CN102503444B - Non-aqueous tape casting slurry and preparation method thereof - Google Patents
Non-aqueous tape casting slurry and preparation method thereof Download PDFInfo
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- CN102503444B CN102503444B CN 201110297045 CN201110297045A CN102503444B CN 102503444 B CN102503444 B CN 102503444B CN 201110297045 CN201110297045 CN 201110297045 CN 201110297045 A CN201110297045 A CN 201110297045A CN 102503444 B CN102503444 B CN 102503444B
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Abstract
The invention discloses non-aqueous tape casting slurry and a preparation method thereof, which relate to the field of manufacturing of semiconductor micro-electronics. The non-aqueous tape casting slurry is made of, by weight, 58-63% of ceramic powder, 10-12% of butanone, 7-8% of ethanol, 0.1-0.5% of glycerol trioleate, 15-20% of liquid binder and 1.5-2% of butyl benzyl phthalate. The preparation method includes steps: firstly, preparing the liquid binder; secondly, ball-milling the butanone, the ethanol, the glycerol trioleate and part of liquid binder for 10-60 minutes; thirdly, adding the ceramic powder into a ball-milling cylinder mentioned at the step two and ball-milling for 2-12 hours; and fourthly, adding the butyl benzyl phthalate and the rest binder into the ball-milling cylinder at the step three and ball-milling for uniform mixing. Tapes made of the slurry prepared by the method by means of tape casting have the advantages of high mechanical strength, high dimensional stability and excellent laminating performance.
Description
Technical field
The present invention relates to semiconductor microactuator electron device preparation field, especially a kind of preparation method of casting slurry.
Background technology
Along with the density of ceramic packing is more and more higher, the manufacturing procedure increasingly complex of ceramic package, raw material also needs through could the ripe porcelain of sintering after punching, filling perforation, printing, lamination, a series of green techniques such as fervent behind flow casting molding.If the physical strength of casting belt material is too low, then in the follow-up course of processing, the easy cracking that occurs falls slag, even the appearance of the situation of whole fracture, has had a strong impact on yield rate.
Casting slurry blending means commonly used is two-phase method: at first porcelain powder, dispersion agent, solvent ball milling for some time are mixed; Add afterwards powder binder and softening agent and continue ball milling to mixing.Do not add binding agent in the ball milling fs among Chinese patent 200610125178.4, the 200710053286.X and 201010153866.8, the raw material that this method is prepared, binding agent and porcelain powder interface are bad, binding agent is not tight to porcelain powder parcel, the effect of binding agent and softening agent is also bad simultaneously, the band material bad mechanical strength that causes curtain coating to go out, plasticity is poor.Casting slurry preparation method of the present invention can effectively address this problem, and can prepare high-quality casting belt material, satisfies the manufacturability requirement of Multi-layer ceramic package.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of non-aqueous tape-casting slurry and preparation method thereof, and the band material that slurry curtain coating of the present invention obtains has that physical strength is large, the well behaved advantage of lamination.
The technical solution used in the present invention is: a kind of non-aqueous tape-casting slurry, raw material are comprised of following material by mass percentage:
Porcelain powder: 58～63% butanone: 10～12% ethanol: 7～8% oleins: 0.1～0.5% liquid adhesive: 15～20% phthalic acid fourth Bian esters: 1.5～2%;
The liquid adhesive raw material is comprised of following material by mass percentage: polyvinyl butyral acetal: 19～25% butanone: 42～50% ethanol: 28～34%.
The purity of preferred butanone, ethanol, olein, phthalic acid fourth Bian ester and polyvinyl butyral acetal is greater than 99%.
A kind of preparation method of non-aqueous tape-casting slurry may further comprise the steps the preparation of (1) liquid adhesive: each material of liquid adhesive raw material is mixed in proportion make liquid adhesive;
(2) the ball milling fs: the butanone in liquid adhesive and the described non-aqueous tape-casting slurry raw material, ethanol and olein were added in the ball mill ball milling 10-60 minute, the quality of the liquid adhesive that the ball milling fs adds be in the described non-aqueous tape-casting slurry raw material total liquid adhesive quality 5～15%;
(3) ball milling subordinate phase: add the porcelain powder in the described non-aqueous tape-casting slurry raw material in the ball grinder of step (2), ball milling 2-12 hour;
(4) add phthalic acid fourth Bian ester and remaining liquid adhesive in the described non-aqueous tape-casting slurry raw material in the ball grinder of step (3), ball milling is to mixing.
Preferred liquid adhesive raw material adopts heating in water bath when mixing, and bath temperature is 25～70 ℃.
Identical raw material, the band material surface uniform that the casting slurry curtain coating that adopts method of the present invention to prepare obtains is fine and close, sees accompanying drawing 3; Cross section binding agent enwrapped granule is abundant, sees accompanying drawing 4; Use conventional methods the band material surface porosity porous that the slurry curtain coating of preparation obtains, see accompanying drawing 1; The cross section becomes stratiform, and particle parcel situation is poor, sees accompanying drawing 2.
The beneficial effect that adopts technique scheme to produce is:
Casting slurry by this hybrid mode preparation, binding agent is owing to be under dissolved state in the adding system, and the solvent system of selecting is good for the solubility property of binding agent, so that the abundant spread apart of binding agent macromolecular chain, thereby obtain good plasticization effect; Owing to added in advance the part binding agent in the ball milling fs, produced with powder granule and wrapped up preferably effect, increased intergranular steric effect, after adding remaining binding agent, form again a concentration gradient, impelled the good distribution of powder granule.Thereby can obtain the casting belt material of satisfactory mechanical property.
Description of drawings
The present invention is further detailed explanation below in conjunction with the drawings and specific embodiments.
Fig. 1 is the SEM photo that adopts the band material surface that the casting slurry curtain coating of traditional method for mixing raw materials preparation obtains;
Fig. 2 is the SEM photo that adopts the band material cross section that the casting slurry curtain coating of traditional method for mixing raw materials preparation obtains;
Fig. 3 is the SEM photo that adopts the band material surface that the casting slurry curtain coating of the inventive method preparation obtains;
Fig. 4 is the SEM photo that adopts the band material cross section that the casting slurry curtain coating of the inventive method preparation obtains;
Raw material and measuring condition are identical.
Embodiment
Embodiment 1:
A kind of non-aqueous tape-casting slurry, raw material are composed of the following components by mass percentage:
Porcelain powder: 63% butanone: 12% ethanol: 7% olein: 0.5%
Liquid adhesive: 16% phthalic acid fourth Bian ester: 1.5%.
Liquid adhesive is composed of the following components by mass percentage: polyvinyl butyral acetal: 21%
Butanone: 50% ethanol: 29%.
The purity of butanone, ethanol, olein, phthalic acid fourth Bian ester and polyvinyl butyral acetal is greater than 99%.
(1) preparation of liquid adhesive: each component of liquid adhesive raw material mixed in proportion make liquid adhesive.
(2) the ball milling fs: the butanone in liquid adhesive and the described non-aqueous tape-casting slurry raw material, ethanol and olein were added in the ball mill ball milling 10 minutes, the quality of liquid adhesive be in the described non-aqueous tape-casting slurry raw material liquid adhesive quality 15%;
(3) ball milling subordinate phase: add the porcelain powder in the described non-aqueous tape-casting slurry raw material in the ball grinder of step (2), ball milling 12 hours;
(4) add phthalic acid fourth Bian ester and remaining liquid adhesive in the ball grinder of step (3), ball milling is to mixing.
The band material that the slurry curtain coating of present embodiment production obtains uses conventional methods the band material tensile strength contrast that the slurry curtain coating of preparation obtains and sees Table 1 with identical raw material:
Table 1
| ? | The tradition invention | The inventive method |
| Elongation at break (%) | 7.75 | 3.19 |
| Tensile strength (MPa) | 1.44 | 2.91 |
| Yield strength (MPa) | 1.12 | 2.67 |
| Maximum load (N) | 1.138 | 2.304 |
Embodiment 2:
A kind of non-aqueous tape-casting slurry, raw material are composed of the following components by mass percentage:
Porcelain powder: 60% butanone: 10% ethanol: 8% olein: 0.5%
Liquid adhesive: 20% phthalic acid fourth Bian ester: 1.5%.
Liquid adhesive is composed of the following components by mass percentage: polyvinyl butyral acetal: 19%
Butanone: 49% ethanol: 32%.
The purity of butanone, ethanol, olein, phthalic acid fourth Bian ester and polyvinyl butyral acetal is greater than 99%.
(1) preparation of liquid adhesive: each component of liquid adhesive raw material mixed in proportion make liquid adhesive;
(2) the ball milling fs: the butanone in liquid adhesive and the described non-aqueous tape-casting slurry raw material, ethanol and olein were added in the ball mill ball milling 60 minutes, the quality of liquid adhesive be in the described non-aqueous tape-casting slurry raw material liquid adhesive quality 5%;
(3) ball milling subordinate phase: add the porcelain powder in the described non-aqueous tape-casting slurry raw material in the ball grinder of step (2), ball milling 2 hours;
(4) add phthalic acid fourth Bian ester and remaining liquid adhesive in the ball grinder of step (3), ball milling is to mixing.
Embodiment 3:
A kind of non-aqueous tape-casting slurry, raw material are composed of the following components by mass percentage:
Porcelain powder: 58% butanone: 11.5% ethanol: 8% olein: 0.5%
Liquid adhesive: 20% phthalic acid fourth Bian ester: 2%.
Liquid adhesive is composed of the following components by mass percentage: polyvinyl butyral acetal: 24%
Butanone: 42% ethanol: 34%.
The purity of butanone, ethanol, olein, phthalic acid fourth Bian ester and polyvinyl butyral acetal is greater than 99%.
(1) preparation of liquid adhesive: each component of liquid adhesive raw material mixed in proportion make liquid adhesive, adopt heating in water bath during mixing, bath temperature is 50 ℃;
(2) the ball milling fs: the butanone in liquid adhesive and the described non-aqueous tape-casting slurry raw material, ethanol and olein were added in the ball mill ball milling 30 minutes, the quality of liquid adhesive be in the described non-aqueous tape-casting slurry raw material liquid adhesive quality 10%;
(3) ball milling subordinate phase: add the porcelain powder in the described non-aqueous tape-casting slurry raw material in the ball grinder of step (2), ball milling 8 hours;
(4) add phthalic acid fourth Bian ester and remaining liquid adhesive in the ball grinder of step (3), ball milling is to mixing.
Embodiment 4:
A kind of non-aqueous tape-casting slurry, raw material are composed of the following components by mass percentage:
Porcelain powder: 61% butanone: 12% ethanol: 8% olein: 0.4%
Liquid adhesive: 16.6% phthalic acid fourth Bian ester: 2%.
Liquid adhesive is composed of the following components by mass percentage: polyvinyl butyral acetal: 22%
Butanone: 50% ethanol: 28%.
The purity of butanone, ethanol, olein, phthalic acid fourth Bian ester and polyvinyl butyral acetal is greater than 99%.
(1) preparation of liquid adhesive: each component of liquid adhesive raw material mixed in proportion make liquid adhesive, adopt heating in water bath during mixing, bath temperature is 25 ℃;
(2) the ball milling fs: the butanone in liquid adhesive and the described non-aqueous tape-casting slurry raw material, ethanol and olein were added in the ball mill ball milling 40 minutes, the quality of liquid adhesive be in the described non-aqueous tape-casting slurry raw material liquid adhesive quality 12%;
(3) ball milling subordinate phase: add the porcelain powder in the described non-aqueous tape-casting slurry raw material in the ball grinder of step (2), ball milling 10 hours;
(4) add phthalic acid fourth Bian ester and remaining liquid adhesive in the ball grinder of step (3), ball milling is to mixing.
Embodiment 5:
A kind of non-aqueous tape-casting slurry, raw material are composed of the following components by mass percentage:
Porcelain powder: 63% butanone: 12% ethanol: 7.9% olein: 0.1%
Liquid adhesive: 15% phthalic acid fourth Bian ester: 2%.
Liquid adhesive is composed of the following components by mass percentage: polyvinyl butyral acetal: 25%
Butanone: 45% ethanol: 30%.
The purity of butanone, ethanol, olein, phthalic acid fourth Bian ester and polyvinyl butyral acetal is greater than 99%.
(1) preparation of liquid adhesive: each component of liquid adhesive raw material mixed in proportion make liquid adhesive, adopt heating in water bath during mixing, bath temperature is 70 ℃;
(2) the ball milling fs: the butanone in liquid adhesive and the described non-aqueous tape-casting slurry raw material, ethanol and olein were added in the ball mill ball milling 50 minutes, the quality of liquid adhesive be in the described non-aqueous tape-casting slurry raw material liquid adhesive quality 10%;
(3) ball milling subordinate phase: add the porcelain powder in the described non-aqueous tape-casting slurry raw material in the ball grinder of step (2), ball milling 8 hours;
(4) add phthalic acid fourth Bian ester and remaining liquid adhesive in the ball grinder of step (3), ball milling is to mixing.
Claims (1)
1. the preparation method of a non-aqueous tape-casting slurry is characterized in that may further comprise the steps the preparation of (1) liquid adhesive: each material of liquid adhesive raw material is mixed in proportion make liquid adhesive;
(2) the ball milling fs: the butanone in liquid adhesive and the described non-aqueous tape-casting slurry raw material, ethanol and olein were added in the ball mill ball milling 10-60 minute, the quality of the liquid adhesive that the ball milling fs adds be in the described non-aqueous tape-casting slurry raw material total liquid adhesive quality 5～15%;
(3) ball milling subordinate phase: add the porcelain powder in the described non-aqueous tape-casting slurry raw material in the ball grinder of step (2), ball milling 2-12 hour;
(4) add phthalic acid fourth Bian ester and remaining liquid adhesive in the described non-aqueous tape-casting slurry raw material in the ball grinder of step (3), ball milling is to mixing;
Described non-aqueous tape-casting slurry, raw material are comprised of following material by mass percentage:
Porcelain powder: 58～63% butanone: 10～12% ethanol: 7～8% oleins: 0.1～0.5% liquid adhesive: 15～20% phthalic acid fourth Bian esters: 1.5～2%;
Described liquid adhesive raw material is comprised of following material by mass percentage: polyvinyl butyral acetal: 19～25% butanone: 42～50% ethanol: 28～34%;
The purity of butanone, ethanol, olein, phthalic acid fourth Bian ester and polyvinyl butyral acetal is greater than 99%.
2A kind of preparation method of non-aqueous tape-casting slurry is characterized in that adopting heating in water bath when the liquid adhesive raw material mixes as claimed in claim 1, and bath temperature is 25～70 ℃.
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| CN114920567B (en) * | 2022-04-21 | 2023-05-26 | 苏州瑞瓷新材料科技有限公司 | Preparation method of alumina slurry and prepared alumina slurry |
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| CN100398491C (en) * | 2006-11-28 | 2008-07-02 | 武汉理工大学 | Silicon nitride non-aqueous tape-casting slurry and its preparation method |
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