CN104370544A - Temperature stable type microwave dielectric ceramic with ultra low dielectric constant capable of being sintered at low temperature and preparation method of temperature stable type microwave dielectric ceramic - Google Patents
Temperature stable type microwave dielectric ceramic with ultra low dielectric constant capable of being sintered at low temperature and preparation method of temperature stable type microwave dielectric ceramic Download PDFInfo
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- CN104370544A CN104370544A CN201410655379.XA CN201410655379A CN104370544A CN 104370544 A CN104370544 A CN 104370544A CN 201410655379 A CN201410655379 A CN 201410655379A CN 104370544 A CN104370544 A CN 104370544A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 12
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 6
- 238000000498 ball milling Methods 0.000 claims abstract description 6
- 239000011230 binding agent Substances 0.000 claims abstract description 6
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000009766 low-temperature sintering Methods 0.000 claims description 6
- 238000000748 compression moulding Methods 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 2
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 2
- 238000005469 granulation Methods 0.000 claims description 2
- 230000003179 granulation Effects 0.000 claims description 2
- 238000005245 sintering Methods 0.000 abstract description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 abstract 2
- 229910052681 coesite Inorganic materials 0.000 abstract 1
- 229910052906 cristobalite Inorganic materials 0.000 abstract 1
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 abstract 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 abstract 1
- 229910052808 lithium carbonate Inorganic materials 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 238000000465 moulding Methods 0.000 abstract 1
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 abstract 1
- 238000005453 pelletization Methods 0.000 abstract 1
- 238000003825 pressing Methods 0.000 abstract 1
- 239000000377 silicon dioxide Substances 0.000 abstract 1
- 235000012239 silicon dioxide Nutrition 0.000 abstract 1
- 229910052682 stishovite Inorganic materials 0.000 abstract 1
- 229910052905 tridymite Inorganic materials 0.000 abstract 1
- 238000005303 weighing Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 11
- 229910010293 ceramic material Inorganic materials 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 8
- 238000004891 communication Methods 0.000 description 6
- 238000011161 development Methods 0.000 description 6
- 229910010413 TiO 2 Inorganic materials 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 5
- 238000011160 research Methods 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000002131 composite material Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 229910000906 Bronze Inorganic materials 0.000 description 1
- 229910020068 MgAl Inorganic materials 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 229910052777 Praseodymium Inorganic materials 0.000 description 1
- 206010037660 Pyrexia Diseases 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000010974 bronze Substances 0.000 description 1
- 239000003985 ceramic capacitor Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002223 garnet Substances 0.000 description 1
- 239000002241 glass-ceramic Substances 0.000 description 1
- 230000001965 increasing effect Effects 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- XHGGEBRKUWZHEK-UHFFFAOYSA-L tellurate Chemical compound [O-][Te]([O-])(=O)=O XHGGEBRKUWZHEK-UHFFFAOYSA-L 0.000 description 1
- 230000035922 thirst Effects 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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- Inorganic Insulating Materials (AREA)
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Abstract
The invention discloses temperature stable type microwave dielectric ceramic with an ultra low dielectric constant capable of being sintered at a low temperature and a preparation method of the temperature stable type microwave dielectric ceramic. The preparation method comprises the specific steps: weighing and dosing original powder, with purity of 99.9% (in percentage by weight) of La2O3, Li2CO3, ZnO and SiO2 according to the composition of La3LiZnSi3O12; then, performing wet type ball-milling and mixing on the raw materials for 12 hours, and pre-sintering for 6 hours at 850 DEG C in an atmosphere, wherein a ball-milling medium is absolute ethyl alcohol; after adding a binder into the prepared powder and pelletizing, pressing and molding; and finally sintering for 4 hours at 900-940 DEG C in the atmosphere; the binder adopts a polyvinyl alcohol solution with mass concentration of 5%, and the adding amount of the polyvinyl alcohol accounts for 3% of the total mass of the powder. The ceramic prepared by the preparation method disclosed by the invention has good sintering performance at 900-940 DEG C, has a dielectric constant of 6.3-6.7, a quality factor Qf value as high as 87000-125000GHz, a small resonant frequency temperature coefficient, and an extremely great application value in industry.
Description
Technical field
The present invention relates to dielectric ceramic material, particularly relate to dielectric ceramic material of the microwave devices such as ceramic substrate, resonator and the wave filter used for the manufacture of microwave frequency and preparation method thereof.
Background technology
Microwave dielectric ceramic refers to and to be applied in microwave frequency band (mainly UHF and SHF frequency range) circuit as dielectric material and to complete the pottery of one or more functions, resonator is widely used as in modern communication, wave filter, the components and parts such as dielectric substrate and medium wave circuit, it is the key foundation material of modern communication technology, at portable mobile phone, automobile telephone, cordless telephone, there is very important application the aspects such as telestar susceptor and military radar, in the miniaturization of modern communication instrument, increasing effect is just being played in integrated process.
Be applied to the dielectric ceramic of microwave frequency band, the requirement of following dielectric characteristics should be met: (1) seriation DIELECTRIC CONSTANT ε
rto adapt to the requirement of different frequency and different application occasion; (2) high quality factor q value or dielectric loss tan δ to reduce noise, general requirement Qf>=3000GHz; (3) the temperature factor τ of resonant frequency
flittle of as far as possible to ensure the thermostability that device has had, general requirement-10ppm/ DEG C≤τ
f≤+10ppm/ DEG C.From late 1930s, just someone attempts dielectric substance to be applied to microwave technology in the world, and prepares TiO
2microwave dielectric filter, but its temperature coefficient of resonance frequency τ
ftoo greatly cannot be practical.Since the seventies in last century, start the large-scale development to medium ceramic material, according to relative permittivity ε
rsize from use frequency range different, usually the microwave-medium ceramics be developed and developing can be divided into 4 classes.
(1) ultralow dielectric microwave dielectric ceramic, main representative is Al
2o
3-TiO
2, Y
2baCuO
5, MgAl
2o
4and Mg
2siO
4deng, its ε
r≤ 20, quality factor q × f>=50000GHz, τ
f≤ 10ppm/ DEG C.Be mainly used in microwave base plate and high-end microwave device.
(2) low ε
rwith the microwave dielectric ceramic of high q-factor, mainly BaO-MgO-Ta
2o
5, BaO-ZnO-Ta
2o
5or BaO-MgO-Nb
2o
5, BaO-ZnO-Nb
2o
5system or the composite system MWDC material between them.Its ε
r=20 ~ 35, Q=(1 ~ 2) × 10
4(under f>=10GHz), τ
f≈ 0.Be mainly used in the microwave communication equipments such as the direct broadcasting satellite of f >=8GHz as dielectric resonance device.
(3) medium ε
rwith the microwave dielectric ceramic of Q value, mainly with BaTi
4o
9, Ba
2ti
9o
20(Zr, Sn) TiO
4deng the MWDC material for base, its ε
r=35 ~ 45, Q=(6 ~ 9) × 10
3(under f=3 ~-4GHz), τ
f≤ 5ppm/ DEG C.Be mainly used in microwave military radar in 4 ~ 8GHz range of frequency and communication system as dielectric resonance device.
(4) high ε
rand the microwave dielectric ceramic that Q value is lower, be mainly used in civilian mobile communcations system in 0.8 ~ 4GHz range of frequency, this is also the emphasis of microwave dielectric ceramic research.Since the eighties, the people such as Kolar, Kato in succession find and have studied perovskite-like tungsten bronze type BaO-Ln
2o
3-TiO
2series (Ln=La, Sm, Nd or Pr etc. are called for short BLT system), complex perovskite structure CaO-Li
2o-Ln
2o
3-TiO
2series, lead base series material, Ca
1-xln
2x/3tiO
3be contour ε
rmicrowave dielectric ceramic, the wherein BaO-Nd of BLT system
2o
3-TiO
2material dielectric constant reaches 90, lead base series (Pb, Ca) ZrO
3specific inductivity reaches 105.
The sintering temperature of these material systems is generally higher than 1300 DEG C above, can not directly and the low melting point metal such as Ag and Cu burn formation laminated ceramic capacitor altogether.In recent years, along with LTCC Technology (Low Temperature Co-firedCeramics, the requirement of development LTCC) and the development of microwave multilayer device, researchist both domestic and external has carried out exploring widely and studying to some low fever's system materials, mainly adopt devitrified glass or glassceramic composites system, because low melting glass has relatively high dielectric loss mutually, the existence of glassy phase substantially increases the dielectric loss of material.Therefore development is the emphasis of current research without the low fired microwave dielectric ceramic material of glassy phase.
Can in the process of low fired microwave dielectric ceramic materials in exploration and development of new, the material systems such as the Li based compound that intrinsic sintering temperature is low, Bi based compound, tungstate architecture compound and tellurate architecture compound get the attention and research, but due to three performance index (ε of microwave dielectric ceramic
rwith Qf and τ
f) between be that the relation of mutually restriction is (see document: the restricting relation between microwave dielectric ceramic materials dielectric properties, Zhu Jianhua, Liang Fei, Wang little Hong, Lv Wenzhong, electronic component and material, phase March the 3rd in 2005), meet three performance requriementss and the single-phase microwave-medium ceramics of low temperature sintering is considerably less, mainly their temperature coefficient of resonance frequency is usually excessive or quality factor are on the low side and cannot application request.Current is the summary of experience drawn by great many of experiments to the research major part of microwave-medium ceramics, but complete theory is not had to set forth the relation of microtexture and dielectric properties, therefore, in theory also cannot predict its microwave dielectric property such as temperature coefficient of resonance frequency and quality factor from the composition of compound and structure, which greatly limits the development of low temperature co-fired technology and microwave multilayer device.Explore and low-temperature sintering can have near-zero resonance frequency temperature coefficient (-10ppm/ DEG C≤τ with exploitation simultaneously
f≤+10ppm/ DEG C) be that those skilled in the art thirst for solving always but are difficult to the difficult problem that succeeds all the time with the microwave dielectric ceramic of higher figure of merit.
Summary of the invention
The object of this invention is to provide and a kind of there is good thermostability and low-loss, simultaneously low temperature sintering ultralow dielectric microwave dielectric ceramic material and preparation method thereof.
The chemical constitution of microwave dielectric ceramic material of the present invention is La
3liZnSi
3o
12.
Preparation method's step of this microwave dielectric ceramic material is:
(1) by purity be the La of more than 99.9% (weight percent)
2o
3, Li
2cO
3, ZnO and SiO
2starting powder press La
3liZnSi
3o
12composition weigh batching.
(2) step (1) raw material wet ball-milling is mixed 12 hours, ball-milling medium is dehydrated alcohol, pre-burning 6 hours in 850 DEG C of air atmosphere after oven dry.
(3) in the powder that step (2) is obtained, binding agent is added and after granulation, then compression moulding, finally in 900 ~ 940 DEG C of air atmosphere, sinter 4 hours; Described binding agent adopts mass concentration to be the polyvinyl alcohol solution of 5%, and polyvinyl alcohol addition accounts for 3% of powder total mass.
Advantage of the present invention: La
3liZnSi
3o
12ceramic sintering temperature is low, and raw materials cost is low; Specific inductivity reaches specific inductivity and reaches 6.3 ~ 6.7, the temperature factor τ of its resonant frequency
flittle, temperature stability is good; Its quality factor q f value is up to 87000-125000GHz, the manufacture of the microwave devices such as various medium substrate, resonator and wave filter can be widely used in, the technology needs of low temperature co-fired technology and microwave multilayer device can be met, industrially have great using value.
Embodiment
Table 1 shows 3 specific embodiments and microwave dielectric property thereof that form different sintering temperature of the present invention.Its preparation method is described above, carries out the evaluation of microwave dielectric property by cylindrical dielectric resonator method.By La
3liZnSi
3o
12powder mixes with the Ag powder accounting for powder quality 20%, after compression moulding, at 940 DEG C, sinter 4 hours; X-ray diffraction material phase analysis and scanning electron microscopic observation all show the La of Ag and cubic garnet structure
3liZnSi
3o
12not there is not chemical reaction, i.e. La
3liZnSi
3o
12can be low temperature co-fired with Ag electrode.
This pottery can be widely used in the manufacture of the microwave devices such as various medium substrate, resonator and wave filter, can meet the technology needs of the system such as mobile communication and satellite communications.
Table 1:
Claims (2)
1. a low temperature sintering temperature-stable ultralow dielectric microwave dielectric ceramic, is characterized in that the chemical constitution of described microwave dielectric ceramic is: La
3liZnSi
3o
12.
2. a preparation method for low temperature sintering temperature-stable ultralow dielectric microwave dielectric ceramic, concrete steps are:
(1) be 99.9%(weight percent by purity) more than La
2o
3, Li
2cO
3, ZnO and SiO
2starting powder press La
3liZnSi
3o
12composition weigh batching;
(2) step (1) raw material wet ball-milling is mixed 12 hours, ball-milling medium is dehydrated alcohol, pre-burning 6 hours in 850 DEG C of air atmosphere after oven dry;
(3) in the powder that step (2) is obtained, binding agent is added and after granulation, then compression moulding, finally in 900 ~ 940 DEG C of air atmosphere, sinter 4 hours; Described binding agent adopts mass concentration to be the polyvinyl alcohol solution of 5%, and polyvinyl alcohol addition accounts for 3% of powder total mass.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105777121A (en) * | 2016-02-17 | 2016-07-20 | 桂林理工大学 | High-quality-factor ultra-low-dielectric constant microwave dielectric ceramic Zn3Sm2Ge3O12 and preparing method thereof |
| CN111925197A (en) * | 2020-07-21 | 2020-11-13 | 深圳顺络电子股份有限公司 | Microwave dielectric ceramic material and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103496959A (en) * | 2013-09-23 | 2014-01-08 | 桂林理工大学 | Low-temperature sintering microwave dielectric ceramic Li2Ca2Si2O7 and preparation method thereof |
| CN103922737A (en) * | 2014-04-06 | 2014-07-16 | 桂林理工大学 | Low-temperature sintered microwave dielectric ceramic Li3Nb3Si2O13 and preparation method thereof |
| CN104003723A (en) * | 2014-05-24 | 2014-08-27 | 桂林理工大学 | Microwave dielectric ceramic Li3Zn4NbO8 capable of realizing low-temperature sintering and preparation method thereof |
-
2014
- 2014-11-18 CN CN201410655379.XA patent/CN104370544B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103496959A (en) * | 2013-09-23 | 2014-01-08 | 桂林理工大学 | Low-temperature sintering microwave dielectric ceramic Li2Ca2Si2O7 and preparation method thereof |
| CN103922737A (en) * | 2014-04-06 | 2014-07-16 | 桂林理工大学 | Low-temperature sintered microwave dielectric ceramic Li3Nb3Si2O13 and preparation method thereof |
| CN104003723A (en) * | 2014-05-24 | 2014-08-27 | 桂林理工大学 | Microwave dielectric ceramic Li3Zn4NbO8 capable of realizing low-temperature sintering and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| GANG DOU ET AL: "Low temperature sintering and microwave dielectric properties of Li2ZnSiO4 ceramics with ZB glass", 《J MATER SCI: MATER ELECTRON》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105777121A (en) * | 2016-02-17 | 2016-07-20 | 桂林理工大学 | High-quality-factor ultra-low-dielectric constant microwave dielectric ceramic Zn3Sm2Ge3O12 and preparing method thereof |
| CN111925197A (en) * | 2020-07-21 | 2020-11-13 | 深圳顺络电子股份有限公司 | Microwave dielectric ceramic material and preparation method thereof |
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| CN104370544B (en) | 2016-03-23 |
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Effective date of registration: 20231225 Address after: No. 23, Wangcheng Road, Yaojiadian Town, Yidu City, Yichang City, Hubei Province 443399 Patentee after: YIDU BOTONG ELECTRONIC Co.,Ltd. Address before: 443002 No. 8, University Road, Yichang, Hubei Patentee before: CHINA THREE GORGES University |
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