CN104446338A - Calcium aluminum silicon glass base low-temperature cofiring ceramic material and preparation method thereof - Google Patents
Calcium aluminum silicon glass base low-temperature cofiring ceramic material and preparation method thereof Download PDFInfo
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- CN104446338A CN104446338A CN201410674962.5A CN201410674962A CN104446338A CN 104446338 A CN104446338 A CN 104446338A CN 201410674962 A CN201410674962 A CN 201410674962A CN 104446338 A CN104446338 A CN 104446338A
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Abstract
The invention provides a calcium aluminum silicon glass base low-temperature cofiring ceramic material and a preparation method thereof. The ceramic material comprises the following components in parts by weight: 40-60 parts of calcium aluminum silicon glass, 2-5 parts of silicon carbide, 10-20 parts of forsterite, and 5-10 parts of carbon nano tube. According to the invention, the calcium aluminum silicon glass is adopted as basic glass; the principal crystalline phase is silicate p-wollostonite adopting a chain structure, and is crossed and arrayed to net in a needle-shaped manner in the glass body; the material is enabled to have characteristics of being abrasion resistant, corrosion-resistant and shock resistant; the silicon carbide, the forsterite and the carbon nano tube are added in the calcium aluminum silicon glass, and the synergistic effect among the materials is utilized, so that the thermal conductivity of the prepared ceramic material is improved; the melting point of the calcium aluminum silicon glass is further reduced; experimental result shows that the coefficient of thermal expansion of the prepared ceramic material is 6.0*10<-6>/K, the dielectric constant of the ceramic material is 5.2 (1 MHz), and the thermal conductivity of the ceramic material is 32 W/mK.
Description
Technical field
The present invention relates to LTCC Technology field, particularly relate to a kind of calcium aluminosilicate glass base low-temperature cofired ceramic material and preparation method thereof.
Background technology
Along with the develop rapidly of modern information technologies, the microminiaturization of electronic circuit, lightweight=integrated and high frequency propose the requirements such as small size, high frequency, high reliability and high integration to electron device.Select suitable to be no more than pottery low temperature co-fired at the temperature of 900 DEG C with electro-conductive materials such as silver, thus prepare sandwich type element or passive device is imbedded in multilayer circuit, become the certainty of above-mentioned trend, the LTCC as passive integration element main medium material also becomes a kind of important development trend.
LTCC (LTCC) technology adopts multilayered structure, usually using silver or the little metal of the resistivity such as copper as interconnecting conductor, multilayer dielectric structure and good metallic conductor can crosstalks between effective address signal, different passive device integration can be got up, realize miniaturization and the multifunction of electronic component.But the thermal conductivity of ltcc substrate material is on the low side, limit its application in more high-power, higher packaging density, thus the thermal conductivity improving ltcc substrate material becomes one of Focal point and difficult point of low temperature co-fired area research.
Prior art has carried out reporting widely to low-temperature co-burning ceramic material and preparation method thereof, such as, application number be 200610022007.9 Chinese patent literature report a kind of low temperature co-fired aluminium nitride ceramics and iolite-base glass composite material, by powder is added mould for hot pressed sintering, obtain the matrix material that thermal conductivity is up to 7.5W/mK.The people such as U.S. J.H.Enloe report a kind of baseplate material of environmental protection, and at 900 ~ 1400 DEG C, sintering obtains AlN-borosilicate glass substrate material, and its thermal conductivity is up to 7W/mK.But the preparation method of the basic material of above-mentioned report all adopts aluminium nitride and glass material compound to improve material thermal conductivity, and the material thermal conductivity prepared is lower, and is 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 ceramic material and preparation method thereof, and the thermal conductivity of calcium aluminosilicate glass base low-temperature cofired ceramic material prepared by the method is higher.
In view of this, the invention provides a kind of calcium aluminosilicate glass base low-temperature cofired ceramic material, consist of the following composition:
Preferably, consist of the following composition:
Accordingly, the present invention also provides a kind of preparation method of calcium aluminosilicate glass base low-temperature cofired ceramic material, comprises the following steps:
Add ethanol, ball-milling processing post-drying after 40 ~ 60 weight part calcium aluminosilicate glass powder, 2 ~ 5 weight part silicon carbide, 10 ~ 20 weight part forsterites and 5 ~ 10 parts by weight of carbon nanotubes being mixed, obtain low-temperature co-fired ceramic powder material;
In described low-temperature co-fired ceramic powder material, add solvent, binding agent, softening agent, dispersion agent and wetting agent, mix rear flow casting molding, after drying, sintering, obtains low-temperature co-burning ceramic material.
Preferably, described calcium aluminosilicate glass is by SiO
2, Al
2o
3prepare with CaO.
Preferably, the particle diameter of described calcium aluminosilicate glass powder is 1 ~ 6 μm.
Preferably, described calcium aluminosilicate glass is 50 ~ 60 weight parts, and described silicon carbide is 4 ~ 5 weight parts, and described forsterite is 10 ~ 15 weight parts, and described carbon nanotube is 8 ~ 10 weight parts.
Preferably, described softening agent is dibutyl phthalate.
Preferably, described dispersion agent is triolein.
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 hour, 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 method thereof, consist of the following composition: calcium aluminosilicate glass 40 ~ 60 weight part; Silicon carbide 2 ~ 5 weight part; Forsterite 10 ~ 20 weight part; Carbon nanotube 5 ~ 10 weight part.The present invention is glass based on calcium aluminosilicate glass, and its principal crystalline phase is the silicate p-wollastonite of chain-like structure, and it is netted with needle form cross arrangement in vitreum, makes material have the characteristics such as wear-resisting, corrosion-resistant and shock resistance.Silicon carbide ceramics has that oxidation-resistance is strong, wear resisting property good, Heat stability is good, hot strength are large, thermal expansivity is little, thermal conductivity is high and the good characteristic such as anti-thermal shock resistance to chemical attack mutually.The present invention, using forsterite as disperse ceramic phase, can improve the thermal conductivity of stupalith to a certain extent; By adding the carbon nanotube with high thermal conductivity, connecting silicon carbide and the forsterite with high thermal conductivity, forming the network-like conductive structure of 3 D stereo, strengthen the heat conductivility of stupalith.Compared with prior art, the present invention by adding silicon carbide, forsterite and carbon nanotube in calcium aluminosilicate glass, utilize synergy each other, improve the thermal conductivity of the low-temperature co-burning ceramic material of preparation, the fusing point of the low calcium aluminosilicate glass of a step-down of going forward side by side.Experimental result shows, the thermal expansivity of low-temperature co-burning ceramic material prepared by the present invention is 6.0 × 10
-6k
-1, specific inductivity is 5.2 (1MHz), and thermal conductivity is 32W/mK.
Embodiment
In order to understand the present invention further, below in conjunction with embodiment, the preferred embodiment of the invention is described, but should be appreciated that these describe just for further illustrating the features and advantages of the present invention, 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, consist of the following composition:
Preferably, described low-temperature co-burning ceramic material consists of the following composition:
The present invention is glass based on calcium aluminosilicate glass, and its principal crystalline phase is the silicate p-wollastonite of chain-like structure, and it is netted with needle form cross arrangement in vitreum, makes material have the characteristics such as wear-resisting, corrosion-resistant and shock resistance.
Take silicon carbide as ceramic phase, this silicon carbide has that oxidation-resistance is strong, wear resisting property good, Heat stability is good, hot strength are large, thermal expansivity is little, thermal conductivity is high and the good characteristic such as anti-thermal shock resistance to chemical attack.The present invention by adding the SiC material of high heat conductance in calcium aluminosilicate glass, both improve ltcc substrate material thermal conductivity, and reduce calcium aluminosilicate glass fusing point, thus achieve the low temperature dense sintering of SiC material, improve the thermal conductivity of the low-temperature co-burning ceramic material of preparation.
Further, the present invention, also using forsterite as disperse ceramic phase, can improve the thermal conductivity of stupalith to a certain extent, and have lower specific inductivity.Described forsterite can be natural, and can be also synthetic, to this present invention, there is no particular restriction.
In addition, the present invention adds the carbon nanotube with high thermal conductivity, connects silicon carbide and the forsterite with high thermal conductivity, forms the network-like conductive structure of 3 D stereo, strengthens the heat conductivility of stupalith further.
Compared with prior art, the present invention by adding silicon carbide, forsterite and carbon nanotube in calcium aluminosilicate glass, utilize synergy each other, improve the thermal conductivity of the low-temperature co-burning ceramic material of preparation, the fusing point of the low calcium aluminosilicate glass of a step-down of going forward side by side.
Accordingly, the present invention also provides a kind of preparation method of calcium aluminosilicate glass base low-temperature cofired ceramic material, comprises the following steps:
Add ethanol, ball-milling processing post-drying after 40 ~ 60 weight part calcium aluminosilicate glass powder, 2 ~ 5 weight part silicon carbide, 10 ~ 20 weight part forsterites and 5 ~ 10 parts by weight of carbon nanotubes being mixed, obtain low-temperature co-fired ceramic powder material;
In described low-temperature co-fired ceramic powder material, add solvent, binding agent, softening agent, dispersion agent and wetting agent, mix rear flow casting molding, after drying, sintering, obtains low-temperature co-burning ceramic material.
Wherein, described calcium aluminosilicate glass is by SiO
2, Al
2o
3prepare with CaO.The present invention is glass based on calcium aluminosilicate glass, and its principal crystalline phase is the silicate p-wollastonite of chain-like structure, and it is netted with needle form cross arrangement in vitreum, makes material have the characteristics such as wear-resisting, corrosion-resistant and shock resistance.The particle diameter of described calcium aluminosilicate glass powder is preferably 1 ~ 6 μm, is more preferably 2 ~ 5 μm.
In above-mentioned preparation process, the ball-milling processing time obtaining low-temperature co-fired ceramic powder material is preferably 6 ~ 10 hours, is more preferably 7 ~ 9 hours.By ball-milling processing, be conducive to obtaining homodisperse slurry, and then carry out flow casting molding and sintering processes.
After obtaining low-temperature co-fired ceramic powder material, in described low-temperature co-fired ceramic powder material, add solvent, binding agent, softening agent, dispersion agent and wetting agent.For the solvent adopted, there is no particular restriction in the present invention, can adopt solvent well known to those skilled in the art, be preferably trieline; For the binding agent adopted, there is no particular restriction in the present invention, can adopt binding agent well known to those skilled in the art, be preferably polyvinyl butyral solution; Described softening agent is preferably dibutyl phthalate; The dispersion agent that the present invention adopts is preferably triolein; Described wetting agent is preferably polyoxyethylene ester.
According to the present invention, described sintering step is specially: be warming up to 400 ~ 450 DEG C of insulations 2 ~ 3 hours, is warming up to 500 ~ 550 DEG C of insulations 1 ~ 5 hour, is then warming up to 650 ~ 680 DEG C of insulations 1 ~ 5 hour.The sintering process that the present invention preferably adopted for three stages heated up, that is: first 400 ~ 450 DEG C of insulations, make glass metal phase sintering, ensure its densified sintering product, the temperature of 400 ~ 450 DEG C is one of key factor affecting the low-temperature co-burning ceramic material obtained, insulating process promotes organic discharge in material, is conducive to the dense sintering controlling sintering shrinkage and be conducive to material.Then be warming up to 500 ~ 550 DEG C of insulations 1 ~ 5 hour, ensure the compactness of material, be then warming up to 650 ~ 680 DEG C, while the further sintering densification of material, slow crystallize out reduces glassy phase, ensures the performance of this low-temperature co-burning ceramic material.
The present invention, by adding silicon carbide, forsterite and carbon nanotube in calcium aluminosilicate glass, utilizes synergy each other, improves the thermal conductivity of the low-temperature co-burning ceramic material of preparation, the fusing point of the low calcium aluminosilicate glass of a step-down of going forward side by side.Experimental result shows, the thermal expansivity of low-temperature co-burning ceramic material prepared by the present invention is 6.0 × 10
-6k
-1, specific inductivity is 5.2 (1MHz), and thermal conductivity is 32W/mK.
In order to understand the present invention further, be described in detail to technical scheme provided by the invention below in conjunction with embodiment, 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) takes 50g calcium aluminosilicate glass powder, 5g SiC powder, 20g forsterite and 5g carbon nanotube, mixing, add and go ethanol to be placed in planetary ball mill grinding jar in right amount to mix 3 hours with 300r/min ball milling, then 120 DEG C of oven dry, low-temperature co-burning ceramic material powder is obtained.
Step (2) adds organic mass percent in described low-temperature co-burning ceramic material powder: the solution of trieline 76%, polyvinyl butyral acetal 14%, dibutyl phthalate 3%, triglycerin acid glyceride 4.8% and polyoxyethylene ester 2.2%, curtain coating is carried out after Homogeneous phase mixing, deaeration, dry, be warming up to 450 DEG C of insulations 2 hours, then 500 DEG C of insulations 5 hours are warming up to, then be warming up to 650 DEG C of insulations 2 hours, obtain calcium aluminosilicate glass base low-temperature cofired ceramic material.
Calcium aluminosilicate glass base low-temperature cofired ceramic material prepared by the present embodiment is measured.After tested, the thermal conductivity of this low-temperature co-burning ceramic material is 32W/mK, and specific inductivity is 5.2 (1MHz), and thermal expansivity is 6.0 × 10
-6k
-1.
Embodiment 2
Step (1) takes 40g calcium aluminosilicate glass powder, 5g SiC powder, 20g forsterite and 10g carbon nanotube, mixing, add and go ethanol to be placed in planetary ball mill grinding jar in right amount to mix 3 hours with 300r/min ball milling, then 120 DEG C of oven dry, low-temperature co-burning ceramic material powder is obtained.
Step (2) adds organic mass percent in described low-temperature co-burning ceramic material powder: the solution of trieline 76%, polyvinyl butyral acetal 14%, dibutyl phthalate 3%, triglycerin acid glyceride 4.8% and polyoxyethylene ester 2.2%, curtain coating is carried out after Homogeneous phase mixing, deaeration, dry, be warming up to 450 DEG C of insulations 2 hours, then 500 DEG C of insulations 5 hours are warming up to, then be warming up to 650 DEG C of insulations 2 hours, obtain calcium aluminosilicate glass base low-temperature cofired ceramic material.
Calcium aluminosilicate glass base low-temperature cofired ceramic material prepared by the present embodiment is measured.After tested, the thermal conductivity of this low-temperature co-burning ceramic material is 31W/mK, and specific inductivity is 5.3 (1MHz), and thermal expansivity is 6.1 × 10
-6k
-1.
Embodiment 2
Step (1) takes 60g calcium aluminosilicate glass powder, 4g SiC powder, 15g forsterite and 8g carbon nanotube, mixing, add and go ethanol to be placed in planetary ball mill grinding jar in right amount to mix 3 hours with 300r/min ball milling, then 120 DEG C of oven dry, low-temperature co-burning ceramic material powder is obtained.
Step (2) adds organic mass percent in described low-temperature co-burning ceramic material powder: the solution of trieline 76%, polyvinyl butyral acetal 14%, dibutyl phthalate 3%, triglycerin acid glyceride 4.8% and polyoxyethylene ester 2.2%, curtain coating is carried out after Homogeneous phase mixing, deaeration, dry, be warming up to 450 DEG C of insulations 2 hours, then 500 DEG C of insulations 5 hours are warming up to, then be warming up to 680 DEG C of insulations 2 hours, obtain calcium aluminosilicate glass base low-temperature cofired ceramic material.
Calcium aluminosilicate glass base low-temperature cofired ceramic material prepared by the present embodiment is measured.After tested, the thermal conductivity of this low-temperature co-burning ceramic material is 30W/mK, and specific inductivity is 5.3 (1MHz), and thermal expansivity is 6.0 × 10
-6k
-1.
The explanation of above embodiment just understands method of the present invention and core concept thereof for helping.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improve and modify 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 are realized or uses the present invention.To be apparent for those skilled in the art to the multiple amendment of these embodiments, General Principle as defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention can not be restricted to these embodiments shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (10)
1. a calcium aluminosilicate glass base low-temperature cofired ceramic material, is characterized in that, consists of the following composition:
2. low-temperature co-burning ceramic material according to claim 1, is characterized in that, consists of the following composition:
3. a preparation method for calcium aluminosilicate glass base low-temperature cofired ceramic material, is characterized in that, comprises the following steps:
Add ethanol, ball-milling processing post-drying after 40 ~ 60 weight part calcium aluminosilicate glass powder, 2 ~ 5 weight part silicon carbide, 10 ~ 20 weight part forsterites and 5 ~ 10 parts by weight of carbon nanotubes being mixed, obtain low-temperature co-fired ceramic powder material;
In described low-temperature co-fired ceramic powder material, add solvent, binding agent, softening agent, dispersion agent and wetting agent, mix rear flow casting molding, after drying, sintering, obtains low-temperature co-burning ceramic material.
4. preparation method according to claim 3, is characterized in that, described calcium aluminosilicate glass is by SiO
2, Al
2o
3prepare with CaO.
5. preparation method according to claim 3, is characterized in that, the particle diameter of described calcium aluminosilicate glass powder is 1 ~ 6 μm.
6. preparation method according to claim 3, is characterized in that, described calcium aluminosilicate glass is 50 ~ 60 weight parts, and described silicon carbide is 4 ~ 5 weight parts, and described forsterite is 10 ~ 15 weight parts, and described carbon nanotube is 8 ~ 10 weight parts.
7. preparation method according to claim 3, is characterized in that, described softening agent is dibutyl phthalate.
8. preparation method according to claim 3, is characterized in that, described dispersion agent is triolein.
9. preparation method according to claim 3, is characterized in that, described wetting agent is polyoxyethylene ester.
10. preparation method according to claim 3, is characterized in that, 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 hour, be then warming up to 650 ~ 680 DEG C of insulations 1 ~ 5 hour.
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| CN110423120A (en) * | 2019-07-18 | 2019-11-08 | 西南科技大学 | A kind of preparation method of SiC base complex phase ceramic solidified body |
| CN116730731A (en) * | 2023-05-09 | 2023-09-12 | 武汉科技大学 | Silicon carbide-based ceramic heat accumulator and preparation method thereof |
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