CN100532490C - Encapsulating material and method for making same - Google Patents
Encapsulating material and method for making same Download PDFInfo
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- CN100532490C CN100532490C CNB2005100891717A CN200510089171A CN100532490C CN 100532490 C CN100532490 C CN 100532490C CN B2005100891717 A CNB2005100891717 A CN B2005100891717A CN 200510089171 A CN200510089171 A CN 200510089171A CN 100532490 C CN100532490 C CN 100532490C
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Abstract
The invention discloses a packing material, which comprises the following parts: 100wt% epoxy resin, 30-150% filler, 1-30wt% solidifier and 0.01-20wt% coupler, wherein the coupler is silane coupler.
Description
Technical field
The present invention relates to packaged material and preparation method thereof, relate more specifically to electronic package material and preparation method thereof.
Background technology
Encapsulation is that each element of electronic product of adopting specific packaged material that layout is connected is solidificated in wherein and the isolated sfgd. of environment.Play preventing the intrusion of moisture, dust and obnoxious flavour, slow down vibrations, prevent the effect of external force damage and stable element parameter electronic component.Therefore, packaged material also will have good high temperature resistant low temperature (40-120 ℃) performance and shock resistance except should having good insulation performance, chemical-resistant and agent of low hygroscopicity.
Existing packaged material mainly contains Resins, epoxy, filler and solidifying agent.Because the material of electronic product has diversity, and exist difference between the thermal expansivity of Resins, epoxy, therefore when the package of packaged material and electronic product composition ties up to temperature shock, the interelement of packaged material and electronic product can produce thermal stresses, the encapsulation system cracks and ftractures, and causes embedding the damage of element.Though add filler can reduce to a certain extent packaged material cure shrinkage, prevent to ftracture, the heat release when reducing to solidify, but filler dispersed relatively poor in Resins, epoxy, the initial viscosity of packaged material is increased, reduce manufacturability, and preventing that the rimose effect is bad, the packaged material that makes still ftractures easily.
Summary of the invention
The objective of the invention is to overcome existing packaged material initial viscosity shortcoming big, easy to crack, provide a kind of initial viscosity little, be difficult for rimose packaged material and preparation method thereof.
Packaged material provided by the invention contains Resins, epoxy, filler and solidifying agent, wherein, this packaged material also contains coupling agent, described coupling agent is a silane coupling agent, described Resins, epoxy with 100 weight parts is benchmark, the content of described filler is the 30-150 weight part, and the content of described solidifying agent is the 1-30 weight part, and the content of described coupling agent is the 0.01-20 weight part.
The preparation method of packaged material provided by the invention comprises coupling agent is added in the solvent, adds filler again, and solvent is removed in the back that is uniformly dispersed, and then the product that obtains and Resins, epoxy and solidifying agent is mixed.
Packaged material provided by the invention has improved the wetting property of filler grain in Resins, epoxy by with coupling agent filling surface being carried out coupling processing, makes filler obtain good dispersion, thereby has reduced the initial viscosity of packaged material and prevented cracking effectively.
Embodiment
Packaged material provided by the invention contains Resins, epoxy, filler and solidifying agent, wherein, this packaged material also contains coupling agent, described coupling agent is a silane coupling agent, described Resins, epoxy with 100 weight parts is benchmark, the content of described filler is the 30-150 weight part, and the content of described solidifying agent is the 1-30 weight part, and the content of described coupling agent is the 0.01-20 weight part.
Described coupling agent is a silane coupling agent, described silane coupling agent is selected from γ-An Bingjisanyiyangjiguiwan, vinyltriethoxysilane, vinyltrimethoxy silane, γ-chloropropyl triethoxysilane, two-(the silica-based propyl group of γ-triethoxy) tetrasulfide, anilinomethyl triethoxysilane, N-β (aminoethyl)-γ-An Bingjisanjiayangjiguiwan, N-(β-aminoethyl)-γ-An Bingjisanyiyangjiguiwan, N-β (aminoethyl)-γ-aminopropyl methyl dimethoxysilane, γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane, γ-(methacryloxypropyl) oxypropyl trimethyl silane, γ-Qiu Jibingjisanjiayangjiguiwan, in γ-sulfydryl propyl-triethoxysilicane one or more; Be preferably γ-(methacryloxypropyl) oxypropyl trimethyl silane, γ-An Bingjisanyiyangjiguiwan; The content of described coupling agent is preferably the 0.1-15 weight part.
The kind of described Resins, epoxy is conventionally known to one of skill in the art, Resins, epoxy is preferably one or more in bisphenol A epoxide resin, the many Resins, epoxy of phenolic aldehyde, glycidyl ester type epoxy resin, the aliphatic epoxy resin, more preferably bisphenol A epoxide resin; The epoxy equivalent (weight) of bisphenol A epoxide resin is 100-900, is preferably 150-500, and described epoxy equivalent (weight) is meant the Resins, epoxy gram number that contains 1 equivalent epoxy group(ing), and unit is [a gram/equivalent].The number-average molecular weight of bisphenol A epoxide resin is 300-7000, is preferably 400-1500; The structural formula of bisphenol A epoxide resin is:
N=0-19 wherein
The kind of described filler is conventionally known to one of skill in the art, and filler is preferably one or more in silica flour, white carbon black, the whiting.In order to improve the dispersing property of filler, in packaged material of the present invention, the average particle diameter of filler (hereinafter to be referred as particle diameter) is the 0.1-200 micron, is preferably the 1-100 micron.The content of filler is preferably the 50-120 weight part.
The kind of described solidifying agent is conventionally known to one of skill in the art.For example, solidifying agent can use carboxylic-acid solidifying agent, amine curing agent, preferably uses amine curing agent.Described amine curing agent comprises aliphatic polyamine such as quadrol, diethylenetriamine, triethylene tetramine, tetraethylene pentamine, two propylene triamines, dimethylaminopropylamine, diethyl amino propylamine, trimethylhexamethylenediamine, dihexyl triamine, hexanediamine, trimethylammonium hexanediamine, diethylamine; Alicyclic ring polyamine such as diaminomethyl hexanaphthene, aminoethyl croak piperazine, hexahydropyridine, isophorone diamine, diamino-cyclohexane, diaminomethyl cyclohexyl-methane, diamino cyclohexyl-methane; Aromatic amine such as mphenylenediamine, m-xylene diamine, diaminodiphenyl-methane, diamino diphenyl sulfone, p-diaminodiphenyl, 4-chlorine O-Phenylene Diamine, benzene dimethylamine tripolymer, phenoxybenzamine base ether; Modification organic amine such as methylol diethyl triamine, methylol quadrol, hydroxyethylethylene diamine, dihydroxy ethyl quadrol, hydroxyethyl diethylenetriamine, dihydroxy ethyl diethylenetriamine, hydroxyethyl hexanediamine, a cyanoethyl quadrol, a cyanoethyl hexanediamine, Dicyanodiamide (dicyanodiamide), dicyanoethyl quadrol, a cyanoethyl diethylenetriamine, two cyanoethyl diethylenetriamine, cyanoethylation dimethylphenylene diamine, diaminodiphenyl-methane; Boracic latent curing agent such as boron trifluoride mono aminoethane, boron trifluoride aniline, boron trifluoride o-toluidine, boron trifluoride benzylamine, boron trifluoride xylidine, boron trifluoride ethylaniline, boron trifluoride pyridine; Imidazole curing agent such as imidazoles, glyoxal ethyline, 2-ethyl imidazol(e), 2,4-methylimidazole, 2-ethyl 4-methylimidazole.The content of described solidifying agent is preferably the 5-20 weight part.
Packaged material provided by the invention can also contain promotor, the kind of promotor and content are conventionally known to one of skill in the art, for example described promotor can be selected from 2,4, in 6-(N, N-dimethylaminomethyl) phenol, boron trifluoride mono aminoethane, 2-ethyl-4-methylimidazole, triethylamine, the pyridine one or more.The content of promotor is the 0-15 weight part, is preferably the 1-10 weight part.
Packaged material provided by the invention can also contain toughner, and described toughner is selected from one or more in dibutyl phthalate, dioctyl phthalate (DOP), the tributyl phosphate.The content of toughner is the 0-30 weight part, is preferably the 2-20 weight part.Toughner can further effectively prevent to solidify cracking and shrinkage phenomenon.
The preparation method of packaged material provided by the invention comprises coupling agent is added in the solvent, adds filler again, and solvent is removed in the back that is uniformly dispersed, and then the product that obtains and Resins, epoxy and solidifying agent is mixed.According to the preparation method of packaged material provided by the invention, described jitter time is 10-100 minute.Described solvent can use any can dissolve coupling agent but not with reaction of filler or coupling agent and the solvent removed easily, as alcohols and ketones solvent.Be preferably acetone, methyl alcohol, butanone, ethanol or their mixture.As long as the consumption of solvent makes coupling agent and fillers dispersed evenly, for example the weight of solvent be coupling agent 10-100 doubly.Can adopt any means of the prior art to remove solvent,, preferably adopt vacuum drying as vacuum drying, seasoning, forced air drying etc.The method of vacuum drying has been conventionally known to one of skill in the art, and for example vacuum tightness is in the scope of 0.05 to 0.08 MPa.Vacuum tightness herein is defined as the absolute value of the difference of absolute pressure and barometric point.In this process, coupling agent has carried out coupling processing to filling surface, is the wetting property of silica flour in Resins, epoxy thereby improved filler, makes filler obtain good distribution.
Resins, epoxy, solidifying agent and do not have specific restriction by the order by merging of the filler of coupling agent treatment under the preferable case, join in the Resins, epoxy with solidifying agent with by the filler of coupling agent treatment.Can adopt existing the whole bag of tricks that above-mentioned each component is mixed, for example use agitator.
The preparation method of packaged material provided by the invention also comprises adding promotor and mixes.The joining day of described promotor does not have specific restriction, under the preferable case, promotor is joined in the Resins, epoxy with solidifying agent with by the filler of coupling agent treatment.
The preparation method of packaged material provided by the invention also comprises adding toughner and mixes that described toughner is selected from one or more in dibutyl phthalate, dioctyl phthalate (DOP), the tributyl phosphate.The joining day of described toughner does not have specific restriction, under the preferable case, toughner is joined in the Resins, epoxy with solidifying agent with by the filler of coupling agent treatment.
Under the preferable case, the preparation method of packaged material provided by the invention can also comprise the deaeration step after said components is mixed.The present invention can use defoaming method known in those skilled in the art to defoaming method without limits, for example adds defoamer, evacuation and centrifugal degassing, vacuum defoamation.The kind of described defoamer and consumption have been conventionally known to one of skill in the art, and for example described defoamer is selected from and contains organo-siloxane type defoamer.With 100 parts by weight of epoxy resin is benchmark, and the consumption of described defoamer is the 0.01-10 weight part, is preferably the 0.1-5 weight part.Deaerating agent can add and mixes with said components, also can add separately after said components mixes again.The method of vacuum defoamation has been conventionally known to one of skill in the art, and for example vacuum tightness is in the scope of 0.05 to 0.08 MPa.Vacuum tightness herein is defined as the absolute value of the difference of absolute pressure and barometric point.
Below by embodiment the present invention is described in more detail.
Embodiment 1
This embodiment is used to illustrate packaged material of the present invention and preparation method thereof.
12 weight part γ-(methacryloxypropyl) propyl trimethoxy silicane is dissolved in the acetone of 300 weight parts, toward wherein adding 100 weight part median sizes is 15 microns silica flour, disperseed 80 minutes, and left standstill final vacuum oven dry (vacuum tightness is 0.06 MPa) in 30 hours.
Silica flour, 16 weight part dicyanodiamide, 15 weight part dibutyl phthalates, 8 weight parts 2 with the above-mentioned processing of process of 108 weight parts, 4,6-(N, the N-dimethylaminomethyl) phenol joins 100 parts of bisphenol A epoxide resin (epoxy equivalent (weight)s 184, number-average molecular weight is 500), mix, vacuum defoamation (vacuum tightness is 0.06 MPa) obtains packaged material A1.
Embodiment 2
This embodiment is used to illustrate packaged material of the present invention and preparation method thereof.
2 weight part γ-An Bingjisanyiyangjiguiwans are dissolved in the acetone of 200 weight parts, are 75 microns silica flour toward wherein adding 60 weight part median sizes, disperse 40 minutes, leave standstill 18 hours final vacuums and dry (vacuum tightness is 0.05 MPa).
Silica flour, 8 weight part dicyanodiamide, the 5 weight part tributyl phosphates of the above-mentioned processing of process of 62 weight parts are joined 100 parts of bisphenol A epoxide resin (epoxy equivalent (weight)s 240, number-average molecular weight is 750), mix, vacuum defoamation (vacuum tightness is 0.05 MPa) obtains packaged material A2.
Embodiment 3
This embodiment is used to illustrate packaged material of the present invention and preparation method thereof.
5 weight part γ-(methacryloxypropyl) propyl trimethoxy silicane is dissolved in the acetone of 200 weight parts, toward wherein adding 80 weight part median sizes is 15 microns silica flour, disperseed 100 minutes, and left standstill final vacuum oven dry (vacuum tightness is 0.07 MPa) in 24 hours.
Silica flour, 12 weight part boron trifluoride ethylaniline, 2 weight parts 2 with the above-mentioned processing of process of 85 weight parts, 4,6-(N, the N-dimethylaminomethyl) phenol joins 100 parts of bisphenol A epoxide resin (epoxy equivalent (weight)s 450, number-average molecular weight is 1300), mix, vacuum defoamation (vacuum tightness is 0.07 MPa) obtains packaged material A3.
Embodiment 4
This embodiment is used to illustrate packaged material of the present invention and preparation method thereof.
1 weight part γ-(methacryloxypropyl) propyl trimethoxy silicane is dissolved in the acetone of 200 weight parts, is 15 microns silica flour toward wherein adding 50 weight part median sizes, disperses 80 minutes, leaves standstill 30 hours final vacuums and dries (vacuum tightness 0.08 MPa).
Silica flour, 10 weight part boron trifluoride ethylaniline, 15 weight part dioctyl phthalate (DOP)s, 5 weight parts 2 with the above-mentioned processing of process of 51 weight parts, 4,6-(N, the N-dimethylaminomethyl) phenol joins 100 parts of bisphenol A epoxide resin (epoxy equivalent (weight)s 184, number-average molecular weight is 500), mix, vacuum defoamation (vacuum tightness 0.08 MPa) obtains packaged material A4.
Comparative Examples 1
This Comparative Examples is used to illustrate reference packaged material and preparation method thereof.
With the median size of 100 weight parts is 15 microns silica flours, 16 weight part dicyanodiamide, 2 weight parts 2,4,6-(N, the N-dimethylaminomethyl) phenol joins 100 parts of bisphenol A epoxide resin (epoxy equivalent (weight)s 184, number-average molecular weight is 500), mix, vacuum defoamation (vacuum tightness is 0.06 MPa) obtains packaged material C1.
Comparative Examples 2
This Comparative Examples is used to illustrate reference packaged material and preparation method thereof.
With 80 weight part median sizes is 75 microns silica flours, 12 weight part boron trifluoride ethylaniline, 2 weight parts 2,4,6-(N, the N-dimethylaminomethyl) phenol joins 100 parts of bisphenol A epoxide resin (epoxy equivalent (weight)s 450, number-average molecular weight is 1300), mix, vacuum defoamation (vacuum tightness is 0.07 MPa) obtains packaged material C2.
Embodiment 5-8
The performance of the packaged material A1-4 that embodiment 5-8 is used for illustrating that respectively embodiment 1-4 obtains.
Measure the viscosity of packaged material A1-4 according to GB/T2794-1995.
Respectively the packaged material A1-4 that obtains among the embodiment 1-4 is kept being warming up to 120 ℃ again in 30 minutes at 80 ℃ and kept 2 hours, obtain cured article.Whether the visual inspection cured article has cracking phenomena.And measure the linear expansivity of cured article according to GB1036-89.
The every performance that records is as shown in table 1.
Comparative Examples 3-4
The performance of the packaged material C1-2 that Comparative Examples 3-4 is used for illustrating that respectively Comparative Examples 1-2 obtains.
According to method and process as embodiment 5-8 every performance of packaged material C1-2 is measured, measurement result is as shown in table 1.
Table 1
| The embodiment numbering | Viscosity (centipoise) | Linear expansivity (α 20-100℃) | The cured article cracking phenomena |
| Embodiment 5 | 4200 | 5.8×10 -5 | Do not have |
| Embodiment 6 | 4350 | 6.1×10 -5 | Do not have |
| Embodiment 7 | 4100 | 5.5×10 -5 | Do not have |
| Embodiment 8 | 3900 | 7.6×10 -5 | Do not have |
| Comparative Examples 3 | 8700 | 4.3×10 -3 | Surface irregularity is arranged |
| Comparative Examples 4 | 10800 | 1.6×10 -2 | Obvious cracking is arranged |
From the measurement result shown in the table 1 as can be seen, compare with the reference packaged material, the viscosity of packaged material provided by the invention reduces, and the cured article of formation does not have cracking phenomena.
Claims (15)
1, a kind of packaged material, this packaged material contains Resins, epoxy, filler and solidifying agent, it is characterized in that, this packaged material also contains coupling agent, and described coupling agent is a silane coupling agent, is benchmark with the described Resins, epoxy of 100 weight parts, the content of described filler is the 30-150 weight part, the content of described solidifying agent is the 1-30 weight part, and the content of described coupling agent is the 0.01-20 weight part
The preparation method of this packaged material comprises: coupling agent is added in the solvent, adds filler again, solvent is removed in the back that is uniformly dispersed, and then the product that obtains and Resins, epoxy and solidifying agent is mixed.
2, packaged material according to claim 1 wherein, is a benchmark with the described Resins, epoxy of 100 weight parts, and the content of described filler is the 50-120 weight part, and the content of described solidifying agent is the 5-20 weight part, and the content of described coupling agent is the 0.1-15 weight part.
3, packaged material according to claim 1 and 2, wherein, described silane coupling agent is selected from γ-An Bingjisanyiyangjiguiwan, vinyltriethoxysilane, vinyltrimethoxy silane, γ-chloropropyl triethoxysilane, two-(the silica-based propyl group of γ-triethoxy) tetrasulfide, anilinomethyl triethoxysilane, N-β (aminoethyl)-γ-An Bingjisanjiayangjiguiwan, N-(β-aminoethyl)-γ-An Bingjisanyiyangjiguiwan, N-β (aminoethyl)-γ-aminopropyl methyl dimethoxysilane, γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane, γ-(methacryloxypropyl) oxypropyl trimethyl silane, γ-Qiu Jibingjisanjiayangjiguiwan, in γ-sulfydryl propyl-triethoxysilicane one or more.
4, packaged material according to claim 1 and 2, wherein, described Resins, epoxy is bisphenol A epoxide resin; The epoxy equivalent (weight) of bisphenol A epoxide resin is 100-900; The number-average molecular weight of bisphenol A epoxide resin is 300-7000.
5, packaged material according to claim 1 and 2, wherein, described filler is selected from one or more in silica flour, white carbon black, the whiting; The median size of described filler is the 0.1-200 micron.
6, packaged material according to claim 1 and 2, wherein, described solidifying agent is an amine curing agent, is selected from aliphatic polyamine, alicyclic ring polyamine, aromatic amine, imidazoles, modification organic amine, and one or more of boracic latent curing agent.
7, packaged material according to claim 1 and 2 wherein, is a benchmark with the described Resins, epoxy of 100 weight parts, and described packaged material also contains the promotor of 0-15 weight part.
8, packaged material according to claim 7, wherein, described promotor is selected from 2,4, one or more in 6-(N, N-dimethylaminomethyl) phenol, boron trifluoride mono aminoethane, 2-ethyl-4-methylimidazole, triethylamine, the pyridine.
9, packaged material according to claim 1 and 2, wherein, described Resins, epoxy with 100 weight parts is benchmark, described packaged material also contains the toughner of 0-30 weight part, and described toughner is selected from one or more in dibutyl phthalate, dioctyl phthalate (DOP), the tributyl phosphate.
10, packaged material according to claim 1, wherein, jitter time is 10-100 minute; Described solvent is acetone, butanone, methyl alcohol, ethanol or its mixture.
11, the preparation method of the described packaged material of claim 1 is characterized in that, this method comprises coupling agent is added in the solvent, adds filler again, and solvent is removed in the back that is uniformly dispersed, and then the product that obtains and Resins, epoxy and solidifying agent is mixed.
12, preparation method according to claim 11, wherein, jitter time is 10-100 minute; Described solvent is acetone, butanone, methyl alcohol, ethanol or its mixture.
13, preparation method according to claim 11, wherein, this method also comprises adding promotor and mixes.
14, preparation method according to claim 13, wherein, this method also comprises adding toughner and mixes that described toughner is selected from one or more in dibutyl phthalate, dioctyl phthalate (DOP), the tributyl phosphate.
15, preparation method according to claim 11, wherein, this method also comprises the deaeration step after mixing.
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| CNB2005100891717A CN100532490C (en) | 2005-08-05 | 2005-08-05 | Encapsulating material and method for making same |
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| CNB2005100891717A CN100532490C (en) | 2005-08-05 | 2005-08-05 | Encapsulating material and method for making same |
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| CN100532490C true CN100532490C (en) | 2009-08-26 |
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| MX2009013786A (en) * | 2007-06-15 | 2010-03-01 | Dow Global Technologies Inc | Process for preparing composites using epoxy resin compositions. |
| CN101503615B (en) * | 2008-12-17 | 2012-07-25 | 武汉钢铁(集团)公司 | Method for preparing single-component high temperature curing sealing material for ironmaking tuyere of blast furnace |
| CN101724368B (en) * | 2009-11-24 | 2013-03-27 | 烟台德邦科技有限公司 | Anti-impact epoxy structural rubber and preparation method thereof |
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| CN102220103A (en) * | 2011-04-21 | 2011-10-19 | 常州华天福杰光电科技有限公司 | Low viscosity heat-conducting adhesive for LED chips |
| CN103468194B (en) * | 2013-09-17 | 2015-05-13 | 广州聚合电子材料有限公司 | Patch inductor packaging single-component glue and preparation method thereof |
| CN103881310A (en) * | 2014-04-11 | 2014-06-25 | 上海神沃电子有限公司 | Halogen-free environment-friendly epoxy resin envelope material for thermistors and application thereof |
| CN106751187A (en) * | 2016-12-13 | 2017-05-31 | 安徽省金正塑业有限公司 | A kind of high leakproofness plastics |
| CN108440930A (en) * | 2018-03-14 | 2018-08-24 | 合肥尚强电气科技有限公司 | High-performance packaging material for storage battery and preparation method thereof |
| CN114479348A (en) * | 2020-11-11 | 2022-05-13 | 中国科学院上海硅酸盐研究所 | Preparation method of matching layer for relaxation ferroelectric single crystal ultrasonic transducer |
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