CN105217958B - 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, it is made up of following components：30wt%~60wt% KBS glass, 30wt%~55wt% Al2O3, and 5wt%~40wt% quartz sand；The mol ratio of the KBS glass is K2O：B2O3：SiO2=x：y：Z, wherein, 0.002<x<0.004,0.2<y<0.3,0.5<z<0.6；The Al2O3For α types Al2O3.Glass ceramic material of the present invention, there is relatively low dielectric constant, it is adjustable from 3.5~4, low (tan δ are lost<3×10‑3), the advantages such as temperature coefficient of resonance frequency is stable, beneficial to promoting the use of.
Description
Technical field
The invention belongs to medium glass ceramic composite substrate Material Field, more particularly to a kind of low-temperature sintering to have relatively low Jie
Electric constant and low-loss glass ceramic material and its method for preparation.
Background technology
The rapid development of modern semiconductors industry, higher requirement is proposed to Electronic Packaging, and multi-layer substrate meets the tendency of
And give birth to.The application of low-temperature co-fired glass ceramic (LTCC) multilager base plate, the transmission speed and wiring density of signal are improved, can be with
Meet the requirement of VLSI high-density packages, be the key foundation material of modern communication technology, defended in portable mobile phone, TV
Star receiver, have highly important application in terms of military radar, the minimizing of modern communication instrument, it is integrated during just
Play increasing effect.The exploitation of low-temperature co-fired glass ceramic material system turns into current Electronic Packaging area research
Focus.
The complication of component, densification and functionalization in electronic device and electronic installation, to package substrate and wiring work
Journey proposes higher and higher requirement, be mainly manifested in it is following some：(1) it is normal to reduce dielectric for the high speed an urgent demand of signal transmission
Number, dielectric loss and reduction lead distance；(2) to reduce volume, many electronic components, such as resistance, even electric capacity, inductance
It is built among substrate；(3) to reduce encapsulation volume, encapsulation link is reduced, bare chip actual load is the most typical.The many of encapsulation
Function, such as it is electrically connected, physical protection, stress relaxes, and radiating is moistureproof, dimensional transitions, normalization, standardization etc., just gradual portion
Divide or fully undertaken by substrate；(4) good chemical stability and mechanical performance.Traditional ceramics Al2O3Low dielectric in having
Constant (9~10), high mechanical properties (>400MPa), excellent chemical stability, it is a kind of good baseplate material.It is however, pure
Al2O3Ceramic sintering temperature is higher (1400~1500 DEG C), it is impossible to is directly burnt altogether with low-melting-point metals such as Ag, Cu.In order to reduce
Sintering temperature, traditional method are a kind of for incorporation low melting point oxide, such as B2O3And V2O5, but free B2O3And V2O5Rear
It is excessive and unstable that slurry viscosity is easily caused in phase casting processes, limits its practical application；Another method is Al2O3- crystallization
Glass, i.e., a small amount of ceramics are participated in crystallized glass and are used 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 big, causes cost higher, strongly limit glass ceramics composite substrate material
Development.
The content of the invention
The goal of the invention of the present invention is：For above-mentioned problem, there is provided one kind can low-temperature sintering (850~900
DEG C), there is low-k (3.5~4), the low Jie's glass ceramic material and its preparation of low-loss and frequency-temperature coefficient stabilization
Method.It can be applied in the civilian and national defense industry such as portable mobile phone, telstar receiver, military radar, technique letter
It is single, it is easy to industrialized production and material property is stable.
The technical solution of the present invention is to provide 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 components：30wt%~60wt% KBS glass, 30wt%~
55wt% Al2O3, and 5wt%~40wt% quartz sand；The mol ratio of the KBS glass is K2O：B2O3：SiO2=
x：y：Z, wherein, 0.002<x<0.004,0.2<y<0.3,0.5<z<0.6；The Al2O3For α types Al2O3。
The preparation method of the low Jie's glass ceramic material of low-temperature sintering as described above, comprises the following steps：
A, according to the component proportion requirement of the KBS glass, by K2CO3、SiO2And H3BO3Powder mixing；
B, by the above-mentioned mixed-powder prepared using deionized water as solvent, wet ball-milling mixing, then dry；
C, the powder after above-mentioned drying is melted in 1500 DEG C of air atmosphere high temperatures, forms KBS glass frits；
D, by above-mentioned KBS glass frits using deionized water as solvent, wet ball-milling, then dry, obtain at 100 DEG C
KBS glass dust；
E, by KBS glass dust with accounting for the Al that its percentage by weight is respectively 50~183%2O3And 8.3~133% stone
Sand mixes, and with deionized water solvent, wet ball-milling mixing, additive capacity accounts for 2~5% propylene of raw material gross mass after drying
Acid solution is granulated as binding agent；
F, the particle obtained above-mentioned granulation is dry-pressing formed, and briquetting pressure is 10~20Mpa；
G, above-mentioned dry-pressing formed material is sintered in 850-900 DEG C of air atmosphere, low Jie's glass ceramic material is made.
Further, the wet ball-milling time in the step b and d is 5~10 hours, the wet ball-milling in step e
Time is 8~24 hours.
Further, in the step c, the time of the air atmosphere high temperature melting at 1500 DEG C is small for 0.5~1 after drying
When, in the step g, sintering time is 0.5~1 hour in 850~900 DEG C of air atmospheres.
Further, the step d also include first by step c gained KBS glass frits crush, then again with from
Sub- water is solvent, carries out wet ball-milling.
Compared with prior art, beneficial effects of the present invention are embodied in：
1st, formula of the invention is free of heavy metal component, can be applied in the product of high frequency field, green pollution-free, full
The RHOS and WEEE of the sufficient newest appearance of the European Community strict standard requirement.
2nd, by traditional sintering process more than 1200 DEG C drop to less than 900 DEG C, the further reduction of sintering temperature, there is energy-conservation
Advantage.
3rd, dielectric constant is adjustable from 3.5~4, and low (tan δ are lost<3×10-3), temperature coefficient of resonance frequency is stable.
4th, the low Jie's glass ceramics composite substrate material of low-temperature sintering of the present invention can improve signal in the application of the communications field
Transmission speed and wiring density, the requirement of VLSI high-density packages can be met, be the key foundation material of modern communication technology,
There is highly important application in terms of portable mobile phone, telstar receiver, military radar, in modern communication instrument
Minimize, it is integrated during just playing increasing effect, there is essential industry application value.
Brief description of the drawings
Fig. 1 is XRD (X-ray diffractogram) of the embodiment 5,6,7,8 in 850 degree of sintering；
Fig. 2 is SEM (scanning electron microscope (SEM) photograph) of the embodiment 5 in 850 degree of sintering；
Fig. 3 is SEM (scanning electron microscope (SEM) photograph) of the embodiment 6 in 850 degree of sintering；
Fig. 4 is SEM (scanning electron microscope (SEM) photograph) of the embodiment 7 in 850 degree of sintering；
Fig. 5 is SEM (scanning electron microscope (SEM) photograph) of the embodiment 8 in 850 degree of sintering.
Embodiment
Below in conjunction with drawings and examples, the present invention is further illustrated.
The low Jie's glass ceramics composite substrate material of a kind of low-temperature sintering, it is characterised in that composed of the following components：30wt%
~60wt% KBS glass, 30wt%~55wt% Al2O3, and 5wt%~40wt% quartz sand；The KBS glass
Mol ratio be K2O：B2O3：SiO2=x：y：Z, wherein, 0.002<x<0.004,0.2<y<0.3,0.5<z<Described in 0.6
Al2O3For α types Al2O3。
The preparation method of the low Jie's glass ceramics composite substrate material of low-temperature sintering as described above, comprises the following steps：
A, according to the component proportion requirement of the KBS glass, by K2CO3、SiO2And H3BO3Powder mixing；
B, by the above-mentioned mixed-powder prepared using deionized water as solvent, wet ball-milling mixing, then dry；
C, the powder after above-mentioned drying is melted in 1500 DEG C of air atmosphere high temperatures, forms KBS glass frits；
D, by above-mentioned KBS glass frits using deionized water as solvent, wet ball-milling, then dry, obtain at 100 DEG C
KBS glass dust；
E, by KBS glass dust with accounting for the Al that its percentage by weight is respectively 50~183%2O3And 8.3~133% stone
Sand mixes, and with deionized water solvent, wet ball-milling mixing, additive capacity accounts for 2~5% propylene of raw material gross mass after drying
Acid solution is granulated as binding agent；
F, the particle obtained above-mentioned granulation is dry-pressing formed, and briquetting pressure is 10~20Mpa；
G, above-mentioned dry-pressing formed material is sintered in 850-900 DEG C of air atmosphere, low Jie's glass ceramic material is made.
Preferably, the wet ball-milling time in the step b and d is 5~10 hours, during wet ball-milling in step e
Between be 8~24 hours；The wet ball-milling time in step b, d and e can be adjusted according to the granularity requirements of setting.
Preferably, in the step c, the time of the air atmosphere high temperature melting at 1500 DEG C is small for 0.5~1 after drying
When, in the step g, sintering time is 0.5~1 hour in 850~900 DEG C of air atmospheres.
Preferably, in the step d, in order to improve the wet ball-milling efficiency of KBS glass and obtain more uniform KBS
Glass dust, first the KBS glass frits obtained in the step c can be crushed, then again using ionized water as solvent, be carried out
Wet ball-milling；The scheme feasible as one, the KBS glass frits obtained in the step c can be directly subjected to water quenching acquisition
Tiny KBS glass fragments
The low Jie's glass ceramic material of low-temperature sintering of the present invention can be used as composite substrate material and extensive use, in KBS glass
Glass powder and Al2O3On the basis of ceramic phase, by adding quartz sand, then KBS glass, Al are adjusted2O3And the matter of quartz sand three
Accounting is measured in suitable scope, so as to realize relatively low dielectric constant and low-loss simultaneously at a relatively low sintering temperature.
What deserves to be explained is quartz sand is added as ceramic fillers in the present invention, the effect for reducing dielectric constant is realized.
Embodiment 1
A, by K2CO3、SiO2And H3BO3Powder mixing, its quality is respectively 0.35g, 28g and 19.15g；
B, by the powder that step a is prepared using deionized water as solvent, wet ball-milling mixes 6 hours, at 1500 DEG C after drying
Air atmosphere high temperature melts 1 hour, forms KBS glass frits；
C, by KBS glass frits using deionized water as solvent, wet ball-milling 6 hours, then dry and obtain at 100 DEG C
KBS glass dust；
D, by above-mentioned KBS glass dust and 52.5g Al2O3Mixing, with deionized water solvent, wet ball-milling mixes 8 hours, dries
2~5% acrylic acid solution that dry rear additive capacity accounts for raw material gross mass is granulated as binding agent；
E, the particle obtained above-mentioned granulation is dry-pressing formed, briquetting pressure 20Mpa；
F, material dry-pressing formed step e is sintered 1 hour in 850 DEG C of air atmospheres, low Jie's glass ceramics material is made
Material.
The low Jie's glass ceramics composite substrate material each component of 1-8 low temperature sinterings of the embodiment of the present invention is listed in table 1
Actual proportioning and sintering temperature.
The micro- of the low Jie's glass ceramics composite substrate material of low-temperature sintering made from 1-8 embodiments of the present invention is given in table 2
Ripple dielectric properties, the embodiment of the present invention carry out the evaluation of microwave dielectric property using cylindrical dielectric resonator method, and detection method is
GB/T 7265.2-1987 open type cell method.
Table 1
Table 2
Embodiment 2
A, by K2CO3、SiO2And H3BO3Powder mixing, its quality is respectively 0.35g, 28g and 19.15g；
B, by the powder that step a is prepared using deionized water as solvent, wet ball-milling mixes 6 hours, at 1500 DEG C after drying
Air atmosphere high temperature melts 1 hour, forms KBS glass frits；
C, by KBS glass frits using deionized water as solvent, wet ball-milling 6 hours, then dry and obtain at 100 DEG C
KBS glass dust；
D, by above-mentioned KBS glass dust and 26.25g Al2O3And the mixing of 26.25g quartz sands, it is wet with deionized water solvent
Formula ball milling mixing 8 hours, additive capacity accounts for 2~5% acrylic acid solution of raw material gross mass as binding agent progress after drying
It is granulated；
E, the particle obtained above-mentioned granulation is dry-pressing formed, briquetting pressure 20Mpa；
F, material dry-pressing formed step e is sintered 1 hour in 850 DEG C of air atmospheres, low Jie's glass ceramics material is made
Material.
Embodiment 3
A, by K2CO3、SiO2And H3BO3Powder mixing, its quality is respectively 0.35g, 28g and 19.15g；
B, by the powder that step a is prepared using deionized water as solvent, wet ball-milling mixes 6 hours, at 1500 DEG C after drying
Air atmosphere high temperature melts 1 hour, forms KBS glass frits；
C, by KBS glass frits using deionized water as solvent, wet ball-milling 6 hours, then dry and obtain at 100 DEG C
KBS glass dust；
D, by above-mentioned KBS glass dust and 21g Al2O3And the mixing of 31.5g quartz sands, with deionized water solvent, wet type ball
Mill mixing 8 hours, additive capacity accounts for 2~5% acrylic acid solution of raw material gross mass and is granulated as binding agent after drying；
E, the particle obtained above-mentioned granulation is dry-pressing formed, briquetting pressure 20Mpa；
F, material dry-pressing formed step e is sintered 1 hour in 850 DEG C of air atmospheres, low Jie's glass ceramics material is made
Material.
Embodiment 4
A, by K2CO3、SiO2And H3BO3Powder mixing, its quality is respectively 0.35g, 28g and 19.15g；
B, by the powder that step a is prepared using deionized water as solvent, wet ball-milling mixes 6 hours, at 1500 DEG C after drying
Air atmosphere high temperature melts 1 hour, forms KBS glass frits；
C, by KBS glass frits using deionized water as solvent, wet ball-milling 6 hours, then dry and obtain at 100 DEG C
KBS glass dust；
D, by above-mentioned KBS glass dust and 15.75g Al2O3And the mixing of 36.75g quartz sands, it is wet with deionized water solvent
Formula ball milling mixing 8 hours, additive capacity accounts for 2~5% acrylic acid solution of raw material gross mass as binding agent progress after drying
It is granulated；
E, the particle obtained above-mentioned granulation is dry-pressing formed, briquetting pressure 20Mpa；
F, material dry-pressing formed step e is sintered 1 hour in 850 DEG C of air atmospheres, low Jie's glass ceramics material is made
Material.
Embodiment 5
A, by K2CO3、SiO2And H3BO3Powder mixing, its quality is respectively 0.55g, 24g and 22.95g；
B, by the powder that step a is prepared using deionized water as solvent, wet ball-milling mixes 6 hours, at 1500 DEG C after drying
Air atmosphere high temperature melts 1 hour, forms KBS glass frits；
C, by KBS glass frits using deionized water as solvent, wet ball-milling 6 hours, then dry and obtain at 100 DEG C
KBS glass dust；
D, by above-mentioned KBS glass dust and 52.5g Al2O3Mixing, with deionized water solvent, wet ball-milling mixes 8 hours, dries
2~5% acrylic acid solution that dry rear additive capacity accounts for raw material gross mass is granulated as binding agent；
E, the particle obtained above-mentioned granulation is dry-pressing formed, briquetting pressure 20Mpa；
F, material dry-pressing formed step e is sintered 1 hour in 850 DEG C of air atmospheres, low Jie's glass ceramics material is made
Material.
Embodiment 6
A, by K2CO3、SiO2And H3BO3Powder mixing, its quality is respectively 0.55g, 24g and 22.95g；
B, by the powder that step a is prepared using deionized water as solvent, wet ball-milling mixes 6 hours, at 1500 DEG C after drying
Air atmosphere high temperature melts 1 hour, forms KBS glass frits；
C, by KBS glass frits using deionized water as solvent, wet ball-milling 6 hours, then dry and obtain at 100 DEG C
KBS glass dust；
D, by above-mentioned KBS glass dust and 26.25g Al2O3And 26.25g mixing, with deionized water solvent, wet ball-milling
Mixing 8 hours, additive capacity accounts for 2~5% acrylic acid solution of raw material gross mass and is granulated as binding agent after drying；
E, the particle obtained above-mentioned granulation is dry-pressing formed, briquetting pressure 20Mpa；
F, material dry-pressing formed step e is sintered 1 hour in 850 DEG C of air atmospheres, low Jie's glass ceramics material is made
Material.
Embodiment 7
A, by K2CO3、SiO2And H3BO3Powder mixing, its quality is respectively 0.55g, 24g and 22.95g；
B, by the powder that step a is prepared using deionized water as solvent, wet ball-milling mixes 6 hours, at 1500 DEG C after drying
Air atmosphere high temperature melts 1 hour, forms KBS glass frits；
C, by KBS glass frits using deionized water as solvent, wet ball-milling 6 hours, then dry and obtain at 100 DEG C
KBS glass dust；
D, by above-mentioned KBS glass dust and 21g Al2O3And the mixing of 31.5g quartz sands, with deionized water solvent, wet type ball
Mill mixing 8 hours, additive capacity accounts for 2~5% acrylic acid solution of raw material gross mass and is granulated as binding agent after drying；
E, the particle obtained above-mentioned granulation is dry-pressing formed, briquetting pressure 20Mpa；
F, material dry-pressing formed step e is sintered 1 hour in 850 DEG C of air atmospheres, low Jie's glass ceramics material is made
Material.
Embodiment 8
A, by K2CO3、SiO2And H3BO3Powder mixing, its quality is respectively 0.55g, 24g and 22.95g；
B, by the powder that step a is prepared using deionized water as solvent, wet ball-milling mixes 6 hours, at 1500 DEG C after drying
Air atmosphere high temperature melts 1 hour, forms KBS glass frits；
C, by KBS glass frits using deionized water as solvent, wet ball-milling 6 hours, then dry and obtain at 100 DEG C
KBS glass dust；
D, by above-mentioned KBS glass dust and 15.75g Al2O3And 36.75g mixing, with deionized water solvent, wet ball-milling
Mixing 8 hours, additive capacity accounts for 2~5% acrylic acid solution of raw material gross mass and is granulated as binding agent after drying；
E, the particle obtained above-mentioned granulation is dry-pressing formed, briquetting pressure 20Mpa；
F, material dry-pressing formed step e is sintered 1 hour in 850 DEG C of air atmospheres, low Jie's glass ceramics material is made
Material.
With reference to knowable to being analyzed Tables 1 and 2, in embodiment 1~4, the quality of the KBS glass in glass ceramic material
When percentage is fixed, addition and Al with quartz sand2O3The reduction of quality accounting, the dielectric constant of glass ceramic material with
And loss gradually reduce, this be due to quartz sand as ceramic phase when, its dielectric constant very little, about 3.5, so serving bright
The aobvious effect for reducing dielectric constant.Analyze embodiment 5~8 to understand, when the mass percent of KBS glass is fixed, with quartz sand
Addition and Al2O3The reduction of quality accounting, the dielectric constant of glass ceramic material still show the change substantially reduced,
At the same time, but there is obvious increase tendency in loss, analyzes its reason, after quartz sand excessive addition, pottery
Wettability between porcelain phase and KBS glass is deteriorated, and many stomatas are formd in sintering process.Because the dielectric constant of air is
1, but loss is very big, so occur as soon as quartz sand quality accounting increase dielectric constant further reduces, but loss occurs
The result significantly increased.So when quartz sand addition within the specific limits, can be achieved glass ceramic material dielectric constant with
And the reduction of loss, by the glass ceramic material for adjusting quartz sand quality accounting acquisition optimum performance.
X-ray diffractogram comparison diagram of the embodiment 5,6,7 and 8 in 850 degree of sintering is shown by Fig. 1, it is seen that with quartz
Sand/Al2O3Ratio increase, SiO2Diffraction maximum it is stronger；The embodiment 5,6,7 being shown respectively by Fig. 2, Fig. 3, Fig. 4 and Fig. 5
With 8 in 850 degree of scanning electron microscope (SEM) photographs sintered, it is seen then that with the increase of quartz sand addition, the microstructure of glass ceramic material
The stomata quantity and area of middle appearance gradually increase, and are more coincide with above-mentioned theory analysis.
One of ordinary skill in the art will be appreciated that embodiment described here is to aid in reader and understands this hair
Bright principle, it should be understood that protection scope of the present invention is not limited to such especially statement and embodiment.This area
Those of ordinary skill can make according to these technical inspirations disclosed by the invention various does not depart from the other each of essence of the invention
The specific deformation of kind and combination, these deform and combined still within the scope of the present invention.
Claims (5)
1. the low Jie's glass ceramic material of a kind of low-temperature sintering, it is characterised in that composed of the following components：30wt%~60wt%'s
KBS glass, 30wt%~55wt% Al2O3, and 5wt%~40wt% quartz sand；The mol ratio of the KBS glass
For K2O：B2O3：SiO2=x：y：Z, wherein, 0.002<x<0.004,0.2<y<0.3,0.5<z<0.6 Al2O3For α types
Al2O3。
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, according to the component proportion requirement of the KBS glass, by K2CO3、SiO2And H3BO3Powder mixing；
B, by the above-mentioned mixed-powder prepared using deionized water as solvent, wet ball-milling mixing, then dry；
C, the powder after above-mentioned drying is melted in 1500 DEG C of air atmosphere high temperatures, forms KBS glass frits；
D, by above-mentioned KBS glass frits using deionized water as solvent, wet ball-milling, then dried at 100 DEG C, obtain KBS glass
Glass powder；
E, by KBS glass dust with accounting for the Al that its percentage by weight is respectively 50~183%2O3And 8.3~133% quartz sand
Mixing, with deionized water solvent, wet ball-milling mixing, after drying additive capacity account for raw material gross mass 2~5% acrylic acid it is molten
Liquid is granulated as binding agent；
F, the particle obtained above-mentioned granulation is dry-pressing formed, and briquetting pressure is 10~20Mpa；
G, above-mentioned dry-pressing formed material is sintered in 850-900 DEG C of air atmosphere, low Jie's glass ceramic material is made.
3. the preparation method of the low Jie's glass ceramic material of low-temperature sintering according to claim 2, it is characterised in that the step
The wet ball-milling time in rapid 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 low-temperature sintering according to Claims 2 or 3, it is characterised in that institute
State in step c, in the time of 1500 DEG C of air atmosphere high temperatures melting be 0.5~1 hour after drying, in the step g
Sintering time is 0.5~1 hour in 850-900 DEG C of air atmosphere.
5. the preparation method of the low Jie's glass ceramic material of low-temperature sintering according to claim 2, it is characterised in that step d
Also include first crushing the KBS glass frits of gained in step c, then again using ionized water as solvent, carry out wet ball-milling.
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