CN103771842A - LTCC (Low Temperature Co-fired Ceramics) microwave ceramic material with low cost, low dielectric constant and low loss and preparation method thereof - Google Patents
LTCC (Low Temperature Co-fired Ceramics) microwave ceramic material with low cost, low dielectric constant and low loss and preparation method thereof Download PDFInfo
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- CN103771842A CN103771842A CN201410012814.7A CN201410012814A CN103771842A CN 103771842 A CN103771842 A CN 103771842A CN 201410012814 A CN201410012814 A CN 201410012814A CN 103771842 A CN103771842 A CN 103771842A
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000000919 ceramic Substances 0.000 title abstract description 7
- 239000000463 material Substances 0.000 claims abstract description 24
- 239000011521 glass Substances 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 238000000498 ball milling Methods 0.000 claims abstract description 10
- 238000005303 weighing Methods 0.000 claims abstract description 4
- 238000005245 sintering Methods 0.000 claims description 27
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 239000003082 abrasive agent Substances 0.000 claims description 3
- 239000003292 glue Substances 0.000 claims description 3
- 238000005469 granulation Methods 0.000 claims description 3
- 230000003179 granulation Effects 0.000 claims description 3
- 239000004570 mortar (masonry) Substances 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 2
- 238000010791 quenching Methods 0.000 claims description 2
- 230000000171 quenching effect Effects 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 229910052844 willemite Inorganic materials 0.000 abstract description 4
- 239000013078 crystal Substances 0.000 abstract description 2
- 239000000758 substrate Substances 0.000 abstract description 2
- 238000010304 firing Methods 0.000 abstract 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 abstract 2
- UPWOEMHINGJHOB-UHFFFAOYSA-N oxo(oxocobaltiooxy)cobalt Chemical compound O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 abstract 2
- 229910052681 coesite Inorganic materials 0.000 abstract 1
- 229910052906 cristobalite Inorganic materials 0.000 abstract 1
- 238000000465 moulding Methods 0.000 abstract 1
- 239000000377 silicon dioxide Substances 0.000 abstract 1
- 235000012239 silicon dioxide Nutrition 0.000 abstract 1
- 229910052682 stishovite Inorganic materials 0.000 abstract 1
- 229910052905 tridymite Inorganic materials 0.000 abstract 1
- 239000011701 zinc Substances 0.000 description 22
- 238000005516 engineering process Methods 0.000 description 7
- 238000000034 method Methods 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 4
- 238000009766 low-temperature sintering Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 230000005496 eutectics Effects 0.000 description 3
- 238000010348 incorporation Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 239000003989 dielectric material Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000004110 Zinc silicate Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000000502 dialysis Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 235000021180 meal component Nutrition 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000010327 methods by industry Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- XSMMCTCMFDWXIX-UHFFFAOYSA-N zinc silicate Chemical compound [Zn+2].[O-][Si]([O-])=O XSMMCTCMFDWXIX-UHFFFAOYSA-N 0.000 description 1
- 235000019352 zinc silicate Nutrition 0.000 description 1
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Abstract
The invention provides a LTCC (Low Temperature Co-fired Ceramics) microwave ceramic material with low cost, low dielectric constant and low loss, which is formed through taking (Zn(1-x)Cox)2SiO4 as a main crystal phase, and a preparation method thereof, wherein x is not smaller than 0.05 and not greater than 0.1. According to the ceramic material, a proper amount of Co<2+> is substituted based on Zn2SiO4 of a willemite structure, the firing temperature is lowered by adopting LBSCA glass assisted firing, the low-temperature firing of 900 DEG C can be realized, the prepared microwave ceramic material has the dielectric constant [epsilon]r of 6.1-6.6 and has extremely low microwave loss, the quality factor Q*f is higher than 30,000GHz and can reach 56,939GHz to the maximum, and the temperature coefficient of resonance frequency ([tau]f) is about -55ppm/DEG C. The preparation method comprises the steps of sequentially carrying out weighing, first-time ball milling, baking, pre-firing, doping, second-time ball milling, baking, granulating, molding and firing on raw materials, namely Co2O3, ZnO and SiO2. The production raw materials are cheap, the production cost is low, and the preparation process is simple. When the microwave ceramic material serves as an LTCC microwave dielectric substrate or device material, the loss of microwave devices or modules can be remarkably lowered.
Description
Technical field
The invention belongs to electron ceramic material and manufacture field thereof, be specifically related to the low Jie's low-loss of a kind of low cost LTCC microwave ceramic material and preparation method thereof.
Background technology
In recent years, be that universal electric complete machine, signal equipment or civilian consumer electronic product are all rapidly to miniaturization, lightweight, integrated, multifunction and high reliability future development in the world.LTCC(LTCC) technology is as a kind of advanced person's 3 D stereo assembling integrated technology, and create condition for passive device and passive/active part mix integrated development, and in lamination sheet type passive device, obtained a wide range of applications rapidly.A lot of electronically materials and component manufacturing enterprises and colleges and universities have all launched research and development and have produced various LTCC planar passive devices and assembly, and in order to obtain high performance LTCC passive integrated devices and assembly, first need to have high performance LTCC material.But the high-performance LTCC material of commercialization at present is mainly abroad monopolized, domesticly fail all the time to obtain key breakthrough in this field, cause LTCC integrated device and the assembly cost of China's research and development very high, be unfavorable for application and the popularization of corresponding product, due under one's control in core key technology, seriously hinder the development of China LTCC industry on the other hand.Therefore it is extremely urgent that, exploitation has the high-performance LTCC material of independent intellectual property right.
LTCC microwave ceramic material is an application branch very widely in LTCC material.General microwave ceramic material sintering temperature all more than 1100 ℃, but for and LTCC technique (being generally between 800 ℃～950 ℃) compatibility, its sintering temperature need be reduced to below 950 ℃.The normal method adopting mainly comprises that interpolation eutectic oxide compound or glass help burning, introduce chemical synthesis process and adopts superfine powder to do raw material etc.; Latter two is with high costs and have certain process limitation, thereby adds eutectic oxide compound or glass is the main method that realizes at present LTCC microwave ceramic material.Even if but take this method, and the sintering temperature of current many microwave ceramic materials is too high, is also difficult to realize low-temperature sintering, and secondly, too much mixing of eutectic oxide compound or glass, also can form very large impact to the drain performance of material, causes Q × f to decline very large.
At first, zinc silicate (Zn
2siO
4) be that it is easy to crystallization in glaze as the crystallizing agent in a kind of crystalline glaze, crystalline substance is spent large and is justified, and is therefore suitable for some ornamental vase series products.Afterwards, Zn
2siO
4used fluorescent material field by the more ion flat-panel monitor that is applied in, pass through Mn
2+doping, forms Zn
2siO
4: Mn2+, this material can demonstrate good luminescent properties under 253nm light wave excites, prepare simple, with low costly due to it, and there are numerous advantages such as chromaticity coordinates is good, relative brightness is high, become the most promising ion flat-panel monitor green fluorescence meal component at present.Zn
2siO
4just study in recent years as microwave dielectric material, its structure is willemite structure, belongs to trigonal system, and space group is R-3, a=1.3971nm, c=0.9334; Each Zn atom and Si atom form tetrahedrons with four Sauerstoffatoms around.Zn
2siO
4sintering temperature be that more than 1400 ℃ dielectric properties are as follows: ε
rbe about 7～8, Q × f and range up to 240000GHz, temperature factor τ
f=(50～-40) ppm/ ℃, over-all properties is fine, and the cost of raw materials is all very low.But Zn
2siO
4an outstanding shortcoming of stupalith is exactly that sintering temperature is too high, by direct oxygenates or glass, sintering temperature is dropped to 900 ℃, and doping needs very large, can cause dielectric loss significantly to increase.At document " Low temperature preparation of the Zn
2siO
4ceramics with the addition of BaO and B
2o
3" people such as Song Chen discloses BaO and B in (J Mater Sci:Mater Electron (2011) 22:1274 – 1281)
2o
3doping of Zn
2siO
4on the impact of its sintering temperature and performance, and under 900 ℃ of sintering temperatures, obtain the following ceramic ε of microwave property
r=6.4～6.7, Q × f=25000GHz, τ
f=-30ppm/ ℃.In document " Low-Temperature Sintering and Microwave Dielectric Propertiesof the Zn2SiO4Ceramics " (J.Am.Ceram.Soc., 91[2] 671 – 674 (2008) DOI:10.1111/j.1551-2916.2007.02187.x), Jin-Seong Kim has reported B
2o
3add Zn to
1.8siO
3.8, obtained good microwave property: ε
r=5.7, Q × f=53000GHz, τ
f=-16ppm/ ℃.Document " Effect of the B
2o
3addition on the sintering behavior and microwave dielectric properties of Ba
3(VO4)
2– Zn
1.87siO
3.87composite ceramics " Yang Lv has reported Ba in (Ceramics International39 (2013) 2545 – 2550)
3(VO
4)
2with Zn
1.87siO
3.87compound, then add B
2o
3reduce sintering temperature, end formulation is 3wt%B
2o
3+ 0.5Ba
3(VO4)
2-0.5Zn
1.87siO
3.87; Although by compound Ba
3(VO
4)
2can reduce sintering temperature and improving performance, but there is very large change in specific inductivity; Its final microwave property parameter is: Q × f=34300GHz, ε
r=9.8, τ
f=-1.1ppm/ ℃.
In sum, LTCC microwave ceramic material of low-k, low lossy microwave and preparation method thereof becomes our research emphasis.
Summary of the invention
The object of the invention is to the defect for prior art, provide a kind of with (Zn
1-xco
x)
2siO
4, the low Jie's low-loss of low cost LTCC microwave ceramic material that 0.05≤x≤0.1 is principal crystalline phase composition and preparation method thereof, can realize 900 ℃ of low-temperature sinterings, is prepared into this microwave ceramic material DIELECTRIC CONSTANT ε
rbe 6.1～6.6, have extremely low lossy microwave, quality factor q × f value all more than 30000GHz, can reach 56939GHz, temperature coefficient of resonance frequency τ
fbe about-55ppm/ ℃; And raw materials for production are cheap, production cost is low, preparation technology is simple.This microwave ceramics, when as LTCC microwave-medium substrate or device material, can significantly reduce the loss of microwave device or module.
Technical scheme of the present invention is: the low Jie's low-loss of low cost LTCC microwave ceramic material, it is characterized in that, and the molecular structure expression formula of this stupalith is (Zn
1-xco
x)
2siO
4, wherein 0.05≤x≤0.1.
Preferably, described stupalith is by raw material ZnO, Co
2o
3, SiO
2znO:Co in molar ratio
2o
3: SiO
2=2 (1-x): x:1 preparations, wherein 0.05≤x≤0.1.
The preparation method of the low Jie's low-loss of described low cost LTCC microwave ceramic material, is characterized in that, comprises the following steps;
Preferably, described LBSCA glass is by raw material Li in molar ratio
2cO
3: B
2o
3: SiO
2: CaO:Al
2o
3=52.45:31.06:11.99:2.25:2.25 preparation, weighs raw material in proportion, and wet mixing packs crucible into after drying, and is warmed up to 1000 ℃ by 3 ℃/point in sintering oven, is incubated after 2 hours and directly from stove, takes out and pour quenching in cold water into, then dries levigate obtaining.
The present invention is at the Zn of willemite structure
2siO
4on basis, carry out the addition of C o
2+substitute, use Co
2+substitute Zn
2+mainly that structure is identical, can reach solid solution condition because their ionic radius is close; And in the time of sintering, introduce Co
2+interionic mobility can be increased, thereby material sintering temperature can be reduced to a certain extent, simultaneously very little on microwave property impact.Adopt LBSCA glass to help burning to be mainly because it has lower melting temperature (400 ℃), in the time of sintering, can form liquid phase, main phase grain is produced to liquid phase parcel, can effectively impel grain growth, improve densification degree, reduce crystal boundary and defect, to reach the object that material system sintering temperature is reduced to 900 ℃.Meanwhile, LBSCA glass and (Zn
1-xco
x)
2siO
4between can there is not obvious composition dialysis, can not cause larger impact to the dielectric loss of material system.
To sum up, the low Jie's low-loss of low cost provided by the invention LTCC microwave ceramic material after tested, its DIELECTRIC CONSTANT ε
rbetween 6.1～6.6; Q × f value all, more than 30000GHz, is up to 56939GHz; Temperature coefficient of resonance frequency τ
fbe about-55ppm/ ℃.
The major advantage of the low Jie's low-loss of low cost provided by the invention LTCC microwave ceramic material is:
1, specific inductivity, in 6.1～6.6 left and right, can be widely used in LTCC microwave base plate, laminated microwave device and module.
2, have extremely low dielectric loss, in the time of 900 ℃ of low-temperature sinterings, Q × f reaches as high as 56939GHz.
3, raw materials for production are cheap, and process engineering is simple, and handled easily being beneficial to reduces costs.
Accompanying drawing explanation
Fig. 1 is preparation technology's schematic flow sheet of the low Jie's low-loss of low cost provided by the invention LTCC microwave ceramic material.
Fig. 2 is prepared into the microwave dielectric property of LTCC microwave ceramic material with LBSCA glass incorporation and sintering temperature variation relation graphic representation in embodiment 1.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is further explained.
The low Jie's low-loss of low cost LTCC microwave ceramic material, the molecular structure expression formula of this stupalith is (Zn
1-xco
x)
2siO
4, wherein 0.05≤x≤0.1.Get x=0.05, its molecular structure expression formula is (Zn
0.95co
0.05)
2siO
4; By raw material ZnO, Co
2o
3, SiO
2znO:Co in molar ratio
2o
3: SiO
2=1.9:0.05:1 preparation.
As shown in Figure 1, concrete preparation method comprises the following steps its preparation technology's flow process:
Low Jie's low-loss LTCC microwave ceramic material performance that this specific embodiments obtains: DIELECTRIC CONSTANT ε
rbe about 6.5, Q × f and be up to 56939GHz, temperature factor is about τ
f=-55ppm/ ℃, illustrates that this dielectric material loss is very low.
In addition, by appropriate change (Zn
1-xco
x)
2siO
4x value and LBSCA glass incorporation y wt% and final sintering temperature (850～950 ℃) in (0.05≤x≤0.1), there is certain variation in the microwave property of material system.Be illustrated in figure 2 and work as x=0.05, when y changes from 1～5, under different sintering temperatures, be prepared into the DIELECTRIC CONSTANT ε of LTCC microwave ceramic material
rvariation relation curve with dielectric loss; Can see and work as x=0.05, LBSCA glass incorporation is 2, and when sintering temperature is 900 ℃, dielectric loss is minimum.
Claims (4)
1. the low Jie's low-loss of low cost LTCC microwave ceramic material, is characterized in that, the molecular structure expression formula of this stupalith is (Zn
1-xco
x)
2siO
4, wherein 0.05≤x≤0.1.
2. by the low Jie's low-loss of low cost LTCC microwave ceramic material described in claim 1, it is characterized in that, described stupalith is by raw material ZnO, Co
2o
3, SiO
2znO:Co in molar ratio
2o
3: SiO
2=2 (1-x): x:1 preparations, wherein 0.05≤x≤0.1.
3. by the preparation method of the low Jie's low-loss of low cost LTCC microwave ceramic material described in claim 1, it is characterized in that, comprise the following steps;
Step 1. with ZnO, Co
2o
3, SiO
2for initial feed, ZnO:Co in molar ratio
2o
3: SiO
2=2 (1-x): x:1 convert out respective quality and carry out weighing, ball milling, the even post-drying of batch mixing, wherein 0.05≤x≤0.1, to form molecular structural formula be (Zn
1-xco
x)
2siO
4, 0.05≤x≤0.1;
Step 2. step 1 gained is dried after material sieves and put into crucible and compacting, rise to 1200 ℃ carry out pre-burning by the temperature rise rate of 3 ℃/point, be incubated 3 hours, furnace cooling obtains Preburning material;
Step 3. the block Preburning material of step 2 gained is taken out from crucible to put into mortar levigate, then add the LBSCA glass powder of 1～5wt% in ball mill, to carry out secondary ball milling;
Step 4. after secondary ball abrasive material that step 3 is obtained is dried, add mass fraction be 30%～40% PVA solution carry out granulation and dry-pressing formed be cylinder;
Step 5. step 4 gained sample is put into sintering oven, slowly rise to 300 ℃ of insulations 2 hours by the temperature rise rates of 2 ℃/point, continue to be warming up to 550 ℃ of insulations 4 hours, to get rid of moisture and the glue in green compact; And then be warming up to 850 ℃～950 ℃ by the temperature rise rate of 4 ℃/point and carry out sintering, being incubated 3 hours, then being cooled to 550 ℃ by the rate of temperature fall of 4 ℃/point, last furnace cooling obtains low Jie's low-loss LTCC microwave ceramic material.
4. by the preparation method of the low Jie's low-loss of low cost LTCC microwave ceramic material described in claim 3, it is characterized in that, described LBSCA glass is by raw material Li in molar ratio
2cO
3: B
2o
3: SiO
2: CaO:Al
2o
3=52.45:31.06:11.99:2.25:2.25 preparation, weighs raw material in proportion, and wet mixing packs crucible into after drying, and is warmed up to 1000 ℃ by 3 ℃/point in sintering oven, is incubated after 2 hours and directly from stove, takes out and pour quenching in cold water into, then dries levigate obtaining.
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Cited By (12)
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| CN104030671A (en) * | 2014-06-09 | 2014-09-10 | 电子科技大学 | LiZnTi ferrite material for LTCC phase shifter and preparation method of material |
| CN104402427A (en) * | 2014-11-27 | 2015-03-11 | 电子科技大学 | Low-coercivity LiZnTi gyromagnetic ferrite material and preparation method thereof |
| CN104829239A (en) * | 2015-03-27 | 2015-08-12 | 电子科技大学 | Low temperature co-fired ceramic (LTCC) power inductor component matrix and ceramic dielectric material matching co-firing method |
| CN108314437A (en) * | 2018-04-11 | 2018-07-24 | 电子科技大学 | A kind of low-temperature sintering low-k ceramic substrate material and preparation method |
| CN110372347A (en) * | 2018-04-12 | 2019-10-25 | 中国科学院上海硅酸盐研究所 | A kind of low-loss dielectric constant microwave ceramic material and preparation method thereof |
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| CN111377721A (en) * | 2018-12-27 | 2020-07-07 | 中国科学院上海硅酸盐研究所 | Low-temperature co-fired ceramic material and preparation method thereof |
| CN112279632A (en) * | 2020-10-31 | 2021-01-29 | 林玉婷 | Microwave dielectric ceramic and preparation method thereof |
| CN112898012A (en) * | 2021-04-12 | 2021-06-04 | 无锡市高宇晟新材料科技有限公司 | Microwave dielectric ceramic material and preparation method thereof |
| CN113292338A (en) * | 2021-06-04 | 2021-08-24 | 电子科技大学 | Ba-Co-V based low dielectric low-firing microwave ceramic material and preparation method thereof |
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| CN104030671A (en) * | 2014-06-09 | 2014-09-10 | 电子科技大学 | LiZnTi ferrite material for LTCC phase shifter and preparation method of material |
| CN104402427A (en) * | 2014-11-27 | 2015-03-11 | 电子科技大学 | Low-coercivity LiZnTi gyromagnetic ferrite material and preparation method thereof |
| CN104829239A (en) * | 2015-03-27 | 2015-08-12 | 电子科技大学 | Low temperature co-fired ceramic (LTCC) power inductor component matrix and ceramic dielectric material matching co-firing method |
| CN108314437B (en) * | 2018-04-11 | 2021-06-15 | 电子科技大学 | Low-temperature sintered low-dielectric-constant ceramic substrate material and preparation method thereof |
| CN108314437A (en) * | 2018-04-11 | 2018-07-24 | 电子科技大学 | A kind of low-temperature sintering low-k ceramic substrate material and preparation method |
| CN110372347B (en) * | 2018-04-12 | 2021-10-01 | 中国科学院上海硅酸盐研究所 | Low-loss low-dielectric-constant microwave ceramic material and preparation method thereof |
| CN110372347A (en) * | 2018-04-12 | 2019-10-25 | 中国科学院上海硅酸盐研究所 | A kind of low-loss dielectric constant microwave ceramic material and preparation method thereof |
| CN111377721A (en) * | 2018-12-27 | 2020-07-07 | 中国科学院上海硅酸盐研究所 | Low-temperature co-fired ceramic material and preparation method thereof |
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