CN103074028A - Organosilicon polyimide insulation adhesive for LED - Google Patents
Organosilicon polyimide insulation adhesive for LED Download PDFInfo
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- CN103074028A CN103074028A CN2011103277760A CN201110327776A CN103074028A CN 103074028 A CN103074028 A CN 103074028A CN 2011103277760 A CN2011103277760 A CN 2011103277760A CN 201110327776 A CN201110327776 A CN 201110327776A CN 103074028 A CN103074028 A CN 103074028A
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- 0 C*(*)[Si](C(C)(C(CCC1C(O2)=O)CC1C2=O)N)(c1ccccc1)O*(C)[Si](C(CCC1C(O2)=O)CC1C2=O)(c1ccccc1)C#N Chemical compound C*(*)[Si](C(C)(C(CCC1C(O2)=O)CC1C2=O)N)(c1ccccc1)O*(C)[Si](C(CCC1C(O2)=O)CC1C2=O)(c1ccccc1)C#N 0.000 description 1
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Abstract
The invention discloses an organosilicon polyimide insulation adhesive for an LED. The adhesive includes, by weight, 10 to 40 parts of amino-terminated silicone oil, 10 to 40 parts of anhydride-terminated silicone oil, 5 to 10 parts of polyamino silicone oil, 2 to 5 parts of a silica filling material, 2 to 5 parts of a titanium dioxide filling material and 0.3 to 1.2 parts of an interfacial strengthening agent-silane coupling agent. According to the invention, the advantages of both an organosilicon resin and a polyimide resin are combined together, and an organosilicon polyamide acid prepolymer is synthesized at first and is finally cured to obtain the organosilicon polyimide insulation adhesive; high temperature resistance of the polyimide resin and light transmittance performance of a polysilicone resin are retained, and the insulation adhesive also has excellent high temperature adhesive properties.
Description
Technical field
The present invention relates to the LED dielectric adhesive, specifically a kind of LED organic silicon polyimide dielectric adhesive.
Background technology
Since striding into 21 century, Energy situation is increasingly serious, and the save energy ratio taps a new source of energy more economical, more environmental protection should be put in the first place.Current, illumination accounts for about 20% of world's total energy consumption.If conventional light source inefficient, high current consumption that the light source of, life-span length low with energy consumption, safety, environmental protection replaces, 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 characteristics, such as power saving, life-span length, vibration resistance, the characteristics such as fast response time, cold light source, be widely used in the fields such as pilot lamp, signal lamp, display screen, illumination, in our daily life everywhere as seen, (Su Shuidao, lucky Aiwa, Zhao Chao such as household electrical appliance, telephone set, dial illumination, automobile anti-fog lamp, traffic lights.The LED encapsulation technology.Shanghai, press of Shanghai Communications University, 2010).The electric energy of ultra-high brightness LED consumption only is 1/10 of conventional light source, has the advantages such as the mercury, the volume that do not use serious environment pollution are little, the life-span is long.Along with the improvement of ultra-high brightness LED performance, great power LED is expected to replace the lighting sources such as incandescent light, become the 4th generation lighting source (Wang Xiaoming, Guo Weiling, high state, etc.LED---lighting source of new generation.Modern demonstration, 2005,53,15～20).
Along with the development of great power LED, the client has proposed more and more higher requirement to the material that uses in the encapsulation process, and new material not only will satisfy the processing requirement that the client produces, and also needing simultaneously has preferably anti-UV and thermotolerance, and enough bonding strengths.Traditional epoxy conductive binding agent has excellent normal temperature adhesiveproperties, but its high temperature bonding performance is not ideal enough, in addition epoxy resin-base not anti-UV often, and under the comprehensive action of UV light and heat, thereby xanthochromia easily occurs and affects the LED luminescent lifetime in it.Therefore, Resins, epoxy is not suitable for the 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 more and more can not satisfy the performance requriements that day by day upgrades.
Polyimide resin refers to contain in minute clamp mechanism polymkeric substance of imide ring, and its structure is as follows:
The good characteristic such as polyimide resin has good high temperature resistant, radiation hardness, wet-heat resisting, modulus is high, rate of moisture absorption is low and thermal expansivity is little is widely used in field of electronics, and traditional polyimide resin rigidity is large, and cured product has color.
The silicon-oxygen backbone structure that the type siloxane tackiness agent has, structural formula is as follows:
Si-O-Si has higher bond energy, has stronger ultra-violet resistance, therefore is applicable to any ultraviolet lighting occasion.The SMP-2800L of Japan SHIN-ETSU HANTOTAI chemical industry, the single-component that Japanese Teng Cang changes into contains solvent organosilicon conductive adhesive (XA-819A of DOTITE and FX-730), is this series products.Because the polarity of the main chain of poly-silica is less, so the cementability of conductive resin described above is relatively poor, chip thrust is less than normal, room temperature small pieces thrust＜5kgf/die (2 * 2mm).
In sum, polyimide and polysiloxane respectively have advantage, and how the advantage with both is combined into the technical issues that need to address of the present invention.Both combinations can make material have resistance to elevated temperatures, anti-UV performance and excellent high temperature bonding performance concurrently.
Summary of the invention
The object of the present invention is to provide a kind of LED organic silicon polyimide dielectric adhesive, advantage combination with silicone resin and polyimide resin, the light transmission that keeps the high temperature resistant and polyorganosiloxane resin of polyimide resin also makes product have excellent adhesiveproperties simultaneously.
The objective of the invention is to be achieved through the following technical solutions:
The LED that the present invention relates to organic silicon polyimide dielectric adhesive comprises the component with following weight part:
According to the present invention, described end amido silicon 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 acid anhydrides 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 median size of described silicon-dioxide and titanium dioxide (ruby-type) filler is 100nm.
According to the present invention, described interface strengthening agent silane coupling agent is 3-glycidyl propyl trimethoxy silicane (Z6040).
LED of the present invention may further comprise the steps with the preparation method of organic silicon polyimide conductive resin:
To hold amido silicon oil, end acid anhydrides silicone oil and polyamino silicone oil mix by a certain percentage, at room temperature stir 6-8 hour, then add silicon-dioxide, titanium dioxide and interface strengthening agent silane coupling agent, use three-roll grinder to grind three times.
Compared with prior art, the present invention has following technique effect:, room temperature chip thrust＞9.3kgf/die (2 * 2mm), and high temperature chip thrust＞1.7kgf/die (2 * 2mm), transmittance＞81%; Namely this tackiness agent has good storage stability, has excellent bonding strength, thermotolerance and light transmission after the curing.
Embodiment
Below in conjunction with specific embodiment, the present invention will be further described.Should be understood that following examples are only for explanation the present invention but not for limiting the scope of the invention.
Silicon-dioxide in following examples and the median size of titanium dioxide filler are 100nm.
Embodiment 1～4
Press shown in the table 1, to hold amido silicon oil SiMNH respectively, end acid anhydrides silicone oil SiMDH and polyamino silicone oil SinNH mix by a certain percentage, at room temperature stirred 6 hours, then add silicon-dioxide, titanium dioxide and interface strengthening agent silane coupling agent, use three-roll grinder to grind three times, namely make the organic silicon polyimide dielectric adhesive.
The component of table 1, organic silicon polyimide dielectric adhesive
Adopt DAGA 4000 thrust machines, the LED that embodiment 1～4 is obtained tests with the performance of organic silicon polyimide dielectric adhesive, and the result is as shown in table 2.
The performance of table 2, organic silicon polyimide dielectric adhesive
By the result of table 2 as seen, the LED of the method preparation of employing embodiment 1～4 is 1.48～1.49 with the specific refractory power of organic silicon polyimide dielectric adhesive, second-order transition temperature is 102～112 ℃, 2 * 2mm chip thrust is 9.3～11.2kgf (25 ℃), 1.7～2.5kgf (250 ℃), and transmittance is 83%～93%.
Embodiment 5～8
Press shown in the table 3, to hold amido silicon oil SiMPNH respectively, end acid anhydrides silicone oil SiMPDH and polyamino silicone oil SinNH mix by a certain percentage, at room temperature stirred 8 hours, then add silicon-dioxide, titanium dioxide and interface strengthening agent silane coupling agent, use three-roll grinder to grind three times, namely make the organic silicon polyimide dielectric adhesive.
The component of table 3, organic silicon polyimide dielectric adhesive
Adopt DAGA 4000 thrust machines, the LED that embodiment 5～8 is obtained tests with the performance of organic silicon polyimide dielectric adhesive, and the result is as shown in table 4.
The performance of table 4, organic silicon polyimide dielectric adhesive
By the result of table 4 as seen, the LED of the method preparation of employing embodiment 5～8 is 1.53 with the specific refractory power of organic silicon polyimide dielectric adhesive, second-order transition temperature is 113～121 ℃, 2 * 2mm chip thrust is 9.4～12.3kgf (25 ℃), 1.9～2.7kgf (250 ℃), and transmittance is 81%～91%.
In conjunction with above-described embodiment, LED of the present invention organic silicon polyimide dielectric adhesive, room temperature chip thrust＞9.3kgf/die (2 * 2mm), and high temperature chip thrust＞1.7kgf/die (2 * 2mm), transmittance＞81%; Namely this tackiness agent has good storage stability, has excellent bonding strength, light transmission, thermotolerance and anti-UV after the curing.
Claims (6)
1. a LED organic silicon polyimide dielectric adhesive is characterized in that, comprises the component with following weight part:
2. dielectric adhesive according to claim 1 is characterized in that, the structural formula of described end amido silicon oil is:
Wherein, n=1～6; Or
Wherein, n=1～6.
3. dielectric adhesive according to claim 1 is characterized in that, the structural formula of described acid anhydrides silicone oil is:
Wherein, n=1～6; Or
Wherein, n=1～6.
4. dielectric adhesive according to claim 1 is characterized in that, the structural formula of described polyamino silicone oil is:
Wherein: n=1～6, m=1-6.
5. dielectric adhesive according to claim 1 is characterized in that, the median size of described silicon-dioxide and titanium dioxide filler is 100nm.
6. each described LED is characterized in that may further comprise the steps with the preparation method of organic silicon polyimide dielectric adhesive in the claim 1～5:
To hold amido silicon oil, end acid anhydrides silicone oil and polyamino silicone oil mix by a certain percentage, at room temperature stir 6-8 hour, then add silicon-dioxide, titanium dioxide and interface strengthening agent silane coupling agent, use three-roll grinder to grind three times.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201110327776.0A CN103074028B (en) | 2011-10-25 | 2011-10-25 | Organosilicon polyimide insulation adhesive for LED |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110327776.0A CN103074028B (en) | 2011-10-25 | 2011-10-25 | Organosilicon polyimide insulation adhesive for LED |
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| CN103074028A true CN103074028A (en) | 2013-05-01 |
| CN103074028B CN103074028B (en) | 2016-06-08 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104230973A (en) * | 2013-06-13 | 2014-12-24 | 达兴材料股份有限公司 | Siloxane dianhydride, polymer, liquid crystal alignment agent, liquid crystal alignment film and liquid crystal display element |
| CN109722211A (en) * | 2018-12-21 | 2019-05-07 | 东华大学 | A kind of BDADDM 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 |
| CN109722209A (en) * | 2018-12-21 | 2019-05-07 | 东华大学 | A kind of YASI organic imides silica gel 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 |
| 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 |
-
2011
- 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 |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104230973A (en) * | 2013-06-13 | 2014-12-24 | 达兴材料股份有限公司 | Siloxane dianhydride, polymer, liquid crystal alignment agent, liquid crystal alignment film and liquid crystal display element |
| JP2015000983A (en) * | 2013-06-13 | 2015-01-05 | 達興材料股▲ふん▼有限公司Ｄａｘｉｎ Ｍａｔｅｒｉａｌｓ Ｃｏｒｐｏｒａｔｉｏｎ | Siloxane diacid anhydride, polymer, liquid crystal aligning agent, liquid crystal alignment film and liquid crystal display |
| CN109722211A (en) * | 2018-12-21 | 2019-05-07 | 东华大学 | A kind of BDADDM 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 |
| CN109722209A (en) * | 2018-12-21 | 2019-05-07 | 东华大学 | A kind of YASI organic imides silica gel 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 |
| 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 |
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| CN103074028B (en) | 2016-06-08 |
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