CN103145336A - Borosilicate glass-spherical alumina low temperature co-fired ceramic green tape and preparation method thereof - Google Patents
Borosilicate glass-spherical alumina low temperature co-fired ceramic green tape and preparation method thereof Download PDFInfo
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- CN103145336A CN103145336A CN201310049370XA CN201310049370A CN103145336A CN 103145336 A CN103145336 A CN 103145336A CN 201310049370X A CN201310049370X A CN 201310049370XA CN 201310049370 A CN201310049370 A CN 201310049370A CN 103145336 A CN103145336 A CN 103145336A
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Abstract
The invention discloses a borosilicate glass-spherical alumina low temperature co-fired ceramic (LTCC) green tape and its preparation method. The green tape is composed of a glass-ceramic composite material and a casting medium. Specifically, the glass-ceramic composite material consists of borosilicate glass and spherical alumina. The casting medium consists of a mixed solvent, a monomer binder, a plasticizer and a dispersing agent. The low temperature co-fired ceramic green tape prepared in the invention has a level and smooth surface, a solid content up to 88-92wt%, and a firing shrinkage rate of 9-11%. The difference between the sintering shrinkage rate of each direction is small. And the green tape can achieve wiring co-firing with Au, Ag and other low melting point metals at 850DEG C. The raw material tape sintered ceramic body provided in the invention has excellent dielectric properties. Under the condition of less than 10GHz, the dielectric constant (epsilon r) of 7-8, the dielectric loss (Tan delta) is less than 2*10<-3>, and effectively solves the anisotropy problem of traditional LTCC green tape 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 is day by day to the future development of microminiaturized, integrated and high frequency, this just to electronic component proposed that size is small, the requirement of high frequency, high reliability, cheap and high integration.LTCC Technology (LTCC) is the type material technology of nineteen eighty-two Hughes Electronics's exploitation, that the low-temperature sintered ceramics powder is made the accurate and fine and close green band of thickness, utilize laser boring on the green band, micropore slip casting, the techniques such as accurate conductor paste printing are made needed circuitous pattern, and with a plurality of passive components (as low appearance value electric capacity, resistance, wave filter, impedance transducer, coupling mechanism etc.) imbed in ceramic substrate, then overlap together, internal and external electrode can use respectively silver, copper, the metals such as gold, at sintering below 900 ℃, make the high assembled density electron device of three-dimensional network.
In order to satisfy this high assembled density product requirement, all materials that relate to must have fine qualities and be repeatable, all processing step needs strict, careful control, the small variation of any processing parameter especially slight change of LTCC material behavior all can affect the performance of resulting devices.Therefore develop closed tolerance, favorable reproducibility, can realize that the green band that burns altogether is significant with other dissimilar materialss.
The key factor that affects LTCC green band quality is the material component factor.The kind of inorganic powder, content, granularity and pattern in the green band, and organic materials such as solvent, binding agent, dispersion agent, the kind of plastic agent and the performance that content directly has influence on LTCC green band.In traditional LTCC green band, solid content (inorganic powder content) is lower, and sintering shrinkage is large, easily unmatched phenomenon occurs in the burning process altogether and causes warpage with other dissimilar materialss; In the green band, inorganic powder is generally glass powder in irregular shape and ceramics powder, the green band of preparing by curtain coating shows a kind of anisotropic structure, to such an extent as to can occur the anisotropy of sintering shrinkage after the ceramic body sintering after punching, printing, lamination, the repeatability that has a strong impact on LTCC device reliability, stability and make has restricted the LTCC device and has further developed towards microminiaturized, integrated, high reliability direction.
Summary of the invention
Purpose of the present invention is exactly the anisotropic problem that has solved traditional LTCC green band sintering shrinkage, and a kind of borosilicate glass and ball-aluminium oxide LTCC green band and preparation method thereof are provided.
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 by the raw material of following parts by weight:
Borosilicate glass 30 ~ 70, ball-aluminium oxide accounts for 40 ~ 60, curtain coating medium 8 ~ 12.
On the basis of technique scheme, following further technical scheme can be arranged:
Described borosilicate glass is made by the raw material of following ratio of weight and number:
B
2O
3?15~25、SiO
2?50~70、Al
2O
3?10~15、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 curtain coating medium is comprised of mixed solvent, binding agent, softening agent and dispersion agent, and the weight percent that each component is occupied machine curtain coating medium total amount is: mixed solvent 75 ~ 85%, monomer 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 the 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%.
The present invention also provides 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 the 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, after being incubated 2 ~ 4h under 1500 ~ 1600 ℃, pours in deionized water, obtain glass fragment transparent, homogeneous;
C, employing corundum pair roller pulverize made glass fragment, obtaining median size is the glass meal of 0.5 ~ 1mm, the glass meal is mixed with deionized water, zirconia ball is as ball-milling medium, in the glass meal: ratio ball milling 5 ~ 10h of ball: water=1:3:0.8, then be placed in 120 ℃ of baking ovens and dry by the fire 4 ~ 6h, obtaining median size is the borosilicate glass powder of 1 ~ 3um;
D, be (30 ~ 70) with ratio of weight and number: the borosilicate glass powder of (40 ~ 60) and ball-aluminium oxide powder form compound, add ethanol medium, according to compound: ratio mixing and ball milling 2 ~ 4h of zirconium ball: ethanol=1:2.5:1, then be placed in 120 ℃ of baking ovens and dry by the fire 4 ~ 6h, obtain the low-temperature co-fired ceramic powder material;
E, add solvent, binding agent, softening agent, dispersion agent in described low-temperature co-fired ceramic powder material, under closed environment, ball milling mixes 8 ~ 12h, vacuum defoamation, adopt the doctor blade method for tape-casting moulding, obtain the green band after drying, wherein: drying temperature is 25 ℃, and be 6 ~ 12h time of drying.
To prepared green band cut into slices, lamination, hot-forming, the ceramic chips that is trimmed to desired shape.Described individual layer green band or laminated ceramic chips at 850 ~ 900 ℃ of lower sintering, are finally obtained 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 the green band, mixed solvent (make and give birth to the rear volatilization fast of band), monomer binding agent (polymerization in green band preparation process) and corresponding softening agent, dispersion agent are prepared the glass-ceramic system LTCC green band of high solids content, and are efficiently solved the anisotropic problem of traditional LTCC green band sintering shrinkage as organic curtain coating medium.
The glass-ceramic system LTCC green band of the present invention's preparation, surfacing, smooth, the X, Y, Z axis sintering shrinkage is 9 ~ 11%, can burn altogether in the wiring of the low melting point metals such as 850 ℃ of realizations and Au, Ag, wherein, that X, Y-axis are respectively is parallel in horizontal plane, perpendicular to the curtain coating direction, Z axis is perpendicular to the curtain coating in-plane.The sintering porcelain body has good dielectric properties: under 10GHz, and specific inductivity (ε
r) be 7 ~ 8, dielectric loss (tan δ) is less than 2 * 10
-3
Description of drawings
Fig. 1 is the present invention's borosilicate glass powder microgram used;
Fig. 2 is the ball-aluminium oxide powder microgram that the present invention adopts;
Fig. 3 is that green band of the present invention is through 850 ℃ of microstructure figure that sinter porcelain body into.
Embodiment
Embodiment 1
Select non-nodularization aluminum oxide powder (3 ~ 5um) fill phase as the pottery in the contained inorganic powder of 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, take respectively B
2O
318kg, SiO
265kg, Al
2O
38kg, MgO 5kg, K
2O 2kg, Na
2O 2kg after mixing 12h, is placed in platinum crucible, is incubated 3h under 1500 ~ 1600 ℃, pours in deionized water, obtains borosilicate glass fragment transparent, homogeneous.
Adopt the corundum pair roller that made glass fragment is pulverized, obtaining median size is the glass meal of 0.5 ~ 1mm, the glass meal is mixed with deionized water, zirconia ball is as ball-milling medium, in expecting: the ratio ball milling 8h of ball: water=1:3:0.8, be placed in 120 ℃ of baking ovens and dry by the fire 4h, obtaining median size is the borosilicate glass powder of 0.5 ~ 2um;
Borosilicate glass powder 55kg and spherical molten aluminum oxide powder 45kg are formed compound, add ethanol medium, according to compound: the ratio ball milling mixing 3h of zirconium ball: ethanol=1:2.5:1, be placed in 120 ℃ of baking ovens and dry by the fire 4h, obtain the low-temperature co-fired ceramic powder material.
Referring to table 1, add solvent, binding agent, softening agent, dispersion agent in described low-temperature co-fired ceramic powder material, under closed environment, ball milling mixes inorganic powder in the 10h(casting slurry and the weight ratio of zirconium ball is 1:4), vacuum defoamation, adopt the doctor blade method for tape-casting moulding, obtain the green band after drying, wherein: drying temperature is 25 ℃, and be 8h time of drying; To prepared green band cut into slices, after lamination in thermocompressor 70 ℃, 20MPa, pressurize 15min.
Table 1 borosilicate glass-each component concentration 1 of aluminum oxide LTCC green band
After green band after lamination hot pressing is cut into required size, be placed in to be incubated at the temperature that rises to setting after the electric furnace binder removal and burn till.The concrete steps of described sintering are: described low-temperature co-burning ceramic material is warming up to 450 ℃ from room temperature with the speed of 2 ℃/min, and insulation 2h is used for binder removal, guarantees organic abundant eliminating in sample; Low-temperature co-burning ceramic material after binder removal is warming up to 850 ℃ from 450 ℃ of beginnings with the speed of 5 ℃/min, and insulation 30min namely sinters porcelain into.Performance test to the sintering porcelain body is as shown in table 2.
Table 2 borosilicate glass-aluminum oxide LTCC green band sintering and dielectric properties 1
Embodiment 2
Select respectively the non-nodularization aluminum oxide powder of 1# (3 ~ 5um), (3 ~ 6um) fill phase as the pottery in the contained inorganic powder of green band to 2# ball-aluminium oxide powder, 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 see Table 3, ceramic phase is respectively non-ball-aluminium oxide in the contained inorganic powder of table 4(1# sample, and 2# is ball-aluminium oxide);
Table 3 borosilicate glass-each component concentration 2 of aluminum oxide LTCC green band
Table 4 borosilicate glass-aluminum oxide LTCC green band sintering and dielectric properties 2
Comparing embodiment 1 and embodiment 2, in the situation that guarantee that slurry viscosity is at suitable curtain coating scope (3 ~ 4 Pa.S), compare with conventional polymer binding agent polyvinyl butyral acetal, adopt monomer binding agent 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 embodiment 2, adopt β-dimethyl-aminoethylmethacrylate, methacrylic acid monomer mixture 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 to fill phase as the pottery of low-temperature co-burning ceramic material, green band solid content slightly increases (88% → 90%), and X-axis, Y-axis, Z-direction sintering shrinkage more be tending towards approaching, efficiently solves the anisotropic problem of traditional LTCC green band sintering shrinkage.
Claims (6)
1. a borosilicate glass and ball-aluminium oxide LTCC green band is characterized in that being made by the raw material of following parts by weight:
Borosilicate glass 30 ~ 70, ball-aluminium oxide accounts for 40 ~ 60, curtain coating medium 8 ~ 12.
2. a kind of borosilicate glass according to claim 1 and ball-aluminium oxide LTCC green band is characterized in that described borosilicate glass made by the raw material of following ratio of weight and number:
B
2O
3?15~25、SiO
2?50~70、Al
2O
3?10~15、MgO?5~10、K
2O?2~3、Na
2O?2~3。
3. a kind of borosilicate glass according to claim 1 and ball-aluminium oxide LTCC green band, it is characterized in that: the median size of borosilicate glass is 1 ~ 3um, the median size of ball-aluminium oxide is 3 ~ 6um.
4. a kind of borosilicate glass according to claim 1 and ball-aluminium oxide LTCC green band, it is characterized in that described curtain coating medium is comprised of mixed solvent, binding agent, softening agent and dispersion agent, the weight percent that each component is occupied machine curtain coating medium total amount is: mixed solvent 75 ~ 85%, monomer binding agent 3 ~ 8%, softening agent 2 ~ 6%, dispersion agent 2 ~ 6%.
5. a kind of borosilicate glass according to claim 4 and ball-aluminium oxide LTCC green band is characterized in that:
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 the 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%.
6. the preparation method of a borosilicate glass and ball-aluminium oxide LTCC green band is characterized in that comprising the following steps:
A, take raw material B by the 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, after being incubated 2 ~ 4h under 1500 ~ 1600 ℃, pours in deionized water, obtain glass fragment transparent, homogeneous;
C, employing corundum pair roller pulverize made glass fragment, obtaining median size is the glass meal of 0.5 ~ 1mm, the glass meal is mixed with deionized water, zirconia ball is as ball-milling medium, in the glass meal: ratio ball milling 5 ~ 10h of ball: water=1:3:0.8, then be placed in 120 ℃ of baking ovens and dry by the fire 4 ~ 6h, obtaining median size is the borosilicate glass powder of 1 ~ 3um;
D, be (30 ~ 70) with ratio of weight and number: the borosilicate glass powder of (40 ~ 60) and ball-aluminium oxide powder form compound, add ethanol medium, according to compound: ratio mixing and ball milling 2 ~ 4h of zirconium ball: ethanol=1:2.5:1, then be placed in 120 ℃ of baking ovens and dry by the fire 4 ~ 6h, obtain the low-temperature co-fired ceramic powder material;
E, add solvent, binding agent, softening agent, dispersion agent in described low-temperature co-fired ceramic powder material, under closed environment, ball milling mixes 8 ~ 12h, vacuum defoamation, adopt the doctor blade method for tape-casting moulding, obtain the green band after drying, wherein: drying temperature is 25 ℃, and be 6 ~ 12h time of drying.
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| CN115745577A (en) * | 2022-10-19 | 2023-03-07 | 中国建筑材料科学研究总院有限公司 | Preparation method of ultrathin low-temperature sintered ceramic substrate |
| CN115745577B (en) * | 2022-10-19 | 2023-09-22 | 中国建筑材料科学研究总院有限公司 | Preparation method of ultrathin low-temperature sintered ceramic substrate |
| CN115974531A (en) * | 2023-02-16 | 2023-04-18 | 浙江矽瓷科技有限公司 | Low-temperature co-fired ceramic tape-casting slurry and preparation method thereof |
| CN115974531B (en) * | 2023-02-16 | 2023-12-26 | 浙江矽瓷科技有限公司 | Low-temperature cofired ceramic tape casting slurry and preparation method thereof |
| CN116462494A (en) * | 2023-03-10 | 2023-07-21 | 浙江矽瓷科技有限公司 | Preparation method of component-controllable low-temperature co-fired ceramic granulating powder |
| CN117049864A (en) * | 2023-10-11 | 2023-11-14 | 有研工程技术研究院有限公司 | Low-temperature co-fired ceramic green ceramic tape, preparation method, ceramic circuit and application |
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