CN103951430B - Low-temperature sintering niobate high-quality factor microwave medium ceramic material - Google Patents
Low-temperature sintering niobate high-quality factor microwave medium ceramic material Download PDFInfo
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- CN103951430B CN103951430B CN201410166374.0A CN201410166374A CN103951430B CN 103951430 B CN103951430 B CN 103951430B CN 201410166374 A CN201410166374 A CN 201410166374A CN 103951430 B CN103951430 B CN 103951430B
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Abstract
The invention discloses a kind of 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, adopts chemical feedstocks ZnO, NiO, Nb
2o
5, TiO
2and CuO, in 850 DEG C of calcining synthesis presomas, in 900 ~ 940 DEG C of sintering.The present invention from the low temperature co-fired angle of LTCC, at Ni
0.04zn
0.96tiNb
2o
8by the low melting point sintering aid CuO that doping is a small amount of in system, while reducing sintering temperature, keep excellent microwave property; Its specific inductivity is 30 ~ 34, and quality factor are 27,800 ~ 41,500GHz, and temperature coefficient of resonance frequency is-35 ~-41 × 10
-6/ DEG C.Preparation technology is simple, and process is pollution-free, has broad application prospects.
Description
Technical field
The invention belongs to a kind of take composition as the ceramic composition of feature, particularly relates 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, to the miniaturization of components and parts, integrated so that modular requirement is also more and more urgent.LTCC LTCC (LowTemperatureCo-firedCeramics) is with the electricity of its excellence, machinery, calorifics and operational characteristic, one of major technique becoming electronic-component module, abroad and Taiwan fast development, industry taper has been formed.It burns temperature altogether generally between 900 DEG C ~ 950 DEG C.Because sintering temperature is low, the low metal of useable resistance rate is as the conductor material of multilayer wiring, packing density, signaling rate can be improved, 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 used at present generally has lower quality factor, easily introduces too high loss in the devices, seriously hinders 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 from the low temperature co-fired angle of LTCC, at Ni
0.04zn
0.96tiNb
2o
8by the low melting point sintering aid CuO that doping is a small amount of in system, its sintering temperature can successfully be down to less than 950 DEG C, meanwhile keeps excellent microwave property.
Summary of the invention
Object of the present invention, is to solve the problem that in prior art, material quality factor is lower, provides a kind of low-temperature sintering niobate high q-factor microwave dielectric ceramic materials and preparation method thereof.
The present invention is achieved by following technical solution.
A kind of 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 Ni respectively
0.04zn
0.96tiNb
2o
8stoichiometric ratio weigh batching.
(2) chemical feedstocks mixing step (1) configured, puts into ball grinder, adds zirconia ball and deionized water, ball milling 4 ~ 6 hours, then dried in infrared drying oven by the raw material after ball milling, sieve;
(3) powder mixed after step (2) being sieved, in 850 DEG C of calcinings, is incubated 3 hours, synthesis presoma;
(4) in the presoma of step (3), additional mass percent is the CuO of 0.70 ~ 1.05% polyvinyl alcohol and (1-4) wt%, put into ball grinder, add zirconia ball and deionized water, ball milling 8 ~ 12 hours, sieve after oven dry, then be base substrate with powder compressing machine pressure forming;
(5) by base substrate in 900 ~ 940 DEG C of sintering, be incubated 3 ~ 6 hours, obtained low-temperature sintering niobate high-quality factor microwave medium ceramic material;
(6) microwave dielectric property of network analyzer test microwave dielectric ceramic materials is adopted.
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 DEG C.
Ni of the present invention
0.04zn
0.96tiNb
2o
8+ (1-4) wt%CuO low-temperature sintering niobate high q-factor microwave dielectric ceramic materials, its sintering temperature is 900 ~ 940 DEG C, 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/ DEG C.In addition, this preparation technology is simple, and process is pollution-free, has broad application prospects.
Embodiment
The present invention adopts purity to be greater than chemical feedstocks ZnO, NiO, Nb of 99.9%
2o
5, TiO
2ni is prepared 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 0.96:0.04:1:1 weigh batching in molar ratio;
2) add in nylon tank after configured raw material being mixed, ball milling 6 hours; Raw material after ball milling is placed in infrared drying oven to dry, sieve;
3) by the powder that mixes after sieving in 850 DEG C of calcinings 3 hours, synthesis precursor;
4) in the precursor of synthesis, additional mass percent be 1.05% polyvinyl alcohol and mass percent is the CuO of 2%, puts into ball grinder, adds zirconia ball and deionized water ball milling 10 hours post-dryings, sieves; Be pressed into the cylinder shape base substrate of Φ 10mm × 5mm again with the pressure of 8MPa with powder compressing machine;
5) by cylinder shape base substrate in 940 DEG C of sintering, be incubated 6 hours, make low-temperature sintering niobate high-quality factor microwave medium ceramic material;
6) microwave dielectric property of network analyzer testing example 1 is adopted; 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 refers to table 1 to CuO addition and relevant dielectric properties thereof.
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 Ni respectively
0.04zn
0.96tiNb
2o
8stoichiometric ratio weigh batching;
(2) chemical feedstocks mixing step (1) configured, puts into ball grinder, adds zirconia ball and deionized water, ball milling 4 ~ 6 hours, then dried in infrared drying oven by the raw material after ball milling, sieve;
(3) powder mixed after step (2) being sieved, in 850 DEG C of calcinings, is incubated 3 hours, synthesis presoma;
(4) in the presoma of step (3), additional mass percent is the CuO of 0.70 ~ 1.05% polyvinyl alcohol and (1-4) wt%, put into ball grinder, add zirconia ball and deionized water, ball milling 8 ~ 12 hours, sieve after oven dry, then be base substrate with powder compressing machine pressure forming;
(5) by base substrate in 900 ~ 940 DEG C of sintering, be incubated 3 ~ 6 hours, obtained low-temperature sintering niobate high-quality factor microwave medium ceramic material;
(6) microwave dielectric property of network analyzer test microwave dielectric ceramic materials is adopted.
2. low-temperature sintering niobate high-quality factor microwave medium ceramic material according to claim 1, it 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 DEG C.
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|---|---|---|---|
| CN201410166374.0A CN103951430B (en) | 2014-04-23 | 2014-04-23 | Low-temperature sintering niobate high-quality factor microwave medium ceramic material |
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| CN201410166374.0A CN103951430B (en) | 2014-04-23 | 2014-04-23 | Low-temperature sintering niobate high-quality factor microwave medium ceramic material |
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| CN103951430B true CN103951430B (en) | 2015-12-02 |
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|---|---|---|---|---|
| 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 |
| CN106904968B (en) * | 2017-02-28 | 2020-02-07 | 天津大学 | Niobium-based composite microwave dielectric 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 |
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2014
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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 |
|---|
| B2O3与CuO掺杂的ZnO-2TiO2-Nb2O5陶瓷与银电极的共烧行为研究;陈秀丽 等;《功能材料》;20101231;224-226 * |
| Phase composition and microwave dielectric properties of (Zn, Ni)TiNb2O8 solid solution;TianKai Chen et al;《J Mater Sci: Mater Electron》;20140330;2494-2500 * |
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