CN104531029A - Chip four-corner binding glue and preparation method thereof - Google Patents
Chip four-corner binding glue and preparation method thereof Download PDFInfo
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- CN104531029A CN104531029A CN201410795290.3A CN201410795290A CN104531029A CN 104531029 A CN104531029 A CN 104531029A CN 201410795290 A CN201410795290 A CN 201410795290A CN 104531029 A CN104531029 A CN 104531029A
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Abstract
The invention belongs to the technical field of chip protective glue and particularly relates to chip four-corner binding glue and a preparation method thereof. The chip four-corner binding glue is prepared from the following components in parts by weight: 20-25 parts of bisphenol A epoxy resin, 35-40 parts of bisphenol F epoxy resin, 0.5-1.0 part of pigment, 4-10 parts of white carbon black, 60-100 parts of spherical filler, 30-50 parts of sulfydryl ester, 1-2 parts of a stabilizer, 4-10 parts of a curing agent and 1-3 parts of a coupling agent. The four-corner binding glue prepared by the preparation method disclosed by the invention is not high in viscosity, good in thixotropy and relatively high in cross-linking density, so that the weather resistance is extremely good, the curing temperature is low, the bonding strength is high, the shrinking percentage is low, the storage is relatively stable and lasting, the preparation process is simple and environmentally friendly, the cost is low and the applied range is wide. Moreover, a product obtained by the preparation method disclosed by the invention is in liquid state, and beneficial to site construction and avoiding generating gas bubbles.
Description
Technical field
The invention belongs to chip protection glue technical field, particularly relate to a kind of chip corner binding glue and preparation method thereof.
Background technology
China has become world's digital product and has produced the first big country; wherein to account for world wide production more than half for mobile digital amount of product throughput; root according to data; the development trend of modern number code product is " thin, light, little "; the requirement of this development to chip also trends towards " thin, light, little ", and this trend requires also greatly to improve to the protection of chip.
Because mobile digital product in use there will be pressure, curved, distortion, the phenomenon such as to fall, and this STRESS VARIATION can be applied on chip naturally, can creep be there is in chip when STRESS VARIATION, long-term applying can cause chip tin ball rupture and occur that chip functions is lost, and causes the damage of whole digital product.In addition, the change of temperature can cause expansion or the contraction of digital product equally, and dilation also can bring destructive destruction to chip.Therefore the protection reducing chip damage is just arisen at the historic moment.
Market there are following two kinds of modes substantially to the protection of chip: 1, chip underfill glue, is commonly referred to as underfill, and this mode is applicable to small chip, play and reduce stress and the function of protect IC; 2, corner binding glue, this mode, mainly for larger chip, at chip surrounding gluing, reduces the stress of chip and brings the protection to chip after solidification.Current notebook computer, e-book and the mode having the protection of the chip of the digital product of larger touch-screen that corner mostly can be used to bind.
At present, traditional on market corner binding glue is: 1, epoxy resin hot setting, but due to the system solidification value of curable epoxide higher, temperature too high after digital product assembles can affect other element function; 2, UV ultra-violet curing; because the curing speed of UV ultra-violet curing glue is fast; curing room can not produce high temperature; this technique should be the best mode of protect IC; but due to the inhibition of oxygen in air; make UV ultraviolet glue solidify rear surface be clamminess, and UV-irradiation less than place also there will be the phenomenon of not solidifying.
Therefore, the corner binding glue material of research and development a kind of solidification low temperature (being no more than 80 DEG C), solidification quick (being less than 10min) will become a kind of inevitable development trend.
Summary of the invention
The present invention is directed to the deficiency that above-mentioned prior art exists, provide that a kind of curing speed is fast, solidification value is low, the high and low cost of reliability, environmental protection, again stability in storage excellence chip corner binding glue and preparation method thereof.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of chip corner binding glue, its component is counted by weight: bisphenol A epoxide resin 20 ~ 25 parts, bisphenol F epoxy resin 35 ~ 40 parts, 0.5 ~ 1.0 part, colorant, white carbon black 4 ~ 10 parts, ball-shaped filling material 60 ~ 100 parts, thiol esters 30 ~ 50 parts, stablizer 1 ~ 2 part, 4 ~ 10 parts, solidifying agent and coupling agent 1 ~ 3 part.
Further, described bisphenol A epoxide resin is liquid bisphenol A epoxy resin 828EL, and described bisphenol F epoxy resin is bisphenol F epoxy resin 830S.
Adopt the beneficial effect of above-mentioned further scheme to be, liquid resin can give the higher cohesive strength of corner binding glue and toughness, and epoxy resin can improve the Tg point (glass transition temperature) after glue curing, improves heat resistance.
Further, described colorant is black cream.
Further, described ball-shaped filling material is silicon-dioxide.
The beneficial effect of above-mentioned further scheme is adopted to be can reduce the contraction problem after the binding adhesive curing of corner by a large amount of interpolations of ball-shaped filling material.
Further, described thiol esters is trimethylolpropane trimethacrylate TMPTMA.
Further, described stablizer is barbituric acid.
Further, described solidifying agent is modified imidazole and the derivative thereof of fineness 5 ~ 10 μm, is preferably modified amine latent curing agent, is more preferably the solidifying agent of trade mark PN-H (Japanese aginomoto).
The beneficial effect of above-mentioned further scheme is adopted to be, the solidifying agent of 5 ~ 10 μm of fineness scopes makes to there will not be stifled pin problem during invocation point glue, and modified amine latent curing agent can improve speed of response, reduce solidification value, simultaneously also helpful to the raising of Tg point (glass transition temperature).
Further, described coupling agent is the silane coupling agent of the trade mark KH550, KH560 or KH570.
Adopt the beneficial effect of above-mentioned further scheme to be of value to the dispersion of ball-shaped filling material, the filling of filler can be strengthened.
The preparation method of binding glue in chip corner described above is: bisphenol A epoxide resin and bisphenol F epoxy resin are toasted 12h at 70 ~ 75 DEG C, then by roasted 20 ~ 25 parts of bisphenol A epoxide resins, 35 ~ 40 parts of bisphenol F epoxy resins, 4 ~ 10 parts of white carbon blacks and 0.5 ~ 1.0 part of colorant are in 20-30 DEG C of mixing 20 ~ 40min, then 60 ~ 100 parts of ball-shaped filling materials are added, 30 ~ 50 parts of thiol esters, 1 ~ 2 part of stablizer, 4 ~ 10 parts of solidifying agent and 1 ~ 3 part of coupling agent, insert in three-roller and mix, repeat mixing three times, add after mixing in reactor, vacuum tightness keeps 90min under-0.1MPa condition.
Further, described be blended in 20 ~ 30 DEG C and carry out under cooling drying condition, control cold water temperature at 15 DEG C.
The beneficial effect of above-mentioned further scheme is adopted to be that, because solidifying agent is responsive to high-temperature, the operation under constant temperature cooling conditions can avoid solidifying agent to lose efficacy, and avoids the stability affecting product.
The liquid corner binding glue that preparation method of the present invention obtains, viscosity is 72-100Pa.s, and yield value is 35-55Pa, and at 80 DEG C, set time is less than 15min.
The invention has the beneficial effects as follows: corner binding adhesive capacity prepared by the present invention is not high and thixotropy good, higher cross-linking density makes its excellent in weather, and solidification value is low, curing speed is fast, and cohesive strength is high, and shrinking percentage is low, it is more stable permanent to store, preparation technology's simple environment protection, cost is low, applied widely.And the product utilizing preparation method of the present invention to obtain is liquid state, is conducive to site operation, avoids the generation of bubble.
Embodiment
Be described principle of the present invention and feature below in conjunction with example, example, only for explaining the present invention, is not intended to limit scope of the present invention.
Embodiment 1
A kind of chip corner binding glue, its component is counted by weight: bisphenol A epoxide resin 828EL (Shel l board, Holland produce) 22.5g, bisphenol F epoxy resin 830S (Japanese DIC board) 37.0g, black cream (Degussa T4 mineral black) 0.5g, white carbon black (R202, Degussa) 4.8g, silicon-dioxide ball-type filler (Toyota Tsusho, FED45B) 88.0g, thiol esters (TMPTMA, Japan) 47.6g, barbituric acid 1.5g, solidifying agent PN-H (Japanese aginomoto) 6.0g and coupling agent KH5602.0g.
By bisphenol A epoxide resin (Shel l board, Holland produces) 22.5g and bisphenol F epoxy resin 830S (Japanese DIC board) 37.0g toasts 12h at 75 DEG C, then by roasted 22.5g bisphenol A epoxide resin, 37.0g bisphenol F epoxy resin, 4.8g white carbon black and 0.5g black cream are in 20 DEG C of mixing 20 ~ 40min, then 88g silicon-dioxide ball-type filler is added, 47.6g thiol esters TMPTMA, 1.5g barbituric acid, 6.0g solidifying agent PN-H and 2.0g coupling agent KH560, insert in three-roller and mix, (namely compound repeats to enter three-roller three times to repeat mixing three times, continuous mixing three times, make mixing of materials more even), add after mixing in reactor, vacuum tightness keeps 90min under-0.1MPa condition.
Above-mentioned obtained chip corner binding glue is adopted the test of DSC differential scanning calorimetry, surveys its solidification value 80 DEG C, solidification needs 7 minutes; Test by GB/T7124-1986 standard, its shearing resistance is 13MPa; CTE (coefficient of linear expansion) a1 is 20ppm, and thermal conductivity is 3.2w/m.k, and 40 DEG C of shelf liveves are 10 months more than 10h, 2-8 DEG C of shelf lives.
Embodiment 2
A kind of chip corner binding glue, its component is counted by weight: bisphenol A epoxide resin 828EL (Shel l board, Holland produce) 20.0g, bisphenol F epoxy resin 830S (Japanese DIC board) 40.0g, black cream (Degussa T4 mineral black) 1.0g, white carbon black (R202, Degussa) 5.0g, silicon-dioxide ball-type filler (Toyota Tsusho, FED45B) 80.0g, thiol esters (TMPTMA, Japan) 48.0g, barbituric acid 1.5g, solidifying agent PN-H (Japanese aginomoto) 4.0g and coupling agent KH5501.0g.
By bisphenol A epoxide resin (Shel l board, Holland produces) 20.0g and bisphenol F epoxy resin 830S (Japanese DIC board) 40.0g toasts 12h at 75 DEG C, then by roasted 20.0g bisphenol A epoxide resin, 40.0g bisphenol F epoxy resin, 5.0g white carbon black and 1.0g black cream are in 30 DEG C of mixing 20 ~ 40min, then 80.0g silicon-dioxide ball-type filler is added, 48.0g thiol esters TMPTMA, 1.5g barbituric acid, 4.0g solidifying agent PN-H and 1.0g coupling agent KH550, insert in three-roller and mix, repeat mixing three times, add after mixing in reactor, vacuum tightness keeps 90min under-0.1MPa condition.
Above-mentioned obtained chip corner binding glue is adopted the test of DSC differential scanning calorimetry, surveys its solidification value 80 DEG C, solidification needs 14 minutes; Test by GB/T7124-1986 standard, its shearing resistance is 10MPa; 40 DEG C of shelf liveves are 10 months more than 10h, 2-8 DEG C of shelf lives.
Embodiment 3
A kind of chip corner binding glue, its component is counted by weight: bisphenol A epoxide resin 828EL (Shel l board, Holland produce) 25.0g, bisphenol F epoxy resin 830S (Japanese DIC board) 35.0g, black cream (Degussa T4 mineral black) 0.8g, white carbon black (R202, Degussa) 10.0g, silicon-dioxide ball-type filler (Toyota Tsusho, FED45B) 60.0g, thiol esters (TMPTMA, Japan) 30.0g, barbituric acid 1.0g, solidifying agent PN-H (Japanese aginomoto) 4.0g and coupling agent KH5701.5g.
By bisphenol A epoxide resin (Shel l board, Holland produces) 25.0g and bisphenol F epoxy resin 830S (Japanese DIC board) 35.0g toasts 12h at 70 DEG C, then by roasted 25.0g bisphenol A epoxide resin, 35.0g bisphenol F epoxy resin, 10.0g white carbon black and 0.8g black cream are in 20 DEG C of mixing 20 ~ 40min, then 60.0g silicon-dioxide ball-type filler is added, 30.0g thiol esters TMPTMA, 1.0g barbituric acid, 4.0g solidifying agent PN-H and 1.5g coupling agent KH570, insert in three-roller and mix, repeat mixing three times, add after mixing in reactor, vacuum tightness keeps 90min under-0.1MPa condition.
Embodiment 4
A kind of chip corner binding glue, its component is counted by weight: bisphenol A epoxide resin 828EL (Shel l board, Holland produce) 22.5g, bisphenol F epoxy resin 830S (Japanese DIC board) 37.0g, black cream (Degussa T4 mineral black) 0.5g, white carbon black (R202, Degussa) 8.0g, silicon-dioxide ball-type filler (Toyota Tsusho, FED45B) 100.0g, thiol esters (TMPTMA, Japan) 50.0g, barbituric acid 2.0g, solidifying agent PN-H (Japanese aginomoto) 10.0g and coupling agent KH5603.0g.
By bisphenol A epoxide resin (Shel l board, Holland produces) 22.5g and bisphenol F epoxy resin 830S (Japanese DIC board) 37.0g toasts 12h at 73 DEG C, then by roasted 22.5g bisphenol A epoxide resin, 37.0g bisphenol F epoxy resin, 8.0g white carbon black and 0.5g black cream are in 30 DEG C of mixing 20 ~ 40min, then 100.0g silicon-dioxide ball-type filler is added, 50.0g thiol esters TMPTMA, 2.0g barbituric acid, 10.0g solidifying agent PN-H and 3.0g coupling agent KH560, insert in three-roller and mix, repeat mixing three times, add after mixing in reactor, vacuum tightness keeps 90min under-0.1MPa condition.
Comparative example 1
The E44 of epoxy resin E51 and 13.2g of 32g is toasted 12h at 70 ~ 75 DEG C, add 0.5g black cream (Degussa T4 mineral black) and mix 20 ~ 40min, then add 600 order silicon powder 80g, dicy-curing agent 4.2g, 1020 (Japanese fuji) curing catalyst 2.4g, coupling agent KH5600.56g and AGE (Shel l H8) 20g mix.
Adopt the test of DSC differential scanning calorimetry, survey its solidification value 120 DEG C, solidification needs 15min; Test by GB/T7124-1986 standard, its shearing resistance is 9MPa; CTE (coefficient of linear expansion) a1 is 54ppm, thermal conductivity 0.3w/m.k; 40 DEG C of shelf liveves are 10 months more than 10h, 2-8 DEG C of shelf lives.
The performance perameter of embodiment 1 with comparative example 1 is contrasted, obtains table 1.
Table 1
| Embodiment 1 | Comparative example 1 | |
| Solidification value (DEG C) | 80 | 120 |
| Solidification duration (min) | 7 | 15 |
| Shearing resistance (MPa) | 13 | 9 |
| CTE a1 | 20 | 54 |
| Thermal conductivity (w/m.k) | 3.2 | 0.3 |
| 40 DEG C of shelf liveves | ≥10h | ≥10h |
| 2-8 DEG C of shelf lives | 10 months | 10 months |
As can be seen from Table 1, embodiment 1 uses bisphenol A epoxide resin and bisphenol F epoxy resin to match, and makes the solidification value of glue low, and curing speed is fast, and the rear good toughness of solidification, cohesive strength are good, have excellent thermal shock resistance.The glue that the present invention obtains has good heat conductivility, extremely low coefficient of linear expansion, the damage to electronic component when can avoid expanding or shrinking.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a chip corner binding glue, is characterized in that its component is counted by weight: bisphenol A epoxide resin 20 ~ 25 parts, bisphenol F epoxy resin 35 ~ 40 parts, 0.5 ~ 1.0 part, colorant, white carbon black 4 ~ 10 parts, ball-shaped filling material 60 ~ 100 parts, thiol esters 30 ~ 50 parts, stablizer 1 ~ 2 part, 4 ~ 10 parts, solidifying agent and coupling agent 1 ~ 3 part.
2. binding glue in chip corner according to claim 1, it is characterized in that described bisphenol A epoxide resin is liquid bisphenol A epoxy resin 828EL, described bisphenol F epoxy resin is bisphenol F epoxy resin 830S.
3. binding glue in chip corner according to claim 1, is characterized in that described colorant is black cream; Described ball-shaped filling material is silicon-dioxide; Described stablizer is barbituric acid.
4. binding glue in chip corner according to claim 1, is characterized in that described thiol esters is trimethylolpropane trimethacrylate TMPTMA.
5. binding glue in chip corner according to claim 1, is characterized in that described solidifying agent is modified imidazole and the derivative thereof of fineness 5 ~ 10 μm.
6. glue is bound in chip corner according to claim 1 or 5, it is characterized in that described solidifying agent is the modified amine latent curing agent of fineness 5 ~ 10 μm.
7. glue is bound in chip corner according to claim 1 or 5, it is characterized in that described solidifying agent is the solidifying agent of trade mark PN-H.
8. binding glue in chip corner according to claim 1, is characterized in that described coupling agent is the silane coupling agent of the trade mark KH550, KH560 or KH570.
9. the preparation method of a binding glue in chip corner according to claim 1, it is characterized in that, bisphenol A epoxide resin and bisphenol F epoxy resin are toasted 12h at 70 ~ 75 DEG C, then by roasted 20 ~ 25 parts of bisphenol A epoxide resins, 35 ~ 40 parts of bisphenol F epoxy resins, 4 ~ 10 parts of white carbon blacks and 0.5 ~ 1.0 part of colorant are in 20-30 DEG C of mixing 20 ~ 40min, then 60 ~ 100 parts of ball-shaped filling materials are added, 30 ~ 50 parts of thiol esters, 1 ~ 2 part of stablizer, 4 ~ 10 parts of solidifying agent and 1 ~ 3 part of coupling agent, insert in three-roller and mix, repeat mixing three times, add after mixing in reactor, vacuum tightness keeps 90min under-0.1MPa condition.
10. the preparation method of chip corner according to claim 9 binding glue, is characterized in that, described be blended in 20 ~ 30 DEG C and carry out under cooling drying condition, controls cold water temperature at 15 DEG C.
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| CN201410795290.3A CN104531029A (en) | 2014-12-18 | 2014-12-18 | Chip four-corner binding glue and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410795290.3A CN104531029A (en) | 2014-12-18 | 2014-12-18 | Chip four-corner binding glue and preparation method thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1871299A (en) * | 2003-09-26 | 2006-11-29 | 伊利诺斯器械工程公司 | Adhesive compositions |
| KR20100095195A (en) * | 2009-02-20 | 2010-08-30 | 도레이첨단소재 주식회사 | Adhesive composition and coverlay film using the same |
| CN103087664A (en) * | 2013-01-29 | 2013-05-08 | 深圳市宝力科技有限公司 | Relay liquid state epoxy resin pouring sealant and preparation method thereof |
-
2014
- 2014-12-18 CN CN201410795290.3A patent/CN104531029A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1871299A (en) * | 2003-09-26 | 2006-11-29 | 伊利诺斯器械工程公司 | Adhesive compositions |
| KR20100095195A (en) * | 2009-02-20 | 2010-08-30 | 도레이첨단소재 주식회사 | Adhesive composition and coverlay film using the same |
| CN103087664A (en) * | 2013-01-29 | 2013-05-08 | 深圳市宝力科技有限公司 | Relay liquid state epoxy resin pouring sealant and preparation method thereof |
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Application publication date: 20150422 |
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