CN103553608A - Low-temperature sinterable microwave dielectric ceramic LiSmNb2O7 and its preparation method - Google Patents
Low-temperature sinterable microwave dielectric ceramic LiSmNb2O7 and its preparation method Download PDFInfo
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- CN103553608A CN103553608A CN201310510722.7A CN201310510722A CN103553608A CN 103553608 A CN103553608 A CN 103553608A CN 201310510722 A CN201310510722 A CN 201310510722A CN 103553608 A CN103553608 A CN 103553608A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 12
- 239000000126 substance Substances 0.000 claims abstract description 7
- 239000011230 binding agent Substances 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 3
- 239000012153 distilled water Substances 0.000 claims abstract description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims abstract 3
- 239000008187 granular material Substances 0.000 claims abstract 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000005245 sintering Methods 0.000 description 11
- 239000000463 material Substances 0.000 description 9
- 238000004891 communication Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 229910010413 TiO 2 Inorganic materials 0.000 description 4
- 229910052797 bismuth Inorganic materials 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000000748 compression moulding Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 229910052714 tellurium Inorganic materials 0.000 description 2
- 229910015808 BaTe Inorganic materials 0.000 description 1
- 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
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000000498 ball milling 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
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 230000001965 increasing effect Effects 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 229910052718 tin Inorganic materials 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
- 229910052725 zinc Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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Abstract
本发明公开了一种可低温烧结的微波介电陶瓷LiSmNb2O7及其制备方法。可低温烧结的微波介电陶瓷的化学组成为LiSmNb2O7。（1）将分析纯的Li2CO3、Sm2O3和Nb2O5的原始粉末按LiSmNb2O7化学式称量配料。（2）将步骤（1）原料与蒸馏水混合湿式球磨12小时，烘干后在850℃大气气氛中预烧6小时。（3）在步骤（2）制得的粉末中添加粘结剂并造粒后，再压制成型，最后在900~930℃大气气氛中烧结4小时；所述的粘结剂采用质量浓度为5%的聚乙烯醇溶液，剂量占粉末总质量的3%。本发明制备的陶瓷在900~930℃烧结良好，其介电常数达到31～32，品质因数Qf值高达74000-88000GHz，谐振频率温度系数小，在工业上有着极大的应用价值。The invention discloses a low-temperature sinterable microwave dielectric ceramic LiSmNb 2 O 7 and a preparation method thereof. The chemical composition of low-temperature sinterable microwave dielectric ceramics is LiSmNb 2 O 7 . (1) The original powders of analytically pure Li 2 CO 3 , Sm 2 O 3 and Nb 2 O 5 were weighed and dosed according to the chemical formula of LiSmNb 2 O 7 . (2) Mix the raw materials in step (1) with distilled water and wet ball mill for 12 hours, dry them and pre-fire them in an atmosphere at 850°C for 6 hours. (3) Add a binder to the powder prepared in step (2) and granulate it, then press it into shape, and finally sinter it in the atmosphere at 900-930°C for 4 hours; the binder is used at a mass concentration of 5 % polyvinyl alcohol solution, the dosage accounts for 3% of the total mass of the powder. The ceramic prepared by the invention is well sintered at 900-930 DEG C, its dielectric constant reaches 31-32, its quality factor Qf value is as high as 74000-88000 GHz, the temperature coefficient of resonance frequency is small, and it has great application value in industry.
Description
Technical field
The present invention relates to dielectric ceramic, particularly relate to microwave dielectric ceramic of the microwave devices such as medium substrate, resonator and wave filter that use in microwave frequency and preparation method thereof.
Background technology
Microwave dielectric ceramic refers to and is applied in microwave frequency band (being mainly UHF, SHF frequency range) circuit as dielectric material and completes the pottery of one or more functions, in modern communication, be widely used as the components and parts such as resonator, wave filter, dielectric substrate and medium guided wave loop, it is the key foundation material of modern communication technology, at aspects such as portable mobile phone, automobile telephone, cordless telephone, telestar susceptor and military radars, there is very important application, in the miniaturization of modern communication instrument, integrated process, just bringing into play increasing effect.
Be applied to the dielectric ceramic of microwave frequency band, should meet the requirement of following dielectric characteristics: (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 are to reduce noise, general requirement Qf>=3000 GHz; (3) the temperature factor τ of resonant frequency
?the as far as possible little thermostability to guarantee that device has had, general requirement-10/ ℃≤τ
?≤+10 ppm/ ℃.From late 1930s, just someone attempts dielectric substance to be applied to microwave technology in the world.
According to relative permittivity ε
rsize from use the different of frequency range, conventionally the microwave dielectric ceramic being developed He 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
?≤ 10 ppm/ ° C.Be mainly used in microwave base plate and high-end microwave device.
(2) low ε
rwith the microwave dielectric ceramic of high Q value, be 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=25～30, Q=(1～2) * 10
4(under the GHz of f>=10), τ
?≈ 0.Be mainly used in the microwave communication equipments such as direct broadcasting satellite of f >=8 GHz as dielectric resonance device.
(3) medium ε
rwith the microwave dielectric ceramic of Q value, be mainly with BaTi
4o
9, Ba
2ti
9o
20(Zr, Sn) TiO
4deng the MWDC material that is base, its ε
r=35 ~ 40, Q=(6～9) * 10
3(under f=3～-4GHz), τ
?≤ 5 ppm/ ° C.Be mainly used in microwave military radar in 4～8 GHz range of frequency and communication system as dielectric resonance device.
(4) high ε
rand the lower microwave dielectric ceramic of Q value is 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 find and have studied perovskite-like tungsten bronze type BaO-Ln in succession
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 ° of C above, can not be directly and the low melting point metal such as Ag and Cu burn altogether formation laminated ceramic capacitor.In recent years, along with device miniaturization and integrated development, microwave-medium ceramics need to burn acquisition chip multilayer structure compared with the low Ag of the metals such as Au, Pd or Cu electrode (fusing point is respectively 961 ℃ and 1042 ℃) altogether with cost, the microwave dielectric property that this just requires material not only to have, and its sintering temperature will be lower than the fusing point of Cu, Ag.The low novel material system of intrinsic sintering temperature of exploring is at present mainly containing Bi
2o
3, Li
2o, TeO
2, V
2o
5deng the multicomponent composite oxide of low-melting component, comprising Bi
2o
3-ZnO-Nb
2o
5system pyrochlore-type compound, BiNbO
4, Bi
2mo
2o
9, Bi
2w
2o
9, Bi
3sbO
7deng Bi sill; Li
1+x-ym
1-x-3yti
x+4yo
3(M=Nb, Ta), Ca (Li
1/3nb
2/3) O
3-&, Li
2tiO
3, Li
3nbO
4, Li
2mgSiO
4, Li
2mgTiO
4, Li
2(M
2+)
2mo
3o
12, Li
3(M
3+) Mo
3o
12li sills such as (M=Zn, Ca, Al, In); BaTe
4o
9, Zn
2te
3o
8, BaTiTe
3o
9deng Te sill.
Due to easy and Ag electrode generation surface reaction and raw material TeO containing compounds such as Bi, Te, Mo
2poisonous the application of these Bi, Te, Mo sill is restricted.We are to consisting of LiSmNb
2o
7pottery carried out sintering characteristic and Study on microwave dielectric property, found that such pottery have excellent comprehensive microwave dielectric property simultaneously sintering temperature lower than 930
°c, can realize low temperature co-fired with Ag, can be widely used in the manufacture of the microwave devices such as various resonators and wave filter, can meet the needs of low temperature co-fired technology and microwave multilayer device.
Summary of the invention
The object of this invention is to provide a kind of have low-loss and good thermostability, simultaneously the low microwave dielectric ceramic of sintering temperature.
The chemical constitution formula of microwave dielectric ceramic of the present invention is: LiSmNb
2o
7.
Preparation method's concrete steps of described microwave dielectric ceramic are:
(1) by analytically pure Li
2cO
3, Sm
2o
3and Nb
2o
5starting powder press LiSmNb
2o
7chemical formula weigh batching.
(2) after will step (1) raw material mixing, add distilled water wet ball-milling 12 hours, pre-burning 6 hours in 850 ℃ of air atmosphere after oven dry.
(3) in the powder making in step (2), add after binding agent granulation, then compression moulding, finally sintering 4 hours in 900 ~ 930 ℃ of air atmosphere; Described binding agent adopts the polyvinyl alcohol solution that mass concentration is 5%, and dosage accounts for 3% of powder total mass.
Therefore pottery prepared by the present invention is good at 900 ~ 930 ℃ of sintering, and its specific inductivity reaches 31～32, and quality factor q f value is up to 74000-88000GHz, and temperature coefficient of resonance frequency is little, has a great using value industrial.
Embodiment
Embodiment:
Table 1 shows 4 specific embodiments and the microwave dielectric property thereof that forms different sintering temperatures of the present invention.Its preparation method as mentioned above, carries out the evaluation of microwave dielectric property by cylindrical dielectric resonator method; By LiSmNb
2o
7powder mixes with the Ag powder that accounts for powder quality 20%, after compression moulding, at 930 ℃, sintering is 4 hours; X ray diffraction material phase analysis and scanning electron microscopic observation all show LiSmNb
2o
7there is not chemical reaction, i.e. LiSmNb with Ag
2o
7can be low temperature co-fired with Ag electrode.
The present invention is never limited to above embodiment.The bound of sintering temperature, interval value can realize the present invention, at this, do not enumerate embodiment.
This pottery can be widely used in the manufacture of the microwave devices such as various medium substrates, resonator and wave filter, can meet the Technology Need of the systems such as mobile communication, satellite communications.
Table 1:
Claims (1)
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310510722.7A CN103553608A (en) | 2013-10-27 | 2013-10-27 | Low-temperature sinterable microwave dielectric ceramic LiSmNb2O7 and its preparation method |
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| CN201310510722.7A CN103553608A (en) | 2013-10-27 | 2013-10-27 | Low-temperature sinterable microwave dielectric ceramic LiSmNb2O7 and its preparation method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104399449A (en) * | 2014-11-21 | 2015-03-11 | 桂林理工大学 | Visible light responsive photocatalyst Li2GaB3O7 and its preparation method |
| CN104628384A (en) * | 2015-02-28 | 2015-05-20 | 桂林理工大学 | Low Loss Temperature Stable Medium Permittivity Microwave Dielectric Ceramic LiBi2NbO6 |
| CN104667905A (en) * | 2015-02-28 | 2015-06-03 | 桂林理工大学 | Visible light responsive photocatalyst LiSm2NbO6 and its preparation method |
| CN105174958A (en) * | 2015-10-09 | 2015-12-23 | 桂林理工大学 | Intermediate permittivity microwave dielectric ceramic Li4La3Nb3O14 and its preparation method |
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| CN1524792A (en) * | 2003-02-28 | 2004-09-01 | 新加坡纳米材料科技有限公司 | A method for preparing various crystalline perovskite compound powders |
| CN101747060A (en) * | 2009-12-25 | 2010-06-23 | 陕西科技大学 | A low-temperature sintered microwave dielectric ceramic material and its preparation method |
| CN103145404A (en) * | 2013-04-02 | 2013-06-12 | 清华大学深圳研究生院 | Low temperature sintered microwave medium ceramic with intermediate dielectric constant and preparation method of medium ceramic |
| CN103193483A (en) * | 2013-04-02 | 2013-07-10 | 桂林理工大学 | Low-temperature sinterable tungstate microwave dielectric ceramic Li3R3W2O12 and its preparation method |
-
2013
- 2013-10-27 CN CN201310510722.7A patent/CN103553608A/en active Pending
Patent Citations (4)
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| CN1524792A (en) * | 2003-02-28 | 2004-09-01 | 新加坡纳米材料科技有限公司 | A method for preparing various crystalline perovskite compound powders |
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Non-Patent Citations (1)
| Title |
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| WEN-CHENG TZOU.ETAL.: "Microwave dielectric characteristics of (Bi11-xSmx)NbO4 ceramics", 《CERAMICS INTERNATIONAL》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104399449A (en) * | 2014-11-21 | 2015-03-11 | 桂林理工大学 | Visible light responsive photocatalyst Li2GaB3O7 and its preparation method |
| CN104628384A (en) * | 2015-02-28 | 2015-05-20 | 桂林理工大学 | Low Loss Temperature Stable Medium Permittivity Microwave Dielectric Ceramic LiBi2NbO6 |
| CN104667905A (en) * | 2015-02-28 | 2015-06-03 | 桂林理工大学 | Visible light responsive photocatalyst LiSm2NbO6 and its preparation method |
| CN105174958A (en) * | 2015-10-09 | 2015-12-23 | 桂林理工大学 | Intermediate permittivity microwave dielectric ceramic Li4La3Nb3O14 and its preparation method |
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Application publication date: 20140205 |