CN104891952A - A low-temperature-sintered low-dielectric-constant glass ceramic composite substrate material and a preparing method thereof - Google Patents

A low-temperature-sintered low-dielectric-constant glass ceramic composite substrate material and a preparing method thereof Download PDF

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CN104891952A
CN104891952A CN201510255805.5A CN201510255805A CN104891952A CN 104891952 A CN104891952 A CN 104891952A CN 201510255805 A CN201510255805 A CN 201510255805A CN 104891952 A CN104891952 A CN 104891952A
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glass
low
kbs
composite substrate
substrate material
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周晓华
杨新石
孙成礼
张玉芹
徐敬业
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University of Electronic Science and Technology of China
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Abstract

A low-temperature-sintered low-dielectric-constant glass ceramic composite substrate material comprises following components: 40-62.5 wt% of KBS glass and 37.5-60 wt% of Al2O3. The KBS glass comprises K2O, B2O3 and SiO2 in a mole ratio of x:y:z, wherein 0.002<x<0.004, 0.2<y<0.3, and 0.5<z<0.6. The Al2O3 is alpha type Al2O3. The material prepared by a preparing method of the glass ceramic composite substrate material is stable in performance, free of heavy metal components, green, and pollution-free, and can be used in high-frequency field products. The sintering temperature reduces from traditional 1200 DEG C or higher to 900 DEG C or lower. The sintering temperature is reduced, thus saving energy. The dielectric constant is adjustable between 4.7 and 5.1. Loss is low (tan[delta]<4*10<-3>). The temperature coefficient of resonance frequency is stable. Mechanical strength is high (higher than 120 MPa).

Description

A kind of low-temperature sintering low Jie's glass-ceramic composite substrate material and preparation method thereof
Technical field
The invention belongs to medium glass ceramic composite substrate Material Field, particularly relate to the method for low-temperature sintering low Jie's glass-ceramic composite substrate material and preparation thereof.
Background technology
The develop rapidly of modern semiconductors industry, has higher requirement to Electronic Packaging, and multi-layer substrate arises at the historic moment.The application of low-temperature co-fired glass ceramic (LTCC) multilager base plate, improve transmission speed and the wiring density of signal, the requirement of VLSI high density packing can be met, it is the key foundation material of modern communication technology, in portable mobile phone, telestar receptor, military radar, there is very important application, in the miniaturization, integrated process of modern communication instrument, just playing increasing effect.The exploitation of low-temperature co-fired glass ceramic material system has become the focus of current Electronic Packaging area research.
Complicated, the densification of components and parts and functionalization in electron device and electronic installation, more and more higher requirement is proposed to base plate for packaging and wiring installation, be mainly manifested in following some: the high speed an urgent demand of (1) Signal transmissions reduces specific inductivity, dielectric loss and reduce lead pitch from; (2) for reducing volume, many electronic components, as resistance, electric capacity, even inductance, be built among substrate; (3) for reducing encapsulation volume, decrease encapsulation link, bare chip actual load is the most typical.Many functions of encapsulation, as electrical connection, physical protection, stress relaxes, and heat radiation is moistureproof, dimensional transitions, and normalization, stdn etc., partly or entirely born by substrate just gradually; (4) good chemical stability and mechanical property.Traditional ceramics Al 2o 3have middle low-k (9 ~ 10), high mechanical strength (>400MPa), excellent chemical stability is a kind of good baseplate material.But, pure Al 2o 3ceramic sintering temperature is higher (1400 ~ 1500 DEG C), can not directly and the low melting point metal such as Ag, Cu burn altogether.In order to reduce sintering temperature, traditional method is a kind of for mixing low melting point oxide, as B 2o 3and V 2o 5, but free B 2o 3and V 2o 5in later stage casting processes, easily cause slurry viscosity excessive and unstable, limit its practical application; Another kind method is Al 2o 3-crystallized glass, in crystallized glass, namely participate in a small amount of pottery as nucleator, the final performance of product is decided by the crystallization degree of sample.But the crystallized glass amount required for this method is very large, causes cost higher, strongly limit the development of glass-ceramic composite substrate material.
Summary of the invention
Goal of the invention of the present invention is: for above-mentioned Problems existing, there is provided one can low-temperature sintering (850 ~ 900 DEG C), there is low-k (4.7 ~ 5.1), low-loss and stable low Jie's glass-ceramic composite substrate material of frequency-temperature coefficient and preparation method thereof.Can be applicable in the civilian and national defense industry such as portable mobile phone, telestar receptor, military radar, technique is simple, is easy to suitability for industrialized production and strong mechanical property.
Technical solution of the present invention is, a kind of low-temperature sintering low Jie's glass-ceramic composite substrate material and preparation method thereof is provided, wherein, low-temperature sintering low Jie's glass-ceramic composite substrate material, composed of the following components: the KBS glass of 40wt% ~ 62.5wt%, and the Al of 37.5wt% ~ 60wt% 2o 3; The mol ratio of described KBS glass is K 2o:B 2o 3: SiO 2=x:y:z, wherein, 0.002<x<0.004,0.2<y<0.3,0.5<z<0.6; Described Al 2o 3for α type Al 2o 3.
The preparation method of low-temperature sintering described above low Jie's glass-ceramic composite substrate material, comprises the following steps:
A, component proportion according to described KBS glass, by K 2cO 3, SiO 2and H 3bO 3powder mixing;
B, be solvent by the mixed powder prepared in step a with deionized water, wet ball-milling mixes, and after oven dry, in 1500 DEG C of air atmosphere, high-temperature fusion forms KBS glass frit;
C, be solvent by step b gained KBS glass frit with deionized water, wet ball-milling, then dries and obtains KBS glass powder at 100 DEG C;
D, by KBS glass powder with account for the Al that its weight percent is 60 ~ 150% 2o 3mixing, with deionized water solvent, wet ball-milling mixes, and the acrylic acid solution that the rear additive capacity of oven dry accounts for 2 ~ 5% of raw material total mass carries out granulation as binding agent;
E, particle steps d granulation obtained are dry-pressing formed, and forming pressure is 10 ~ 20Mpa;
F, material dry-pressing formed for step e to be sintered in 850 ~ 900 DEG C of air atmosphere, make low Jie's glass-ceramic composite substrate material.
Further, the wet ball-milling time in described step b and c is 5 ~ 10 hours, and the wet ball-milling time in steps d is 8 ~ 24 hours.
Further, in described step b, in 1500 DEG C of air atmosphere, the time of high-temperature fusion is 0.5 ~ 1 hour after the drying, and in described steps d, in 850 ~ 900 DEG C of air atmosphere, sintering time is 0.5 ~ 1 hour.
Compared with prior art, beneficial effect of the present invention is embodied in:
1, formula of the present invention is not containing heavy metal component, and can apply in the product of high frequency field, environmental protection is pollution-free, meets the strict standard requirement of RHOS and WEEE of the up-to-date appearance of the European Community.
2, drop to less than 900 DEG C by traditional sintering process more than 1200 DEG C, the further reduction of sintering temperature, has power savings advantages.
3, specific inductivity is adjustable from 4.7 ~ 5.1, low (tan δ <4 × 10 of loss -3), temperature coefficient of resonance frequency is stablized, physical strength high (> 120MPa).
4, the application of low-temperature sintering of the present invention low Jie's glass-ceramic composite substrate material in the communications field, transmission speed and the wiring density of signal can be improved, the requirement of VLSI high density packing can be met, it is the key foundation material of modern communication technology, very important application is had in portable mobile phone, telestar receptor, military radar, in the miniaturization, integrated process of modern communication instrument, just playing increasing effect, there is essential industry using value.
Accompanying drawing explanation
Fig. 1 is the XRD (X-ray diffractogram) of embodiment 3 at 850 degree of sintering;
Fig. 2 is the XRD (X-ray diffractogram) of embodiment 5 at 850 degree of sintering;
Fig. 3 is the XRD (X-ray diffractogram) of embodiment 7 at 850 degree of sintering;
Fig. 4 is the SEM (scanning electron microscope (SEM) photograph) of embodiment 3 at 850 degree of sintering;
Fig. 5 is the SEM (scanning electron microscope (SEM) photograph) of embodiment 5 at 850 degree of sintering;
Fig. 6 is the SEM (scanning electron microscope (SEM) photograph) of embodiment 7 at 850 degree of sintering.
Embodiment
Below in conjunction with drawings and Examples, the present invention is further illustrated.
A kind of low-temperature sintering low Jie's glass-ceramic composite substrate material, is characterized in that, composed of the following components: the KBS glass of 40wt% ~ 62.5wt%, and the Al of 37.5wt% ~ 60wt% 2o 3; The mol ratio of described KBS glass is K 2o:B 2o 3: SiO 2=x:y:z, wherein, Al described in 0.002<x<0.004,0.2<y<0.3,0.5<z<0.6 2o 3for α type Al 2o 3.
The preparation method of low-temperature sintering described above low Jie's glass-ceramic composite substrate material, comprises the following steps:
A, component proportion according to described KBS glass, by K 2cO 3, SiO 2and H 3bO 3powder mixing;
B, be solvent by the mixed powder prepared in step a with deionized water, wet ball-milling mixes, and after oven dry, in 1500 DEG C of air atmosphere, high-temperature fusion forms KBS glass frit;
C, be solvent by step b gained KBS glass frit with deionized water, wet ball-milling, then dries and obtains KBS glass powder at 100 DEG C;
D, by KBS glass powder with account for the Al that its weight percent is 60 ~ 150% 2o 3mixing, with deionized water solvent, wet ball-milling mixes, and the acrylic acid solution that the rear additive capacity of oven dry accounts for 2 ~ 5% of raw material total mass carries out granulation as binding agent;
E, particle steps d granulation obtained are dry-pressing formed, and forming pressure is 10 ~ 20Mpa;
F, material dry-pressing formed for step e to be sintered in 850 ~ 900 DEG C of air atmosphere, make low Jie's glass-ceramic composite substrate material.
As preferably, the wet ball-milling time in described step b and c is 5 ~ 10 hours, and the wet ball-milling time in steps d is 8 ~ 24 hours.
As preferably, in described step b, in 1500 DEG C of air atmosphere, the time of high-temperature fusion is 0.5 ~ 1 hour after the drying, and in described steps d, in 850 ~ 900 DEG C of air atmosphere, sintering time is 0.5 ~ 1 hour.
Embodiment 1
A, by K 2cO 3, SiO 2and H 3bO 3powder mixing, its quality is respectively 0.25g, 30g and 17.25g;
B, the powder prepared by step a take deionized water as solvent, and wet ball-milling mixes 6 hours, after oven dry in 1500 DEG C of air atmosphere high-temperature fusion 1 hour, form KBS glass frit;
C, take deionized water as solvent by KBS glass frit, wet ball-milling 6 hours, then dries and obtains KBS glass powder at 100 DEG C;
D, by above-mentioned KBS glass powder and 52.5g Al 2o 3mixing, with deionized water solvent, wet ball-milling mixes 8 hours, and the acrylic acid solution that the rear additive capacity of oven dry accounts for 2 ~ 5% of raw material total mass carries out granulation as binding agent;
E, the particle above-mentioned granulation obtained are dry-pressing formed, and forming pressure is 20Mpa;
F, material dry-pressing formed for step e is sintered 1 hour in 850 DEG C of air atmosphere, make low Jie's glass-ceramic composite substrate material.
Actual proportioning and the sintering temperature of each component of embodiment of the present invention 1-8 low temperature sintering low Jie glass-ceramic composite substrate material is listed in table 1.
The microwave dielectric property of low-temperature sintering low Jie's glass-ceramic composite substrate material that 1-8 embodiment of the present invention obtains is given in table 2, the embodiment of the present invention adopts cylindrical dielectric resonator method to carry out the evaluation of microwave dielectric property, and detection method is GB/T 7265.2-1987 open type cell method.
Table 1
Table 2
Embodiment 2
A, by K 2cO 3, SiO 2and H 3bO 3powder mixing, its quality is respectively 0.25g, 30g and 17.25g;
B, the powder prepared by step a take deionized water as solvent, and wet ball-milling mixes 6 hours, after oven dry in 1500 DEG C of air atmosphere high-temperature fusion 1 hour, form KBS glass frit;
C, take deionized water as solvent by KBS glass frit, wet ball-milling 6 hours, then dries and obtains KBS glass powder at 100 DEG C;
D, by above-mentioned KBS glass powder and 52.5g Al 2o 3mixing, with deionized water solvent, wet ball-milling mixes 8 hours, and the acrylic acid solution that the rear additive capacity of oven dry accounts for 2 ~ 5% of raw material total mass carries out granulation as binding agent;
E, the particle above-mentioned granulation obtained are dry-pressing formed, and forming pressure is 20Mpa;
F, material dry-pressing formed for step e is sintered 1 hour in 875 DEG C of air atmosphere, make low Jie's glass-ceramic composite substrate material.
Embodiment 3
A, by K 2cO 3, SiO 2and H 3bO 3powder mixing, its quality is respectively 0.35g, 28g and 19.15g;
B, the powder prepared by step a take deionized water as solvent, and wet ball-milling mixes 6 hours, after oven dry in 1500 DEG C of air atmosphere high-temperature fusion 1 hour, form KBS glass frit;
C, take deionized water as solvent by KBS glass frit, wet ball-milling 6 hours, then dries and obtains KBS glass powder at 100 DEG C;
D, by above-mentioned KBS glass powder and 52.5g Al 2o 3mixing, with deionized water solvent, wet ball-milling mixes 8 hours, and the acrylic acid solution that the rear additive capacity of oven dry accounts for 2 ~ 5% of raw material total mass carries out granulation as binding agent;
E, the particle above-mentioned granulation obtained are dry-pressing formed, and forming pressure is 20Mpa;
F, material dry-pressing formed for step e is sintered 1 hour in 850 DEG C of air atmosphere, make low Jie's glass-ceramic composite substrate material.
Embodiment 4
A, by K 2cO 3, SiO 2and H 3bO 3powder mixing, its quality is respectively 0.35g, 28g and 19.15g;
B, the powder prepared by step a take deionized water as solvent, and wet ball-milling mixes 6 hours, after oven dry in 1500 DEG C of air atmosphere high-temperature fusion 1 hour, form KBS glass frit;
C, take deionized water as solvent by KBS glass frit, wet ball-milling 6 hours, then dries and obtains KBS glass powder at 100 DEG C;
D, by above-mentioned KBS glass powder and 52.5g Al 2o 3mixing, with deionized water solvent, wet ball-milling mixes 8 hours, and the acrylic acid solution that the rear additive capacity of oven dry accounts for 2 ~ 5% of raw material total mass carries out granulation as binding agent;
E, the particle above-mentioned granulation obtained are dry-pressing formed, and forming pressure is 20Mpa;
F, material dry-pressing formed for step e is sintered 1 hour in 875 DEG C of air atmosphere, make low Jie's glass-ceramic composite substrate material.
Embodiment 5
A, by K 2cO 3, SiO 2and H 3bO 3powder mixing, its quality is respectively 0.45g, 26g and 21.05g;
B, the powder prepared by step a take deionized water as solvent, and wet ball-milling mixes 6 hours, after oven dry in 1500 DEG C of air atmosphere high-temperature fusion 1 hour, form KBS glass frit;
C, take deionized water as solvent by KBS glass frit, wet ball-milling 6 hours, then dries and obtains KBS glass powder at 100 DEG C;
D, by above-mentioned KBS glass powder and 52.5g Al 2o 3mixing, with deionized water solvent, wet ball-milling mixes 8 hours, and the acrylic acid solution that the rear additive capacity of oven dry accounts for 2 ~ 5% of raw material total mass carries out granulation as binding agent;
E, the particle above-mentioned granulation obtained are dry-pressing formed, and forming pressure is 20Mpa;
F, material dry-pressing formed for step e is sintered 1 hour in 850 DEG C of air atmosphere, make low Jie's glass-ceramic composite substrate material.
Embodiment 6
A, by K 2cO 3, SiO 2and H 3bO 3powder mixing, its quality is respectively 0.45g, 26g and 21.05g;
B, the powder prepared by step a take deionized water as solvent, and wet ball-milling mixes 6 hours, after oven dry in 1500 DEG C of air atmosphere high-temperature fusion 1 hour, form KBS glass frit;
C, take deionized water as solvent by KBS glass frit, wet ball-milling 6 hours, then dries and obtains KBS glass powder at 100 DEG C;
D, by above-mentioned KBS glass powder and 52.5g Al 2o 3mixing, with deionized water solvent, wet ball-milling mixes 8 hours, and the acrylic acid solution that the rear additive capacity of oven dry accounts for 2 ~ 5% of raw material total mass carries out granulation as binding agent;
E, the particle above-mentioned granulation obtained are dry-pressing formed, and forming pressure is 20Mpa;
F, material dry-pressing formed for step e is sintered 1 hour in 875 DEG C of air atmosphere, make low Jie's glass-ceramic composite substrate material.
Embodiment 7
A, by K 2cO 3, SiO 2and H 3bO 3powder mixing, its quality is respectively 0.55g, 24g and 22.95g;
B, the powder prepared by step a take deionized water as solvent, and wet ball-milling mixes 6 hours, after oven dry in 1500 DEG C of air atmosphere high-temperature fusion 1 hour, form KBS glass frit;
C, take deionized water as solvent by KBS glass frit, wet ball-milling 6 hours, then dries and obtains KBS glass powder at 100 DEG C;
D, by above-mentioned KBS glass powder and 52.5g Al 2o 3mixing, with deionized water solvent, wet ball-milling mixes 8 hours, and the acrylic acid solution that the rear additive capacity of oven dry accounts for 2 ~ 5% of raw material total mass carries out granulation as binding agent;
E, the particle above-mentioned granulation obtained are dry-pressing formed, and forming pressure is 20Mpa;
F, material dry-pressing formed for step e is sintered 1 hour in 850 DEG C of air atmosphere, make low Jie's glass-ceramic composite substrate material.
Embodiment 8
A, by K 2cO 3, SiO 2and H 3bO 3powder mixing, its quality is respectively 0.53g, 24g and 22.95g;
B, the powder prepared by step a take deionized water as solvent, and wet ball-milling mixes 6 hours, after oven dry in 1500 DEG C of air atmosphere high-temperature fusion 1 hour, form KBS glass frit;
C, take deionized water as solvent by KBS glass frit, wet ball-milling 6 hours, then dries and obtains KBS glass powder at 100 DEG C;
D, by above-mentioned KBS glass powder and 52.5g Al 2o 3mixing, with deionized water solvent, wet ball-milling mixes 8 hours, and the acrylic acid solution that the rear additive capacity of oven dry accounts for 2 ~ 5% of raw material total mass carries out granulation as binding agent;
E, the particle above-mentioned granulation obtained are dry-pressing formed, and forming pressure is 20Mpa;
F, material dry-pressing formed for step e is sintered 1 hour in 875 DEG C of air atmosphere, make low Jie's glass-ceramic composite substrate material.
The X-ray diffractogram that the embodiment 3,5 and 7 illustrated respectively by Fig. 1, Fig. 2 and Fig. 3 sinters at 850 degree, as seen along with K 2cO 3the no third that adds generate mutually; Fig. 4 illustrates the scanning electron microscope (SEM) photograph of embodiment 3 at 850 degree of sintering, and the embodiment 3,5 and 7 illustrated respectively by Fig. 4, Fig. 5 and Fig. 6 is at the scanning electron microscope (SEM) photograph of 850 degree of sintering, visible, K within the specific limits 2cO 3greatly facilitate sintered density, thus improve dielectric properties and the physical strength of glass-ceramic.
Those of ordinary skill in the art will appreciate that, embodiment described here is to help reader understanding's principle of the present invention, should be understood to that protection scope of the present invention is not limited to so special statement and embodiment.Those of ordinary skill in the art can make various other various concrete distortion and combination of not departing from essence of the present invention according to these technology enlightenment disclosed by the invention, and these distortion and combination are still in protection scope of the present invention.

Claims (5)

1. low-temperature sintering low Jie's glass-ceramic composite substrate material, is characterized in that, composed of the following components: the KBS glass of 40wt% ~ 62.5wt%, and the Al of 37.5wt% ~ 60wt% 2o 3; The mol ratio of described KBS glass is K 2o:B 2o 3: SiO 2=x:y:z, wherein, Al described in 0.002<x<0.004,0.2<y<0.3,0.5<z<0.6 2o 3for α type Al 2o 3.
2. the preparation method of low-temperature sintering low Jie's glass-ceramic composite substrate material as claimed in claim 1, comprises the following steps:
A, component proportion requirement according to described KBS glass, by K 2cO 3, SiO 2and H 3bO 3powder mixing;
B, be solvent by the above-mentioned mixed powder prepared with deionized water, wet ball-milling mixes, and then dries;
C, by the high-temperature fusion in 1500 DEG C of air atmosphere of the powder after above-mentioned oven dry, form KBS glass frit;
D, be solvent by above-mentioned KBS glass frit with deionized water, wet ball-milling, then dries at 100 DEG C, obtains KBS glass powder;
E, by KBS glass powder with account for the Al that its weight percent is 60 ~ 150% 2o 3mixing, with deionized water solvent, wet ball-milling mixes, and the acrylic acid solution that the rear additive capacity of oven dry accounts for 2 ~ 5% of raw material total mass carries out granulation as binding agent;
F, the particle above-mentioned granulation obtained are dry-pressing formed, and forming pressure is 10 ~ 20Mpa;
G, above-mentioned dry-pressing formed material to be sintered in 850-900 DEG C of air atmosphere, make low Jie's glass-ceramic composite substrate material.
3. the preparation method of low-temperature sintering according to claim 2 low Jie's glass-ceramic composite substrate material, is characterized in that, the wet ball-milling time in described step b and d is 5 ~ 10 hours, and the wet ball-milling time in step e is 8 ~ 24 hours.
4. the preparation method of the low Jie's glass-ceramic of the low-temperature sintering according to Claims 2 or 3 composite substrate material, it is characterized in that, in described step c, in 1500 DEG C of air atmosphere, the time of high-temperature fusion is 0.5 ~ 1 hour after the drying, and in described step g, in 850-900 DEG C of air atmosphere, sintering time is 0.5 ~ 1 hour.
5. the preparation method of low-temperature sintering according to claim 2 low Jie's glass-ceramic composite substrate material, it is characterized in that, steps d also comprises first to be pulverized the KBS glass frit of gained in step c, and then by its with account for the Al that its weight percent is 60 ~ 150% 2o 3mixing.
CN201510255805.5A 2015-05-19 2015-05-19 A low-temperature-sintered low-dielectric-constant glass ceramic composite substrate material and a preparing method thereof Pending CN104891952A (en)

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CN109650871A (en) * 2019-01-29 2019-04-19 电子科技大学 A kind of ZnAl2O4Ceramic systems material and preparation method thereof
CN113845355A (en) * 2021-10-18 2021-12-28 安徽蓝讯通信技术有限公司 Preparation method of LTCC green tape slurry

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106187131A (en) * 2016-07-13 2016-12-07 吴迪 A kind of preparation method of high compactness piezoceramic material
CN109650871A (en) * 2019-01-29 2019-04-19 电子科技大学 A kind of ZnAl2O4Ceramic systems material and preparation method thereof
CN113845355A (en) * 2021-10-18 2021-12-28 安徽蓝讯通信技术有限公司 Preparation method of LTCC green tape slurry

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Application publication date: 20150909