CN102504741A - High-heat conductivity and electric conductivity die bonding adhesive for carbon nano tube-filled high-power light-emitting diode (LED) - Google Patents

High-heat conductivity and electric conductivity die bonding adhesive for carbon nano tube-filled high-power light-emitting diode (LED) Download PDF

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CN102504741A
CN102504741A CN2011103295203A CN201110329520A CN102504741A CN 102504741 A CN102504741 A CN 102504741A CN 2011103295203 A CN2011103295203 A CN 2011103295203A CN 201110329520 A CN201110329520 A CN 201110329520A CN 102504741 A CN102504741 A CN 102504741A
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high
led
carbon nanotubes
filled
die bonding
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CN2011103295203A
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Chinese (zh)
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丁磊
万超
何丽娇
曹诺
李勋平
杜彬
王宏芹
王玲
王鹏程
符永高
胡嘉琦
赵新
邓梅玲
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中国电器科学研究院有限公司
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Abstract

The invention relates to a high-heat conductivity and electric conductivity die bonding adhesive for a carbon nano tube-filled high-power light-emitting diode (LED), which belongs to the technical field of LED packaging materials, and comprises the following raw materials in weight percentage: 15-25 percent of epoxy resin, 0.5-1.5 parts of carbon nano tube, 1-2 parts of coupling agent, 1.2-2 percent of curing agent, 0.4-0.7 percent of curing accelerator and 75-80 percent of electric conduction filler. The raw materials are evenly mixed and stirred, and vacuum defoaming is performed so as to obtain the high-heat conductivity and electric conductivity die bonding adhesive for the carbon nano tube-filled high-power LED. In the high-heat conductivity and electric conductivity die bonding adhesive for the carbon nano tube-filled high-power LED, the epoxy resin with low viscosity is adopted, thereby, the system viscosity of the resin is improved, and the dispersion of the electric conduction filler is promoted, and moreover, the electric conductivity and the heat conductivity of the electrically conductive adhesive are improved through adding the carbon nano tube. The prepared electrically conductive adhesive has better electric conductivity, heat conductivity and shearing strength after being cured.

Description

一种碳纳米管填充型大功率LED用高导热导电固晶胶粘剂 A carbon nanotube filled with a high thermal conductivity power LED die bonding adhesive

技术领域 FIELD

[0001] 本发明涉及混合物型导电粘结剂,尤其是涉及一种碳纳米管填充型大功率LED用高导热导电固晶胶粘剂;适用于大功率LED固晶封装应用场合,主要起到力学固定、电气连接及导热效用。 [0001] The present invention relates to a mixture of type conductive adhesive, particularly to a carbon nanotube filled with a high thermal conductivity power LED die bonding adhesive; solid crystal suitable for high-power LED package applications, primarily as a fixed mechanical , electrical connections and thermal effects. 本发明还涉及上述胶粘剂的制备方法。 The present invention also relates to a method for preparing the adhesive.

背景技术 Background technique

[0002] LED作为一种特殊的光电子半导体器件,由于具有抗震耐冲击、光响应速度快、省电和寿命长等特点,广泛应用于各种室内、户外显示屏,汽车,背光源等方面;随功率型LED 的发展,具备节能环保特征的LED照明成为世界各国的重点发展产业之一。 [0002] LED as a special optoelectronic semiconductor device, since an impact shock resistance, the light response speed, power consumption, and long life characteristics, is widely used in a variety of indoor and outdoor displays, automotive, and other aspects of the backlight; with the development of power LED type, with energy saving features LED lighting has become one of key industries around the world. 然而当前大功率LED制造产业的共性问题是散热管理,开发高导热性能的LED固晶封装材料成为解决LED 制造产业瓶颈问题的关键技术之一。 However, common problems of current high-power LED manufacturing industry is thermal management, development of high thermal conductivity of the solid crystal LED encapsulant LED technology to solve one of the key manufacturing industry bottlenecks.

[0003] 环氧树脂具有优良的粘接性、耐热性、耐化学腐蚀性和机械强度,且价格相对便宜,在热固性树脂领域中处于主导地位。 [0003] The epoxy resin has excellent adhesion, heat resistance, chemical resistance and mechanical strength, and relatively inexpensive, in a dominant position in the field of thermosetting resins. 然而,环氧树脂作为聚合物基体使用其缺点主要是热导率低和韧性差。 However, the disadvantage of the epoxy resin used as the polymer matrix which is mainly a low thermal conductivity and poor toughness. LED产业中目前最常用的导热导电固晶胶也是环氧树脂基体的,同样存在热导率低及韧性差的特征。 LED industry, the most commonly used die attach adhesive is thermally and electrically conductive epoxy matrix, the same low thermal conductivity and flexibility characteristics difference exists.

发明内容 SUMMARY

[0004] 本发明的目的在于提供一种碳纳米管填充型大功率LED用高导热导电固晶胶粘剂,为解决大功率LED的散热问题而研发一种高导热性能、高力学性能的固晶胶粘剂。 [0004] The object of the present invention is to provide a carbon nanotube filled with a high thermal conductivity power LED die bonding adhesive, in order to solve the heat dissipation problem of developing a high-power LED and the high thermal conductivity, high mechanical performance die bonding adhesive .

[0005] 另外,本发明还涉及上述胶粘剂的制备方法。 [0005] The present invention further relates to a method for preparing the adhesive.

[0006] 本发明的目的通过以下的技术措施来实现:一种碳纳米管填充型大功率LED用高导热导电固晶胶粘剂,它包括如下质量百分比的组分: [0006] The object of the present invention is achieved by the following technical measures: A carbon nanotube filled with a high thermal conductivity power LED die bonding adhesive comprising the mass percentages of components:

环氧树脂 15 - -25%稀释剂 0. 5〜 1. 5%碳纳米管 0. 5 〜1%固化剂 1. 2 〜2%酰胺类固化促进剂 0. 4〜 0. 7%偶联剂 1〜2% 导电填料 75 - -80%将以上成分混合均勻, 真空脱泡。 Epoxy 15---25 diluent 0.5% -5 to 1.5% carbon nanotubes 0.5 1.2 ~ 1% ~ 2% hardener amide-based curing accelerator 0.5 4 ~ 0.7% coupling agent 1 ~ 2% conductive filler 75---80% the above ingredients were uniformly mixed, vacuum defoaming.

[0007] 所述的环氧树脂为双酚F型、双酚A型、脂环族环氧树脂、脂肪族缩水甘油醚类环氧树脂中的一种或共混物。 [0007] The epoxy resin is a bisphenol F type, bisphenol A type, alicyclic epoxy resins, aliphatic ether type epoxy resin or a blend of one.

[0008] 所述的双酚F型环氧树脂为双酚F170或双酚F862等。 [0008] The epoxy resin is bisphenol F type bisphenol or bisphenol F170 F862 like.

[0009] 所述的碳纳米管为单壁或多壁碳纳米管。 [0009] The single-walled carbon nanotubes or multi-walled carbon nanotubes.

[0010] 所述的稀释剂为乙二醇丁醚、二乙二醇己醚等。 [0010] The diluent is ethylene glycol butyl ether, diethylene glycol hexyl ether.

[0011] 所述的偶联剂为硅烷类偶联剂KH550、KH560或KH570。 [0011] The coupling agent is a silane coupling agent KH550, KH560 or KH570. [0012] 所述的固化剂为咪唑类固化剂、双氰胺或酸酐类固化剂。 Curing Agent [0012] the curing agent is an imidazole, dicyandiamide or acid anhydride curing agent.

[0013] 所述的导电填料为银粉及银合金粉的共混物。 [0013] The conductive filler is silver powder or silver alloy powder blend.

[0014] 所述的银粉为片状银粉,粒径为2〜5μπι。 [0014] The silver flake silver powder is a particle size of 2~5μπι.

[0015] 本发明的另一个目的,通过以下的技术措施实现,上述胶粘剂的制备方法:包括: (1)将多壁碳纳米管置于酸溶液中,在50°C下于超声波中振荡10-1¾,接着用2倍酸溶液体积的去离子水进行稀释,利用离心机过滤出多壁碳纳米管,并用去离子水洗至中性,然后在80°C下真空干燥20-2¾,得到的表面处理后的碳纳米管产物; [0015] Another object of the present invention, implemented by the following technical measures, the preparation method of the adhesive: comprising: (1) Multi-walled carbon nanotubes placed in the acid solution in an ultrasonic oscillation at 50 ° C 10 -1¾, followed by deionized water with 2 volumes of dilute acid solution, filtered off using a centrifuge carbon nanotubes, and washed with deionized water until neutral, then dried in vacuo 20-2¾ at 80 ° C, to give the surface-treated carbon nano tube products;

(2)将上述处理后的碳纳米管加入到树脂基体中,利用离心消泡机进行充分搅拌均勻。 (2) the process after the carbon nanotube is added to the resin matrix, a centrifugal defoaming machine stir. 添加其他成分,充分搅拌均勻并真空脱泡。 Adding other ingredients, and stir to vacuum defoaming.

[0016] 本发明所述的制备方法,所述碳纳米管在偶联剂KH560试剂中浸泡20-M小时后, 再加入到树脂基体中。 After the preparation method of [0016] the present invention, the carbon nanotubes are immersed in a coupling reagent 20-M KH560 hours, then added to the resin matrix. 所述多壁碳纳米管和混合酸的重量体积比为1:1。 Weight to volume ratio of the MWNTs and the mixed acid is 1: 1.

[0017] 本发明首先对碳纳米管进行表面功能化处理,然后将处理后的碳纳米管加入到含有一定稀释剂的环氧树脂基体中,利用离心机进行充分搅拌,进而添加固化剂、促进剂、偶联剂及银粉等组分,进行充分搅拌,确保碳纳米管在聚合物中的均勻分散,充分发挥其优异性能,制备出高导热高韧性的导电胶。 [0017] First, the present invention features carbon nanotubes subjected to a surface treatment, and then added to the carbon nanotubes treated epoxy resin matrix containing some diluent, sufficiently stirred by using a centrifuge, and then adding a curing agent to promote agents, coupling agents and silver powder components were thoroughly stirred to ensure uniform dispersion of carbon nanotubes in the polymer, give full play to their excellent performance, a high thermal conductive adhesive to prepare a high toughness. 其在150°c下固化lh,体积电阻率彡10_4Ω. cm,剪切拉伸强度大于12. OMpa的导电胶,导热系数大于20W/M°C,适用于对导热导电有较高要求的LED封装场合。 Which is 150 ° c LH curing, the volume resistivity San 10_4Ω. Cm, a shear tensile strength greater than 12. OMpa conductive paste, thermal conductivity greater than 20W / M ° C, is suitable for an LED to have a relatively high electrical and thermal conductivity requirements packaging applications.

[0018] 具体实例方式 [0018] Specific examples of the way

为了更好地理解本发明,下面结合实例进一步阐明本发明的内容,但本发明不仅仅局限于下面的实施例。 For a better understanding of the present invention, the following examples in conjunction with the present invention is further illustrated, but the present invention is not limited to the following examples.

[0019] 实施例1 : [0019] Example 1:

将IOOmg的多壁碳纳米管置于IOOml的70%浓硫酸和70%浓硝酸形成的混合酸中(V 浓硫酸:V浓硝酸=3:1),在501:下于100W超声波中振荡12h,接着用200ml去离子水进行稀释,利用离心机过滤出多壁碳纳米管,并用去离子水洗至中性,然后在80°C下真空干燥Mh,得到的表面处理后的碳纳米管产物。 Multi-walled carbon nanotube was placed IOOmg mixed acid formed of 70% concentrated sulfuric acid and 70% concentrated nitric acid in IOOml (V concentrated sulfuric acid: concentrated nitric acid V = 3: 1), 501: shaken under a 100W ultrasonic 12h , followed by 200ml of deionized water for dilution, using a centrifuge filtered carbon nanotubes, and washed with deionized water until neutral, then dried in vacuo Mh at 80 ° C, the product was obtained carbon nanotubes surface-treated. 按以下重量的组分: The following components by weight:

双酚F170 16g Bisphenol F170 16g

乙二醇丁醚 0. 7 g 0. 7 g ethylene glycol butyl ether

多壁碳纳米管 0. 5 g MWCNTs 0. 5 g

双氰胺 1. 2 g 1. 2 g of dicyandiamide

酰胺类固化促进剂 0.6 g Amide-based curing accelerator 0.6 g

偶联剂KH560 1 g Coupling agent KH560 1 g

片状银粉 80 g 80 g silver flake

将乙二醇丁醚和双酚F170混合,上述处理后的多壁碳纳米管加入到混合后的双酚F170树脂基体中,利用离心消泡机进行充分搅拌均勻。 F170 bisphenol resin matrix after the mixing ethylene glycol butyl ether and bisphenol F170, multiwall carbon nanotubes were added to the above-described mixing process, a centrifugal defoaming machine stir. 继续依次添加其他各个组分双氰胺、 酰胺类固化促进剂、偶联剂KH560、粒径为2〜5 μ m的片状银粉,充分搅拌均勻并真空脱泡, 然后在150°C下固化lh,测得体积电阻率为4. 9 X 10_4 Ω . cm,剪切拉伸强度为12. 5Mpa,导热系数为23W/M°C。 Continue to add various other components sequentially dicyandiamide, amide-based curing accelerator, coupling of KH560, 2~5 μ m particle size of the silver flake, fully stirred and defoamed under vacuum, and then cured at 150 ° C for lh, the volume resistivity was measured to 4. 9 X 10_4 Ω. cm, a tensile shear strength was 12. 5Mpa, a thermal conductivity of 23W / M ° C. [0020] 实施例2 : [0020] Example 2:

将200mg的多壁碳纳米管置于200ml的70%浓硝酸中,在50°C下于100W超声波中振荡10h,接着用400ml去离子水进行稀释,利用离心机过滤出多壁碳纳米管,并用去离子水洗至中性,然后在80°C下真空干燥20h,得到的表面处理后的碳纳米管产物。 Multi-walled carbon nanotube was placed in 200ml of 200mg of 70% concentrated nitric acid and shaken at 50 ° C for 10H 100W ultrasonic waves, followed by dilution with 400ml of deionized water, filtered using a centrifuge MWCNT with deionized water until neutral, and then dried 20h under vacuum at 80 ° C, the product was obtained carbon nanotubes surface-treated. 按以下重量的 In the following weight

组分: Components:

MM F862 20g MM F862 20g

乙二醇丁醚 1. 2 g 1. 2 g of ethylene glycol monobutyl ether

多壁碳纳米管 1. 0 g MWCNTs 1. 0 g

双氰胺 1. 2 g 1. 2 g of dicyandiamide

酰胺类固化促进剂 0.6 g Amide-based curing accelerator 0.6 g

偶联剂KH560 1 g Coupling agent KH560 1 g

片状银粉 75 g 75 g of silver flake

将乙二醇丁醚和双酚F862混合,上述处理后的多壁碳纳米管加入到混合后双酚F862 树脂基体中,利用离心消泡机进行充分搅拌均勻。 The mixed ethylene glycol butyl ether and bisphenol F862, multiwall carbon nanotubes were added to the above-described processing after F862 bisphenol mixed in a resin matrix, a centrifugal defoaming machine stir. 继续依次添加其他各个组分双氰胺、酰胺类固化促进剂、偶联剂KH560、粒径为2〜5 μ m的片状银粉,充分搅拌均勻并真空脱泡,然后在150°C下固化lh,测得体积电阻率为5. 9X 10_4Ω . cm,剪切拉伸强度为13. 5Mpa,导热系数为21W/M°C。 Continue to add various other components sequentially dicyandiamide, amide-based curing accelerator, coupling of KH560, 2~5 μ m particle size of the silver flake, fully stirred and defoamed under vacuum, and then cured at 150 ° C for lh, the volume resistivity was measured to 5. 9X 10_4Ω. cm, a tensile shear strength was 13. 5Mpa, a thermal conductivity of 21W / M ° C. [0021] 实施例3: [0021] Example 3:

将IOOmg的多壁碳纳米管置于IOOml的70%浓硫酸中,在100W超声波作用下于90°C处理15h,接着用200ml去离子水进行稀释,利用离心机过滤出多壁碳纳米管,并用去离子水洗至中性,然后在80°C下真空干燥25h,得到的表面处理后的碳纳米管产物。 The multiwall carbon nanotubes IOOmg 70% concentrated sulfuric acid was placed in IOOml at 100W ultrasonic treatment at 90 ° C 15h, then diluted with 200ml of deionized water, filtered using a centrifuge MWCNT with deionized water until neutral, and then dried 25h under vacuum at 80 ° C, the product was obtained carbon nanotubes surface-treated. 按以下重量的组分: The following components by weight:

脂环族环氧树脂TDE- -85 18g二乙二醇己醚 0.7 g多壁碳纳米管 0.5 g双氰胺 1.2g酰胺类固化促进剂 0. 6g偶联剂KH560 Ig片状银粉 78g Alicyclic epoxy resins TDE- -85 18g diethylene glycol hexyl ether 0.7 g 0.5 g MWCNTs amides 1.2g dicyandiamide curing accelerator 0. 6g coupling KH560 Ig flake silver 78g

将二乙二醇己醚和TDE-85混合,上述处理过的多壁碳纳米管加入到混合后TDE-85树脂基体中,利用离心消泡机进行充分搅拌均勻。 Mixing the diethylene glycol hexyl ether, and TDE-85, the above-treated MWCNTs TDE-85 was added to the resin matrix after mixing, a centrifugal defoaming machine stir. 继续依次添加其他各个组分双氰胺、酰胺类固化促进剂、偶联剂KH560、粒径为2〜5 μ m的片状银粉,充分搅拌均勻并真空脱泡,然后在150°C下固化lh,测得体积电阻率为5. 4Χ10_4Ω. cm,剪切拉伸强度为12. 5Mpa,导热系数为20ff/M°C。 Continue to add various other components sequentially dicyandiamide, amide-based curing accelerator, coupling of KH560, 2~5 μ m particle size of the silver flake, fully stirred and defoamed under vacuum, and then cured at 150 ° C for lh, a volume resistivity was measured 5. 4Χ10_4Ω. cm, a tensile shear strength was 12. 5Mpa, thermal conductivity 20ff / M ° C.

[0022] 实施例4 : [0022] Example 4:

将150mg的多壁碳纳米管置于150ml的70%浓硝酸中,在100W超声波作用下于90°C 处理15h,接着用300ml去离子水进行稀释,利用离心机过滤出多壁碳纳米管,并用去离子水洗至中性,然后在80°C下真空干燥Mh。 The multiwall carbon nanotubes 150mg of 70% was placed in 150ml of concentrated nitric acid, treated at 100W ultrasonic waves at 90 ° C 15h, followed by dilution 300ml of deionized water, filtered using a centrifuge MWCNT with deionized water until neutral, then dried in vacuo Mh at 80 ° C. 为了让碳纳米管更好分散,将干燥的碳纳米管在偶联剂KH560试剂中浸泡20-M小时后(该浸泡用的偶联剂KH560不是指组分中的偶联剂KH560)取出,得到的表面处理后的碳纳米管产物。 To give a better dispersion of the carbon nanotubes, the carbon nanotubes was immersed in dried coupling reagent 20-M KH560 hours (soaked in the coupling agent does not refer KH560 KH560 coupling component) is removed, the product obtained after the carbon nanotube surface-treated.

[0023] 按以下重量的组分:双酚F862 [0023] by weight of the following components: bisphenol F862

二乙二醇己醚多壁碳纳米管双氰胺 Diethylene glycol hexyl ether MWCNTs dicyandiamide

酰胺类固化促进剂偶联剂KH560 片状银粉 Amide-based curing accelerator flake silver coupling KH560

19g 0. 5g 1.2g 1.2g 0. 6g 0. 5g 77g 19g 0. 5g 1.2g 1.2g 0. 6g 0. 5g 77g

将二乙二醇己醚和双酚F862混合,上述处理过的多壁碳纳米管加入到混合后双酚F862树脂基体中,利用离心消泡机进行充分搅拌均勻。 After diethylene glycol hexyl ether, and bisphenol F862 mixing the treated MWCNTs added to a mixture of bisphenol F862 resin matrix, a centrifugal defoaming machine stir. 继续依次添加其他各个组分双氰胺、 酰胺类固化促进剂、偶联剂KH560、粒径为2〜5 μ m的片状银粉,充分搅拌均勻并真空脱泡, 然后在150°C下固化lh,测得体积电阻率为3. 4X ΙΟ"4 Ω . cm,剪切拉伸强度为15. 5Mpa,导热系数为。 Continue to add various other components sequentially dicyandiamide, amide-based curing accelerator, coupling of KH560, 2~5 μ m particle size of the silver flake, fully stirred and defoamed under vacuum, and then cured at 150 ° C for lh, the volume resistivity was measured as 3. 4X ΙΟ "4 Ω. cm, a tensile shear strength was 15. 5Mpa, thermal conductivity.

[0024] 上述实施例为本发明较佳的实施方式,但本发明的实施方式并不受上述实施例的限制,如环氧树脂还可为双酚F型、双酚A型、脂肪族缩水甘油醚类环氧树脂中的一种或共混物;碳纳米管还可为单壁壁碳纳米管;偶联剂还可为硅烷类偶联剂KH550、KH570、或钛酸酯类偶联剂;固化剂还可为咪唑类固化剂、或酸酐类固化剂;导电填料还可为银合金粉的共混物。 [0024] The preferred embodiment of the present invention embodiment, but the embodiment of the present invention is not limited to the above embodiments, the epoxy resin may also be a bisphenol F type, bisphenol A type, glycidyl aliphatic epoxy ethers of glycerol or a blend; single-walled carbon nanotube may also walled carbon nanotubes; coupling agent may also be a silane coupling agent KH550, KH570, or a titanate-based coupling agent; imidazole curing agent as a curing agent may also, or an acid anhydride curing agent; conductive fillers may also be a silver alloy powder blend. 其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化,均应为等效的置换方式,都包含在本发明的保护范围。 Other changes made under the spirit and principle of Any without departing from the present invention, modifications, substitutions, combinations, simplification of the replacement pattern of equivalent effect, are included in the scope of the present invention.

Claims (10)

1. 一种碳纳米管填充型大功率LED用高导热导电固晶胶粘剂,特征在于它包括如下质量百分比的组分:环氧树脂 15 - -25%稀释剂 0. 5〜 1. 5%碳纳米管 0. 5 〜1%固化剂 1. 2 〜2%酰胺类固化促进剂 0. 4 - -0. 7%偶联剂 1〜 2%导电填料 75 〜80%将以上混合均勻,真空脱泡,即得。 A carbon nanotube filled with a high thermal conductivity power LED die bonding adhesive, characterized in that it comprises the following mass percent composition: Epoxy 15---25 diluent 0.5% -5 to 1.5% carbon 0.5 ~ 1% of nanotubes curing agent 1.2 ~ 2% amide-based curing accelerator 0.4 - -07% coupling agent 1 ~ 2% 75 ~ 80% conductive filler mixed more uniformly, vacuum degassing bubble, that is, too.
2.根据权利要求1所述的一种碳纳米管填充型大功率LED用高导热导电固晶胶粘剂, 其特征在于:所述的环氧树脂为双酚F型、双酚A型、脂环族环氧树脂、脂肪族缩水甘油醚类环氧树脂中的一种或其共混物。 The carbon nanotube-filled power LED with highly thermally conductive die attach adhesive according to claim 1, wherein: said epoxy resin is a bisphenol F type, bisphenol A type, an alicyclic aromatic epoxy resin, an aliphatic ether type epoxy resin of one or blends thereof.
3.根据权利要求2所述的一种碳纳米管填充型大功率LED用高导热导电固晶胶粘剂, 其特征在于:所述的双酚F型环氧树脂为双酚F170或双酚F862树脂。 3. The carbon nanotube-filled high power LED with highly thermally conductive die attach adhesive according to claim 2, wherein: said epoxy resin is bisphenol F type bisphenol or bisphenol F170 F862 resin .
4.根据权利要求1所述的一种碳纳米管填充型大功率LED用高导热导电固晶胶粘剂, 其特征在于:所述的偶联剂为硅烷类偶联剂KH550、KH560或KH570。 The carbon nanotube-filled power LED with highly thermally conductive die attach adhesive according to claim 1, wherein: said coupling agent is a silane coupling agent KH550, KH560 or KH570.
5.根据权利要求1所述的一种碳纳米管填充型大功率LED用高导热导电固晶胶粘剂, 其特征在于:所述的固化剂为咪唑类固化剂、双氰胺或酸酐类固化剂。 The bulking power of the carbon nanotubes with high thermal conductivity 1 LED die bonding adhesive claim, wherein: said curing agent is an imidazole curing agent, dicyandiamide or an acid anhydride type curing agent .
6.根据权利要求1所述的一种碳纳米管填充型大功率LED用高导热导电固晶胶粘剂, 其特征在于:所述的导电填料为银粉,所述的银粉为片状银粉,粒径为2〜5μπι。 The bulking power of the carbon nanotubes with high thermal conductivity 1 LED die bonding adhesive claim, wherein: said conductive filler is silver powder, the silver powder is silver flake particle size as 2~5μπι.
7.根据权利要求7所述的一种碳纳米管填充型大功率LED用高导热导电固晶胶粘剂, 其特征在于:所述的碳纳米管为单壁或多壁碳纳米管。 According to claim power A carbon nanotube filled with a high thermal conductivity LED die bonding adhesive of claim 7, wherein: the carbon nanotubes are single-walled or multi-walled carbon nanotubes.
8.权利要求1所述一种碳纳米管填充型大功率LED用高导热导电固晶胶粘剂的制备方法,其特征在于:(1)将多壁碳纳米管置于酸溶液中,在50°C下于超声波中振荡10-1¾,接着用2倍酸溶液体积的去离子水进行稀释,利用离心机过滤出多壁碳纳米管,并用去离子水洗至中性,然后在80°C下真空干燥20-2¾,得到的表面处理后的碳纳米管产物;(2)将上述处理后的碳纳米管加入到树脂基体中,利用离心消泡机进行充分搅拌均勻, 添加其他成分,充分搅拌均勻并真空脱泡。 Claim 8. A method for producing a high-power LED is filled with a highly thermally conductive die attach adhesive carbon nanotube, characterized in that: (1) Multi-walled carbon nanotubes to be placed in an acid solution, at 50 ° C under ultrasonic shaking in 10-1¾, then was diluted with deionized water two times the volume of the acid solution, filtered off using a centrifuge carbon nanotubes, and washed with deionized water until neutral, and then vacuum at 80 ° C for drying 20-2¾, the carbon nanotubes obtained product was treated surface; (2) the process after the carbon nanotube is added to the resin matrix, a centrifugal defoaming machine, stir, add the other ingredients, stir and vacuum degassing.
9.根据权利要求8所述的制备方法,其特征在于:所述碳纳米管在偶联剂KH560试剂中浸泡20-M小时后,再加入到树脂基体中。 9. A method of preparation according to claim 8, wherein: the carbon nanotubes after immersion in KH560 coupling reagent 20-M h, then added to the resin matrix.
10.根据权利要求8所述的制备方法,其特征在于:所述多壁碳纳米管和混合酸的重量体积比为1:1。 10. The production method according to claim 8, wherein: the weight ratio of multi-walled carbon nanotubes by volume and mixed acid is 1: 1.
CN2011103295203A 2011-10-26 2011-10-26 High-heat conductivity and electric conductivity die bonding adhesive for carbon nano tube-filled high-power light-emitting diode (LED) CN102504741A (en)

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CN103805118A (en) * 2014-02-21 2014-05-21 厦门大学 Compound conductive adhesive for electronic packaging and preparation method thereof
CN103805118B (en) * 2014-02-21 2015-01-07 厦门大学 Compound conductive adhesive for electronic packaging and preparation method thereof
CN104599740A (en) * 2015-01-08 2015-05-06 安徽凤阳德诚科技有限公司 Conductive silver paste with nanocarbon
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CN105802531A (en) * 2016-04-15 2016-07-27 安庆市晶科电子有限公司 Electric-heating flame-retardant conductive silver adhesive for circuit board
CN105860901A (en) * 2016-06-08 2016-08-17 蚌埠市正园电子科技有限公司 Composite carbon nano tube filled and modified epoxy pouring sealant for LED display screen

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