CN103951430A - Low-temperature-sintered niobate high-quality-factor microwave dielectric ceramic material - Google Patents
Low-temperature-sintered niobate high-quality-factor microwave dielectric ceramic material Download PDFInfo
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- CN103951430A CN103951430A CN201410166374.0A CN201410166374A CN103951430A CN 103951430 A CN103951430 A CN 103951430A CN 201410166374 A CN201410166374 A CN 201410166374A CN 103951430 A CN103951430 A CN 103951430A
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Abstract
The invention discloses a low-temperature-sintered niobate high-quality-factor microwave dielectric ceramic material of which the chemical formula is Ni0.04Zn0.96TiNb2O8+(1-4)wt%CuO. The microwave dielectric ceramic material is prepared by the following steps: calcining chemical raw materials ZnO, NiO, Nb2O5, TiO2 and CuO at 850 DEG C to synthesize a precursor, and sintering at 900-940 DEG C. From the angle of LTCC (low temperature co-fired ceramic), a small amount of low-melting-point sintering assistant CuO is doped in the Ni0.04Zn0.96TiNb2O8 system, thereby keeping excellent microwave behaviors under the condition of lowering the sintering temperature; and the dielectric constant is 30-34, the quality factor is 27800-41500GHz, and the temperature coefficient of resonance frequency is -35 to -41*10<-6>/DEG C. The microwave dielectric ceramic material has the advantages of simple preparation technique and no pollution in the process, and has wide application prospects.
Description
Technical field
The invention belongs to a kind of ceramic composition that composition is feature of take, relate in particular to a kind of low-temperature sintering niobate high quality factor (Q value) microwave dielectric ceramic materials.
Background technology
Along with electronic information technology is constantly to high frequency and digitizing future development, the miniaturization to components and parts, integrated so that modular requirement is also more and more urgent.LTCC LTCC (Low Temperature Co-fired Ceramics) is with its excellent electricity, machinery, calorifics and operational characteristic, become one of major technique of electronic-component module, abroad and Taiwan fast development, formed industry taper.It burns temperature altogether generally between 900 ℃～950 ℃.Because sintering temperature is low, the low metal of available resistivity is as the conductor material of multilayer wiring, can improve packing density, signaling rate, and can in be embedded in the various laminar microwave electronic devices of multilager base plate once-firing, be therefore widely used in high-speed and high-density and interconnect among polynary ceramic component (MCM).But the material using at present generally has lower quality factor, easily in device, introduces too high loss, has seriously hindered the further raising of device performance.
The invention provides a kind of low-temperature sintering high-quality factor microwave medium ceramic material and preparation method thereof, this low-temperature sintered microwave dielectric ceramic material is from the low temperature co-fired angle of LTCC, at Ni
0.04zn
0.96tiNb
2o
8in system, by a small amount of low melting point sintering aid CuO of doping, its sintering temperature can be successfully down to below 950 ℃, meanwhile keeps excellent microwave property.
Summary of the invention
Object of the present invention, is to solve the lower problem of material quality factor in prior art, and the high Q value of a kind of low-temperature sintering niobate microwave dielectric ceramic materials and preparation method thereof is provided.
The present invention is achieved by following technical solution.
A low-temperature sintering niobate high-quality factor microwave medium ceramic material, its chemical formula is Ni
0.04zn
0.96tiNb
2o
8+ (1-4) wt%CuO;
The preparation method of this low-temperature sintering niobate high-quality factor microwave medium ceramic material, has following steps:
(1) by chemical feedstocks ZnO, NiO, Nb
2o
5and TiO
2press respectively Ni
0.04zn
0.96tiNb
2o
8stoichiometric ratio weigh batching.
(2) chemical feedstocks step (1) being configured mixes, and puts into ball grinder, adds zirconia ball and deionized water, ball milling 4～6 hours, then the raw material after ball milling is dried in infrared drying oven, sieve;
(3) powder mixing after step (2) is sieved, in 850 ℃ of calcinings, is incubated 3 hours, synthetic presoma;
(4) in the presoma of step (3), additional mass percent is 0.70～1.05% polyvinyl alcohol and (1-4) CuO of wt%, put into ball grinder, add zirconia ball and deionized water, ball milling 8～12 hours, after oven dry, sieve, then be base substrate with powder compressing machine pressure forming;
(5) by base substrate in 900～940 ℃ of sintering, be incubated 3～6 hours, make low-temperature sintering niobate high-quality factor microwave medium ceramic material;
(6) microwave dielectric property of Adoption Network analyser test microwave dielectric ceramic materials.
The purity of the chemical feedstocks of described step (1) is greater than 99.9%.
The powder compressing machine of described step (4) is with the pressure forming of 4～6MPa, and base substrate is the right cylinder of Φ 10mm * 5mm.
The preferred sintering temperature of described step (5) is 940 ℃.
Ni of the present invention
0.04zn
0.96tiNb
2o
8+ (1-4) the high Q value of wt%CuO low-temperature sintering niobate microwave dielectric ceramic materials, its sintering temperature is 900～940 ℃, and specific inductivity is 30～34, and quality factor are 27,800～41,500GHz, and temperature coefficient of resonance frequency is-35～-41 * 10
-6/ ℃.In addition, this preparation technology is simple, and process is pollution-free, has broad application prospects.
Embodiment
Chemical feedstocks ZnO, NiO, Nb that the present invention adopts purity to be greater than 99.9%
2o
5, TiO
2prepare Ni with CuO
0.04zn
0.96tiNb
2o
8+ (1-4) wt%CuO microwave-medium ceramics, specific embodiment is as follows:
Embodiment 1
1) by ZnO, NiO, Nb
2o
5, TiO
2difference is 0.96:0.04:1:1 weigh batching in molar ratio;
2) will after configure raw material mixing, add in nylon tank ball milling 6 hours; Raw material after ball milling is placed in to infrared drying oven dries, sieves;
3) by the powder mixing after sieving in 850 ℃ of calcinings 3 hours, synthetic precursor;
4) in synthetic precursor, additional mass percent is the CuO that 1.05% polyvinyl alcohol and mass percent are 2%, puts into ball grinder, adds 10 hours post-dryings of zirconia ball and deionized water ball milling, sieves; With powder compressing machine, with the pressure of 8MPa, be pressed into again the cylinder shape base substrate of Φ 10mm * 5mm;
5) by cylinder shape base substrate in 940 ℃ of sintering, be incubated 6 hours, make low-temperature sintering niobate high-quality factor microwave medium ceramic material;
6) microwave dielectric property of Adoption Network analyser test implementation example 1; Obtain its performance as follows:
Specific inductivity is: 34.13
Quality factor are: 41013GHz
Temperature coefficient of resonance frequency is :-37 * 10
-6
Embodiment 2～5
The preparation process of embodiment 2～5 is substantially the same manner as Example 1, and difference is the difference of sintering temperature and CuO addition; The concrete sintering temperature of embodiment 2～5 and CuO addition and relevant dielectric properties thereof refer to table 1.
Table 1
Claims (4)
1. a low-temperature sintering niobate high-quality factor microwave medium ceramic material, its chemical formula is Ni
0.04zn
0.96tiNb
2o
8+ (1-4) wt%CuO;
The preparation method of this low-temperature sintering niobate high-quality factor microwave medium ceramic material, has following steps:
(1) by chemical feedstocks ZnO, NiO, Nb
2o
5and TiO
2press respectively Ni
0.04zn
0.
96tiNb
2o
8stoichiometric ratio weigh batching.
(2) chemical feedstocks step (1) being configured mixes, and puts into ball grinder, adds zirconia ball and deionized water, ball milling 4～6 hours, then the raw material after ball milling is dried in infrared drying oven, sieve;
(3) powder mixing after step (2) is sieved, in 850 ℃ of calcinings, is incubated 3 hours, synthetic presoma;
(4) in the presoma of step (3), additional mass percent is 0.70～1.05% polyvinyl alcohol and (1-4) CuO of wt%, put into ball grinder, add zirconia ball and deionized water, ball milling 8～12 hours, after oven dry, sieve, then be base substrate with powder compressing machine pressure forming;
(5) by base substrate in 900～940 ℃ of sintering, be incubated 3～6 hours, make low-temperature sintering niobate high-quality factor microwave medium ceramic material;
(6) microwave dielectric property of Adoption Network analyser test microwave dielectric ceramic materials.
2. low-temperature sintering niobate high-quality factor microwave medium ceramic material according to claim 1, is characterized in that, the purity of the chemical feedstocks of described step (1) is greater than 99.9%.
3. low-temperature sintering niobate high-quality factor microwave medium ceramic material according to claim 1, is characterized in that, the powder compressing machine of described step (4) is with the pressure forming of 4～6MPa, and base substrate is the right cylinder of Φ 10mm * 5mm.
4. low-temperature sintering niobate high-quality factor microwave medium ceramic material according to claim 1, is characterized in that, the preferred sintering temperature of described step (5) is 940 ℃.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105777120A (en) * | 2016-03-09 | 2016-07-20 | 同济大学 | CuO-doped leadless piezoelectric ceramic and low-temperature sintering method thereof |
| CN106904968A (en) * | 2017-02-28 | 2017-06-30 | 天津大学 | A kind of niobium base composite microwave medium ceramic material and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102617142A (en) * | 2012-04-05 | 2012-08-01 | 天津大学 | Novel medium-temperature-sintering temperature stabilization type microwave dielectric ceramic |
| CN103467093A (en) * | 2013-08-28 | 2013-12-25 | 天津大学 | Nickel oxide-doped niobium zinc titanate microwave dielectric ceramic and preparation method thereof |
-
2014
- 2014-04-23 CN CN201410166374.0A patent/CN103951430B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102617142A (en) * | 2012-04-05 | 2012-08-01 | 天津大学 | Novel medium-temperature-sintering temperature stabilization type microwave dielectric ceramic |
| CN103467093A (en) * | 2013-08-28 | 2013-12-25 | 天津大学 | Nickel oxide-doped niobium zinc titanate microwave dielectric ceramic and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| TIANKAI CHEN ET AL: "Phase composition and microwave dielectric properties of (Zn, Ni)TiNb2O8 solid solution", 《J MATER SCI: MATER ELECTRON》, 30 March 2014 (2014-03-30), pages 2494 - 2500 * |
| 陈秀丽 等: "B2O3与CuO掺杂的ZnO-2TiO2-Nb2O5陶瓷与银电极的共烧行为研究", 《功能材料》, 31 December 2010 (2010-12-31), pages 224 - 226 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105777120A (en) * | 2016-03-09 | 2016-07-20 | 同济大学 | CuO-doped leadless piezoelectric ceramic and low-temperature sintering method thereof |
| CN105777120B (en) * | 2016-03-09 | 2018-06-26 | 同济大学 | A kind of cupric oxide doped leadless piezoelectric ceramics and its low-temperature sintering method |
| CN106904968A (en) * | 2017-02-28 | 2017-06-30 | 天津大学 | A kind of niobium base composite microwave medium ceramic material and preparation method thereof |
| CN106904968B (en) * | 2017-02-28 | 2020-02-07 | 天津大学 | Niobium-based composite microwave dielectric ceramic material and preparation method thereof |
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