CN103145336B - A kind of borosilicate glass and ball-aluminium oxide LTCC green band and preparation method thereof - Google Patents
A kind of borosilicate glass and ball-aluminium oxide LTCC green band and preparation method thereof Download PDFInfo
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- CN103145336B CN103145336B CN201310049370.XA CN201310049370A CN103145336B CN 103145336 B CN103145336 B CN 103145336B CN 201310049370 A CN201310049370 A CN 201310049370A CN 103145336 B CN103145336 B CN 103145336B
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Abstract
The invention discloses a kind of borosilicate glass and ball-aluminium oxide LTCC green band and preparation method thereof, this green band is made up of glassceramic composites and casting medium, and wherein glassceramic composites is made up of borosilicate glass, ball-aluminium oxide; Casting medium is made up of mixed solvent, monomeric binder, plastic agent and dispersion agent.LTCC green tape surfacing prepared by the present invention, smooth, green tape solid content can reach 88 ~ 92wt%, and percent of firing shrinkage is 9 ~ 11%, and all directions sintering shrinkage difference is little, can realize connect up with the low melting point metal such as Au, Ag common burning at 850 DEG C.Raw material band sintering porcelain body provided by the invention has excellent dielectric properties: under 10GHz, specific inductivity (ε
r) be 7 ~ 8, dielectric loss (tan δ) is less than 2 × 10
-3, and efficiently solve the anisotropic problem of traditional LTCC green band sintering shrinkage.
Description
Technical field
The present invention relates to a kind of composite glass-ceramic system low-temperature co-burning ceramic material, belong to high density packing function ceramic field.
Background technology
In recent years, the demand for development high-speed data of information technology and high current density transmission, electronic circuit day by day to future development that is microminiaturized, integrated and high frequency, to electronic component, this just proposes that size is small, high frequency, high reliability, cheap and high integration requirement.LTCC Technology (LTCC) is the type material technology of nineteen eighty-two Hughes Electronics's exploitation, low-temperature sintered ceramics powder is made the accurate and fine and close green band of thickness, green band utilizes laser boring, micropore slip casting, the techniques such as accurate conductor paste printing make required circuitous pattern, and by multiple passive component (as low capacitance electric capacity, resistance, wave filter, impedance transducer, coupling mechanism etc.) imbed in ceramic substrate, then overlap together, internal and external electrode can use silver respectively, copper, the metals such as gold, sinter below 900 DEG C, make the high assembled density electron device of three-dimensional network.
In order to meet this high assembled density product requirement, all materials related to must have fine qualities and repeatability, all processing step needs strictly, carefully to control, and the slight change of the small change of any processing parameter especially LTCC material behavior all can affect the performance of resulting devices.Therefore develop closed tolerance, favorable reproducibility, the green band that can realize burning altogether with other dissimilar materialss are significant.
The key factor affecting LTCC green band quality is material component factor.The kind of inorganic powder, content, granularity and pattern in green band, and the kind of organic materials such as solvent, binding agent, dispersion agent, plastic agent and content directly have influence on the performance of LTCC green band.In traditional LTCC green band, solid content (inorganic powder content) is lower, and sintering shrinkage is large, causes warpage with easily there is unmatched phenomenon in other dissimilar materialss altogether burning process; In green band, inorganic powder is generally glass powder in irregular shape and ceramics powder, the green band prepared by curtain coating shows a kind of anisotropic structure, to such an extent as to punching, printing, there will be the anisotropy of sintering shrinkage after ceramic body sintering after lamination, have a strong impact on the repeatability of the reliability of LTCC device, stability and manufacture, constrain LTCC device and further develop towards microminiaturized, integrated, high reliability direction.
Summary of the invention
Object of the present invention is exactly the anisotropic problem solving traditional LTCC green band sintering shrinkage, provides a kind of borosilicate glass and ball-aluminium oxide LTCC green band and preparation method thereof.
In order to solve above technical problem, the invention provides following technical scheme:
A kind of borosilicate glass and ball-aluminium oxide LTCC green band, is characterized in that being made up of the raw material of following parts by weight:
Borosilicate glass 30 ~ 70, ball-aluminium oxide accounts for 40 ~ 60, casting medium 8 ~ 12.
On the basis of technique scheme, following further technical scheme can be had:
Described borosilicate glass is made up of the raw material of following ratio of weight and number:
B
2O
315~25、SiO
250~70、Al
2O
310~15、MgO 5~10、K
2O 2~3、Na
2O 2~3。
The median size of borosilicate glass is 1 ~ 3um, and the median size of ball-aluminium oxide is 3 ~ 6um.
Described casting medium is made up of mixed solvent, binding agent, softening agent and dispersion agent, and the weight percent that each component occupies machine curtain coating medium total amount is: mixed solvent 75 ~ 85%, monomeric binder 3 ~ 8%, softening agent 2 ~ 6%, dispersion agent 2 ~ 6%;
Described mixed solvent is ethanol, dimethylbenzene, acetone mixture; Binding agent is β-dimethyl-aminoethylmethacrylate and methacrylic acid mixture; Softening agent is dibutyl phthalate; Dispersion agent is Viscotrol C;
The weight percent that wherein in mixed solvent, each composition accounts for solvent total amount is respectively: ethanol 30 ~ 60%, dimethylbenzene 30 ~ 60%, acetone 10 ~ 30%;
In binding agent, each monomer accounts for weight of binder per-cent and is: β-dimethyl-aminoethylmethacrylate 80 ~ 90%, methacrylic acid 5 ~ 15%.
Present invention also offers the preparation method of a kind of borosilicate glass and ball-aluminium oxide LTCC green band, it is characterized in that comprising the following steps:
A, take raw material B by borosilicate glass formula
2o
3, SiO
2, Al
2o
3, MgO, K
2o, Na
2o, preserves 12 ~ 24h after mixing;
B, above-mentioned mixing raw material powder is placed in platinum crucible, be incubated 2 ~ 4h at 1500 ~ 1600 DEG C after, pour in deionized water, obtain transparent, homogeneous glass fragment;
Made glass fragment pulverizes by c, employing corundum pair roller, obtain the glass meal that median size is 0.5 ~ 1mm, glass meal is mixed with deionized water, zirconia ball is as ball-milling medium, in glass meal: ball: the ratio ball milling 5 ~ 10h of water=1:3:0.8, then be placed in 120 DEG C of baking ovens and dry 4 ~ 6h, obtain the borosilicate glass powder that median size is 1 ~ 3um;
D, be (30 ~ 70) by ratio of weight and number: borosilicate glass powder and the spherical alumina aluminium powder of (40 ~ 60) form compound, add ethanol medium, according to compound: zirconium ball: the ratio mixing and ball milling 2 ~ 4h of ethanol=1:2.5:1, then be placed in 120 DEG C of baking ovens and dry 4 ~ 6h, obtain low-temperature co-fired ceramic powder material;
E, in described low-temperature co-fired ceramic powder material, add solvent, binding agent, softening agent, dispersion agent, under closed environment, ball milling mixes 8 ~ 12h, vacuum defoamation, employing doctor blade method for tape-casting is shaping, obtain green band after drying, wherein: drying temperature is 25 DEG C, time of drying is 6 ~ 12h.
Prepared green band is cut into slices, lamination, hot-forming, the ceramic chips that is trimmed to desired shape.Described individual layer green band or laminated ceramic chips are sintered at 850 ~ 900 DEG C, finally obtains borosilicate glass and ball-aluminium oxide low-temperature co-fired ceramic substrate.
The present invention selects Superfine Boron silicate glass, ball-aluminium oxide as the inorganic powder in green band, mixed solvent (volatilizing fast after making green tape), monomeric binder (being polymerized in green band preparation process) and corresponding softening agent, dispersion agent prepare the glass-ceramic systems LTCC green band of high solids content as organic curtain coating medium, and efficiently solve the anisotropic problem of traditional LTCC green band sintering shrinkage.
Glass-ceramic system LTCC green band prepared by the present invention, surfacing, smooth, X, Y, Z axis sintering shrinkage is 9 ~ 11%, can connect up at low melting point metals such as 850 DEG C of realizations and Au, Ag and burn altogether, wherein, X, Y-axis are respectively parallel in horizontal plane, perpendicular to curtain coating direction, Z axis is perpendicular to curtain coating in-plane.Sintering porcelain body has excellent dielectric properties: under 10GHz, specific inductivity (ε
r) be 7 ~ 8, dielectric loss (tan δ) is less than 2 × 10
-3.
Accompanying drawing explanation
Fig. 1 is the present invention's borosilicate glass powder microgram used;
Fig. 2 is the spherical alumina aluminium powder microgram that the present invention adopts;
Fig. 3 is that green band of the present invention sinters the microstructure figure of porcelain body into through 850 DEG C.
Embodiment
embodiment 1
Select the aluminum oxide powder (3 ~ 5um) of non-nodularization as the ceramic filler phase in inorganic powder contained by green band, select polyvinyl butyral acetal as the binding agent in organic curtain coating system, compare with the present invention:
By ratio of weight and the number of copies, B is taken respectively
2o
318kg, SiO
265kg, Al
2o
38kg, MgO 5kg, K
2o 2kg, Na
2o 2kg, after mixing 12h, is placed in platinum crucible, at 1500 ~ 1600 DEG C, is incubated 3h, pour in deionized water, obtain transparent, homogeneous borosilicate glass fragment.
Corundum pair roller is adopted to be pulverized by made glass fragment, obtain the glass meal that median size is 0.5 ~ 1mm, glass meal is mixed with deionized water, zirconia ball is as ball-milling medium, in material: ball: the ratio ball milling 8h of water=1:3:0.8, be placed in 120 DEG C of baking ovens and dry 4h, obtain the borosilicate glass powder that median size is 0.5 ~ 2um;
Borosilicate glass powder 55kg and spherical molten aluminum oxide powder 45kg is formed compound, adds ethanol medium, according to compound: zirconium ball: the ratio ball milling mixing 3h of ethanol=1:2.5:1, is placed in 120 DEG C of baking ovens and dries 4h, obtain low-temperature co-fired ceramic powder material.
See table 1, solvent, binding agent, softening agent, dispersion agent is added in described low-temperature co-fired ceramic powder material, under closed environment, ball milling mixes the weight ratio of inorganic powder in 10h(casting slurry and zirconium ball is 1:4), vacuum defoamation, employing doctor blade method for tape-casting is shaping, obtain green band after drying, wherein: drying temperature is 25 DEG C, time of drying is 8h; Prepared green band is cut into slices, after lamination in thermocompressor 70 DEG C, 20MPa, pressurize 15min.
Table 1 borosilicate glass-each component concentration 1 of alumina low temperature common burning porcelain green band
After green band after lamination hot pressing is cut into required size, be incubated under rising to the temperature of setting after being placed in electric furnace binder removal and burn till.The concrete steps of described sintering are: by described low-temperature co-burning ceramic material from room temperature with the ramp to 450 DEG C of 2 DEG C/min, insulation 2h be used for binder removal, guarantee organic abundant eliminating in sample; Low-temperature co-burning ceramic material after binder removal begins from 450 DEG C with the ramp to 850 DEG C of 5 DEG C/min, and namely insulation 30min sinters porcelain into.As shown in table 2 to the performance test of sintering porcelain body.
Table 2 borosilicate glass-alumina low temperature common burning porcelain green band sintering and dielectric properties 1
embodiment 2
Select 1# non-nodularization aluminum oxide powder (3 ~ 5um), 2# spherical alumina aluminium powder (3 ~ 6um) as the ceramic filler phase in inorganic powder contained by green band respectively, select β-dimethyl-aminoethylmethacrylate, methacrylic acid as the binding agent in organic curtain coating medium, the preparation method of green band is as embodiment 1, green band formula and sintering porcelain body performance are respectively aspherical aluminum oxide in ceramic phase in inorganic powder contained by table 3, table 4(1# sample, and 2# is ball-aluminium oxide);
Table 3 borosilicate glass-each component concentration 2 of alumina low temperature common burning porcelain green band
Table 4 borosilicate glass-alumina low temperature common burning porcelain green band sintering and dielectric properties 2
Comparing embodiment 1 and embodiment 2, ensureing that slurry viscosity is when suitable curtain coating scope (3 ~ 4 Pa.S), compared with conventional polymer binding agent polyvinyl butyral acetal, employing monomeric binder β-dimethyl-aminoethylmethacrylate, methacrylic acid can significantly improve the solid content of curtain coating green band.In embodiment 1, adopt polyvinyl butyral as binding agent, green band solid content is 82%, and in example 2, β-dimethyl-aminoethylmethacrylate, methacrylic acid monomer mixture is adopted to replace polyvinyl butyral, green band solid content can reach 88%, and correspondingly, the sintering shrinkage of green band also decreases.
In embodiment 2, select ball-aluminium oxide as the ceramic filler phase of low-temperature co-burning ceramic material, green band solid content slightly increases (88% → 90%), and X-axis, Y-axis, Z-direction sintering shrinkage are more tending towards close, efficiently solves the anisotropic problem of traditional LTCC green band sintering shrinkage.
Claims (1)
1. a preparation method for borosilicate glass and ball-aluminium oxide LTCC green band, adopt the raw material of following parts by weight: borosilicate glass 30 ~ 70, ball-aluminium oxide accounts for 40 ~ 60, casting medium 8 ~ 12;
Described borosilicate glass is made up of the raw material of following ratio of weight and number: B
2o
315 ~ 25, SiO
250 ~ 70, Al
2o
310 ~ 15, MgO 5 ~ 10, K
2o 2 ~ 3, Na
2o 2 ~ 3, the median size of borosilicate glass is 1 ~ 3 μm, and the median size of ball-aluminium oxide is 3 ~ 6 μm;
Described casting medium is made up of mixed solvent, binding agent, softening agent and dispersion agent, and the weight percent that each component accounts for curtain coating medium total amount is: mixed solvent 75 ~ 85%, binding agent 3 ~ 8%, softening agent 2 ~ 6%, dispersion agent 2 ~ 6%; Described mixed solvent is ethanol, dimethylbenzene, acetone mixture; Binding agent is β-dimethyl-aminoethylmethacrylate and methacrylic acid mixture; Softening agent is dibutyl phthalate; Dispersion agent is Viscotrol C; The weight percent that wherein in mixed solvent, each composition accounts for solvent total amount is respectively: ethanol 30 ~ 60%, dimethylbenzene 30 ~ 60%, acetone 10 ~ 30%; In binding agent, each monomer accounts for weight of binder per-cent and is: β-dimethyl-aminoethylmethacrylate 80 ~ 90%, methacrylic acid 5 ~ 15%;
It is characterized in that comprising the following steps:
A, take raw material B by borosilicate glass formula
2o
3, SiO
2, Al
2o
3, MgO, K
2o, Na
2o, preserves 12 ~ 24h after mixing;
B, be placed in platinum crucible by above-mentioned by borosilicate glass mixed mixing raw material of filling a prescription, be incubated 2 ~ 4h at 1500 ~ 1600 DEG C after, pour in deionized water, obtain transparent, homogeneous glass fragment;
Made glass fragment pulverizes by c, employing corundum pair roller, obtain the glass meal that median size is 0.5 ~ 1mm, glass meal is mixed with deionized water, zirconia ball is as ball-milling medium, in glass meal: ball: the ratio ball milling 5 ~ 10h of water=1:3:0.8, then be placed in 120 DEG C of baking ovens and dry 4 ~ 6h, obtain the borosilicate glass powder that median size is 1 ~ 3 μm;
D, be (30 ~ 70) by ratio of weight and number: borosilicate glass powder and the spherical alumina aluminium powder of (40 ~ 60) form compound, add ethanol medium, according to compound: zirconium ball: the ratio mixing and ball milling 2 ~ 4h of ethanol=1:2.5:1, then be placed in 120 DEG C of baking ovens and dry 4 ~ 6h, obtain low-temperature co-fired ceramic powder material;
E, in described low-temperature co-fired ceramic powder material, add mixed solvent, binding agent, softening agent, dispersion agent, under closed environment, ball milling mixes 8 ~ 12h, vacuum defoamation, employing doctor blade method for tape-casting is shaping, obtain green band after drying, wherein: drying temperature is 25 DEG C, time of drying is 6 ~ 12h.
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Address after: No.1047 Tushan Road, Bengbu City, Anhui Province 233000 Patentee after: CHINA BUILDING MATERIALS BENGBU GLASS INDUSTRY DESIGN & RESEARCH INSTITUTE Co.,Ltd. Patentee after: China Triumph International Engineering Co.,Ltd. Address before: 233010 Tushan Road 1047, Yuhui District, Bengbu City, Anhui Province Patentee before: BENGBU DESIGN & Research Institute FOR GLASS INDUSTRY Patentee before: China Triumph International Engineering Co.,Ltd. |
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Effective date of registration: 20210122 Address after: 233100 Fengyang Industrial Park, Chuzhou City, Anhui Province Patentee after: Fengyang Kaisheng silicon material Co.,Ltd. Address before: No.1047 Tushan Road, Bengbu City, Anhui Province 233000 Patentee before: CHINA BUILDING MATERIALS BENGBU GLASS INDUSTRY DESIGN & RESEARCH INSTITUTE Co.,Ltd. Patentee before: China Triumph International Engineering Co.,Ltd. |