CN101967058B - High Q value microwave medium ceramic and preparation method thereof - Google Patents
High Q value microwave medium ceramic and preparation method thereof Download PDFInfo
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- CN101967058B CN101967058B CN201010237748.5A CN201010237748A CN101967058B CN 101967058 B CN101967058 B CN 101967058B CN 201010237748 A CN201010237748 A CN 201010237748A CN 101967058 B CN101967058 B CN 101967058B
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- microwave
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- ceramic
- medium ceramics
- niobate
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- 239000000919 ceramic Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 229910052725 zinc Inorganic materials 0.000 claims description 15
- 239000011701 zinc Substances 0.000 claims description 15
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 13
- 239000000843 powder Substances 0.000 claims description 13
- 239000002253 acid Substances 0.000 claims description 12
- 238000009413 insulation Methods 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 9
- 238000001238 wet grinding Methods 0.000 claims description 9
- 239000011230 binding agent Substances 0.000 claims description 6
- 238000010304 firing Methods 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 238000005469 granulation Methods 0.000 claims description 5
- 230000003179 granulation Effects 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 4
- 230000000977 initiatory effect Effects 0.000 claims description 4
- 229910052758 niobium Inorganic materials 0.000 claims description 4
- 229910052715 tantalum Inorganic materials 0.000 claims description 4
- 238000010792 warming Methods 0.000 claims description 4
- 238000005304 joining Methods 0.000 claims description 2
- 238000004891 communication Methods 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 5
- 238000010295 mobile communication Methods 0.000 abstract description 4
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 abstract 2
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 abstract 2
- 229920002451 polyvinyl alcohol Polymers 0.000 abstract 2
- 238000013329 compounding Methods 0.000 abstract 1
- 238000000748 compression moulding Methods 0.000 abstract 1
- 238000005245 sintering Methods 0.000 abstract 1
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 abstract 1
- 150000001875 compounds Chemical class 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 5
- 239000000956 alloy Substances 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
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- Inorganic Insulating Materials (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention discloses high Q value microwave medium ceramic and a preparation method thereof, and belongs to the field of a microwave medium ceramic material and preparation technology thereof. The ceramic is formed by compounding MgNb2O6 and ZnTa2O6, wherein the MgNb2O6 is synthesized by using MgO and Nb2O5 serving as raw materials; the ZnTa2O6 is synthesized by using ZnO and Ta2O5 serving as raw material; the MgNb2O6 and the ZnTa2O6 are mixed; polyvinyl alcohol (PVA) is added into the mixture for compression molding; and the microwave medium ceramic is prepared by sintering the mixture ina high-temperature furnace for 2 to 4 hours. The relative dielectric constant of the microwave medium ceramic of the invention ranges from 29.7 to 31.4, the Qf value ranges from 66,280 to 67,370, and the temperature coefficient of resonance frequency is adjustable; and the ceramic can be widely applied to manufacturing various microwave devices, such as a medium resonator, a filter and the like, and meets the technical requirements of a mobile communication system, a satellite communication system and the like.
Description
Technical field
The present invention relates to a kind of take oxide as the basis the ceramic compound take composition as feature, more precisely, be with magnesium-niobate (MgNb about a kind of
2O
6) and tantalic acid zinc (ZnTa
2O
6) compound ceramic compound and preparation method thereof, belong to materials science field.
Background technology
Microwave-medium ceramics refers to be applied to microwave frequency band, and (finishing the pottery of one or more functions in the circuit of 300MHz～3000GHz) as dielectric material, is the core material of microwave device.Recent two decades comes, because microwave technology equipment is to miniaturization, integrated and high frequency, especially to the developing rapidly of the large output of the product for civilian use, low price direction, has developed large quantities of microwave dielectric ceramic materials that are applicable to microwave frequency band at present.Be applied to the media ceramic of microwave circuit, should satisfy the requirement of following dielectric characterization: the relative dielectric constant ε that (1) is high
rTo reduce the size of device, General Requirements ε
r〉=20; (2) high quality factor q is to reduce noise, General Requirements Q * f 〉=3000; (3) approach zero frequency-temperature coefficient τ
fTo guarantee the temperature stability of device.According to the performance of microwave material, microwave-medium ceramics can be divided three classes: the microwave-medium ceramics of (1) high-k low reactance-resistance ratio is mainly used in the hand-held mobile communication equipment that microminiaturization is had relatively high expectations; (2) high Q value dielectric constant microwave ceramic medium is mainly used in millimeter wave communication and microwave circuit substrate.(3) microwave-medium ceramics of high Q value near-zero resonance frequency temperature coefficient is used for the higher satellite of the transmission quantity of information and required precision and the base station of ground communications.MgNb
2O
6And ZnTa
2O
6All has excellent microwave dielectric property.Deliver one piece such as " Japanese Applied Physics " magazine (Japanese journal of applied physics) in 1997 and be entitled as " AB under the microwave frequency
2O
6The dielectric property of compound (A=Ca, Mg, Mn, Co, Ni, Zn, and B=Nb, Ta) " (Dielectric Properties of AB
2O
6Compounds at MicrowaveFrequencies (A=Ca, Mg, Mn, Co, Ni, Zn, and B=Nb, Ta)) (Japanese journalof applied physics, vol.36, issue Part 2, No.10A, PP.L1318-L1320) in reported 1300 ℃ of MgNb that burn till 2 hours
2O
6Microwave dielectric property be ε
r=21.4, τ
f=-70, Qf=93800GHz." micro-structural was to ZnTa at one piece of article in 2002 for " alloy and compound " magazine (Journal of Alloys and Compounds)
2O
6The impact of low-dielectric loss ceramic microwave dielectric property " (Influence of microstructure on microwave dielectric properties ofZnTa
2O
6Ceramics with low dielectric loss) (Journal of Alloys andCompounds, vol.337, issue 1-2, pp.303-308) reported 1400 ℃ of ZnTa that burn till 2 hours
2O
6Dielectric property are ε
r=32.3, τ
f=9.5, Qf=67580GHz.These two kinds of microwave-medium ceramics all have higher quality factor, in order to obtain the microwave dielectric ceramic materials that temperature coefficient of resonance frequency is adjustable and have higher Q value, method commonly used is exactly to carry out two kinds of potteries with opposite temperature coefficient of resonance frequency compound.
Have not yet to see MgNb
2O
6With ZnTa
2O
6Be combined into the report of the nearly frequency-temperature coefficient adjustable microwave of high Q value media ceramic.
Summary of the invention
The present invention seeks to overcome independent magnesium-niobate and or the non-adjustable shortcoming of sour zinc microwave-medium ceramics frequency-temperature coefficient, the microwave-medium ceramics that a kind of frequency-temperature coefficient of compound acquisition by both is adjustable, have the higher quality factor provides simultaneously the compositing formula of magnesium-niobate and tantalic acid zinc composite microwave medium ceramic and has made the method for this media ceramic product.
The present invention is achieved by following scheme.
A kind of high Q value microwave-medium ceramics is characterized in that by magnesium-niobate (MgNb
2O
6) and tantalic acid zinc (ZnTa
2O
6) form.
By weight percentage, wherein:
Magnesium-niobate 2.5%～12.5%;
Tantalic acid zinc 87.5%～97.5%.
Further, described high Q value microwave-medium ceramics is preferably by weight percentage:
Magnesium-niobate 10.0%;
Tantalic acid zinc 90.0%.
The preparation method of a kind of high Q value microwave-medium ceramics of the present invention comprises the steps:
(1) take purity as 98.5% MgO and 99.99% Nb
2O
5Be initiation material, synthesize MgNb 1000 ℃ of calcinings after the raw material wet-milling is mixed, dries, sieves
2O
6Ceramic powder;
(2) take purity as 99.0% ZnO and 99.99% Ta
2O
5Be initiation material, synthesize ZnTa 1100 ℃ of calcinings after the raw material wet-milling is mixed, dries, sieves
2O
6Ceramic powder;
(3) magnesium-niobate that step (1) and step (2) is synthesized and tantalic acid zinc is by weight:
Magnesium-niobate 2.5%～12.5%
Tantalic acid zinc 87.5%～97.5%
Form batching, institute adds binding agent and granulation after joining powder wet-milling 4h oven dry, and is compressing again, then is warming up to 500 ℃ of insulation 1h and carries out binder removal in high temperature furnace, cools off with stove after continuing to be warming up to firing temperature insulation 2～4h.
Further, in the above-mentioned steps (3), the binding agent of described adding is that concentration is 5%, weight percent content is 3～10% the PVA aqueous solution.
Further, the firing temperature in the described step (3) is 1300～1450 ℃.
Further, the firing time in the described step (3) is 2～4 hours.
The present invention can be widely used in the manufacturing of the various microwave devices such as various dielectric resonators, filter, can satisfy the Technology Need of the systems such as mobile communication, satellite communication.
Description of drawings
Fig. 1 is MgNb of the present invention
2O
6The X-ray diffractogram of ceramic powder.
Fig. 2 is ZnTa of the present invention
2O
6The X-ray diffractogram of ceramic powder.
Fig. 3 is the X-ray diffractogram of the pottery that synthesizes of three embodiment of the present invention.1 represents embodiment 1,2 represents embodiment 2,3 and represents embodiment 3
Embodiment
The present invention further describes with reference to following embodiment, certainly the scope that is not meant to limit the present invention of these embodiment.
MgNb
2O
6Synthetic:
Get MgO 8.0600g and Nb
2O
553.1640g in absolute ethyl alcohol ball milling 4 as a child post-drying, sieve, then in high temperature furnace, heat up with the heating rate of 5 ℃/min, rise to 1000 ℃ of insulations and cool to the synthetic MgNb of room temperature with the furnace after 2 hours
2O
6Ceramic powder.
ZnTa
2O
6Synthetic:
Get ZnO 16.2780g and Ta
2O
588.3780g ball milling 4 was as a child dried, sieved in absolute ethyl alcohol, then the heating rate with 5 ℃/min heats up in high temperature furnace, rises to 1100 ℃ of insulations and cools to the synthetic ZnTa of room temperature in 2 hours afterwards with the furnace
2O
6Ceramic powder.
Get MgNb in ratio in the table 1
2O
6And ZnTa
2O
6Powder, wet-milling 4 hours.Material after the oven dry adds 5% PVA aqueous solution 1g granulation, then use the pressure of 200MPa compressing, heating rate with 5 ℃/min in high temperature furnace rises to 1350 ℃ of insulations 3 hours, makes microwave-medium ceramics, and the dielectric property testing result of its pottery under 10GHz sees Table 2.
Embodiment 2:
Get MgNb in ratio in the table 1
2O
6And ZnTa
2O
6Powder, wet-milling 4 hours.Material after the oven dry adds 5% PVA aqueous solution 1g granulation, then use the pressure of 200MPa compressing, heating rate with 5 ℃/min in high temperature furnace rises to 1350 ℃ of insulations 3 hours, makes microwave-medium ceramics, and the dielectric property testing result of its pottery under 10GHz sees Table 2.
Embodiment 3:
Get MgNb in ratio in the table 1
2O
6And ZnTac
2O
6Powder, wet-milling 4 hours.Material after the oven dry adds 5% PVA aqueous solution 1g granulation, then use the pressure of 200MPa compressing, heating rate with 5 ℃/min in high temperature furnace rises to 1350 ℃ of insulations 3 hours, makes microwave-medium ceramics, and the dielectric property testing result of its pottery under 10GHz sees Table 2.
Table 1 microwave-medium ceramics forms
The dielectric property of table 2 microwave-medium ceramics under 10GHz
| Pottery forms | εr | Qf(GHz) | τf(ppm/℃) |
| |
31.3 | 67320 | 6.3 |
| |
30.9 | 66850 | 2.6 |
| |
30.4 | 66330 | -0.4 |
The present invention can be widely used in the manufacturing of the various microwave devices such as various dielectric resonators, filter, can satisfy the Technology Need of the systems such as mobile communication, satellite communication.
Claims (6)
1. one kind high Q value microwave-medium ceramics is characterized in that: by magnesium-niobate (MgNb
2O
6) and tantalic acid zinc (ZnTa
2O
6) form, by weight percentage:
Magnesium-niobate 2.5%～12.5%;
Tantalic acid zinc 87.5%～97.5%.
2. a kind of high Q value microwave-medium ceramics according to claim 1 is characterized in that, by weight percentage:
Magnesium-niobate 10.0%;
Tantalic acid zinc 90.0%.
3. the preparation method of a kind of high Q value microwave-medium ceramics according to claim 1 is characterized in that comprising the steps:
(1) take purity as 98.5% MgO and 99.99% Nb
2O
5Be initiation material, synthesize MgNb 1000 ℃ of calcinings after the raw material wet-milling is mixed, dries, sieves
2O
6Ceramic powder;
(2) take purity as 99.0% ZnO and 99.99% Ta
2O
5Be initiation material, synthesize ZnTa 1100 ℃ of calcinings after the raw material wet-milling is mixed, dries, sieves
2O
6Ceramic powder;
(3) magnesium-niobate that step (1) and step (2) is synthesized and tantalic acid zinc is by weight:
Magnesium-niobate 2.5%～12.5%
Tantalic acid zinc 87.5%～97.5%
Form batching, institute adds binding agent and granulation after joining powder wet-milling 4h oven dry, and is compressing again, then is warming up to 500 ℃ of insulation 1h and carries out binder removal in high temperature furnace, cools off with stove after continuing to be warming up to firing temperature insulation 2～4h.
4. the preparation method of a kind of high Q value microwave-medium ceramics according to claim 3 is characterized in that: in the step (3), the binding agent of described adding is that concentration is 5%, weight percent content is 3～10% the PVA aqueous solution.
5. the preparation method of a kind of high Q value microwave-medium ceramics according to claim 3, it is characterized in that: the firing temperature in the described step (3) is 1300～1450 ℃.
6. the preparation method of a kind of high Q value microwave-medium ceramics according to claim 3, it is characterized in that: the firing time in the described step (3) is 2～4 hours.
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| CN201010237748.5A CN101967058B (en) | 2010-07-23 | 2010-07-23 | High Q value microwave medium ceramic and preparation method thereof |
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| CN201010237748.5A CN101967058B (en) | 2010-07-23 | 2010-07-23 | High Q value microwave medium ceramic and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN101967058A CN101967058A (en) | 2011-02-09 |
| CN101967058B true CN101967058B (en) | 2013-02-06 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102765939B (en) * | 2012-07-23 | 2014-02-12 | 天津大学 | Microwave dielectric ceramic with moderate dielectric constant and low loss |
| CN103011802B (en) * | 2012-12-21 | 2014-12-03 | 武汉理工大学 | Microwave dialect ceramic material and preparation method thereof |
| CN104016684B (en) * | 2014-06-25 | 2017-04-19 | 嘉兴职业技术学院 | Preparation method and ball mill for microwave dielectric ceramic test piece |
| CN104609860A (en) * | 2015-01-25 | 2015-05-13 | 济南唯博新材料有限公司 | Preparation for magnesium niobate microwave ceramic powder through sol-gel technology |
| CN107382313B (en) * | 2017-06-02 | 2020-06-12 | 中国科学院上海硅酸盐研究所 | Microwave dielectric ceramic with ultrahigh quality factor, medium-low dielectric constant and near-zero temperature coefficient and preparation method thereof |
| CN114520114B (en) * | 2022-02-24 | 2023-06-16 | 电子科技大学 | High-temperature-stability bismuth sodium titanate-based medium energy storage ceramic and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1148582A (en) * | 1996-07-31 | 1997-04-30 | 清华大学 | Nb-Mg-acid-load group temp. stabilized relaxation ferroelectric ceramic composition and its preparation methodology |
| CN101100376A (en) * | 2007-07-17 | 2008-01-09 | 上海师范大学 | Lead magnesio-niobate-lead titanate binary system high-heat electricity-release ceramic material and preparation technique thereof |
| CN101560106A (en) * | 2009-05-21 | 2009-10-21 | 深圳市金雨叶新材料科技有限公司 | Method for preparing textured piezoelectric ceramics with high piezoelectric strain constant |
-
2010
- 2010-07-23 CN CN201010237748.5A patent/CN101967058B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1148582A (en) * | 1996-07-31 | 1997-04-30 | 清华大学 | Nb-Mg-acid-load group temp. stabilized relaxation ferroelectric ceramic composition and its preparation methodology |
| CN101100376A (en) * | 2007-07-17 | 2008-01-09 | 上海师范大学 | Lead magnesio-niobate-lead titanate binary system high-heat electricity-release ceramic material and preparation technique thereof |
| CN101560106A (en) * | 2009-05-21 | 2009-10-21 | 深圳市金雨叶新材料科技有限公司 | Method for preparing textured piezoelectric ceramics with high piezoelectric strain constant |
Non-Patent Citations (1)
| Title |
|---|
| 张迎春 等.高Q值(1-x)ZnNb2O6-xZnTa2O6系微波介质陶瓷.《中国硅酸盐学会2003年学术年会论文摘要集》.2003,第312页. * |
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