CN103496981A - Low-temperature sintering temperature-stable microwave dielectric ceramic Bi14W2O27 and preparation method thereof - Google Patents
Low-temperature sintering temperature-stable microwave dielectric ceramic Bi14W2O27 and preparation method thereof Download PDFInfo
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- CN103496981A CN103496981A CN201310444130.XA CN201310444130A CN103496981A CN 103496981 A CN103496981 A CN 103496981A CN 201310444130 A CN201310444130 A CN 201310444130A CN 103496981 A CN103496981 A CN 103496981A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 238000009766 low-temperature sintering Methods 0.000 title claims abstract description 6
- 239000000843 powder Substances 0.000 claims abstract description 12
- 238000005245 sintering Methods 0.000 claims abstract description 12
- 239000011230 binding agent Substances 0.000 claims abstract description 7
- 239000012298 atmosphere Substances 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims abstract description 6
- 238000000748 compression moulding Methods 0.000 claims abstract description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 3
- 238000000498 ball milling Methods 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
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 239000002904 solvent Substances 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000002131 composite material Substances 0.000 claims description 5
- 238000005469 granulation Methods 0.000 claims description 2
- 230000003179 granulation Effects 0.000 claims description 2
- 239000000203 mixture Substances 0.000 abstract description 2
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 abstract 2
- 238000001035 drying Methods 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 238000005303 weighing Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 9
- 238000004891 communication Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 229910010413 TiO 2 Inorganic materials 0.000 description 4
- 238000011161 development Methods 0.000 description 4
- 229910010293 ceramic material Inorganic materials 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 239000011521 glass Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000011160 research Methods 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
- 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
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 229910052709 silver 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
- 229910052726 zirconium Inorganic materials 0.000 description 1
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- Inorganic Insulating Materials (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention discloses a low-temperature sintering temperature-stable microwave dielectric ceramic and a preparation method thereof. The composition formula of the low-temperature sintering temperature-stable microwave dielectric ceramic is Bi14W2O27. The preparation method comprises the steps of (1) weighing and batching original powder of Bi2O3 and WO3 with the purity being over 99.9% according to the chemical formula Bi14W2O27; (2) carrying out wet ball-milling and mixing on raw materials obtained in the step (1) for 12 hours, taking distilled water as a solvent, drying, and then, pre-sintering in an air atmosphere for 6 hours at the temperature of 700 DEG C; (3) adding a binder into powder prepared in the step (2), granulating, then, carrying out compression molding, and finally, sintering in the air atmosphere for 4 hours at the temperature of 800-820 DEG C, wherein a polyvinyl alcohol solution with the mass concentration of 5% is adopted as the binder, and the dosage of the binder accounts for 3% of the total mass of the powder. According to the ceramic prepared by the preparation method, the sintering at the temperature of 800-820 DEG C is good, the dielectric constant reaches 12-13, the quality factor (Qf) reaches up to 61,000-84,000GHz, the temperature coefficient of resonance frequency is small, and the ceramic can be subjected to low-temperature co-sintering together with a Ag electrode, so that the ceramic has a great application value in industries.
Description
Technical field
The present invention relates to dielectric ceramic material, particularly relate to microwave dielectric ceramic material 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, be widely used as the components and parts such as resonator, wave filter, dielectric substrate and medium guided wave loop in modern communication, 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, very important application is arranged, 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 is applied to microwave technology in the world.
According to relative permittivity ε
rsize from use the different of frequency range, usually the microwave dielectric ceramic be developed He developing can be divided into to 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 f>=10 GHz), τ
?≈ 0.Be mainly used in the microwave communication equipments such as direct broadcasting satellite of f >=8 GHz as the 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(f=3～-4GHz under), τ
?≤ 5 ppm/ ° C.Be mainly used in the interior microwave military radar of 4～8 GHz range of frequency and communication system as the 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 above these material systems is generally higher than 1300 ° of C, can not be directly and the low melting point metals such as Ag and Cu burn altogether the formation laminated ceramic capacitor.In recent years, along with LTCC Technology (Low Temperature Co-fired Ceramics, 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 to adopt devitrified glass or glass-ceramic composite system, because low melting glass has relatively high dielectric loss mutually, the existence of glassy phase has improved the dielectric loss of material greatly.Therefore development is the emphasis of current research without the low fired microwave dielectric ceramic material of glassy phase, low temperature sintering high performance microwave media ceramic system is still very limited at present, and this has limited the development of low temperature co-fired technology and microwave multilayer device to a great extent.
Summary of the invention
The purpose of this invention is to provide a kind of have low-loss and good temperature stability, high-frequency dielectric constant reaches 12 ~ 13, Qf value up to 61000-84000GHz simultaneously, can be at microwave dielectric ceramic of 800-820 ℃ of sintering and preparation method thereof.
The chemical constitution formula of microwave dielectric ceramic of the present invention is: Bi
14w
2o
27.
Preparation method's concrete steps of described microwave dielectric ceramic are:
(1) by purity, be the Bi more than 99.9%
2o
3and WO
3starting powder press Bi
14w
2o
27the chemical formula weigh batching.
(2) step (1) raw material wet ball-milling is mixed 12 hours, solvent is distilled water, pre-burning 6 hours in 700 ℃ of air atmosphere after oven dry.
(3) after adding binding agent granulation in the powder made in step (2), then compression moulding, last sintering 4 hours in 800 ~ 820 ℃ 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.
Pottery prepared by the present invention is good at 800-820 ℃ of sintering, its specific inductivity reaches 12～13, and quality factor q f value is up to 61000-84000GHz, and temperature coefficient of resonance frequency is little, and can be low temperature co-fired with the Ag electrode, therefore industrial great using value arranged.
Embodiment
Embodiment:
Table 1 shows 3 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 the cylindrical dielectric resonator method; By powder with the Ag powder that accounts for powder quality 20%, mix, after compression moulding, 820 ℃ of sintering 4 hours; X ray diffraction material phase analysis and scanning electron microscopic observation all show Bi
14w
2o
27with Ag, chemical reaction, i.e. Bi do not occur
14w
2o
27can be low temperature co-fired with the Ag electrode.
The present invention never is 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)
1. composite oxides, as the application of low-temperature sintering temperature-stable microwave dielectric ceramic, is characterized in that the chemical constitution formula of described composite oxides is: Bi
14w
2o
27;
Preparation method's concrete steps of described composite oxides are:
(1) by purity, be the Bi more than 99.9%
2o
3and WO
3starting powder press Bi
14w
2o
27the chemical formula weigh batching;
(2) step (1) raw material wet ball-milling is mixed 12 hours, solvent is distilled water, pre-burning 6 hours in 700 ℃ of air atmosphere after oven dry;
(3) after adding binding agent granulation in the powder made in step (2), then compression moulding, last sintering 4 hours in 800 ~ 820 ℃ 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.
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|---|---|---|---|
| CN201310444130.XA CN103496981B (en) | 2013-09-26 | 2013-09-26 | Low-temperature sintering temperature-stable microwave dielectric ceramic Bi14W2O27 and preparation method thereof |
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|---|---|---|---|
| CN201310444130.XA CN103496981B (en) | 2013-09-26 | 2013-09-26 | Low-temperature sintering temperature-stable microwave dielectric ceramic Bi14W2O27 and preparation method thereof |
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| Publication Number | Publication Date |
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| CN103496981B CN103496981B (en) | 2015-01-07 |
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|---|---|---|---|
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104230339A (en) * | 2014-09-20 | 2014-12-24 | 桂林理工大学 | Microwave dielectric ceramic Bi2ZnW4O16 with low dielectric constant and capacity of low temperature sintering |
| CN104261827A (en) * | 2014-09-21 | 2015-01-07 | 桂林理工大学 | Low-temperature sinterable microwave dielectric ceramic Bi2MgW5O19 with low dielectric constant |
| CN104261824A (en) * | 2014-09-19 | 2015-01-07 | 桂林理工大学 | Low-temperature-sintering ultralow-dielectric-constant microwave dielectric ceramic Bi2ZnW3O13 |
| CN104446474A (en) * | 2014-12-28 | 2015-03-25 | 桂林理工大学 | Microwave dielectric ceramic NdBiWO6 with near-zero resonant frequency temperature coefficient |
| CN108840666A (en) * | 2018-07-23 | 2018-11-20 | 淄博宇海电子陶瓷有限公司 | Low-temperature sintered microwave dielectric ceramic material and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103319177A (en) * | 2013-06-25 | 2013-09-25 | 桂林理工大学 | Microwave dielectric ceramic Ba3WTiO8 with low-temperature sintering characteristic and preparation method thereof |
-
2013
- 2013-09-26 CN CN201310444130.XA patent/CN103496981B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103319177A (en) * | 2013-06-25 | 2013-09-25 | 桂林理工大学 | Microwave dielectric ceramic Ba3WTiO8 with low-temperature sintering characteristic and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| ANTONIO FETEIRA ET AL.: "Microwave Dielectric Properties of Low Firing Temperature Bi2W2O9 Ceramics", 《J. AM. CERAM. SOC.》 * |
| SYED N.HODA ET AL.: "Phase Relations in the System Bi2O3-WO3", 《JOURNAL OF THE AMERICAN CERAMIC SOCIETY》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104261824A (en) * | 2014-09-19 | 2015-01-07 | 桂林理工大学 | Low-temperature-sintering ultralow-dielectric-constant microwave dielectric ceramic Bi2ZnW3O13 |
| CN104261824B (en) * | 2014-09-19 | 2016-01-13 | 桂林理工大学 | Low temperature sintering ultralow dielectric microwave dielectric ceramic Bi 2znW 3o 13 |
| CN104230339A (en) * | 2014-09-20 | 2014-12-24 | 桂林理工大学 | Microwave dielectric ceramic Bi2ZnW4O16 with low dielectric constant and capacity of low temperature sintering |
| CN104261827A (en) * | 2014-09-21 | 2015-01-07 | 桂林理工大学 | Low-temperature sinterable microwave dielectric ceramic Bi2MgW5O19 with low dielectric constant |
| CN104446474A (en) * | 2014-12-28 | 2015-03-25 | 桂林理工大学 | Microwave dielectric ceramic NdBiWO6 with near-zero resonant frequency temperature coefficient |
| CN108840666A (en) * | 2018-07-23 | 2018-11-20 | 淄博宇海电子陶瓷有限公司 | Low-temperature sintered microwave dielectric ceramic material and preparation method thereof |
| CN108840666B (en) * | 2018-07-23 | 2020-09-04 | 淄博宇海电子陶瓷有限公司 | Low-temperature sintered microwave dielectric ceramic material and preparation method thereof |
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| CN103496981B (en) | 2015-01-07 |
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