature not only increases production cost, and cannot can not be applied on LTCC devices with Ag electrode cofirings, affect its
Commercial large-scale application.Therefore the research and development low temperature co-fired LTCC microwave dielectric ceramic materials of novel high-performance are of far-reaching significance.
Invention content
The object of the present invention is to provide a kind of sintered at ultra low temperature, ultralow dielectric microwave dielectric material and its preparation sides
Method.
Thinking of the present invention：LiAlB is designed first2O5Sintering temperature and low LTCC microwave dielectric materials.On this basis, it adds
A small amount of CaTiO3To adjust LiAlB2O5Basis materialτ f Value, to obtain a kind of sintering temperature and low, have excellent performance it is novel
Low temperature co-fired LTCC microwave dielectric ceramic materials.
The sintered at ultra low temperature of the present invention, the chemical constitution formula of ultralow dielectric microwave dielectric material are LiAlB2O5-xCaTiO3(0≤x≤ 15%), whereinxFor mass fraction.
Prepare above-mentioned sintered at ultra low temperature, ultralow dielectric microwave dielectric material the specific steps are：
(1) with the Li of purity >=99%2CO3、Al2O3And H3BO3For primary raw material, by LiAlB2O5Molecular formula dispensing, according to nothing
Water-ethanol:Powder:The mass ratio of zirconium ball is 1:1:2 absolute ethyl alcohol and zirconium ball are added into powder, mix 4h using wet grinding, so
It is dried at 110 ~ 120 DEG C afterwards, is sieved with the sieve of 80 mesh, block stock is pressed into after sieving, finally with the heating of 5 DEG C/min
The block stock of compacting is risen to 600 DEG C by room temperature and keeps the temperature 4 h at this temperature by rate, and LiAlB is made2O5Pre-burning block.
(2) by LiAlB made from step (1)2O5Pre-burning block is ground into powder, respectively according to absolute ethyl alcohol:Powder:Zirconium
The mass ratio of ball is 1:1:2 absolute ethyl alcohol and zirconium ball are added into powder, are put into nylon tank and are taken out after 4 h of ball milling, are placed in baking
It is dried at 110 ~ 120 DEG C in stove, LiAlB is made2O5Powder.
(3) with the CaCO of purity >=99%3And TiO2For primary raw material, by CaTiO3Molecular formula dispensing, according to anhydrous second
Alcohol:Powder:The mass ratio of zirconium ball is 1:1:2 absolute ethyl alcohol and zirconium ball are added into powder, mix 4h using wet grinding, then exist
It is dried at 110 ~ 120 DEG C, is sieved with the sieve of 80 mesh, block stock is pressed into after sieving, finally with the heating rate of 5 DEG C/min
The block stock of compacting is risen to 1100 DEG C by room temperature and keeps the temperature 4h at this temperature, CaTiO is made3(CT) pre-burning block.
(4) by CaTiO made from step (3)3Pre-burning block crushes, respectively according to absolute ethyl alcohol:Powder:The matter of zirconium ball
Amount is than being 1:1:2 absolute ethyl alcohol and zirconium ball are added into powder, are put into nylon tank and are taken out after ball milling 4h, are placed in baker
It is dried at 110 ~ 120 DEG C, CaTiO is made3Powder.
(5) LiAlB obtained with step (2)2O5The CaTiO that powder and step (4) obtain3Powder is raw material, is pressed
LiAlB2O5-xCaTiO3(0≤x≤ 15%) it is weighed, then batch mixing；Respectively according to absolute ethyl alcohol:Powder:The quality of zirconium ball
Than being 1:1:Absolute ethyl alcohol and zirconium ball are added into powder for 2 ratio, are put into nylon tank and are taken out after ball milling 4h, are placed in baker
It is dried at 110 ~ 120 DEG C, powder is made.
(6) a diameter of 12mm will be pressed into after granulation for powders made from step (5), thickness is the small column of 4 ~ 6mm, in
Dumping 4h at 500 ~ 600 DEG C obtains porcelain, then porcelain is sintered 4h at 650 ~ 750 DEG C after furnace cooling, obtain ultralow temperature
Sintering, ultralow dielectric microwave dielectric material.
The method of the present invention is easy to operate, and the microwave-medium ceramics prepared, sintering temperature are low（≤750℃）, microwave
It can be excellent：Dielectric constant is low（ε r ）,Q×fValue height and τ f It is worth nearly zero；Wherein LiAlB2O5-15%CaTiO3Component is in low temperature 675
Sintering has preferable performance at DEG C（ε r ~3.66, Q × f∼18,412 GHz, τ f ~ -2.7 ppm/°C）, can be used for humorous
It shakes the manufactures of the microwave devices such as device, antenna, filter.
Specific implementation mode
Embodiment 1:
(1) with the Li of purity >=99%2CO3、Al2O3And H3BO3For primary raw material, by LiAlB2O5Molecular formula dispensing, according to nothing
Water-ethanol:Powder:The mass ratio of zirconium ball is 1:1:2 absolute ethyl alcohol and zirconium ball are added into powder, mix 4h using wet grinding, so
It is dried at 115 DEG C afterwards, is sieved with the sieve of 80 mesh, block stock is pressed into after sieving, finally with the heating rate of 5 DEG C/min
The block stock of compacting is risen to 600 DEG C by room temperature and keeps the temperature 4 h at this temperature, LiAlB is made2O5Pre-burning block.
(2) by LiAlB made from step (1)2O5Pre-burning block is ground into powder, respectively according to absolute ethyl alcohol:Powder:Zirconium
The mass ratio of ball is 1:1:2 absolute ethyl alcohol and zirconium ball are added into powder, are put into nylon tank and are taken out after 4 h of ball milling, are placed in baking
It is dried at 115 DEG C in stove, LiAlB is made2O5Powder.
(3) with the CaCO of purity >=99%3And TiO2For primary raw material, by CaTiO3Molecular formula dispensing, according to anhydrous second
Alcohol:Powder:The mass ratio of zirconium ball is 1:1:2 absolute ethyl alcohol and zirconium ball are added into powder, mix 4h using wet grinding, then exist
It is dried at 115 DEG C, is sieved with the sieve of 80 mesh, block stock is pressed into after sieving, will finally pressed with the heating rate of 5 DEG C/min
The block stock of system rises to 1100 DEG C by room temperature and keeps the temperature 4h at this temperature, and CaTiO is made3Pre-burning block.
(4) by CaTiO made from step (3)3Pre-burning block crushes, respectively according to absolute ethyl alcohol:Powder:The matter of zirconium ball
Amount is than being 1:1:2 absolute ethyl alcohol and zirconium ball are added into powder, are put into nylon tank and are taken out after ball milling 4h, are placed in baker
It is dried at 115 DEG C, CaTiO is made3Powder.
(5) LiAlB obtained with step (2)2O5The CaTiO that powder and step (4) obtain3Powder is raw material, is pressed
LiAlB2O5-xCaTiO3(x=0) it is weighed, then batch mixing；Respectively according to absolute ethyl alcohol:Powder:The mass ratio of zirconium ball is 1:
1:Absolute ethyl alcohol and zirconium ball are added into powder for 2 ratio, are put into nylon tank and are taken out after ball milling 4h, are placed in baker 115
It is dried at DEG C, powder is made.
(6) a diameter of 12mm will be pressed into after granulation for powders made from step (5), thickness is the small column of 5mm, in 550
Dumping 4h at DEG C obtains porcelain, then porcelain is sintered 4h at 675 DEG C after furnace cooling, obtain sintered at ultra low temperature, ultralow Jie
Electric constant microwave dielectric material.
Embodiment 2 ~ 13：
In addition to will be in step (5)xOther than sintering temperature in value and step (6) in table 1 according to being adjusted, embodiment 2 ~ 13
Preparation process with embodiment 1, specificallyxValue and sintering temperature are shown in Table 1.Embodiment 1 ~ 13 is made with cylindrical dielectric resonator method
Microwave dielectric material carry out the evaluation of microwave dielectric property, concrete outcome is shown in Table 1.
From experimental data it can be seen that this ceramics can be widely used for the microwave electrons such as various medium substrates, antenna and filter
The manufacture of component meets the technology needs of Modern Mobile Communications Systems.
The design parameter of 1 embodiment 1 ~ 13 of table
Claims (2)
1. a kind of sintered at ultra low temperature, ultralow dielectric microwave dielectric material, it is characterised in that the sintered at ultra low temperature, ultralow dielectric
The chemical constitution formula of constant microwave dielectric material is LiAlB2O5-xCaTiO3, whereinxFor mass fraction, and 0≤x≤15%。
2. the preparation method of a kind of sintered at ultra low temperature as described in claim 1, ultralow dielectric microwave dielectric material, special
Sign be the specific steps are：
(1) with the Li of purity >=99%2CO3、Al2O3And H3BO3For primary raw material, by LiAlB2O5Molecular formula dispensing, according to anhydrous
Ethyl alcohol:Powder:The mass ratio of zirconium ball is 1:1:2 absolute ethyl alcohol and zirconium ball are added into powder, mix 4h using wet grinding, then
It is dried at 110 ~ 120 DEG C, is sieved with the sieve of 80 mesh, block stock is pressed into after sieving, finally with the heating of 5 DEG C/min speed
The block stock of compacting is risen to 600 DEG C by room temperature and keeps the temperature 4 h at this temperature by rate, and LiAlB is made2O5Pre-burning block；
(2) by LiAlB made from step (1)2O5Pre-burning block is ground into powder, respectively according to absolute ethyl alcohol:Powder:Zirconium ball
Mass ratio is 1:1:2 absolute ethyl alcohol and zirconium ball are added into powder, are put into nylon tank and are taken out after 4 h of ball milling, are placed in baker
It is dried at 110 ~ 120 DEG C, LiAlB is made2O5Powder；
(3) with the CaCO of purity >=99%3And TiO2For primary raw material, by CaTiO3Molecular formula dispensing, according to absolute ethyl alcohol:Powder
Body:The mass ratio of zirconium ball is 1:1:2 absolute ethyl alcohol and zirconium ball are added into powder, and 4h is mixed using wet grinding, then 110 ~
It is dried at 120 DEG C, is sieved with the sieve of 80 mesh, block stock is pressed into after sieving, will finally pressed with the heating rate of 5 DEG C/min
The block stock of system rises to 1100 DEG C by room temperature and keeps the temperature 4h at this temperature, and CaTiO is made3Pre-burning block；
(4) by CaTiO made from step (3)3Pre-burning block crushes, respectively according to absolute ethyl alcohol:Powder:The mass ratio of zirconium ball is
1:1:2 absolute ethyl alcohol and zirconium ball are added into powder, are put into nylon tank and are taken out after ball milling 4h, are placed in baker 110 ~ 120
It is dried at DEG C, CaTiO is made3Powder；
(5) LiAlB obtained with step (2)2O5The CaTiO that powder and step (4) obtain3Powder is raw material, by LiAlB2O5-xCaTiO3Weighing batch mixing is carried out, wherein 0≤x≤15%；Respectively according to absolute ethyl alcohol:Powder:The mass ratio of zirconium ball is 1:1:2
Ratio absolute ethyl alcohol and zirconium ball are added into powder, be put into nylon tank and taken out after ball milling 4h, is placed in baker 110 ~ 120
It is dried at DEG C, powder is made；
(6) a diameter of 12mm will be pressed into after granulation for powders made from step (5), thickness is the small column of 4 ~ 6mm, in 500 ~
Dumping 4h at 600 DEG C obtains porcelain, then porcelain is sintered 4h at 650 ~ 750 DEG C after furnace cooling, obtain ultralow temperature burning
Knot, ultralow dielectric microwave dielectric material.
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Citations (7)
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|---|---|---|---|---|
| EP0312923A1 (en) * | 1987-10-19 | 1989-04-26 | Tam Ceramics, Inc. | Low-firing dielectric composition |
| CN102417350A (en) * | 2011-09-03 | 2012-04-18 | 桂林理工大学 | Temperature-stable low-cost microwave dielectric ceramic material and preparation method thereof |
| CN102424579A (en) * | 2011-09-03 | 2012-04-25 | 桂林理工大学 | Microwave dielectric ceramic material with low intrinsic sintering temperature and preparation method thereof |
| CN104446379A (en) * | 2014-12-27 | 2015-03-25 | 桂林理工大学 | Temperature-stable microwave dielectric ceramics with ultralow dielectric constant and preparation method thereof |
| CN104478409A (en) * | 2014-12-02 | 2015-04-01 | 桂林理工大学 | Temperature-stabilized microwave dielectric ceramic Li2AlB3O7 and preparation method thereof |
| CN104557019A (en) * | 2014-12-27 | 2015-04-29 | 桂林理工大学 | Ultralow sintering temperature stable type microwave dielectric ceramic LiBiB2O5 and preparation method thereof |
| CN107253856A (en) * | 2017-06-26 | 2017-10-17 | 桂林理工大学 | A kind of microwave dielectric material of near-zero resonance frequency temperature coefficient and preparation method thereof |
-
2018
- 2018-02-05 CN CN201810109585.9A patent/CN108395234A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0312923A1 (en) * | 1987-10-19 | 1989-04-26 | Tam Ceramics, Inc. | Low-firing dielectric composition |
| CN102417350A (en) * | 2011-09-03 | 2012-04-18 | 桂林理工大学 | Temperature-stable low-cost microwave dielectric ceramic material and preparation method thereof |
| CN102424579A (en) * | 2011-09-03 | 2012-04-25 | 桂林理工大学 | Microwave dielectric ceramic material with low intrinsic sintering temperature and preparation method thereof |
| CN104478409A (en) * | 2014-12-02 | 2015-04-01 | 桂林理工大学 | Temperature-stabilized microwave dielectric ceramic Li2AlB3O7 and preparation method thereof |
| CN104446379A (en) * | 2014-12-27 | 2015-03-25 | 桂林理工大学 | Temperature-stable microwave dielectric ceramics with ultralow dielectric constant and preparation method thereof |
| CN104557019A (en) * | 2014-12-27 | 2015-04-29 | 桂林理工大学 | Ultralow sintering temperature stable type microwave dielectric ceramic LiBiB2O5 and preparation method thereof |
| CN107253856A (en) * | 2017-06-26 | 2017-10-17 | 桂林理工大学 | A kind of microwave dielectric material of near-zero resonance frequency temperature coefficient and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| M. HE ET AL.: "Ab Initio Structure Determination of New Compound LiAlB2O5", 《JOURNAL OF SOLID STATE CHEMISTRY》 * |
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Application publication date: 20180814 |