CN103074028B - Organosilicon polyimide insulation adhesive for LED - Google Patents
Organosilicon polyimide insulation adhesive for LED Download PDFInfo
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- CN103074028B CN103074028B CN201110327776.0A CN201110327776A CN103074028B CN 103074028 B CN103074028 B CN 103074028B CN 201110327776 A CN201110327776 A CN 201110327776A CN 103074028 B CN103074028 B CN 103074028B
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Abstract
The invention discloses a kind of Organosilicon polyimide insulation adhesive for LED, comprise 10��40 weight portion Amino End Group silicone oil, 10��40 weight portion end anhydride silicone oil, 5��10 weight portion polyamino silicone oil, 2��5 parts by weight of silica fillers, 2��5 parts by weight of titanium dioxide fillers, 0.3��1.2 weight portion interface reinforcing agent silane coupler. The advantage of organic siliconresin and polyimide resin is combined by the insulating cement of the present invention, first synthesizing organo-silicon polyamide acid prepolymer, and final solidification obtains organic silicon polyimide insulating cement. Present invention preserves the light transmission of the high temperature resistant of polyimide resin and polyorganosiloxane resin, also make product have the high temperature bonding performance of excellence simultaneously.
Description
Technical field
The present invention relates to LED dielectric adhesive, specifically a kind of Organosilicon polyimide insulation 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.
Polyimide resin refers to the polymer in molecular machinery containing imide ring, and its structure is as follows:
Polyimide 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, and traditional polyimide resin rigidity is big, and cured product has color.
The silicon-oxygen backbone structure that type siloxane 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, polyimides and polysiloxanes are respectively arranged with advantage, how both advantages are combined into the technical issues that need to address of the present invention. Both combinations can make material have the high temperature bonding performance of resistance to elevated temperatures, uv-resistance energy and excellence concurrently.
Summary of the invention
It is an object of the invention to provide a kind of Organosilicon polyimide insulation adhesive for LED, the advantage of organic siliconresin and polyimide resin is combined, retain the light transmission of the high temperature resistant and polyorganosiloxane resin of polyimide 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 polyimide insulation adhesive for LED that the present invention relates to, comprises the component with following weight portion:
According to the present invention, described Amino End Group silicone oil is:
(1) SiMNH, its structural formula is:
Wherein, n=1��6; Or
(2) SiMPNH, its structural formula is:
Wherein, n=1��6.
According to the present invention, described end anhydride silicone oil is:
(1) SiMDH, its structural formula is:
Wherein, n=1��6; Or
(2) SiMPDH, its structural formula is:
Wherein, n=1��6.
According to the present invention, the structural formula of described polyamino silicone oil (SinNH) is:
Wherein: n=1-6, m=1-6.
According to the present invention, the mean diameter of described silicon dioxide and titanium dioxide (ruby-type) filler is 100nm.
According to the present invention, described interface reinforcing agent silane coupler is 3-glycidylpropyl trimethoxy silane (Z6040).
The preparation method of the LED organic silicon polyimide insulating cement of the present invention comprises the following steps:
By Amino End Group silicone oil, end anhydride silicone oil and polyamino silicone oil mix by a certain percentage, at room temperature stirring 6-8 hour, then add silicon dioxide, titanium dioxide and interface reinforcing agent silane coupler, use three-roll grinder to grind three times.
Compared with prior art, the present invention has the following technical effect that, room temperature chip thrust > 9.3kgf/die (2 �� 2mm), high temperature chip thrust > 1.7kgf/die (2 �� 2mm), light transmittance > 81%; Namely this adhesive has good bin stability, has the adhesive strength of excellence, thermostability and light transmission 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.
Silicon dioxide and the mean diameter of titanium dioxide filler in following example are 100nm.
Embodiment 1��4
Shown in table 1, respectively by Amino End Group silicone oil SiMNH, end anhydride silicone oil SiMDH and polyamino silicone oil SinNH mixes by a certain percentage, at room temperature stirring 6 hours, it is subsequently adding silicon dioxide, titanium dioxide and interface reinforcing agent silane coupler, use three-roll grinder to grind three times, namely prepare Organosilicon polyimide insulation adhesive.
Table 1, Organosilicon polyimide insulation adhesive component
Adopting DAGA4000 thrust machine, the performance of the Organosilicon polyimide insulation adhesive for LED that embodiment 1��4 obtains is tested, result is as shown in table 2.
Table 2, Organosilicon polyimide insulation adhesive performance
Result from table 2, the refractive index of Organosilicon polyimide insulation adhesive for LED prepared by the method for employing embodiment 1��4 is 1.48��1.49, glass transition temperature is 102��112 DEG C, 2 �� 2mm chip thrust is 9.3��11.2kgf (25 DEG C), 1.7��2.5kgf (250 DEG C), and light transmittance is 83%��93%.
Embodiment 5��8
Shown in table 3, respectively by Amino End Group silicone oil SiMPNH, end anhydride silicone oil SiMPDH and polyamino silicone oil SinNH mixes by a certain percentage, at room temperature stirring 8 hours, it is subsequently adding silicon dioxide, titanium dioxide and interface reinforcing agent silane coupler, use three-roll grinder to grind three times, namely prepare Organosilicon polyimide insulation adhesive.
Table 3, Organosilicon polyimide insulation adhesive component
Adopting DAGA4000 thrust machine, the performance of the Organosilicon polyimide insulation adhesive for LED that embodiment 5��8 obtains is tested, result is as shown in table 4.
Table 4, Organosilicon polyimide insulation adhesive performance
Result from table 4, the refractive index of Organosilicon polyimide insulation adhesive for LED prepared by the method for employing embodiment 5��8 is 1.53, glass transition temperature is 113��121 DEG C, 2 �� 2mm chip thrust is 9.4��12.3kgf (25 DEG C), 1.9��2.7kgf (250 DEG C), and light transmittance is 81%��91%.
In conjunction with above-described embodiment, the Organosilicon polyimide insulation adhesive for LED of the present invention, room temperature chip thrust > 9.3kgf/die (2 �� 2mm), high temperature chip thrust > 1.7kgf/die (2 �� 2mm), light transmittance > 81%; Namely this adhesive has good bin stability, has the adhesive strength of excellence, light transmission, thermostability and uv-resistance after solidification.
Claims (3)
1. an Organosilicon polyimide insulation adhesive for LED, it is characterised in that comprise the component with following weight portion:
Interface reinforcing agent silane coupler 0.3��1.2;
Wherein, the structural formula of described Amino End Group silicone oil is:
Wherein, n=1��6; Or
Wherein, n=1��6;
The structural formula of described end anhydride silicone oil is:
Wherein, n=1��6; Or
Wherein, n=1��6;
The structural formula of described polyamino silicone oil is:
Wherein: n=1-6, m=1-6.
2. dielectric adhesive according to claim 1, it is characterised in that the mean diameter of described silicon dioxide and titanium dioxide filler is 100nm.
3. the preparation method of the Organosilicon polyimide insulation adhesive for LED described in claim 1 or 2, it is characterised in that comprise the following steps:
By Amino End Group silicone oil, end anhydride silicone oil and polyamino silicone oil mix by a certain percentage, at room temperature stirring 6-8 hour, then add silicon dioxide, titanium dioxide and interface reinforcing agent silane coupler, use three-roll grinder to grind three times.
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Families Citing this family (6)
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TWI468415B (en) * | 2013-06-13 | 2015-01-11 | Daxin Materials Corp | Siloxane dianhydride, polymer, liquid crystal alignment agent, liquid crystal alignment film, and liquid crystal display device |
CN109722209A (en) * | 2018-12-21 | 2019-05-07 | 东华大学 | A kind of YASI organic imides silica gel and preparation method thereof |
CN109722211A (en) * | 2018-12-21 | 2019-05-07 | 东华大学 | A kind of BDADDM type silicon-containing adhesive and preparation method thereof |
CN109722208A (en) * | 2018-12-21 | 2019-05-07 | 东华大学 | A kind of 12BDAPB type silicon-containing adhesive and preparation method thereof |
CN109722210A (en) * | 2018-12-21 | 2019-05-07 | 东华大学 | A kind of TADE type silicon-containing adhesive and preparation method thereof |
CN111640845A (en) * | 2020-05-29 | 2020-09-08 | 旭宇光电(深圳)股份有限公司 | Deep ultraviolet LED light source and packaging method thereof |
Citations (4)
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CN1332779A (en) * | 1998-12-28 | 2002-01-23 | 西洋化学公司 | Polyamideimidesiloxane hot melt adhesive |
JP2005113059A (en) * | 2003-10-09 | 2005-04-28 | Shin Etsu Chem Co Ltd | Curable resin composition and electrically conductive adhesive |
JP2008138124A (en) * | 2006-12-04 | 2008-06-19 | Shin Etsu Chem Co Ltd | Adhesive composition and adhesive film |
CN102127388A (en) * | 2011-01-19 | 2011-07-20 | 常州市耀辉涂料有限公司 | Acid-resistant high-temperature-resistant elastic adhesive |
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- 2011-10-25 CN CN201110327776.0A patent/CN103074028B/en active Active
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1332779A (en) * | 1998-12-28 | 2002-01-23 | 西洋化学公司 | Polyamideimidesiloxane hot melt adhesive |
JP2005113059A (en) * | 2003-10-09 | 2005-04-28 | Shin Etsu Chem Co Ltd | Curable resin composition and electrically conductive adhesive |
JP2008138124A (en) * | 2006-12-04 | 2008-06-19 | Shin Etsu Chem Co Ltd | Adhesive composition and adhesive film |
CN102127388A (en) * | 2011-01-19 | 2011-07-20 | 常州市耀辉涂料有限公司 | Acid-resistant high-temperature-resistant elastic adhesive |
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