CN104446338B - A kind of calcium aluminosilicate glass base low-temperature cofired ceramic material and preparation method thereof - Google Patents
A kind of calcium aluminosilicate glass base low-temperature cofired ceramic material and preparation method thereof Download PDFInfo
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- CN104446338B CN104446338B CN201410674962.5A CN201410674962A CN104446338B CN 104446338 B CN104446338 B CN 104446338B CN 201410674962 A CN201410674962 A CN 201410674962A CN 104446338 B CN104446338 B CN 104446338B
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Abstract
The invention provides a kind of calcium aluminosilicate glass base low-temperature cofired ceramic material and preparation method thereof, consist of the following composition: calcium aluminosilicate glass 40～60 weight portions; Carborundum 2～5 weight portions; Forsterite 10～20 weight portions; CNT 5～10 weight portions. The present invention is taking calcium aluminosilicate glass as parent glass, the silicate p-wollastonite that its principal crystalline phase is chain structure, and it is netted with the cross arrangement of needle-like form in vitreum, makes material have the characteristics such as wear-resisting, corrosion-resistant and shock resistance. The present invention, by add carborundum, forsterite and CNT in calcium aluminosilicate glass, utilizes synergy each other, has improved the thermal conductivity of the low-temperature co-burning ceramic material of preparation, and further reduces the fusing point of calcium aluminosilicate glass. Experimental result shows, the thermal coefficient of expansion of low-temperature co-burning ceramic material prepared by the present invention is 6.0 × 10-6K-1, dielectric constant is 5.2 (1MHz), thermal conductivity is 32W/mK.
Description
Technical field
The present invention relates to LTCC Technology field, relate in particular to a kind of calcium aluminosilicate glass baseLow-temperature co-burning ceramic material and preparation method thereof.
Background technology
Along with the develop rapidly of modern information technologies, the microminiaturization of electronic circuit, lightweight=collectionOne-tenthization and high frequency have proposed small size, high-frequency, high reliability and high integrated to electronic deviceThe requirements such as degree. Select suitable bending down in the temperature that is no more than 900 DEG C with conductive materials such as silverThe pottery that temperature is burnt altogether, thus prepare sandwich type element or passive device is imbedded in multilayer circuit, becomeFor the certainty of above-mentioned trend, as the LTCC of passive integration element main medium materialAlso become a kind of important development trend.
LTCC (LTCC) technology is to adopt sandwich construction, conventionally with silver or copper etc.The little metal of resistivity is as interconnecting conductor, and multilayer dielectric structure and good metallic conductor are passableCrosstalking between effective address signal, can get up different passive device integrations, realizes electronics unitThe miniaturization of part and multifunction. But the thermal conductivity of ltcc substrate material is on the low side, restrictionIts application in more high-power, higher packaging density, thereby improve ltcc substrate materialThermal conductivity become one of Focal point and difficult point of low temperature co-fired area research.
Prior art has been carried out report widely to low-temperature co-burning ceramic material and preparation method thereof,For example, the Chinese patent literature that application number is 200610022007.9 has been reported a kind of low temperature co-firedAluminium nitride ceramics and cordierite-base glass composite material, by adding powder hot pressing in mould to burnKnot, obtains thermal conductivity and is up to the composite of 7.5W/mK. People's reports such as U.S. J.H.EnloeRoad a kind of baseplate material of environmental protection, at 900～1400 DEG C, sintering obtains AlN-borosilicateGlass substrate material, its thermal conductivity is up to 7W/mK. But, the stock of above-mentioned reportPreparation method all adopt aluminium nitride and the compound raising material thermal conductivity of glass material, prepareMaterial thermal conductivity lower, and be unfavorable for large-scale industrial production.
Summary of the invention
The technical problem that the present invention solves is to provide a kind of calcium aluminosilicate glass base low-temperature cofired potteryCeramic material and preparation method thereof, calcium aluminosilicate glass base low-temperature cofired ceramic material prepared by the methodThermal conductivity higher.
In view of this, the invention provides a kind of calcium aluminosilicate glass base low-temperature cofired ceramic material,Made by following composition:
Preferably, made by following composition:
Accordingly, the present invention also provides a kind of system of calcium aluminosilicate glass base low-temperature cofired ceramic materialPreparation Method, comprises the following steps:
By 40～60 weight portion calcium aluminosilicate glass, 2～5 weight portion carborundum, 10～20 weight portionsForsterite and 5～10 weight portion CNTs add ethanol after mixing, ball-milling treatment post-drying,Obtain low-temperature co-fired ceramic powder material;
In described low-temperature co-fired ceramic powder material, add solvent, binding agent, plasticizer, dispersantAnd wetting agent, mixing rear flow casting molding, sintering after drying, obtains LTCC materialMaterial.
Preferably, described calcium aluminosilicate glass is by SiO2、Al2O3Prepare with CaO.
Preferably, the particle diameter of described calcium aluminosilicate glass is 1～6 μ m.
Preferably, described calcium aluminosilicate glass is 50～60 weight portions, and described carborundum is 4～5 weightsAmount part, described forsterite is 10～15 weight portions, described CNT is 8～10 weightsAmount part.
Preferably, described plasticizer is dibutyl phthalate.
Preferably, described dispersant is olein.
Preferably, described wetting agent is polyoxyethylene ester.
Preferably, described sintering step is specially:
Be warming up to 400～450 DEG C of insulations 2～3 hours, be warming up to 500～550 DEG C of insulations 1～5 littleTime, be then warming up to 650～680 DEG C of insulations 1～5 hour.
The invention provides a kind of calcium aluminosilicate glass base low-temperature cofired ceramic material and preparation side thereofMethod, consists of the following composition: calcium aluminosilicate glass 40～60 weight portions; Carborundum 2～5 weight portions;Forsterite 10～20 weight portions; CNT 5～10 weight portions. The present invention is with calcium aluminium silicon glassGlass is parent glass, the silicate p-wollastonite that its principal crystalline phase is chain structure, and it is at vitreumIn be netted with the cross arrangement of needle-like form, make material there are wear-resisting, corrosion-resistant and shock resistance etc.Characteristic. Silicon carbide ceramics has that non-oxidizability is strong, anti-wear performance good mutually, Heat stability is good, heightTemperature intensity is large, thermal coefficient of expansion is little, thermal conductivity is high and the good spy such as anti-thermal shock resistance to chemical attackProperty. The present invention, using forsterite as disperse ceramic phase, can improve ceramic material to a certain extentThe thermal conductivity of material; There is the CNT of high thermal conductivity by interpolation, connect and there is high thermal conductivityCarborundum and forsterite, form the network-like conductive structure of 3 D stereo, strengthen potteryThe heat conductivility of material. Compared with prior art, the present invention by adding in calcium aluminosilicate glassCarborundum, forsterite and CNT, utilize synergy each other, improved systemThe thermal conductivity of standby low-temperature co-burning ceramic material, and further reduce the fusing point of calcium aluminosilicate glass.Experimental result shows, the thermal coefficient of expansion of low-temperature co-burning ceramic material prepared by the present invention is6.0×10-6K-1, dielectric constant is 5.2 (1MHz), thermal conductivity is 32W/mK.
Detailed description of the invention
In order further to understand the present invention, below in conjunction with embodiment to the preferred embodiment of the inventionBe described, but should be appreciated that these are described is for further illustrating feature of the present inventionAnd advantage, instead of limiting to the claimed invention.
The embodiment of the invention discloses a kind of calcium aluminosilicate glass base low-temperature cofired ceramic material, by withLower composition is made:
As preferred version, described low-temperature co-burning ceramic material is made up of following composition:
The present invention is taking calcium aluminosilicate glass as parent glass, the silicate that its principal crystalline phase is chain structureP-wollastonite, it is netted with the cross arrangement of needle-like form in vitreum, material is had resistance toThe characteristics such as mill, corrosion-resistant and shock resistance.
Taking carborundum as ceramic phase, this carborundum has that non-oxidizability is strong, anti-wear performance good, hotGood stability, elevated temperature strength is large, thermal coefficient of expansion is little, thermal conductivity is high and anti-thermal shock chemically-resistantThe good characteristics such as corrosion. The present invention by adding the SiC material of high heat conductance in calcium aluminosilicate glassMaterial, had both improved ltcc substrate material thermal conductivity, and had reduced calcium aluminosilicate glass fusing point, fromAnd realized the low temperature dense sintering of SiC material, improve the low-temperature co-burning ceramic material of preparationThermal conductivity.
And the present invention, also using forsterite as disperse ceramic phase, can carry to a certain extentThe thermal conductivity of high ceramic material, and there is lower dielectric constant. Described forsterite is passableBeing natural, can be also artificial synthetic, and to this present invention, there is no particular restriction.
In addition, the present invention adds the CNT with high thermal conductivity, connects and has high thermal conductivityCarborundum and forsterite, form the network-like conductive structure of 3 D stereo, further increaseThe heat conductivility of strong ceramic material.
Compared with prior art, the present invention by adding carborundum, magnesium olive in calcium aluminosilicate glassOlive stone and CNT, utilize synergy each other, improved the low temperature co-fired of preparationThe thermal conductivity of ceramic material, and further reduce the fusing point of calcium aluminosilicate glass.
Accordingly, the present invention also provides a kind of system of calcium aluminosilicate glass base low-temperature cofired ceramic materialPreparation Method, comprises the following steps:
By 40～60 weight portion calcium aluminosilicate glass, 2～5 weight portion carborundum, 10～20 weight portionsForsterite and 5～10 weight portion CNTs add ethanol after mixing, ball-milling treatment post-drying,Obtain low-temperature co-fired ceramic powder material;
In described low-temperature co-fired ceramic powder material, add solvent, binding agent, plasticizer, dispersantAnd wetting agent, mixing rear flow casting molding, sintering after drying, obtains LTCC materialMaterial.
Wherein, described calcium aluminosilicate glass is by SiO2、Al2O3Prepare with CaO. The present invention is with calciumAluminosilicate glass is parent glass, the silicate p-wollastonite that its principal crystalline phase is chain structure, itsIn vitreum, be netted with the cross arrangement of needle-like form, material had wear-resisting, corrosion-resistant and anti-The characteristics such as impact. The particle diameter of described calcium aluminosilicate glass is preferably 1～6 μ m, more preferably 2～5 μm。
In above-mentioned preparation process, the ball-milling treatment time that obtains low-temperature co-fired ceramic powder material is preferredBe 6～10 hours, more preferably 7～9 hours. By ball-milling treatment, be conducive to obtain evenlyThe slurry disperseing, and then carry out flow casting molding and sintering processes.
Obtain after low-temperature co-fired ceramic powder material, molten to adding in described low-temperature co-fired ceramic powder materialAgent, binding agent, plasticizer, dispersant and wetting agent. The present invention there is no for the solvent adoptingSpecial restriction, can adopt solvent well known to those skilled in the art, is preferably trichloro-ethylene;For the binding agent adopting, there is no particular restriction in the present invention, can adopt those skilled in the art ripeThe binding agent of knowing, is preferably polyvinyl butyral resin solution; Described plasticizer is preferably adjacent benzene twoFormic acid dibutyl ester; The dispersant that the present invention adopts is preferably olein; Described wetting agentBe preferably polyoxyethylene ester.
According to the present invention, described sintering step is specially: be warming up to 400～450 DEG C of insulations 2～3Hour, be warming up to 500～550 DEG C of insulations 1～5 hour, be then warming up to 650～680 DEG C of insulations1～5 hour. The present invention preferably adopts the sintering process of three stages intensification, that is: first at 400～450 DEG CInsulation, makes glass metal phase sintering, ensures its densified sintering product, and the temperature of 400～450 DEG C is shadowRing one of key factor of the low-temperature co-burning ceramic material obtaining, insulating process promotes have in materialThe discharge of machine thing, is conducive to the dense sintering of controlling sintering shrinkage and being conducive to material. ThenBe warming up to 500～550 DEG C of insulations 1～5 hour, ensure the compactness of material, be then warming up to650～680 DEG C, when the further sintering densification of material, slow crystallize out reduces glassy phase,Ensure the performance of this low-temperature co-burning ceramic material.
The present invention is by add carborundum, forsterite and CNT in calcium aluminosilicate glass,Utilize synergy each other, improved the thermal conductivity of the low-temperature co-burning ceramic material of preparation,And further reduce the fusing point of calcium aluminosilicate glass. Experimental result shows, low temperature prepared by the present inventionThe thermal coefficient of expansion of material of ceramics burned together is 6.0 × 10-6K-1, dielectric constant is 5.2 (1MHz),Thermal conductivity is 32W/mK.
In order further to understand the present invention, below in conjunction with embodiment to technical side provided by the inventionCase is elaborated, and protection scope of the present invention is not limited by the following examples.
The chemical reagent that the embodiment of the present invention adopts is commercial.
Embodiment 1
Step (1) take 50g calcium aluminosilicate glass, 5gSiC powder, 20g forsterite and5g CNT, mixes, add go in right amount ethanol be placed in planetary ball mill grinding jar with300r/min ball milling mixes 3 hours, then, 120 DEG C of oven dry, obtains LTCC materialMaterial powder.
Step (2) adds organic quality hundred in described low-temperature co-burning ceramic material powderProportion by subtraction is: trichloro-ethylene 76%, polyvinyl butyral resin 14%, dibutyl phthalate 3%,The solution of triglycerin acid glyceride 4.8% and polyoxyethylene ester 2.2%, evenly after mixing, deaerationCarry out curtain coating, dry, be warming up to 450 DEG C of insulations 2 hours, be then warming up to 500 DEG C of insulations 5Hour, be then warming up to 650 DEG C of insulations 2 hours, obtain the base low-temperature cofired pottery of calcium aluminosilicate glassCeramic material.
Calcium aluminosilicate glass base low-temperature cofired ceramic material prepared by the present embodiment is measured. WarpTest, the thermal conductivity of this low-temperature co-burning ceramic material is 32W/mK, dielectric constant is5.2 (1MHz), thermal coefficient of expansion is 6.0 × 10-6K-1。
Embodiment 2
Step (1) take 40g calcium aluminosilicate glass, 5gSiC powder, 20g forsterite and10g CNT, mixes, add go in right amount ethanol be placed in planetary ball mill grinding jar with300r/min ball milling mixes 3 hours, then, 120 DEG C of oven dry, obtains LTCC materialMaterial powder.
Step (2) adds organic quality hundred in described low-temperature co-burning ceramic material powderProportion by subtraction is: trichloro-ethylene 76%, polyvinyl butyral resin 14%, dibutyl phthalate 3%,The solution of triglycerin acid glyceride 4.8% and polyoxyethylene ester 2.2%, evenly after mixing, deaerationCarry out curtain coating, dry, be warming up to 450 DEG C of insulations 2 hours, be then warming up to 500 DEG C of insulations 5Hour, be then warming up to 650 DEG C of insulations 2 hours, obtain the base low-temperature cofired pottery of calcium aluminosilicate glassCeramic material.
Calcium aluminosilicate glass base low-temperature cofired ceramic material prepared by the present embodiment is measured. WarpTest, the thermal conductivity of this low-temperature co-burning ceramic material is 31W/mK, dielectric constant is5.3 (1MHz), thermal coefficient of expansion is 6.1 × 10-6K-1。
Embodiment 2
Step (1) take 60g calcium aluminosilicate glass, 4gSiC powder, 15g forsterite and8g CNT, mixes, add go in right amount ethanol be placed in planetary ball mill grinding jar with300r/min ball milling mixes 3 hours, then, 120 DEG C of oven dry, obtains LTCC materialMaterial powder.
Step (2) adds organic quality hundred in described low-temperature co-burning ceramic material powderProportion by subtraction is: trichloro-ethylene 76%, polyvinyl butyral resin 14%, dibutyl phthalate 3%,The solution of triglycerin acid glyceride 4.8% and polyoxyethylene ester 2.2%, evenly after mixing, deaerationCarry out curtain coating, dry, be warming up to 450 DEG C of insulations 2 hours, be then warming up to 500 DEG C of insulations 5Hour, be then warming up to 680 DEG C of insulations 2 hours, obtain the base low-temperature cofired pottery of calcium aluminosilicate glassCeramic material.
Calcium aluminosilicate glass base low-temperature cofired ceramic material prepared by the present embodiment is measured. WarpTest, the thermal conductivity of this low-temperature co-burning ceramic material is 30W/mK, dielectric constant is5.3 (1MHz), thermal coefficient of expansion is 6.0 × 10-6K-1。
The explanation of above embodiment is just for helping to understand method of the present invention and core think of thereofThink. It should be pointed out that for those skilled in the art, do not departing from thisUnder the prerequisite of bright principle, can also carry out some improvement and modification to the present invention, these improve andModify and also fall in the protection domain of the claims in the present invention.
To the above-mentioned explanation of the disclosed embodiments, professional and technical personnel in the field can be realizedOr use the present invention. The multiple amendment of these embodiment is come those skilled in the artSay it will will be apparent, General Principle as defined herein can do not depart from of the present inventionIn the situation of spirit or scope, realize in other embodiments. Therefore, the present invention will be not can be byBe limited to these embodiment shown in this article, but will meet and principle disclosed herein and newGrain husk feature the widest consistent scope.
Claims (10)
1. a calcium aluminosilicate glass base low-temperature cofired ceramic material, is characterized in that, by belowComposition is made:
2. low-temperature co-burning ceramic material according to claim 1, is characterized in that, byFollowing composition is made:
3. a preparation method for calcium aluminosilicate glass base low-temperature cofired ceramic material, its feature existsIn, comprise the following steps:
By 40～60 weight portion calcium aluminosilicate glass, 2～5 weight portion carborundum, 10～20 weight portionsForsterite and 5～10 weight portion CNTs add ethanol after mixing, ball-milling treatment post-drying,Obtain low-temperature co-fired ceramic powder material;
In described low-temperature co-fired ceramic powder material, add solvent, binding agent, plasticizer, dispersantAnd wetting agent, mixing rear flow casting molding, sintering after drying, obtains LTCC materialMaterial.
4. preparation method according to claim 3, is characterized in that, described calcium aluminium siliconGlass is by SiO2、Al2O3Prepare with CaO.
5. preparation method according to claim 3, is characterized in that, described calcium aluminium siliconThe particle diameter of glass is 1～6 μ m.
6. preparation method according to claim 3, is characterized in that, described calcium aluminium siliconGlass is 50～60 weight portions, and described carborundum is 4～5 weight portions, and described forsterite is10～15 weight portions, described CNT is 8～10 weight portions.
7. preparation method according to claim 3, is characterized in that, described plasticizerFor dibutyl phthalate.
8. preparation method according to claim 3, is characterized in that, described dispersantFor olein.
9. preparation method according to claim 3, is characterized in that, described wetting agentFor polyoxyethylene ester.
10. preparation method according to claim 3, is characterized in that, described sintering stepSuddenly be specially:
Be warming up to 400～450 DEG C of insulations 2～3 hours, be warming up to 500～550 DEG C of insulations 1～5 littleTime, be then warming up to 650～680 DEG C of insulations 1～5 hour.
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| CN101161605A (en) * | 2006-10-09 | 2008-04-16 | 九豪精密陶瓷股份有限公司 | Low-temperature sintered ceramic material |
| JP2010208944A (en) * | 2010-06-18 | 2010-09-24 | Kyocera Corp | Glass ceramic, method of manufacturing the same, and wiring board using the same |
| CN102531392A (en) * | 2012-02-01 | 2012-07-04 | 云南云天化股份有限公司 | Low-temperature co-fired ceramic material and preparation method thereof |
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| CN101161605A (en) * | 2006-10-09 | 2008-04-16 | 九豪精密陶瓷股份有限公司 | Low-temperature sintered ceramic material |
| JP2010208944A (en) * | 2010-06-18 | 2010-09-24 | Kyocera Corp | Glass ceramic, method of manufacturing the same, and wiring board using the same |
| CN102531392A (en) * | 2012-02-01 | 2012-07-04 | 云南云天化股份有限公司 | Low-temperature co-fired ceramic material and preparation method thereof |
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