CN103074021B - Organosilicon bimaleimide-epoxy conductive adhesive for LED - Google Patents
Organosilicon bimaleimide-epoxy conductive adhesive for LED Download PDFInfo
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- CN103074021B CN103074021B CN201110327740.2A CN201110327740A CN103074021B CN 103074021 B CN103074021 B CN 103074021B CN 201110327740 A CN201110327740 A CN 201110327740A CN 103074021 B CN103074021 B CN 103074021B
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Abstract
The invention discloses a kind of Organosilicon bimaleimide-epoxy conductive adhesive for LED, comprise 5～25 parts by weight epoxy resin, 5～25 weight portion organosilicon BMIs, 60～80 parts by weight of silver powder conductive fillers, 0.3～0.7 weight portion curing accelerator, 0.3～0.7 weight portion interface reinforcing agent silane coupler.The advantage of organosilicon BMI and epoxy resin is combined by the conducting resinl of the present invention, remains resistance to elevated temperatures and the uv-resistance energy of polyorganosiloxane resin, also makes product have the adhesive property of excellence simultaneously.
Description
Technical field
The present invention relates to LED conductive adhesive, specifically a kind of Organosilicon bimaleimide-epoxy conductive adhesive for LED.
Background technology
Since striding into 21 century, Energy situation is increasingly serious, and saves energy ratio and tap a new source of energy more economical, more environmental protection, should put in the first place.Currently, illumination accounts for about the 20% of world's total energy consumption.If, life-span length, safe and environment-friendly light source low by energy consumption replace the conventional light source of power consumption inefficient, high, will bring undoubtedly a global illumination revolution (Yang Xiongfa, Wu Chuan, Dong Hong, etc..The progress of LED organosilicon material for packaging.Organosilicon material, 2009,23,47～50).
LED is with its intrinsic feature, such as power saving, life-span length, vibration resistance, the feature such as fast response time, cold light source, it is widely used in the fields such as display lamp, signal lights, display screen, illumination, in our daily life visible everywhere, such as household electrical appliance, telephone set, dial illumination, automobile anti-fog lamp, traffic light etc. (Su Yongdao, lucky Aiwa, Zhao Chao.LED encapsulation technology.Shanghai, publishing house of Shanghai Communications University, 2010).The electric energy of ultra-high brightness LED consumption is only the 1/10 of conventional light source, has advantages such as not using little, the life-span length of the hydrargyrum of serious environment pollution, volume.Along with the improvement of ultra-high brightness LED performance, great power LED is expected to replace the lighting source such as electric filament lamp, become forth generation lighting source (Wang Xiaoming, Guo Weiling, Gao Guo, etc..LED a new generation lighting source.Modern display, 2005,53,15～20).
Along with the development of great power LED, the material used in encapsulation process is proposed increasingly higher requirement by client, and new material not only to meet the technological requirement that client produces, and has also needed to good uv-resistance and thermostability and enough adhesive strengths simultaneously.Traditional epoxy conductive binding agent has the room temperature adhesive property of excellence, but its high temperature bonding performance is not ideal enough, and epoxy resin-base is often weak to UV in addition, and under the comprehensive function of UV light and heat, it easily xanthochromia occurs thus affecting LED luminescent lifetime.Therefore, epoxy resin is not suitable for high temperature occasion, or can launch LED and the great power LED of ultraviolet wavelength, and uses out of doors.In sum, traditional epoxy conductive binding agent increasingly can not meet the performance requirement day by day updated, it is necessary to it is modified.
Epoxy resin refers to containing the organic high molecular compound of two or more epoxide groups in molecule, and molecular structure is to be its feature containing active epoxide group in strand, and epoxide group may be located at the end of strand, centre or structure circlewise.Due to its dielectric properties, mechanical property, adhesive property, excellent anti-corrosion performance, cure shrinkage and linear expansion coefficient are little, good stability of the dimension, good manufacturability, combination property is splendid, more due to the motility of epoxy material formula design and multiformity so that it is widely used in field of electronics.
BMI resin refer to maleimide be active end group difunctional BMI monomer and relevant copolymerization component formed a class thermosetting resin, the formula of BMI is as follows:
BMI resin has good high temperature resistant, the good characteristic such as radiation hardness, wet-heat resisting, modulus high, hydroscopicity is low and thermal coefficient of expansion is little, is widely used in field of electronics, but traditional B MI resin rigidity is relatively big, and the transparency is poor.
The silicon-oxygen backbone structure that polysiloxane-based adhesive has, structural formula is as follows:
Si-O-Si has higher bond energy, has stronger ultra-violet resistance, is therefore applicable to any ultraviolet lighting occasion.The SMP-2800L of SHIN-ETSU HANTOTAI of Japan chemical industry, the one-component of Japan's Teng Cang chemical conversion, containing solvent organosilicon conductive adhesive (XA-819A and the FX-730 of DOTITE), is this series products.Because the polarity of the main chain of poly-silica is less, so the cementability of conducting resinl described above is poor, chip thrust is less than normal, room temperature small pieces thrust < 5kgf/die (2 × 2mm).
In sum, epoxy resin, BMI and polysiloxanes are respectively arranged with advantage, how the advantage of three are combined into the technical issues that need to address of the present invention.The combination of three can make material have the high temperature bonding performance of resistance to elevated temperatures, light transmission and excellence concurrently.This patent uses containing the machine silicon BMI of polysiloxane structure and epoxy resin copolymerization, generation there is the conductive adhesive of excellent properties.
Summary of the invention
It is an object of the invention to provide a kind of Organosilicon bimaleimide-epoxy conductive adhesive for LED, the advantage of epoxy resin, organosilicon BMI and polyorganosiloxane resin three is combined, retain the high transparent of the high temperature resistant and polyorganosiloxane resin of the high adhesiveness energy of epoxy resin, bimaleimide resin, also make product have the adhesive property of excellence simultaneously.
It is an object of the invention to be achieved through the following technical solutions:
The Organosilicon bimaleimide-epoxy conductive adhesive for LED that the present invention relates to, comprises the component with following weight portion:
According to the present invention, described epoxy resin is hydrogenated bisphenol A epoxy (HEP), and its structural formula is:
According to the present invention, described organosilicon BMI is the material shown in below formula (I) or formula (II):
A, methylsiloxane BMI (SiMBMI), its structure is shown in formula (I):
Wherein, n=1～6；
B, aminomethyl phenyl organosilicon BMI (SiMPBMI), its structure is shown in formula (II):
Wherein, n=1～6.
According to the present invention, described curing accelerator is 2-methylimidazole (2MZ) or 2-ethyl-4-methylimidazole (2E4MZ).
According to the present invention, described argentum powder conductive filler is the granule D90 argentum powder less than 50 microns；Described argentum powder is flake silver powder, spherical argentum powder, unformed argentum powder or their any mixture.
According to the present invention, described interface reinforcing agent silane coupler is 3-glycidylpropyl trimethoxy silane (Z6040).
The preparation method of the Organosilicon bimaleimide-epoxy conductive adhesive for LED of the present invention comprises the following steps:
A) organosilicon BMI, curing accelerator and the mixing of interface reinforcing agent silane coupler, then pass through three-roll grinder grinding and obtain uniform resin；
B) argentum powder is added in the resin after grinding, stir 1 hour.
Compared with prior art, the present invention has the following technical effect that the Organosilicon bimaleimide-epoxy conductive adhesive for LED of the present invention, room temperature chip thrust > 11.6kgf/die (2 × 2mm), high temperature chip thrust > 2.2kgf/die (2 × 2mm), specific insulation≤3.7 × 10-4Ω·cm；Namely this adhesive has good bin stability, has the adhesive strength of excellence, electric conductivity, thermostability and uv-resistance after solidification.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention will be further described.Should be understood that following example are merely to illustrate the present invention not for restriction the scope of the present invention.
Flake silver powder in following example, spherical argentum powder, unformed argentum powder are all that granule D90 (referring to that the cumulative particle sizes distribution number of sample reaches particle diameter corresponding when 90%) is less than 50 microns.
Embodiment 1～9
By the proportioning shown in table 1, first by organosilicon BMI, curing accelerator and interface reinforcing agent silane coupler mix, and then pass through three-roll grinder grinding and obtain uniform resin；Then argentum powder is added in the resin after grinding, stir 1 hour, namely obtain Organosilicon bimaleimide-epoxy conductive adhesive.
Table 1, Organosilicon bimaleimide-epoxy conductive adhesive component
The DAGA4000 thrust machine adopted, tests the performance of the Organosilicon bismaleimide conductive adhesive for LED that embodiment 1～9 obtains, and result is as shown in table 2.
Table 2, Organosilicon bimaleimide-epoxy conductive adhesive performance
Result from table 2, the refractive index of Organosilicon bimaleimide-epoxy conductive adhesive for LED prepared by the method for employing embodiment 1～9 is 1.47～1.51, glass transition temperature is 123～132 DEG C, 2 × 2mm chip thrust is 11.6～13.1kgf (25 DEG C), 2.2～2.9kgf (250 DEG C), and specific insulation is 1.9 × 10-4～3.7 × 10-4Ω.cm。
Embodiment 10～18
Shown in table 3, first by organosilicon BMI, curing accelerator and interface reinforcing agent silane coupler mix, and then pass through three-roll grinder grinding and obtain uniform resin；Then argentum powder is added in the resin after grinding, stir 1 hour, obtain Organosilicon bimaleimide-epoxy conductive adhesive.
Table 3, Organosilicon bimaleimide-epoxy conductive adhesive component
Adopting DAGA4000 thrust machine, the performance of the Organosilicon bismaleimide conductive adhesive for LED that embodiment 10～18 obtains is tested, result is as shown in table 4.
Table 4, Organosilicon bimaleimide-epoxy conductive adhesive performance
Result from table 4, the refractive index of Organosilicon bimaleimide-epoxy conductive adhesive for LED prepared by the method for employing embodiment 10～18 is 1.52～1.53, glass transition temperature is 126～132 DEG C, 2 × 2mm chip thrust is 12.6～13.9kgf (25 DEG C), 2.2～3.1kgf (250 DEG C), and specific insulation is 1.3 × 10-4～3.5 × 10-4Ω.cm。
In conjunction with above-described embodiment, the Organosilicon bimaleimide-epoxy conductive adhesive for LED of the present invention, room temperature chip thrust > 11.6kgf/die (2 × 2mm), high temperature chip thrust > 2.2kgf/die (2 × 2mm), specific insulation≤3.7 × 10-4Ω·cm；Namely this adhesive has good bin stability, has the adhesive strength of excellence, electric conductivity, thermostability and uv-resistance after solidification.
Claims (7)
1. an Organosilicon bimaleimide-epoxy conductive adhesive for LED, it is characterised in that comprise the component with following weight portion:
Wherein, described epoxy resin is hydrogenated bisphenol A epoxy, and its structural formula is:
2. conductive adhesive according to claim 1, it is characterised in that described organosilicon BMI is the material shown in below formula (1) or formula (II):
A, methylsiloxane BMI, its structure is shown in formula (I):
Wherein, n=1～6；
B, aminomethyl phenyl organosilicon BMI, its structure is shown in formula (II):
Wherein, n=1～6.
3. conductive adhesive according to claim 1, it is characterised in that described argentum powder conductive filler is the granule D90 argentum powder less than 50 microns；Wherein, described granule D90 refers to that the cumulative particle sizes distribution number of sample reaches particle diameter corresponding when 90%.
4. conductive adhesive according to claim 3, it is characterised in that described argentum powder is flake silver powder, spherical argentum powder, unformed argentum powder or their any mixture.
5. conductive adhesive according to claim 1, it is characterised in that described curing accelerator is 2-methylimidazole or 2-ethyl-4-methylimidazole.
6. conductive adhesive according to claim 1, it is characterised in that described interface reinforcing agent silane coupler is 3-glycidylpropyl trimethoxy silane.
7. the preparation method of the Organosilicon bimaleimide-epoxy conductive adhesive for LED according to any one of claim 1～6, it is characterised in that comprise the following steps:
A) epoxy resin, organosilicon BMI, curing accelerator and interface reinforcing agent silane coupler mixing, then pass through three-roll grinder grind obtain uniform resin；
B) argentum powder is added in the resin after grinding, stir 1 hour.
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| CN201110327740.2A CN103074021B (en) | 2011-10-25 | 2011-10-25 | Organosilicon bimaleimide-epoxy conductive adhesive for LED |
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| CN201110327740.2A CN103074021B (en) | 2011-10-25 | 2011-10-25 | Organosilicon bimaleimide-epoxy conductive adhesive for LED |
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| CN103074021B true CN103074021B (en) | 2016-07-20 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103602309B (en) * | 2013-11-28 | 2014-10-22 | 烟台德邦先进硅材料有限公司 | High-power packaging silica gel for LED (Light Emitting Diode) |
| CN104817989B (en) * | 2015-04-10 | 2017-11-10 | 深圳广恒威科技有限公司 | A kind of Underfill adhesive composition and preparation method thereof |
| JP7024660B2 (en) * | 2018-08-10 | 2022-02-24 | 信越化学工業株式会社 | Thermosetting resin compositions and semiconductor devices |
| JP7020341B2 (en) * | 2018-08-10 | 2022-02-16 | 信越化学工業株式会社 | Thermosetting resin composition for semiconductor encapsulation and semiconductor devices |
| CN113736401A (en) * | 2021-09-06 | 2021-12-03 | 艾蒙特成都新材料科技有限公司 | High-heat-resistance single-component adhesive and preparation method thereof |
| CN114231230B (en) * | 2021-12-30 | 2023-10-20 | 黑龙江省科学院石油化学研究院 | Adhesive capable of reducing stress and improving temperature resistance and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6238597B1 (en) * | 1999-03-10 | 2001-05-29 | Korea Advanced Institute Of Science And Technology | Preparation method of anisotropic conductive adhesive for flip chip interconnection on organic substrate |
| CN102391811A (en) * | 2011-09-23 | 2012-03-28 | 上海景涵实业有限公司 | Bismaleimide-epoxy conductive adhesive with high adhesive strength for light emitting diode (LED) |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6238597B1 (en) * | 1999-03-10 | 2001-05-29 | Korea Advanced Institute Of Science And Technology | Preparation method of anisotropic conductive adhesive for flip chip interconnection on organic substrate |
| CN102391811A (en) * | 2011-09-23 | 2012-03-28 | 上海景涵实业有限公司 | Bismaleimide-epoxy conductive adhesive with high adhesive strength for light emitting diode (LED) |
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