CN105217958A - Low Jie's glass ceramic material of a kind of low-temperature sintering and preparation method thereof - Google Patents
Low Jie's glass ceramic material of a kind of low-temperature sintering and preparation method thereof Download PDFInfo
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Abstract
The invention discloses low Jie's glass ceramic material of a kind of low-temperature sintering and preparation method thereof, wherein, the low Jie's glass ceramic material of low-temperature sintering, is made up of following component: the KBS glass of 30wt% ~ 60wt%, the Al of 30wt% ~ 55wt%
2o
3, and the quartz sand of 5wt% ~ 40wt%; The mol ratio of described KBS glass is K
2o:B
2o
3: SiO
2=x:y:z, wherein, 0.002 & lt; X & lt; 0.004,0.2 & lt; Y & lt; 0.3,0.5 & lt; Z & lt; 0.6; Described Al
2o
3for α type Al
2o
3.Glass ceramic material of the present invention, has lower specific inductivity, adjustable from 3.5 ~ 4, low (the tan δ & lt of loss; 3 × 10
-3), the advantages such as temperature coefficient of resonance frequency is stable, are beneficial to and promote the use of.
Description
Technical field
The invention belongs to medium glass ceramic composite substrate Material Field, particularly relate to a kind of low-temperature sintering and there is method compared with low-k and low-loss glass ceramic 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 (3.5 ~ 4), low-loss and stable low Jie's glass ceramic 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, provides low Jie's glass ceramic material of a kind of low-temperature sintering and preparation method thereof, and wherein, the low Jie's glass ceramic material of low-temperature sintering, is made up of following component: the KBS glass of 30wt% ~ 60wt%, the Al of 30wt% ~ 55wt%
2o
3, and the quartz sand of 5wt% ~ 40wt%; 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 the low Jie's glass ceramic material of low-temperature sintering described above, 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 respectively 50 ~ 183%
2o
3and the quartz sand mixing of 8.3 ~ 133%, 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 material.
Further, 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.
Further, in described step c, after oven dry, in 1500 DEG C of air atmosphere, the time of high-temperature fusion is 0.5 ~ 1 hour, and in described step g, in 850 ~ 900 DEG C of air atmosphere, sintering time is 0.5 ~ 1 hour.
Further, described steps d also comprises first to be pulverized the KBS glass frit of gained in step c, and then is solvent with ionized water, carries out wet ball-milling.
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 3.5 ~ 4, low (tan δ <3 × 10 of loss
-3), temperature coefficient of resonance frequency is stablized.
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 5,6,7,8 at 850 degree of sintering;
Fig. 2 is the SEM (scanning electron microscope (SEM) photograph) of embodiment 5 at 850 degree of sintering;
Fig. 3 is the SEM (scanning electron microscope (SEM) photograph) of embodiment 6 at 850 degree of sintering;
Fig. 4 is the SEM (scanning electron microscope (SEM) photograph) of embodiment 7 at 850 degree of sintering;
Fig. 5 is the SEM (scanning electron microscope (SEM) photograph) of embodiment 8 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 30wt% ~ 60wt%, the Al of 30wt% ~ 55wt%
2o
3, and the quartz sand of 5wt% ~ 40wt%; 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 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 respectively 50 ~ 183%
2o
3and the quartz sand mixing of 8.3 ~ 133%, 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 material.
Preferably, 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; The wet ball-milling time in described step b, d and e can regulate according to the granularity requirements of setting.
Preferably, in described step c, after oven dry, in 1500 DEG C of air atmosphere, the time of high-temperature fusion is 0.5 ~ 1 hour, and in described step g, in 850 ~ 900 DEG C of air atmosphere, sintering time is 0.5 ~ 1 hour.
Preferably, in described steps d, in order to improve the wet ball-milling efficiency of KBS glass and obtain more uniform KBS glass powder, first the KBS glass frit obtained in described step c can be pulverized, and then be solvent with ionized water, carry out wet ball-milling; As a feasible scheme, the KBS glass frit obtained directly can be carried out shrend and obtain tiny KBS glass fragment in described step c.
The low Jie's glass ceramic material of low-temperature sintering of the present invention can be used as composite substrate material and widespread use, at KBS glass powder and Al
2o
3on the basis of ceramic phase, by adding quartz sand, then regulate KBS glass, Al
2o
3and the quality accounting of quartz sand three is in suitable scope, thus realize lower specific inductivity and low-loss at a relatively low sintering temperature simultaneously.What deserves to be explained is, in the present invention, quartz sand adds as ceramic fillers, realizes the effect reducing specific inductivity.
Embodiment 1
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 52.5gAl
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 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/T7265.2-1987 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 0.35g, 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 26.25gAl
2o
3and the mixing of 26.25g quartz sand, 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 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 21gAl
2o
3and the mixing of 31.5g quartz sand, 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 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 15.75gAl
2o
3and the mixing of 36.75g quartz sand, 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 material.
Embodiment 5
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 52.5gAl
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 material.
Embodiment 6
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 26.25gAl
2o
3and 26.25g mixing, 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 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 21gAl
2o
3and the mixing of 31.5g quartz sand, 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 material.
Embodiment 8
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 15.75gAl
2o
3and 36.75g mixing, 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 material.
It is known that associative list 1 and table 2 carry out analysis, in embodiment 1 ~ 4, when the mass percent of the KBS glass in glass ceramic material is fixed, along with adding and Al of quartz sand
2o
3the reduction of quality accounting, specific inductivity and the loss of glass ceramic material reduce gradually, this be due to quartz sand as ceramic phase time, its specific inductivity is very little, is about 3.5, so serve the effect obviously reducing specific inductivity.Analyze embodiment 5 ~ 8 known, when the mass percent of KBS glass is fixed, along with adding and Al of quartz sand
2o
3the reduction of quality accounting, the specific inductivity of glass ceramic material still shows the change obviously reduced, meanwhile, but there is obvious increase tendency in loss, analyze its reason, mainly due to quartz sand add excessive after, the wettability between ceramic phase and KBS glass is deteriorated, and defines a lot of pore in sintering process.Specific inductivity due to air is 1, but loss is very large, so just occur reducing further along with quartz sand quality accounting increases specific inductivity, but the obvious result increased appears in loss.So, when quartz sand addition within the specific limits, the reduction of glass ceramic material specific inductivity and loss can be realized, obtained the glass ceramic material of optimum performance by adjustment quartz sand quality accounting.
The X-ray diffractogram comparison diagram of embodiment 5,6,7 and 8 at 850 degree of sintering is shown, as seen along with quartz sand/Al by Fig. 1
2o
3ratio increase, SiO
2diffraction peak stronger; The embodiment 5,6,7 and 8 illustrated respectively by Fig. 2, Fig. 3, Fig. 4 and Fig. 5 is at the scanning electron microscope (SEM) photograph of 850 degree of sintering, visible, along with the increase of quartz sand addition, the pore quantity occurred in the microstructure of glass ceramic material and area increase gradually, comparatively identical with above-mentioned theory analysis.
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. the low Jie's glass ceramic material of low-temperature sintering, is characterized in that, composed of the following components: the KBS glass of 30wt% ~ 60wt%, the Al of 30wt% ~ 55wt%
2o
3, and the quartz sand of 5wt% ~ 40wt%; 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 the low Jie's glass ceramic material of low-temperature sintering 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 respectively 50 ~ 183%
2o
3and the quartz sand mixing of 8.3 ~ 133%, 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 material.
3. the preparation method of the low Jie's glass ceramic material of low-temperature sintering according to claim 2, 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 material of the low-temperature sintering according to Claims 2 or 3, it is characterized in that, in described step c, after oven dry, in 1500 DEG C of air atmosphere, the time of high-temperature fusion is 0.5 ~ 1 hour, 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 the low Jie's glass ceramic material of low-temperature sintering according to claim 2, is characterized in that, steps d also comprises first to be pulverized the KBS glass frit of gained in step c, and then is solvent with ionized water, carries out wet ball-milling.
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CN113979640A (en) * | 2021-10-08 | 2022-01-28 | 云南银峰新材料有限公司 | High-bending-strength low-temperature co-fired ceramic material for microwave substrate and preparation method thereof |
CN113979640B (en) * | 2021-10-08 | 2023-03-24 | 云南银峰新材料有限公司 | High-bending-strength low-temperature co-fired ceramic material for microwave substrate and preparation method thereof |
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