CN114014669B - Preparation method of stretch-proof aluminum nitride raw porcelain substrate - Google Patents
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Abstract
The invention relates to the technical field of electronic packaging ceramics, and particularly discloses a preparation method of a stretch-resistant aluminum nitride green ceramic substrate. According to the preparation method of the stretch-proof aluminum nitride raw ceramic substrate, provided by the invention, the dispersion and stability of the tape casting slurry are improved through a specific material adding sequence and a staged ball milling method, the distribution of coarse particle size particles in powder is reduced, the uniformity of slurry components is obviously improved, the specific drying temperature arrangement mode of the tape casting process is further combined, the generation of surface defects of the raw ceramic substrate is effectively inhibited, the preparation of the aluminum nitride raw ceramic substrate with good stretch-proof performance and high uniformity is facilitated, meanwhile, the drying efficiency of the tape casting material is improved, the preparation process is simple to operate and easy to control, and the preparation method has higher popularization and application values.
Description
Technical Field
The invention relates to the technical field of electronic packaging ceramics, in particular to a preparation method of a stretch-proof aluminum nitride green ceramic substrate.
Background
The method is that aluminum nitride powder, solvent, dispersant, adhesive, plasticizer and other materials are ball milled to prepare slurry with flowability and certain viscosity, and the slurry is cast with casting machine to prepare green ceramic substrate with certain tensile strength; then punching, hole filling, printing, lamination, hot cutting, glue discharging and sintering are carried out through a subsequent ceramic production process to obtain the ceramic element. The tensile strength of the raw porcelain substrate is an effective index for representing the processing performance of the raw porcelain substrate, and the higher the tensile strength of the raw porcelain substrate is, the less problems such as mucous membrane, tearing, porcelain shortage, powder falling and the like are generated in the processing process of the raw porcelain, so that the higher the yield of the final product is facilitated.
However, since aluminum nitride powder is difficult to sinter, a high sintering temperature is required, and aluminum nitride powder having a small particle size and a large specific surface area is currently used as a raw material in order to reduce the sintering temperature and to facilitate the control of the sintering process. However, when aluminum nitride powder with small particle size and high specific surface is prepared into slurry, more binder and plasticizer are needed to be added, more organic components are needed in the slurry, the uniformity of the slurry is poor, defoaming is incomplete, and quality defects such as cracking, dark cracking, pinholes, non-drying of a blank roll, poor thickness consistency and the like are easily generated in the casting process, so that the tensile resistance of the prepared green ceramic substrate is poor, and the subsequent sintering quality is indirectly influenced. Therefore, there is a need to develop a method for producing an aluminum nitride green ceramic substrate which can reduce the surface defects of the green ceramic substrate and improve the tensile properties of the green ceramic substrate.
Disclosure of Invention
Aiming at the problems of more surface defects and poor stretch resistance of the aluminum nitride raw ceramic substrate prepared by the prior art, the invention provides a preparation method of the stretch-resistant aluminum nitride raw ceramic substrate.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a preparation method of a stretch-proof aluminum nitride green ceramic substrate comprises the following steps:
step a, uniformly mixing a binder, a plasticizer and an organic solvent to obtain a mixed solution;
step b, adding a dispersing agent, an organic solvent and a sintering aid into a ball mill to perform first pre-ball milling, and then adding aluminum nitride powder to perform second pre-ball milling to obtain pre-milled powder;
step c, adding the mixed solution into a pre-grinding powder for ball milling, and then performing vacuum defoaming under the negative pressure condition until the viscosity of the slurry is 2000 CPS-20000 CPS, so as to obtain a casting slurry;
step d, adopting a 4-section zoned temperature control type casting machine to cast and mold the casting slurry, and drying to obtain an aluminum nitride raw porcelain substrate; wherein the temperature of the first drying bin area of the zoned temperature control casting machine is 70-90 ℃, the temperature of the second drying bin area is 50-70 ℃, the temperature of the third drying bin area is 40-50 ℃, and the temperature of the fourth drying bin area is 90-110 ℃.
Compared with the prior art, the preparation method of the stretch-proof aluminum nitride green ceramic substrate improves the dispersibility and stability of the casting slurry, reduces the distribution of coarse particle size particles in powder, remarkably improves the uniformity of slurry components, further combines a specific drying temperature arrangement mode of a casting procedure, effectively inhibits the generation of surface defects of the green ceramic substrate, is beneficial to obtaining the aluminum nitride green ceramic substrate with good stretch-proof performance and high uniformity, simultaneously improves the drying efficiency of the casting strip, has simple operation and easy control of the preparation process, and has higher popularization and application values.
Preferably, in step a, the amounts of the components are: 2 to 10 parts of binder, 0.5 to 5.0 parts of plasticizer and 20 to 25 parts of organic solvent.
Preferably, in step a, the binder is polyvinyl butyral.
Preferably, in step a, the plasticizer is dibutyl phthalate, butyl benzyl phthalate, dibutyl phthalate, a carbonic acid acrylate or polyethylene glycol.
Preferably, in the step a and the step b, the organic solvent is a binary solvent consisting of any two of absolute ethyl alcohol, butanone, methyl isobutyl ketone or toluene.
Further preferably, in the step a and the step b, the organic solvent is a binary solvent consisting of ethanol and methyl isobutyl ketone, absolute ethanol and butanone, absolute ethanol and toluene, butanone and toluene or methyl isobutyl ketone and toluene.
The invention has no specific requirement on the proportion of each component in the binary organic solvent, the specific proportion composition can be obtained by routine test adjustment, and the basically equivalent technical effects can be achieved.
In step a, the binder, plasticizer and organic solvent are mixed uniformly at 40 to 60 ℃.
The optimized binder and plasticizer are pre-dissolved, so that the influence of undissolved micelles in the casting slurry is avoided, and more uniform casting slurry is obtained.
Preferably, in step b, the amounts of the components are: 0.5 to 2.0 parts of dispersing agent, 50 to 80 parts of organic solvent, 1 to 8 parts of sintering aid and 90 to 100 parts of aluminum nitride powder.
Preferably, in step b, the dispersant is oleic acid, linoleic acid, stearic acid, polyacrylate dispersant or herring fish oil.
Preferably, in the step b, the sintering aid is at least one of samarium oxide, yttrium oxide, dysprosium oxide or europium oxide.
When the sintering aid is a combination of a plurality of rare earth metal oxides, the proportion of each component is not particularly required, and the sintering aid can be obtained by conventional test adjustment and can achieve basically equivalent technical effects.
After premixing and ball milling a small amount of sintering aid, a dispersing agent and an organic solvent, mixing and ball milling with aluminum nitride powder, so that the sintering aid and aluminum nitride powder are fully mixed, the function of the sintering aid is fully exerted, the performance of the prepared green ceramic substrate is improved, and the stability of subsequent processing application is improved.
Preferably, in the step b, the rotating speed of the first pre-ball milling is 20 rpm-40 rpm, and the ball milling time is 2-4 h.
Preferably, in the step b, the rotation speed of the second pre-ball milling is 20 rpm-40 rpm, and the ball milling time is 24-48 h.
Preferably, in the step c, the rotating speed of the ball milling is 20 rpm-40 rpm, and the ball milling time is 24-48 h.
The ball milling rotating speed of each step is preferable, so that the dispersibility of each material is improved, and the uniformity of a system is improved, and the stability of the casting substrate and the molding uniformity of sintering of ceramic products are improved.
Preferably, in the step c, the vacuum degree of the negative pressure condition is 0.05MPa to 0.095MPa.
The preferable negative pressure condition is favorable for sufficiently removing micro bubbles in the casting slurry, so that the aluminum nitride ceramic green body substrate obtained by casting has lower porosity, and the defect of the aluminum nitride green body substrate is reduced.
Preferably, in step d, the casting belt speed is 0.3m/min to 0.8m/min.
The preferable tape is matched with a specific tape casting drying temperature arrangement mode, so that the surface of the slurry can be dried and shaped quickly, the problem of microcrack caused by too fast evaporation of the solvent can be avoided, the problem of deformation or adhesion of a tape casting material can be avoided, and the quality and the yield of the prepared aluminum nitride raw ceramic substrate can be improved.
The preparation method of the stretch-proof aluminum nitride raw ceramic substrate provided by the invention can effectively reduce the occurrence of surface defects of the prepared aluminum nitride ceramic substrate and improve the component uniformity of the raw ceramic substrate, so that the prepared aluminum nitride raw ceramic substrate has higher stretch-proof performance, and the preparation method is simple, high in production efficiency and has higher application prospect.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) image of an aluminum nitride green porcelain substrate prepared in example 1 of the present invention;
FIG. 2 is a photograph showing the surface state of an aluminum nitride green porcelain substrate prepared in example 1 of the present invention;
FIG. 3 is a Scanning Electron Microscope (SEM) image of an aluminum nitride green porcelain substrate prepared according to comparative example 1 of the present invention;
FIG. 4 is a photograph showing the surface state of an aluminum nitride green porcelain substrate prepared in comparative example 1 of the present invention;
FIG. 5 is a graph showing the tensile strength of the aluminum nitride green porcelain substrates prepared in example 1 and comparative example 1 according to the present invention, wherein a is example 1 and b is comparative example 2.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Example 1
A preparation method of a stretch-proof aluminum nitride green ceramic substrate comprises the following steps:
s1, weighing 5 parts of polyvinyl butyral and 2 parts of dibutyl phthalate, adding the polyvinyl butyral and the dibutyl phthalate into a mixed solvent (volume ratio of 1:2) of 22 parts of absolute ethyl alcohol and toluene, and stirring at 50 ℃ for 35 hours to obtain a mixed solution;
s2, weighing 1 part of oleic acid, 65 parts of the mixed solvent of the absolute ethyl alcohol and the toluene and 5 parts of europium oxide, adding into a ball mill, ball milling for 3 hours at 30rpm to uniformly disperse, adding 95 parts of aluminum nitride powder, and ball milling for 36 hours at 30rpm to uniformly disperse to obtain pre-ground powder;
s3, adding the mixed solution into a pre-grinding powder, continuously ball-milling for 36 hours, and then vacuum defoaming under the condition of-0.07 MPa until the viscosity of the slurry is 8000CPS;
s4, adopting a 4-section type zoned temperature control type casting machine to carry out casting, wherein the casting belt speed is 0.5m/min, and drying to obtain an aluminum nitride raw porcelain substrate with the thickness of 0.20+/-0.01 mm; wherein the temperature of the first region of the drying bin of the casting machine is set to 80 ℃, the second region is set to 70 ℃, the third region is set to 45 ℃, and the fourth region is set to 100 ℃.
A Scanning Electron Microscope (SEM) image of the aluminum nitride green porcelain substrate prepared in this example is shown in FIG. 1. As can be seen from the figure, the aluminum nitride green porcelain substrate prepared in the embodiment has better component uniformity.
The photo of the surface state of the aluminum nitride green ceramic substrate prepared in this example is shown in fig. 2, and it can be seen from the figure that the surface of the substrate prepared in this example is fine and smooth and has no microcrack.
The green ceramic substrate prepared in this example was tested for surface roughness according to GB/T131-2006 standard, with a roughness of 0.37. Mu.m.
The green ceramic substrate prepared in the embodiment has a tensile strength of 2.5MPa according to GB/T12683-2009 standard test.
Example 2
A preparation method of a stretch-proof aluminum nitride green ceramic substrate comprises the following steps:
s1, weighing 10 parts of polyvinyl butyral and 0.5 part of butyl benzyl phthalate, adding the polyvinyl butyral and the butyl benzyl phthalate into a mixed solvent (volume ratio of 2:1) of 25 parts of absolute ethyl alcohol and butanone, and stirring at 40 ℃ for 48 hours to obtain a mixed solution;
s2, weighing 2 parts of linoleic acid, 80 parts of the mixed solvent of the absolute ethyl alcohol and butanone and 1 part of yttrium oxide, adding into a ball mill, ball milling for 4 hours at 20rpm to uniformly disperse, adding 100 parts of aluminum nitride powder, and ball milling for 48 hours at 20rpm to uniformly disperse to obtain pre-ground powder;
s3, adding the mixed solution into a pre-grinding powder, continuously ball-milling for 48 hours, and then vacuum defoaming under the condition of-0.095 MPa until the viscosity of the slurry is 20000CPS;
s4, adopting a 4-section type zoned temperature control type casting machine to carry out casting, wherein the casting belt speed is 0.8m/min, and drying to obtain an aluminum nitride raw porcelain substrate with the thickness of 0.20+/-0.01 mm; wherein the temperature of the first region of the drying bin of the casting machine is set to 70 ℃, the second region is set to 50 ℃, the third region is set to 40 ℃, and the fourth region is set to 90 ℃.
The green ceramic substrate prepared in this example was tested for surface roughness according to GB/T131-2006 standard, with a roughness of 0.39. Mu.m.
The green ceramic substrate prepared in the embodiment has a tensile strength of 2.2MPa according to GB/T12683-2009 standard test.
Example 3
A preparation method of a stretch-proof aluminum nitride green ceramic substrate comprises the following steps:
s1, weighing 2 parts of polyvinyl butyral and 5 parts of dibutyl phthalate, adding the polyvinyl butyral and the dibutyl phthalate into a mixed solvent (volume ratio of 1:1) of 20 parts of absolute ethyl alcohol and methyl isobutyl ketone, and stirring at 60 ℃ for 24 hours to obtain a mixed solution;
s2, weighing 0.5 part of herring fish oil, 50 parts of the mixed solvent of the absolute ethyl alcohol and the methyl isobutyl ketone and 8 parts of samarium oxide, adding into a ball mill, ball milling for 2 hours at 40rpm to uniformly disperse, adding 90 parts of aluminum nitride powder, and ball milling for 48 hours at 40rpm to uniformly disperse to obtain pre-ground powder;
s3, adding the mixed solution into a pre-grinding powder, continuously ball-milling for 48 hours, and then vacuum defoaming under the condition of-0.05 MPa until the viscosity of the slurry is 2000CPS;
s4, adopting a 4-section type zoned temperature control type casting machine to carry out casting, wherein the casting belt speed is 0.3m/min, and drying to obtain an aluminum nitride raw porcelain substrate with the thickness of 0.20+/-0.01 mm; wherein the temperature of the first region of the drying bin of the casting machine is set to 90 ℃, the second region is set to 60 ℃, the third region is set to 50 ℃, and the fourth region is set to 110 ℃.
The green ceramic substrate prepared in this example was tested for surface roughness according to GB/T131-2006 standard, with a roughness of 0.40. Mu.m.
The green ceramic substrate prepared in the embodiment has a tensile strength of 2.1MPa according to GB/T12683-2009 standard test.
Comparative example 1
The preparation method of the aluminum nitride green porcelain substrate of this comparative example is the same as that of example 1, except that the binder and the plasticizer are not subjected to the pre-dissolution step, and the specific steps are as follows:
s1, weighing 5 parts of polyvinyl butyral, 2 parts of dibutyl phthalate, 1 part of oleic acid, 5 parts of europium oxide and 87 parts of a mixed solvent of absolute ethyl alcohol and toluene (volume ratio is 1:2), adding into a ball mill, ball milling for 3 hours at 30rpm to uniformly disperse, adding 95 parts of aluminum nitride powder, and ball milling for 72 hours at 30rpm to uniformly disperse to obtain slurry;
s2, vacuum defoaming under the condition of-0.07 MPa until the viscosity of the slurry is 8000CPS;
s3, adopting a 4-section type zoned temperature control type casting machine to carry out casting, wherein the casting belt speed is 0.5m/min, and drying to obtain an aluminum nitride raw porcelain substrate with the thickness of 0.20+/-0.01; wherein the temperature of the first region of the drying bin of the casting machine is set to 80 ℃, the second region is set to 70 ℃, the third region is set to 45 ℃, and the fourth region is set to 100 ℃.
A Scanning Electron Microscope (SEM) image of the aluminum nitride green porcelain substrate prepared in this comparative example is shown in FIG. 3. As can be seen from the figure, the aluminum nitride green porcelain substrate prepared in this comparative example was inferior in uniformity of composition.
The photograph of the surface state of the aluminum nitride green porcelain substrate prepared in this example is shown in fig. 4, and it can be seen from the figure that the substrate prepared in this example has a rough surface and microcracks.
Comparative example 2
The preparation method of the aluminum nitride green porcelain substrate of the comparative example is the same as that of the example 1, and the difference is that the temperature arrangement mode of the drying bin of the casting machine in the step S4 is different, and the specific steps are as follows:
s1, weighing 5 parts of polyvinyl butyral and 2 parts of dibutyl phthalate, adding the polyvinyl butyral and the dibutyl phthalate into a mixed solvent (volume ratio of 1:2) of 22 parts of absolute ethyl alcohol and toluene, and stirring at 50 ℃ for 35 hours to obtain a mixed solution;
s2, weighing 1 part of oleic acid, 65 parts of the mixed solvent of the absolute ethyl alcohol and the toluene and 5 parts of europium oxide, adding into a ball mill, ball milling for 3 hours at 30rpm to uniformly disperse, adding 95 parts of aluminum nitride powder, and ball milling for 36 hours at 30rpm to uniformly disperse to obtain pre-ground powder;
s3, adding the mixed solution into a pre-grinding powder, continuously ball-milling for 36 hours, and then vacuum defoaming under the condition of-0.07 MPa until the viscosity of the slurry is 8000CPS;
s4, adopting a 4-section type zoned temperature control type casting machine to carry out casting, wherein the casting belt speed is 0.5m/min, and drying to obtain an aluminum nitride raw porcelain substrate with the thickness of 0.20+/-0.01 mm; wherein the temperature of the first region of the drying bin of the casting machine is set to be 50 ℃, the second region is set to be 70 ℃, the third region is set to be 80 ℃, and the fourth region is set to be 100 ℃.
The tensile strength of the aluminum nitride raw porcelain substrates prepared in the example 1 and the comparative example 2 is compared according to the method of GB 13022-1991 Plastic film tensile Property test, and the result is shown in FIG. 5, and it can be seen from the graph that the tensile strength of the aluminum nitride raw porcelain substrate prepared in the example of the invention is obviously better than that of the comparative example 2.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, or alternatives falling within the spirit and principles of the invention.
Claims (9)
1. A preparation method of a stretch-proof aluminum nitride green ceramic substrate is characterized by comprising the following steps:
step a, uniformly mixing a binder, a plasticizer and an organic solvent to obtain a mixed solution;
step b, adding a dispersing agent, an organic solvent and a sintering aid into a ball mill to perform first pre-ball milling, and then adding aluminum nitride powder to perform second pre-ball milling to obtain pre-milled powder;
step c, adding the mixed solution into a pre-grinding powder for ball milling, and then performing vacuum defoaming under the negative pressure condition until the viscosity of the slurry is 2000 CPS-20000 CPS, so as to obtain a casting slurry;
the vacuum degree of the negative pressure condition is 0.05 MPa-0.095 MPa;
step d, adopting a 4-section zoned temperature control type casting machine to cast and mold the casting slurry, and drying to obtain an aluminum nitride raw porcelain substrate; wherein the temperature of a first drying bin area of the zoned temperature control casting machine is 70-90 ℃, the temperature of a second drying bin area is 50-70 ℃, the temperature of a third drying bin area is 40-50 ℃, and the temperature of a fourth drying bin area is 90-110 ℃;
in the step a and the step b, the organic solvent is a binary solvent consisting of any two of absolute ethyl alcohol, butanone, methyl isobutyl ketone or toluene.
2. The method for producing a stretch-proof aluminum nitride green porcelain substrate according to claim 1, wherein in the step a, the amounts of the respective components are as follows: 2 to 10 parts of binder, 0.5 to 5.0 parts of plasticizer and 20 to 25 parts of organic solvent.
3. The method of producing a stretch-proof aluminum nitride green porcelain substrate according to claim 1 or 2, wherein in the step a, the binder is polyvinyl butyral; and/or
In the step a, the plasticizer is dibutyl phthalate, butyl benzyl phthalate, dibutyl phthalate, carbonic acid acrylic ester or polyethylene glycol.
4. The method of producing a stretch-proof aluminum nitride green ceramic substrate according to claim 3, wherein in the step a and the step b, the organic solvent is a binary solvent composed of absolute ethyl alcohol and methyl isobutyl ketone, absolute ethyl alcohol and butanone, absolute ethyl alcohol and toluene, butanone and toluene, or methyl isobutyl ketone and toluene.
5. The method of producing a stretch-proof aluminum nitride green porcelain substrate according to claim 1, wherein in the step b, the amounts of the respective components are as follows: 0.5 to 2.0 parts of dispersing agent, 50 to 80 parts of organic solvent, 1 to 8 parts of sintering aid and 90 to 100 parts of aluminum nitride powder.
6. The method of producing a stretch-proof aluminum nitride green ceramic substrate according to claim 1 or 5, wherein in the step b, the dispersant is oleic acid, linoleic acid, stearic acid, polyacrylate dispersant or herring fish oil; and/or
In the step b, the sintering aid is at least one of samarium oxide, yttrium oxide, dysprosium oxide or europium oxide.
7. The method for producing a stretch-proof aluminum nitride green ceramic substrate according to claim 1, wherein in the step b, the rotation speed of the first preliminary ball milling is 20rpm to 40rpm, and the ball milling time is 2h to 4h; and/or
In the step b, the rotating speed of the second pre-ball milling is 20 rpm-40 rpm, and the ball milling time is 24-48 h.
8. The method for producing a stretch-proof aluminum nitride green ceramic substrate according to claim 1, wherein in the step c, the rotation speed of the ball mill is 20rpm to 40rpm, and the ball milling time is 24 hours to 48 hours.
9. The method for producing a stretch-proof aluminum nitride green ceramic substrate according to claim 1, wherein in the step d, the casting belt speed is 0.3m/min to 0.8m/min.
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