CN100522877C - Low-temperature melt Ba3Ti4Nb4O21 microwave dielectric ceramic material and method for producing the same - Google Patents

Low-temperature melt Ba3Ti4Nb4O21 microwave dielectric ceramic material and method for producing the same Download PDF

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CN100522877C
CN100522877C CNB2007101561465A CN200710156146A CN100522877C CN 100522877 C CN100522877 C CN 100522877C CN B2007101561465 A CNB2007101561465 A CN B2007101561465A CN 200710156146 A CN200710156146 A CN 200710156146A CN 100522877 C CN100522877 C CN 100522877C
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microwave
low
cuo
sintering
dielectric ceramic
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CN101172858A (en
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张启龙
杨辉
史灵杭
邹栋
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Zhejiang University ZJU
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Zhejiang University ZJU
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Abstract

The invention discloses low-temperature sintered Ba3Ti4Nb4O21 microwave medium porcelain material, wherein, Ba3Ti4Nb4O21 is the main component and MnCO3+CuO are used as the sintering addition agent. The components include Ba3Ti4Nb4O21, awt xMnCO3+(1-x)CuO, wherein, x is larger than 0 but lower than 1, and a is larger than 0 but lower than 10, and a is the weight point of the Ba3Ti4Nb4O21. The invention also discloses the preparation method of the porcelain. The porcelain of the invention can be sintered in the condition of low temperature, thereby satisfying the requirement of the co-sintering with silver electrode with microwave dielectric performance. The constant of the dielectric is 58 to 66, being high Qf value (6000 to 13400GHz). The invention can be used for preparing the new sheet-type multilayer microwave apparatuses such as capacitors, filters and syntonizer, and is provided with significant industrial application value.

Description

A kind of low-temperature sintering Ba 3Ti 4Nb 4O 21Microwave dielectric ceramic materials and preparation method thereof
Technical field
The present invention relates to be applied to a kind of low-temperature sintering Ba of chip multilayer microwave device 3Ti 4Nb 4O 21Microwave dielectric ceramic materials and preparation method thereof belongs to materials science field.
Background technology
Be the requirement of integrated, the miniaturization of satisfying modern communication equipment, the microwave-medium device also is badly in need of miniaturization and lightweight as one of main element.The important channel of realizing this goal is to adopt multilevel integration technology (being called for short MLIC).In the design of multilayer sheet type microwave device,, generally adopt the Cu of high conductivity and Ag to make electrode, and the fusing point of Cu and Ag is 1064 ℃ and 961 ℃ respectively in order to reduce cost.Therefore, exploitation can be very important with the low-temperature sintering microwave medium pottery that Ag or Cu burn altogether.At present, realized BiNbO 4, ZnO-TiO 2, MgO-TiO 2, CaO-SiO 2, Li 2O-Nb 2O 5-TiO 2, BaO-Nd 2O 3-TiO 2, BaO-Nb 2O 5Low-temperature sintering etc. a plurality of material systems.
" the New low loss microwavedielectric ceramics in the BaO-TiO that Sebastian M T etc. deliver at " Journal of Materials Science-Materials inElectronics " 10 phase 475-478 pages or leaves in 1999 2-Nb 2O 5/ Ta 2O 5System " Ba is disclosed in the literary composition 3Ti 4Nb 4O 21Pottery is at 1300 ℃ microwave dielectric property: DIELECTRIC CONSTANT rBe 55, quality factor q f value is 9000GHz, frequency-temperature coefficient τ fBe 100 * 10 -6/ ℃, can be applicable to preparation temperature building-out capacitor, dielectric resonator and antenna.For reducing Ba 3Ti 4Nb 4O 21The sintering temperature of pottery, " the Low-temperature sintering and microwave dielectric properties ofBa that Ko WJ etc. deliver at " Journal of the Korean Physical society " 49 phase 1234-1238 pages or leaves in 2006 3Ti 4-xZr xNb 4O 21Ceramics with the substitution of Zr for Ti " literary composition discloses a kind of glass auxiliary agent by admixture 7wt%, and can be in 875 ℃ of agglomerating technical schemes, its dielectric properties: DIELECTRIC CONSTANT rBe 52, quality factor q f value is 3000GHz, frequency-temperature coefficient τ fBe 5 * 10 -6/ ℃, because the introducing of a large amount of glass auxiliary agents, its Qf value descends significantly.
Therefore, how effectively reducing the microwave-medium ceramics sintering temperature and to keep higher quality factor q f value is Ba 3Ti 4Nb 4O 21The a great problem in microwave-medium ceramics low-temperature sintering technology field.
Summary of the invention
The present invention overcomes the above-mentioned defective that prior art exists, and a kind of have high Qf value, low-temperature sintering Ba that sintering temperature is low are provided 3Ti 4Nb 4O 21Microwave-medium ceramics, and corresponding preparation method is provided.
Low-temperature sintering Ba of the present invention 3Ti 4Nb 4O 21The technical scheme of microwave-medium ceramics adopts the significant MnCO of cooling-down effect 3+ CuO reduces the system sintering temperature as sintering aid, improves its microwave dielectric property.
A kind of low-temperature sintering Ba 3Ti 4Nb 4O 21Microwave dielectric ceramic materials, its raw material consists of: Ba 3Ti 4Nb 4O 21+ awt%[xMnCO 3+ (1-x) CuO], wherein: 0＜x＜1,0＜a＜10, a is for accounting for Ba 3Ti 4Nb 4O 21 weight fraction.
The prioritization scheme of above-mentioned composition is: a kind of low-temperature sintering Ba 3Ti 4Nb 4O 21Microwave dielectric ceramic materials, its raw material consists of: Ba 3Ti 4Nb4O 21+1wt% (0.2MnCO 3+ 0.8CuO).
A kind of low-temperature sintering Ba 3Ti 4Nb 4O 21The preparation technology of microwave dielectric ceramic materials may further comprise the steps:
1) presses Ba 3Ti 4Nb 4O 21Chemical formula proportioning weighing major ingredient BaCO 3, TiO 2, Nb 2O 5, major ingredient is mixed, pre-burning 2～4h prepares Ba under 1100～1200 ℃ condition 3Ti 4Nb 4O 21The pottery base-material, and grind standby;
2) with xMnCO 3+ (1-x) CuO is mixed in proportion, drying, and pre-burning obtains MnCO under 700～800 ℃ of conditions 3-MnO 2Mixture, with above-mentioned ceramic base-material according to Ba 3Ti 4Nb 4O 21+ awt%[xMnCO 3+ (1-x) CuO] mix, wherein: 0＜x＜1,0＜a＜10, a is for accounting for Ba 3Ti 4Nb 4O 21Weight fraction, obtain being used to prepare the powder of microwave-medium ceramics;
3) the described powder that is used to prepare microwave-medium ceramics is pressed into the circle sheet of diameter 18mm, thickness 8～10mm, at 900～980 ℃ of sintering, insulation 1～4h can obtain material of the present invention.
The present invention who adopts above-mentioned prescription and technology to form, (6000～13000GHz), specific inductivity is 58～66, satisfies with low-cost Ag electrode and burns the low-temperature sintering Ba of requirement altogether can to obtain having high Qf value 3Ti 4Nb 4O 21Microwave-medium ceramics can be used for preparing novel chip multilayer microwave devices such as electrical condenser, wave filter, resonator, coupling mechanism.Material of the present invention does not have particular requirement to production technique and production unit, and technology is simple, favorable reproducibility, low cost of manufacture.Therefore, material of the present invention has great using value.
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.
Embodiment
1.Ba 3Ti 4Nb 4O 21The preparation of pottery base-material
Press Ba 3Ti 4Nb 4O 21Chemical formula proportioning (BaCO 3, TiO 2And Nb 2O 5Mol ratio be 3:4:2) weighing BaCO 3, TiO 2And Nb 2O 5, place urethane ball milling bucket then, added zirconia ball and deionized water ball milling 16 hours, oven dry places box-type furnace or tunnel furnace pre-burning 2～4h under 1100～1200 ℃ condition, and cooling back ball milling makes the about 1um of its median size standby.
2.MnCO 3The preparation of+CuO mixture
With xMnCO 3+ (1-x) CuO weighing MnCO in proportion 3And CuO, place urethane ball milling bucket then, added zirconia ball and deionized water ball milling 12 hours, drying is placed on box-type furnace or tunnel furnace pre-burning under 700～800 ℃ of conditions obtains MnCO 3-MnO 2Mixture, cooling back ball milling makes the about 1um of its median size standby.
To prepare Ba 3Ti 4Nb 4O 21Pottery base-material and MnCO 3+ CuO mixture places urethane ball milling bucket in proportion, add zirconia ball and deionized water and mixed 20 hours, add the granulation of 5wt% polyvinyl alcohol (PVA) tackiness agent, under 80Mpa pressure, be pressed into diameter 18mm, the circle sheet of thickness 10mm is at 900～980 ℃ of sintering 2h.The sample surfaces of preparation with diamond polishing after, (0.05～13.5GHz) network analyzer is measured DIELECTRIC CONSTANT according to Hakki-Coleman to adopt Ailment 8719ET rWith quality factor q f, temperature coefficient of resonance frequency τ fAdopt the cavity method to measure, calculate by following formula: τ f=(f 80-f 25)/(f 25* 55), f wherein 80And f 25It is respectively the resonance mid-frequency under 80 ℃ and 25 ℃.Concrete prescription forms and microwave dielectric property sees table 1 for details.
Table 1 ceramic composition and performance table
Numbering X a ε r Qf(GHz) τ f(10 -6/℃) Sintering temperature (℃)
1 0.6 1 64.2 10500 61.6 950
2 0.6 2 62.8 9340 60.3 950
3 0.6 4 61.3 8050 59.5 930
4 0.6 8 58.4 6320 60.8 900
5 0.33 1 65.1 12500 63.2 950
6 0.33 2 64.3 9800 61.5 950
7 0.33 4 62.4 7600 62.3 930
8 0.33 8 58.1 6750 59.8 900
9 0.2 1 66.0 13400 60.2 950
10 0.2 2 64.2 11600 58.4 950
11 0.2 4 63.5 9200 57.3 930
12 0.2 8 59.5 7300 59.5 900

Claims (3)

1. low-temperature sintering Ba 3Ti 4Nb 4O 21Microwave dielectric ceramic materials is characterized in that its raw material consists of:
Ba 3Ti 4Nb 4O 21+awt％[xMnCO 3+(1-x)CuO]
Wherein: 0＜x＜1,0＜a＜10
A is for accounting for Ba 3Ti 4Nb 4O 21Weight fraction.
2. low-temperature sintering Ba according to claim 1 3Ti 4Nb 4O 21Microwave dielectric ceramic materials is characterized in that raw material consists of: Ba 3Ti 4Nb 4O 21+ 1wt% (0.2MnCO 3+ 0.8CuO).
3. low-temperature sintering Ba 3Ti 4Nb 4O 21The preparation method of microwave dielectric ceramic materials is characterized in that preparation technology may further comprise the steps:
1) presses Ba 3Ti 4Nb 4O 21Chemical formula proportioning weighing major ingredient BaCO 3, TiO 2, Nb 2O 5, major ingredient is mixed, pre-burning 2～4h prepares Ba under 1100～1200 ℃ condition 3Ti 4Nb 4O 21The pottery base-material, and grind standby;
2) with xMnCO 3+ (1-x) CuO is mixed in proportion, drying, and pre-burning obtains MnCO under 700～800 ℃ of conditions 3-MnO 2Mixture, with above-mentioned ceramic base-material according to Ba 3Ti 4Nb 4O 21+ awt%[xMnCO 3+ (1-x) CuO] mix, wherein: 0＜x＜1,0＜a＜10, a is for accounting for Ba 3Ti 4Nb 4O 21Weight fraction, obtain being used to prepare the powder of microwave-medium ceramics;
3) the described powder that is used to prepare microwave-medium ceramics is pressed into the circle sheet of diameter 18mm, thickness 8～10mm, at 900～980 ℃ of sintering, insulation 1～4h.
CNB2007101561465A 2007-10-19 2007-10-19 Low-temperature melt Ba3Ti4Nb4O21 microwave dielectric ceramic material and method for producing the same Active CN100522877C (en)

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