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CN107189447A - LED packaging silicon rubbers of wet-heat resisting and its preparation method and application - Google Patents

LED packaging silicon rubbers of wet-heat resisting and its preparation method and application Download PDF

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CN107189447A
CN107189447A CN201710566871.3A CN201710566871A CN107189447A CN 107189447 A CN107189447 A CN 107189447A CN 201710566871 A CN201710566871 A CN 201710566871A CN 107189447 A CN107189447 A CN 107189447A
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silicone resin
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CN107189447B (en
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肖少岗
韩小兵
蔡国章
郑长利
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Guangzhou Hui Li Electron Material Co Ltd
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    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
    • C08L83/04Polysiloxanes
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    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/08Macromolecular additives
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • C09J183/00Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
    • C09J183/04Polysiloxanes
    • HELECTRICITY
    • H10SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10HINORGANIC LIGHT-EMITTING SEMICONDUCTOR DEVICES HAVING POTENTIAL BARRIERS
    • H10H20/00Individual inorganic light-emitting semiconductor devices having potential barriers, e.g. light-emitting diodes [LED]
    • H10H20/80Constructional details
    • H10H20/85Packages
    • H10H20/852Encapsulations
    • H10H20/854Encapsulations characterised by their material, e.g. epoxy or silicone resins
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    • C08L2201/08Stabilised against heat, light or radiation or oxydation
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  • Led Device Packages (AREA)
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Abstract

本发明涉及一种耐湿热的LED封装硅胶及其制备方法和应用,属于材料化学技术领域。该耐湿热的LED封装硅胶由A组分和B组分构成,其中,A部分包括:甲基苯基乙烯基硅树脂、铂金催化剂、加成型增粘剂;B部分包括:甲基苯基乙烯基硅树脂、甲基苯基含氢硅树脂、反应抑制剂。该耐湿热的LED封装硅胶,通过选用特定的原料相互配合,得到了耐湿热的LED封装硅胶,提高了SMD器件的耐湿热性能,解决了SMD器件储存过程中吸潮,在无铅回流焊制程中时易裂胶和脱胶的问题,进而降低了风险,提高了生产效率。

The invention relates to heat-and-humidity-resistant LED packaging silica gel, a preparation method and application thereof, and belongs to the technical field of material chemistry. The heat-and-humidity-resistant LED encapsulation silicone is composed of component A and component B, wherein part A includes: methyl phenyl vinyl silicone resin, platinum catalyst, and addition type tackifier; part B includes: methyl phenyl vinyl Base silicone resin, methyl phenyl hydrogen silicone resin, reaction inhibitor. The heat and humidity resistant LED packaging silica gel, through the selection of specific raw materials to cooperate with each other, has obtained the heat and humidity resistant LED packaging silica gel, which improves the heat and humidity resistance of SMD devices and solves the problem of moisture absorption in the storage process of SMD devices and the lead-free reflow soldering process. The problem of easy cracking and degumming in the medium and long term reduces the risk and improves the production efficiency.

Description

耐湿热的LED封装硅胶及其制备方法和应用Moisture and heat resistant LED encapsulation silica gel and its preparation method and application

技术领域technical field

本发明涉及材料化学技术领域,特别是涉及一种耐湿热的LED封装硅胶及其制备方法和应用。The invention relates to the technical field of material chemistry, in particular to a heat-and-humidity-resistant LED packaging silica gel and a preparation method and application thereof.

背景技术Background technique

目前,目前商业化的LED照明器件很大一部分是采用SMD(表面贴装式)的封装形式,而高折LED硅树脂具有优异的透明性、耐热性及抗UV老化性,因此成为SMD器件主要的封装材料。At present, a large part of the current commercialized LED lighting devices are packaged in SMD (Surface Mount Type), and high-fold LED silicone resin has excellent transparency, heat resistance and UV aging resistance, so it has become a popular choice for SMD devices. The main packaging material.

然而,在实际应用过程中,SMD器件在使用高折硅树脂封装完成后,因密封性或封装材料的吸湿性和气体透过性,在储存过程中难免会吸收水汽,而SMD器件需要贴装在PCB电路板上,在无铅回流焊制程中,吸潮的SMD器件极易发生胶体破裂及脱离现象,从而使封装结构遭到破坏。However, in the actual application process, after the SMD device is packaged with high-fold silicone resin, due to the sealing property or the hygroscopicity and gas permeability of the packaging material, it will inevitably absorb water vapor during the storage process, and the SMD device needs to be mounted. On the PCB circuit board, in the lead-free reflow soldering process, the moisture-absorbing SMD devices are prone to colloidal cracking and detachment, which will damage the packaging structure.

发明内容Contents of the invention

基于此,有必要针对上述问题,提供一种耐湿热的LED封装硅胶,采用该耐湿热的LED封装硅胶,提高了SMD器件的耐湿热性能,解决了SMD器件储存过程中吸潮,在无铅回流焊制程中时易裂胶和脱胶的问题,进而降低了风险,提高了生产效率。Based on this, it is necessary to address the above problems and provide a heat-and-humidity-resistant LED packaging silica gel, which improves the heat-and-moisture resistance of SMD devices and solves the problem of moisture absorption in the storage process of SMD devices. The problem of easy cracking and degumming during the reflow soldering process reduces the risk and improves production efficiency.

一种耐湿热的LED封装硅胶,由A组分和B组分构成,A kind of heat and humidity resistant LED encapsulation silicone, composed of A component and B component,

所述A组分由以下重量百分比的原料制备而成:The A component is prepared from the following raw materials in weight percentage:

甲基苯基乙烯基硅树脂 40%-60%Methylphenyl vinyl silicone resin 40%-60%

铂金催化剂 0.0002%-0.002%Platinum catalyst 0.0002%-0.002%

加成型增粘剂 0.1%-5%Additive tackifier 0.1%-5%

所述B组分主要由以下重量百分比的原料制备而成:The B component is mainly prepared from the following raw materials in weight percentage:

甲基苯基乙烯基硅树脂 10%-40%Methylphenyl vinyl silicone resin 10%-40%

甲基苯基含氢硅树脂 10%-45%Methylphenyl hydrogen silicone resin 10%-45%

反应抑制剂 0.01%-0.2%Reaction inhibitor 0.01%-0.2%

所述A组分和B组分原料总和为100%。The sum of the A component and B component raw materials is 100%.

上述耐湿热的LED封装硅胶,选择特定结构的甲基苯基乙烯基硅树脂,可保证MDT型苯基乙烯基硅树脂固化物的强度和柔韧性并降低固化物的吸湿性;并且,选择硅硼型增粘剂,主要作用是提高胶体与基材之间的粘结力,上述硅硼型增粘剂是在固化过程中极大的提高与PPA和镀银金属的粘接力,尤其是在一段高温烘烤之后如一个标准的烘烤条件170℃/3hrs,硅硼型增粘剂的加入提高了胶体与基材之间的密封性,减少了水汽由胶体与基材之间的界面进入SMD器件的可能性;且配合MDT型甲基苯基含氢硅树脂,可保证固化物的交联密度,又可以提升韧性,降低固化物的吸湿性。For the above heat and humidity resistant LED packaging silica gel, select a methylphenyl vinyl silicone resin with a specific structure, which can ensure the strength and flexibility of the cured product of the MDT type phenyl vinyl silicone resin and reduce the hygroscopicity of the cured product; and, choose silicon The main function of boron-type tackifier is to improve the cohesive force between the colloid and the substrate. The above-mentioned silicon-boron-type tackifier greatly improves the bonding force with PPA and silver-plated metal during the curing process, especially After a period of high-temperature baking, such as a standard baking condition of 170°C/3hrs, the addition of silicon-boron tackifier improves the sealing between the colloid and the substrate, and reduces the water vapor from the interface between the colloid and the substrate. Possibility of entering SMD devices; and with MDT type methyl phenyl hydrogen silicone resin, it can ensure the cross-linking density of the cured product, improve the toughness and reduce the hygroscopicity of the cured product.

在其中一个实施例中,所述A组分由以下重量百分比的原料制备而成:In one of the embodiments, the A component is prepared from the following raw materials in weight percent:

甲基苯基乙烯基硅树脂 45%-55%Methylphenyl vinyl silicone resin 45%-55%

铂金催化剂 0.0004%-0.001%Platinum catalyst 0.0004%-0.001%

加成型增粘剂 1%-3%Additive tackifier 1%-3%

所述B组分主要由以下重量百分比的原料制备而成:The B component is mainly prepared from the following raw materials in weight percentage:

甲基苯基乙烯基硅树脂 15%-35%Methylphenyl vinyl silicone resin 15%-35%

甲基苯基含氢硅树脂 25%-45%Methylphenyl hydrogen silicone resin 25%-45%

反应抑制剂 0.05%-0.1%。Reaction inhibitor 0.05%-0.1%.

上述甲苯苯基乙烯基硅树脂在配方中的添加量优选为45%-55%,甲基苯基乙烯基硅树脂的添加量依据SiH/Vi的比例确定,SiH/vi值在1-2.0之间,当甲基苯基含氢硅树脂含量过低时,得不到一个期望的硬度,而当甲基苯基含氢硅树脂含量过高时,可能会影响胶液的固化。The addition amount of the above-mentioned toluene phenyl vinyl silicone resin in the formula is preferably 45%-55%, the addition amount of the methyl phenyl vinyl silicone resin is determined according to the ratio of SiH/Vi, and the SiH/vi value is between 1-2.0 Meanwhile, when the content of the methylphenyl hydrogen-containing silicone resin is too low, a desired hardness cannot be obtained, and when the content of the methylphenyl hydrogen-containing silicone resin is too high, the curing of the glue may be affected.

铂金催化剂的添加量过少时,固化时间延长,固化程度不完全,当添加量过大时,固化物可能会产生黄变现象,由此导致透明度下降,将其添加量控制在上述范围内,具有较佳的效果。When the amount of platinum catalyst added is too small, the curing time will be prolonged and the degree of curing will be incomplete. better effect.

加成型增粘剂的添加量优选为1%-2%,当添加量过少时起不到应有的粘接效果,当添加量过多时,会影响胶体的透明性及胶液的固化。The addition amount of the addition-type tackifier is preferably 1%-2%. When the amount is too small, the proper bonding effect cannot be achieved. When the amount is too much, the transparency of the colloid and the curing of the glue will be affected.

而混合后为使得胶水有较长的使用周期和粘度稳定性,选择加入反应抑制剂,且添加量范围0.01%~0.2%,当添加量过少时,起不到良好的抑制效果,当添加量过多时,胶体的固化时间延长,固化程度降低,得不到期望的硬度,添加量优选为0.05%~0.1%。After mixing, in order to make the glue have a longer service life and viscosity stability, a reaction inhibitor is selected to be added, and the added amount ranges from 0.01% to 0.2%. When the added amount is too small, a good inhibitory effect cannot be achieved. If it is too much, the curing time of the colloid will be prolonged, the degree of curing will be reduced, and the desired hardness cannot be obtained. The added amount is preferably 0.05% to 0.1%.

在其中一个实施例中,所述甲基苯基乙烯基硅树脂具有如下化学式:In one of the embodiments, the methylphenyl vinyl silicone resin has the following chemical formula:

(PhSiO3/2)a(Ph2SiO2/2)b(Me2SiO2/2)c(ViMe2SiO1/2)d(PhSiO 3/2 )a(Ph 2 SiO 2/2 )b(Me 2 SiO 2/2 )c(ViMe 2 SiO 1/2 )d

其中,a+b+c+d=1,并且0<a<0.6,0<b<0.4,0<C<0.4,0<d<0.3;Wherein, a+b+c+d=1, and 0<a<0.6, 0<b<0.4, 0<C<0.4, 0<d<0.3;

所述甲基苯基含氢硅树脂具有如下化学式:The methylphenyl hydrogen-containing silicone resin has the following chemical formula:

(PhSiO3/2)a(Ph2SiO2/2)b(HMe2SiO1/2)c(PhSiO 3/2 )a(Ph 2 SiO 2/2 )b(HMe 2 SiO 1/2 )c

其中,a+b+c=1 0<a<0.5,0<b<0.4,0<C<0.4;Among them, a+b+c=1 0<a<0.5, 0<b<0.4, 0<C<0.4;

所述加成型增粘剂选自硅硼型加成型增粘剂,具有以下结构:The addition type tackifier is selected from silicon boron type addition type tackifier, has the following structure:

CH2OCHCH3H6(CH3O)2Si0(Ph2SiO2/2)a(MeSiO2/2)b(BO3/2)cOSi(OCH3)2CH2OCHCH3H6,其中0<a<0.7,0<b<0.3,0<c<0.1CH 2 OCHCH 3 H 6 (CH 3 O) 2 Si0(Ph 2 SiO 2 /2)a(MeSiO 2 /2)b(BO 3 /2)cOSi(OCH 3 ) 2 CH 2 OCHCH 3 H 6 , where 0 <a<0.7, 0<b<0.3, 0<c<0.1

当硅硼型增粘剂中硼含量过高时,可能会导致在空气中潮解的问题,因此,控制(BO3/2)c单元的摩尔百分率在0<c<0.1,When the boron content in the silicon-boron type tackifier is too high, it may cause the problem of deliquescence in the air. Therefore, the molar percentage of the (BO 3 /2)c unit is controlled at 0<c<0.1,

由Ph为苯基、Me为甲基、Vi为乙烯基、Si为硅、O为氧、H为氢,a、b、c、d代表结构单元在大分子中的平均摩尔百分率。Ph is phenyl, Me is methyl, Vi is vinyl, Si is silicon, O is oxygen, H is hydrogen, and a, b, c, d represent the average mole percentage of structural units in macromolecules.

在其中一个实施例中,所述LED封装硅胶中,SiH/Vi的摩尔比为1-2。优选1.2-1.5。当SiH/vi当在此范围时,固化反应最完全(固化物中残留的可反应基团最小),表现出最优性能,并且固化物的吸湿性降低,湿气阻隔性能提高。In one of the embodiments, the molar ratio of SiH/Vi in the LED packaging silica gel is 1-2. Preferably 1.2-1.5. When SiH/vi is in this range, the curing reaction is the most complete (residual reactive groups in the cured product are the smallest), showing optimal performance, and the hygroscopicity of the cured product is reduced, and the moisture barrier performance is improved.

在其中一个实施例中,所述甲基苯基含氢硅树脂中,0.2<a<0.45,0.1<b<0.25,0.1<C<0.35,且(HMe2SiO1/2)基团为封端基团。所述甲基苯基含氢硅树脂为MDT型结构,分子链呈支化状,结构中“T”(PhSiO3/2)链节起到补强作用,“D”(Ph2SiO2/2)链节则提供“柔性”链段以提高柔韧性,并且D链节中侧端为苯基,提高了空间位阻效应,有效提高了湿气阻隔性,“T”链节的摩尔百分率在0-50%之间,优选为20%~45%,“D”链节的摩尔百分率在0%~40%之间,优选为10%-25%,M链节为含氢官能团,其摩尔百分率为0~40%,优选为10%~35%,尤其是M链节为封端基团,每个分子链中至少含有2个M单元。In one embodiment, in the methylphenyl hydrogen-containing silicone resin, 0.2<a<0.45, 0.1<b<0.25, 0.1<C<0.35, and the (HMe 2 SiO 1/2 ) group is an encapsulating end group. The methylphenyl hydrogen-containing silicone resin has an MDT structure, and the molecular chain is branched. In the structure, the "T" (PhSiO 3/2 ) chain links play a reinforcing role, and the "D" (Ph 2 SiO 2/ 2) The chain link provides a "flexible" segment to improve flexibility, and the side end of the D chain link is a phenyl group, which improves the steric hindrance effect and effectively improves the moisture barrier property. The molar percentage of the "T" link Between 0-50%, preferably 20%-45%, the molar percentage of "D" chain link is between 0%-40%, preferably 10%-25%, the M chain link is a hydrogen-containing functional group, its The molar percentage is 0-40%, preferably 10%-35%, especially the M chain section is a capping group, and each molecular chain contains at least 2 M units.

在其中一个实施例中,所述甲基苯基乙烯基硅树脂的折射率不小于1.54,25℃时粘度为5000cps-100000cps;(优选为30000-60000cps),分子量为200-1500,多分散性指数(PDI)小于1.3,且分子量小于500的分子摩尔百分含量小于1%;In one of the embodiments, the refractive index of the methylphenyl vinyl silicone resin is not less than 1.54, the viscosity at 25°C is 5000cps-100000cps; (preferably 30000-60000cps), the molecular weight is 200-1500, and the polydispersity The index (PDI) is less than 1.3, and the mole percentage of molecules with molecular weight less than 500 is less than 1%;

所述甲基苯基含氢硅树脂的折射率为不小于1.54,25℃时粘度为200cps-5000cps,(优选为1000-2000cps),分子量为500-1000,H的质量分数为0.1%-0.6%(优选为0.2%-0.5%)。当氢含量过少时,导致交联密度下降,吸湿性增加,氢含量过高时,交联密度升高,但同时脆性增加,柔韧性下降,将H含量控制在上述范围,具有较好的效果。The refractive index of the methylphenyl hydrogen-containing silicone resin is not less than 1.54, the viscosity at 25°C is 200cps-5000cps, (preferably 1000-2000cps), the molecular weight is 500-1000, and the mass fraction of H is 0.1%-0.6 % (preferably 0.2%-0.5%). When the hydrogen content is too small, the crosslinking density will decrease and the hygroscopicity will increase. When the hydrogen content is too high, the crosslinking density will increase, but at the same time the brittleness will increase and the flexibility will decrease. Controlling the H content in the above range will have a better effect .

在其中一个实施例中,所述铂金催化剂选自:1,3-二乙烯基-1,1,3,3-四甲基二硅氧烷铂(0),1,3-二乙烯基-1,1,3,3-四甲基二硅氧烷铂(0),六氯合铂氢酸中的至少一种;In one embodiment, the platinum catalyst is selected from: 1,3-divinyl-1,1,3,3-tetramethyldisiloxane platinum(0), 1,3-divinyl- At least one of 1,1,3,3-tetramethyldisiloxane platinum(0), hexachloroplatinum hydride;

优选为1,3-二乙烯基-1,1,3,3-四甲基二硅氧烷铂(0)甲苯溶液,1,3-二乙烯基-1,1,3,3-四甲基二硅氧烷铂(0)异丙醇溶液,六氯合铂氢酸异丙醇溶液中的至少一种;Preferred is 1,3-divinyl-1,1,3,3-tetramethyldisiloxane platinum(0) toluene solution, 1,3-divinyl-1,1,3,3-tetramethyl Platinum disiloxane platinum (0) isopropanol solution, at least one of hexachloroplatinum hydrogen acid isopropanol solution;

所述反应抑制剂选自:乙炔基环己醇、多乙烯基化合物、硅烷改性炔醇中的至少一种。The reaction inhibitor is selected from at least one of ethynyl cyclohexanol, polyvinyl compounds, and silane-modified acetylenic alcohols.

在其中一个实施例中,所述铂金催化剂为1,3-二乙烯基-1,1,3,3-四甲基二硅氧烷铂(0)。In one embodiment, the platinum catalyst is 1,3-divinyl-1,1,3,3-tetramethyldisiloxane platinum(0).

本法明还公开了上述的耐湿热的LED封装硅胶的制备方法,包括以下步骤:This Faming also discloses the preparation method of the above-mentioned heat-and-humidity resistant LED encapsulation silica gel, comprising the following steps:

制备A组分:将A组分的各原料混合均匀,即得;Preparation of component A: Mix the raw materials of component A evenly to obtain;

制备B组分:将B组分的各原料混合均匀,即得。Preparation of component B: Mix all the ingredients of component B evenly to get ready.

上述耐湿热的LED封装硅胶的制备方法,具有工艺简单,可靠性高的特点,可方便得应用于工业生产中。The above method for preparing the heat-and-humidity-resistant LED encapsulating silica gel has the characteristics of simple process and high reliability, and can be conveniently applied in industrial production.

在其中一个实施例中,所述制备A组分步骤中,将各原料分别加入搅拌机中,在常温下搅拌均匀,抽真空去除起泡,即得;优选将各原料分别加入行星搅拌机中,自转速率35-45r/min,常温下搅拌0.8-1.2h,停止搅拌,抽真空脱泡。In one of the embodiments, in the step of preparing component A, each raw material is added to the mixer respectively, stirred evenly at room temperature, vacuumized to remove foaming, and then obtained; preferably, each raw material is respectively added to the planetary mixer, and the rotation The speed is 35-45r/min, stir at room temperature for 0.8-1.2h, stop stirring, and vacuumize for defoaming.

所述制备B组分步骤中,将各原料分别加入搅拌机中,在常温下搅拌均匀,抽真空去除起泡,即得。优选将各原料分别加入行星搅拌机中,自转速率35-45r/min,常温下搅拌0.8-1.2h,停止搅拌,抽真空脱泡。In the step of preparing component B, add each raw material into a blender, stir evenly at room temperature, and vacuumize to remove foaming. Preferably, each raw material is added to a planetary mixer respectively, the rotation rate is 35-45r/min, stirred at room temperature for 0.8-1.2h, the stirring is stopped, and the vacuum is used for defoaming.

上述常温指的是15-35℃,优选25℃。The above normal temperature refers to 15-35°C, preferably 25°C.

本法明还公开了上述的耐湿热的LED封装硅胶在用于封装LED中的应用。The present invention also discloses the application of the above-mentioned heat-and-humidity-resistant LED encapsulating silica gel in encapsulating LEDs.

与现有技术相比,本发明具有以下有益效果:Compared with the prior art, the present invention has the following beneficial effects:

本发明的耐湿热的LED封装硅胶,通过选择特定的原料相互配合提高了SMD器件的耐湿热性能,解决了SMD器件储存过程中吸潮,在无铅回流焊制程中时易裂胶和脱胶的问题,进而降低了风险,提高了生产效率。The heat-and-humidity-resistant LED packaging silica gel of the present invention improves the heat-and-humidity resistance of SMD devices by selecting specific raw materials to cooperate with each other, and solves the problems of moisture absorption in the storage process of SMD devices and easy cracking and degumming in the lead-free reflow soldering process. problems, thereby reducing risks and improving production efficiency.

本发明的耐湿热的LED封装硅胶的制备方法,具有工艺简单,可靠性高的特点,可方便得应用于工业生产中。The preparation method of the heat-and-humidity-resistant LED packaging silica gel of the present invention has the characteristics of simple process and high reliability, and can be conveniently applied in industrial production.

该耐湿热的LED封装硅胶在可用于封装LED中,特别是使用该LED封装胶封装SMD器件,极大的提高了SMD器件的耐湿热性能。The heat-and-moisture-resistant LED encapsulating silica gel can be used in encapsulating LEDs, especially the use of the LED encapsulating glue to encapsulate SMD devices can greatly improve the heat-and-moisture resistance performance of the SMD devices.

附图说明Description of drawings

图1为背景技术中对于LED芯片和封装胶水涂覆关系示意图;Fig. 1 is a schematic diagram of the relationship between LED chip and packaging glue coating in the background technology;

其中:1.封装胶水;2.荧光粉;3.金线;4.支架;5.芯片。Among them: 1. Packaging glue; 2. Phosphor powder; 3. Gold wire; 4. Bracket; 5. Chip.

具体实施方式detailed description

为了便于理解本发明,下面将参照相关附图对本发明进行更全面的描述。附图中给出了本发明的较佳实施例。但是,本发明可以以许多不同的形式来实现,并不限于本文所描述的实施例。相反地,提供这些实施例的目的是使对本发明的公开内容的理解更加透彻全面。In order to facilitate the understanding of the present invention, the present invention will be described more fully below with reference to the associated drawings. Preferred embodiments of the invention are shown in the accompanying drawings. However, the present invention can be embodied in many different forms and is not limited to the embodiments described herein. On the contrary, these embodiments are provided to make the understanding of the disclosure of the present invention more thorough and comprehensive.

除非另有定义,本文所使用的所有的技术和科学术语与属于本发明的技术领域的技术人员通常理解的含义相同。本文中在本发明的说明书中所使用的术语只是为了描述具体的实施例的目的,不是旨在于限制本发明。本文所使用的术语“和/或”包括一个或多个相关的所列项目的任意的和所有的组合。Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the technical field of the invention. The terms used herein in the description of the present invention are for the purpose of describing specific embodiments only, and are not intended to limit the present invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.

以下实施例中所用原料均为市售购得。The raw materials used in the following examples are all commercially available.

实施例1Example 1

一种耐湿热的LED封装硅胶,由A组分和B组分构成,A kind of heat and humidity resistant LED encapsulation silicone, composed of A component and B component,

所述A组分由以下原料制备而成:The A component is prepared from the following raw materials:

甲基苯基乙烯基硅树脂((PhSiO3/2)0.48(Ph2SiO2/2)0.16(Me2SiO2/2)0.09(ViMe2SiO1/2)0.27,粘度为30000cps,折射率为1.543,分子量MW=951,PDI=1.253) 50gMethylphenyl vinyl silicone resin ((PhSiO 3/2 )0.48(Ph 2 SiO 2/2 )0.16(Me 2 SiO 2/2 )0.09(ViMe 2 SiO 1/2 )0.27, viscosity 30000cps, refractive index 1.543, molecular weight MW=951, PDI=1.253) 50g

铂金催化剂(含量为5000ppm的Pt-1,3,5,7四甲基-二乙烯基硅烷甲苯溶液) 0.2gPlatinum catalyst (content is 5000ppm Pt-1,3,5,7 tetramethyl-divinylsilane toluene solution) 0.2g

加成型增粘剂(含硼型增粘剂,Addition type tackifier (boron type tackifier,

CH2OCHCH3H6(CH3O)2Si0(Ph2SiO2/2)0.68(MeSiO2/2)0.25(BO3/2)0.07OSi(OCH3)2CH2OCHCH3H6)CH 2 OCHCH 3 H 6 (CH 3 O) 2 Si0(Ph 2 SiO 2 /2)0.68(MeSiO 2 /2)0.25(BO 3 /2)0.07OSi(OCH 3 ) 2 CH 2 OCHCH 3 H 6 )

1.0g1.0g

所述B组分主要由以下原料制备而成:The B component is mainly prepared from the following raw materials:

甲基苯基乙烯基硅树脂((PhSiO3/2)0.48(Ph2SiO2/2)0.16(Me2SiO2/2)0.09(ViMe2SiO1/2)0.27,粘度为30000cps,折射率为1.543,分子量MW=951,PDI=1.253) 20gMethylphenyl vinyl silicone resin ((PhSiO 3/2 )0.48(Ph 2 SiO 2/2 )0.16(Me 2 SiO 2/2 )0.09(ViMe 2 SiO 1/2 )0.27, viscosity 30000cps, refractive index 1.543, molecular weight MW=951, PDI=1.253) 20g

甲基苯基含氢硅树脂((PhSiO3/2)0.51(Ph2SiO2/2)0.25(HMe2SiO1/2)0.24,粘度为1000cps,折射率1.54,分子量mw=975,氢含量0.3%) 30gMethylphenyl hydrogen-containing silicone resin ((PhSiO 3/2 )0.51(Ph 2 SiO 2/2 )0.25(HMe 2 SiO 1/2 )0.24, viscosity 1000cps, refractive index 1.54, molecular weight mw=975, hydrogen content 0.3%) 30g

反应抑制剂(1-乙炔基环己醇) 0.03gReaction inhibitor (1-ethynyl cyclohexanol) 0.03g

本实施例的耐湿热的LED封装硅胶通过以下方法制备得到:The heat-and-humidity-resistant LED encapsulation silica gel of this embodiment is prepared by the following method:

一、制备A组分。1. Preparation of component A.

将A组分中的各原料分别加入到行星搅拌机中,在常温下混合搅拌1.0h,抽真空脱泡,得到A组分。Add each raw material in component A into a planetary mixer, mix and stir at room temperature for 1.0 h, vacuumize and defoam to obtain component A.

二、制备B组分。2. Preparation of component B.

将B组分中的各原料分别加入到行星搅拌机中,在常温下混合搅拌1.0h,抽真空脱泡,得到B组分。Add each raw material in component B into a planetary mixer, mix and stir at room temperature for 1.0 h, vacuumize and defoam to obtain component B.

实施例2Example 2

一种耐湿热的LED封装硅胶,由A组分和B组分构成,A kind of heat and humidity resistant LED encapsulation silicone, composed of A component and B component,

所述A组分由以下原料制备而成:The A component is prepared from the following raw materials:

甲基苯基乙烯基硅树脂((PhSiO3/2)0.5(Ph2SiO2/2)0.16(Me2SiO2/2)0.07(ViMe2SiO1/2)0.27,粘度为40000cps,折射率为1.545,分子量MW=1025,PDI=1.237) 50gMethylphenyl vinyl silicone resin ((PhSiO 3/2 )0.5(Ph 2 SiO 2/2 )0.16(Me 2 SiO 2/2 )0.07(ViMe 2 SiO 1/2 )0.27, viscosity 40000cps, refractive index 1.545, molecular weight MW=1025, PDI=1.237) 50g

铂金催化剂(含量为5000ppm的Pt-1,3,5,7四甲基-二乙烯基硅烷甲苯溶液) 0.2gPlatinum catalyst (content is 5000ppm Pt-1,3,5,7 tetramethyl-divinylsilane toluene solution) 0.2g

加成型增粘剂(含硼型增粘剂,Addition type tackifier (boron type tackifier,

CH2OCHCH3H6(CH3O)2Si0(Ph2SiO2/2)0.68(MeSiO2/2)0.25(BO3/2)0.07OSi(OCH3)2CH2OCHCH3H6)CH 2 OCHCH 3 H 6 (CH 3 O) 2 Si0(Ph 2 SiO 2 /2)0.68(MeSiO 2 /2)0.25(BO 3 /2)0.07OSi(OCH 3 ) 2 CH 2 OCHCH 3 H 6 )

1.0g1.0g

所述B组分主要由以下原料制备而成:The B component is mainly prepared from the following raw materials:

甲基苯基乙烯基硅树脂((PhSiO3/2)0.5(Ph2SiO2/2)0.16(Me2SiO2/2)0.07(ViMe2SiO1/2)0.27,粘度为40000cps,折射率为1.545,分子量MW=1025,PDI=1.237) 15gMethylphenyl vinyl silicone resin ((PhSiO 3/2 )0.5(Ph 2 SiO 2/2 )0.16(Me 2 SiO 2/2 )0.07(ViMe 2 SiO 1/2 )0.27, viscosity 40000cps, refractive index 1.545, molecular weight MW=1025, PDI=1.237) 15g

甲基苯基含氢硅树脂((PhSiO3/2)0.48(Ph2SiO2/2)0.27(HMe2SiO1/2)0.25,粘度为2000cps,折射率1.54,分子量mw=700,氢含量0.25%) 35gMethylphenyl hydrogen-containing silicone resin ((PhSiO 3/2 ) 0.48 (Ph 2 SiO 2/2 ) 0.27 (HMe 2 SiO 1/2 ) 0.25, viscosity 2000cps, refractive index 1.54, molecular weight mw=700, hydrogen content 0.25%) 35g

反应抑制剂(1-乙炔基环己醇) 0.03gReaction inhibitor (1-ethynyl cyclohexanol) 0.03g

本实施例的耐湿热的LED封装硅胶通过以下方法制备得到:The heat-and-humidity-resistant LED encapsulation silica gel of this embodiment is prepared by the following method:

一、制备A组分。1. Preparation of component A.

将A组分中的各原料分别加入到行星搅拌机中,在常温下混合搅拌1.0h,抽真空脱泡,得到A组分。Add each raw material in component A into a planetary mixer, mix and stir at room temperature for 1.0 h, vacuumize and defoam to obtain component A.

二、制备B组分。2. Preparation of component B.

将B组分中的各原料分别加入到行星搅拌机中,在常温下混合搅拌1.0h,抽真空脱泡,得到B组分。Add each raw material in component B into a planetary mixer, mix and stir at room temperature for 1.0 h, vacuumize and defoam to obtain component B.

实施例3Example 3

一种耐湿热的LED封装硅胶,由A组分和B组分构成,A kind of heat and humidity resistant LED encapsulation silicone, composed of A component and B component,

所述A组分由以下原料制备而成:The A component is prepared from the following raw materials:

甲基苯基乙烯基硅树脂((PhSiO3/2)0.51(Ph2SiO2/2)0.15(Me2SiO2/2)0.07(ViMe2SiO1/2)0.27,粘度为45000cps,折射率为1.543,分子量MW=1105,PDI=1.221) 50gMethylphenyl vinyl silicone resin ((PhSiO 3/2 )0.51(Ph 2 SiO 2/2 )0.15(Me 2 SiO 2/2 )0.07(ViMe 2 SiO 1/2 )0.27, viscosity 45000cps, refractive index 1.543, molecular weight MW=1105, PDI=1.221) 50g

铂金催化剂(含量为5000ppm的Pt-1,3,5,7四甲基-二乙烯基硅烷甲苯溶液)Platinum catalyst (5000ppm Pt-1,3,5,7 tetramethyl-divinylsilane toluene solution)

0.2g 0.2g

加成型增粘剂(含硼型增粘剂,Addition type tackifier (boron type tackifier,

CH2OCHCH3H6(CH3O)2Si0(Ph2SiO2/2)0.68(MeSiO2/2)0.25(BO3/2)0.07OSi(OCH3)2CH2OCHCH3H6) 1.0gCH 2 OCHCH 3 H 6 (CH 3 O) 2 Si0(Ph 2 SiO 2 /2)0.68(MeSiO 2 /2)0.25(BO 3 /2)0.07OSi(OCH 3 ) 2 CH 2 OCHCH 3 H 6 ) 1.0 g

所述B组分主要由以下原料制备而成:The B component is mainly prepared from the following raw materials:

甲基苯基乙烯基硅树脂(((PhSiO3/2)0.51(Ph2SiO2/2)0.15(Me2SiO2/2)0.07(ViMe2SiO1/2)0.27,粘度为45000cps,折射率为1.543,分子量MW=1105,PDI=1.221) 12gMethylphenyl vinyl silicone resin (((PhSiO 3/2 )0.51(Ph 2 SiO 2/2 )0.15(Me 2 SiO 2/2 )0.07(ViMe 2 SiO 1/2 )0.27, viscosity is 45000cps, refractive Rate is 1.543, molecular weight MW=1105, PDI=1.221) 12g

甲基苯基含氢硅树脂((PhSiO3/2)0.48(Ph2SiO2/2)0.27(HMe2SiO1/2)0.25粘度为2000cps,折射率1.54,分子量mw=700,氢含量0.25%) 38gMethylphenyl hydrogen-containing silicone resin ((PhSiO 3/2 ) 0.48 (Ph 2 SiO 2/2 ) 0.27 (HMe 2 SiO 1/2 ) 0.25 has a viscosity of 2000cps, a refractive index of 1.54, a molecular weight of mw=700, and a hydrogen content of 0.25 %) 38g

反应抑制剂(1-乙炔基环己醇) 0.03gReaction inhibitor (1-ethynyl cyclohexanol) 0.03g

本实施例的耐湿热的LED封装硅胶通过以下方法制备得到:The heat-and-humidity-resistant LED encapsulation silica gel of this embodiment is prepared by the following method:

一、制备A组分。1. Preparation of component A.

将A组分中的各原料分别加入到行星搅拌机中,在常温下混合搅拌1.0h,抽真空脱泡,得到A组分。Add each raw material in component A into a planetary mixer, mix and stir at room temperature for 1.0 h, vacuumize and defoam to obtain component A.

二、制备B组分。2. Preparation of component B.

将B组分中的各原料分别加入到行星搅拌机中,在常温下混合搅拌1.0h,抽真空脱泡,得到B组分。Add each raw material in component B into a planetary mixer, mix and stir at room temperature for 1.0 h, vacuumize and defoam to obtain component B.

实施例4Example 4

一种耐湿热的LED封装硅胶,由A组分和B组分构成,A kind of heat and humidity resistant LED encapsulation silicone, composed of A component and B component,

所述A组分由以下原料制备而成:The A component is prepared from the following raw materials:

甲基苯基乙烯基硅树脂((PhSiO3/2)0.52(Ph2SiO2/2)0.15(Me2SiO2/2)0.08(ViMe2SiO1/2)0.25,粘度为50000cps,折射率为1.543,分子量MW=1208,PDI=1.228) 50gMethylphenyl vinyl silicone resin ((PhSiO 3/2 )0.52(Ph 2 SiO 2/2 )0.15(Me 2 SiO 2/2 )0.08(ViMe 2 SiO 1/2 )0.25, viscosity is 50000cps, refractive index 1.543, molecular weight MW=1208, PDI=1.228) 50g

铂金催化剂(含量为5000ppm的Pt-1,3,5,7四甲基-二乙烯基硅烷甲苯溶液) 0.2gPlatinum catalyst (content is 5000ppm Pt-1,3,5,7 tetramethyl-divinylsilane toluene solution) 0.2g

加成型增粘剂(含硼型增粘剂,Addition type tackifier (boron type tackifier,

CH2OCHCH3H6(CH3O)2Si0(Ph2SiO2/2)0.68(MeSiO2/2)0.25(BO3/2)0.07OSi(OCH3)2CH2OCHCH3H6)CH 2 OCHCH 3 H 6 (CH 3 O) 2 Si0(Ph 2 SiO 2 /2)0.68(MeSiO 2 /2)0.25(BO 3 /2)0.07OSi(OCH 3 ) 2 CH 2 OCHCH 3 H 6 )

1.0g1.0g

所述B组分主要由以下原料制备而成:The B component is mainly prepared from the following raw materials:

甲基苯基乙烯基硅树脂((PhSiO3/2)0.52(Ph2SiO2/2)0.15(Me2SiO2/2)0.08(ViMe2SiO1/2)0.25,粘度为50000cps,折射率为1.543,分子量MW=1208,PDI=1.228) 8gMethylphenyl vinyl silicone resin ((PhSiO 3/2 )0.52(Ph 2 SiO 2/2 )0.15(Me 2 SiO 2/2 )0.08(ViMe 2 SiO 1/2 )0.25, viscosity 50000cps, refractive index 1.543, molecular weight MW=1208, PDI=1.228) 8g

甲基苯基含氢硅树脂((PhSiO3/2)0.51(Ph2SiO2/2)0.25(HMe2SiO1/2)0.24,粘度为2000cps,折射率1.54,分子量mw=700,氢含量0.2%) 42gMethylphenyl hydrogen-containing silicone resin ((PhSiO 3/2 )0.51(Ph 2 SiO 2/2 )0.25(HMe 2 SiO 1/2 )0.24, viscosity 2000cps, refractive index 1.54, molecular weight mw=700, hydrogen content 0.2%) 42g

反应抑制剂(1-乙炔基环己醇) 0.03gReaction inhibitor (1-ethynyl cyclohexanol) 0.03g

本实施例的耐湿热的LED封装硅胶通过以下方法制备得到:The heat-and-humidity-resistant LED encapsulation silica gel of this embodiment is prepared by the following method:

一、制备A组分。1. Preparation of component A.

将A组分中的各原料分别加入到行星搅拌机中,在常温下混合搅拌1.0h,抽真空脱泡,得到A组分。Add each raw material in component A into a planetary mixer, mix and stir at room temperature for 1.0 h, vacuumize and defoam to obtain component A.

二、制备B组分。2. Preparation of component B.

将B组分中的各原料分别加入到行星搅拌机中,在常温下混合搅拌1.0h,抽真空脱泡,得到B组分。Add each raw material in component B into a planetary mixer, mix and stir at room temperature for 1.0 h, vacuumize and defoam to obtain component B.

实施例5Example 5

一种耐湿热的LED封装硅胶,由A组分和B组分构成,A kind of heat and humidity resistant LED encapsulation silicone, composed of A component and B component,

所述A组分由以下原料制备而成:The A component is prepared from the following raw materials:

甲基苯基乙烯基硅树脂((PhSiO3/2)0.53(Ph2SiO2/2)0.17(Me2SiO2/2)0.04(ViMe2SiO1/2)0.26,粘度为50000cps,折射率为1.543,分子量MW=1208,PDI=1.228) 50gMethylphenyl vinyl silicone resin ((PhSiO 3/2 )0.53(Ph 2 SiO 2/2 )0.17(Me 2 SiO 2/2 )0.04(ViMe 2 SiO 1/2 )0.26, viscosity 50000cps, refractive index 1.543, molecular weight MW=1208, PDI=1.228) 50g

铂金催化剂(含量为5000ppm的Pt-1,3,5,7四甲基-二乙烯基硅烷甲苯溶液) 0.2gPlatinum catalyst (content is 5000ppm Pt-1,3,5,7 tetramethyl-divinylsilane toluene solution) 0.2g

加成型增粘剂(含硼型增粘剂,Addition type tackifier (boron type tackifier,

CH2OCHCH3H6(CH3O)2Si0(Ph2SiO2/2)0.68(MeSiO2/2)0.25(BO3/2)0.07OSi(OCH3)2CH2OCHCH3H6)CH 2 OCHCH 3 H 6 (CH 3 O) 2 Si0(Ph 2 SiO 2 /2)0.68(MeSiO 2 /2)0.25(BO 3 /2)0.07OSi(OCH 3 ) 2 CH 2 OCHCH 3 H 6 )

1.0g1.0g

所述B组分主要由以下原料制备而成:The B component is mainly prepared from the following raw materials:

甲基苯基乙烯基硅树脂((PhSiO3/2)0.52(Ph2SiO2/2)0.17(Me2SiO2/2)0.04(ViMe2SiO1/2)0.26,粘度为50000cps,折射率为1.543,分子量MW=1208,PDI=1.228) 5gMethylphenyl vinyl silicone resin ((PhSiO 3/2 )0.52(Ph 2 SiO 2/2 )0.17(Me 2 SiO 2/2 )0.04(ViMe 2 SiO 1/2 )0.26, viscosity 50000cps, refractive index 1.543, molecular weight MW=1208, PDI=1.228) 5g

甲基苯基含氢硅树脂((PhSiO3/2)0.51(Ph2SiO2/2)0.25(HMe2SiO1/2)0.24,粘度为1500cps,折射率1.54,分子量mw=600,氢含量0.25%) 45gMethylphenyl hydrogen-containing silicone resin ((PhSiO 3/2 )0.51(Ph 2 SiO 2/2 )0.25(HMe 2 SiO 1/2 )0.24, viscosity 1500cps, refractive index 1.54, molecular weight mw=600, hydrogen content 0.25%) 45g

反应抑制剂(1-乙炔基环己醇) 0.03gReaction inhibitor (1-ethynyl cyclohexanol) 0.03g

本实施例的耐湿热的LED封装硅胶通过以下方法制备得到:The heat-and-humidity-resistant LED encapsulation silica gel of this embodiment is prepared by the following method:

一、制备A组分。1. Preparation of component A.

将A组分中的各原料分别加入到行星搅拌机中,在常温下混合搅拌1.0h,抽真空脱泡,得到A组分。Add each raw material in component A into a planetary mixer, mix and stir at room temperature for 1.0 h, vacuumize and defoam to obtain component A.

二、制备B组分。2. Preparation of component B.

将B组分中的各原料分别加入到行星搅拌机中,在常温下混合搅拌1.0h,抽真空脱泡,得到B组分。Add each raw material in component B into a planetary mixer, mix and stir at room temperature for 1.0 h, vacuumize and defoam to obtain component B.

对比例1Comparative example 1

一种耐湿热的LED封装硅胶,与实施例1的硅胶基本相似,区别在于:A heat-and-humidity-resistant LED packaging silica gel, which is basically similar to the silica gel in Example 1, the difference is:

本对比例1中的A组分添加有6g甲基苯基乙烯基硅油。Component A in Comparative Example 1 was added with 6g of methylphenylvinyl silicone oil.

对比例2Comparative example 2

一种耐湿热的LED封装硅胶,与实施例2的硅胶基本相似,区别在于:A heat-and-humidity-resistant LED packaging silica gel, which is basically similar to the silica gel in Example 2, the difference is:

本对比例2中的硅硼型增粘剂替换为信越化学KBM-403增粘剂,该增粘剂的成分为r-环氧丙氧基三甲基硅烷。The silicon-boron type tackifier in this comparative example 2 was replaced by Shin-Etsu Chemical KBM-403 tackifier, and the tackifier was composed of r-glycidoxytrimethylsilane.

对比例3Comparative example 3

一种耐湿热的LED封装硅胶,与实施例3的硅胶基本相似,区别在于:A heat-and-humidity-resistant LED packaging silica gel, which is basically similar to the silica gel in Example 3, the difference is:

本对比例3中的B组分添加有5g的含氢硅油,该含氢硅油的成分为四甲基二苯基三硅氧烷,结构如下式:Component B in Comparative Example 3 is added with 5g of hydrogen-containing silicone oil, the composition of which is tetramethyldiphenyltrisiloxane, and its structure is as follows:

对比例4Comparative example 4

一种耐湿热的LED封装硅胶,与实施例4的硅胶基本相似,区别在于:A heat-and-humidity-resistant LED packaging silica gel, which is basically similar to the silica gel of Example 4, the difference is:

本对比例4中的A组分添加有6g的乙烯基硅油,该乙烯基硅油的结构式如下式:The A component in this comparative example 4 is added with the vinyl silicone oil of 6g, and the structural formula of this vinyl silicone oil is as follows:

对比例5Comparative example 5

一种耐湿热的LED封装硅胶,与实施例5的硅胶基本相似,区别在于:A heat-and-humidity-resistant LED encapsulating silica gel, which is basically similar to the silica gel in Example 5, the difference is that:

本对比例5中的B组分添加有6g的甲基苯基乙烯基硅油和6g的甲基苯基含氢硅油,该甲基苯基乙烯基硅油的成分如下式:Component B in Comparative Example 5 is added with 6g of methylphenyl vinyl silicone oil and 6g of methylphenyl hydrogen-containing silicone oil. The composition of the methylphenyl vinyl silicone oil is as follows:

该甲基苯基含氢硅油的成分如下式:The composition of this methyl phenyl hydrogen silicone oil is as follows:

实验例Experimental example

将不同实施例和对比例制备得到耐湿热的LED封装胶进行性能测试。The heat-and-humidity-resistant LED encapsulants prepared from different examples and comparative examples were tested for performance.

测试方方法如下:The test method is as follows:

1、将A剂、B剂以一定比例混合均匀,SMD5050贴片上点胶;1. Mix agent A and agent B evenly in a certain proportion, and dispense glue on the SMD5050 patch;

2、80℃/1hrs+170℃/3hrs烘烤固化;2. Baking and curing at 80℃/1hrs+170℃/3hrs;

3、将固化好的SMD5050贴片放入恒温恒湿机中,湿度RH=85%,温度Ta=85%;分别放置24h,48h,72h;3. Put the cured SMD5050 patch into the constant temperature and humidity machine, the humidity RH=85%, the temperature Ta=85%; place them for 24h, 48h, 72h respectively;

4、取出贴片,在标准实验室中恢复20分钟,4. Take out the patch and recover for 20 minutes in a standard laboratory,

5、进行无铅回流焊制程,260℃/30s,过3次,记录裂胶及脱胶数量;裂胶或脱胶记为失效。5. Carry out lead-free reflow soldering process, 260℃/30s, 3 times, record the number of cracked and degummed glue; cracked or degummed glue is recorded as failure.

测试结果如下表所示。The test results are shown in the table below.

表1.各LED封装胶配方及性能测试结果Table 1. Formulas and performance test results of various LED encapsulation adhesives

从上述结果中可以看出,当配方中含氢硅树脂的用量增大(Vi/SiH值从小到大),固化后胶体的硬度上升,表现为MSL测试失效百分率下降(最优结果为实施例4vi/SiH=1/1.5),但当配方中加入苯基乙烯基硅油时,固化后胶体的硬度下降,表现为MSL测试失效百分率上升。As can be seen from the above results, when the amount of hydrogen-containing silicone resin in the formula increases (Vi/SiH value increases from small to large), the hardness of the colloid after curing increases, showing that the failure percentage of the MSL test decreases (the best result is the embodiment). 4vi/SiH=1/1.5), but when phenylvinyl silicone oil is added to the formula, the hardness of the cured colloid decreases, which is manifested as an increase in the failure percentage of the MSL test.

以上所述实施例的各技术特征可以进行任意的组合,为使描述简洁,未对上述实施例中的各个技术特征所有可能的组合都进行描述,然而,只要这些技术特征的组合不存在矛盾,都应当认为是本说明书记载的范围。The technical features of the above-mentioned embodiments can be combined arbitrarily. To make the description concise, all possible combinations of the technical features in the above-mentioned embodiments are not described. However, as long as there is no contradiction in the combination of these technical features, should be considered as within the scope of this specification.

以上所述实施例仅表达了本发明的几种实施方式,其描述较为具体和详细,但并不能因此而理解为对发明专利范围的限制。应当指出的是,对于本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形和改进,这些都属于本发明的保护范围。因此,本发明专利的保护范围应以所附权利要求为准。The above-mentioned embodiments only express several implementation modes of the present invention, and the descriptions thereof are relatively specific and detailed, but should not be construed as limiting the patent scope of the invention. It should be pointed out that those skilled in the art can make several modifications and improvements without departing from the concept of the present invention, and these all belong to the protection scope of the present invention. Therefore, the protection scope of the patent for the present invention should be based on the appended claims.

Claims (10)

1.一种耐湿热的LED封装硅胶,其特征在于,由A组分和B组分构成,1. A heat-and-humidity-resistant LED encapsulation silica gel, characterized in that it consists of component A and component B, 所述A组分由以下重量百分比的原料制备而成:The A component is prepared from the following raw materials in weight percentage: 甲基苯基乙烯基硅树脂 40%-60%Methylphenyl vinyl silicone resin 40%-60% 铂金催化剂 0.0002%-0.002%Platinum catalyst 0.0002%-0.002% 加成型增粘剂 0.1%-5%Additive tackifier 0.1%-5% 所述B组分主要由以下重量百分比的原料制备而成:The B component is mainly prepared from the following raw materials in weight percentage: 甲基苯基乙烯基硅树脂 10%-40%Methylphenyl vinyl silicone resin 10%-40% 甲基苯基含氢硅树脂 10%-45%Methylphenyl hydrogen silicone resin 10%-45% 反应抑制剂 0.01%-0.2%Reaction inhibitor 0.01%-0.2% 所述A组分和B组分原料总和为100%。The sum of the A component and B component raw materials is 100%. 2.根据权利要求1所述的耐湿热的LED封装硅胶,其特征在于,所述A组分由以下重量百分比的原料制备而成:2. The heat-and-humidity-resistant LED packaging silica gel according to claim 1, characterized in that, the A component is prepared from the following raw materials in weight percentage: 甲基苯基乙烯基硅树脂 45%-55%Methylphenyl vinyl silicone resin 45%-55% 铂金催化剂 0.0004%-0.001%Platinum catalyst 0.0004%-0.001% 加成型增粘剂 1%-3%Additive tackifier 1%-3% 所述B组分主要由以下重量百分比的原料制备而成:The B component is mainly prepared from the following raw materials in weight percentage: 甲基苯基乙烯基硅树脂 15%-35%Methylphenyl vinyl silicone resin 15%-35% 甲基苯基含氢硅树脂 25%-45%Methylphenyl hydrogen silicone resin 25%-45% 反应抑制剂 0.05%-0.1%。Reaction inhibitor 0.05%-0.1%. 3.根据权利要求1或2所述的耐湿热的LED封装硅胶,其特征在于,所述甲基苯基乙烯基硅树脂具有如下化学式:3. The heat-and-humidity-resistant LED packaging silica gel according to claim 1 or 2, wherein the methylphenyl vinyl silicone resin has the following chemical formula: (PhSiO3/2)a(Ph2SiO2/2)b(Me2SiO2/2)c(ViMe2SiO1/2)d(PhSiO 3/2 )a(Ph 2 SiO 2/2 )b(Me 2 SiO 2/2 )c(ViMe 2 SiO 1/2 )d 其中,a+b+c+d=1,并且0<a<0.6,0<b<0.4,0<C<0.4,0<d<0.3;Wherein, a+b+c+d=1, and 0<a<0.6, 0<b<0.4, 0<C<0.4, 0<d<0.3; 所述甲基苯基含氢硅树脂具有如下化学式:The methylphenyl hydrogen-containing silicone resin has the following chemical formula: (PhSiO3/2)a(Ph2SiO2/2)b(HMe2SiO1/2)c(PhSiO 3/2 )a(Ph 2 SiO 2/2 )b(HMe 2 SiO 1/2 )c 其中,a+b+c=1 0<a<0.5,0<b<0.4,0<C<0.4;Among them, a+b+c=1 0<a<0.5, 0<b<0.4, 0<C<0.4; 所述加成型增粘剂选自硅硼型加成型增粘剂,具有以下结构:The addition type tackifier is selected from silicon boron type addition type tackifier, has the following structure: CH2OCHCH3H6(CH3O)2Si0(Ph2SiO2/2)a(MeSiO2/2)b(BO3/2)cOSi(OCH3)2CH2OCHCH3H6;其中,Ph为苯基、Me为甲基、B为硼原子,a、b、c分别代表各结构单元在分子中的平均摩尔百分率,其中0<a<0.7,0<b<0.3,0<c<0.1CH 2 OCHCH 3 H 6 (CH 3 O) 2 Si0(Ph 2 SiO 2 /2)a(MeSiO 2 /2)b(BO 3 /2)cOSi(OCH 3 ) 2 CH 2 OCHCH 3 H 6 ; where, Ph is a phenyl group, Me is a methyl group, B is a boron atom, a, b, and c represent the average mole percentage of each structural unit in the molecule, among which 0<a<0.7, 0<b<0.3, 0<c< 0.1 Ph为苯基、Me为甲基、Vi为乙烯基、Si为硅、O为氧、H为氢,a、b、c、d代表结构单元在大分子中的平均摩尔百分率。Ph is phenyl, Me is methyl, Vi is vinyl, Si is silicon, O is oxygen, H is hydrogen, and a, b, c, d represent the average mole percentage of structural units in macromolecules. 4.根据权利要求3所述的耐湿热的LED封装硅胶,其特征在于,所述LED封装硅胶中,SiH/Vi的摩尔比为1-2。4. The heat-and-humidity resistant LED packaging silica gel according to claim 3, characterized in that, in the LED packaging silica gel, the molar ratio of SiH/Vi is 1-2. 5.根据权利要求3所述的耐湿热的LED封装硅胶,其特征在于,所述甲基苯基含氢硅树脂中,0.2<a<0.45,0.1<b<0.25,0.1<C<0.35,且(HMe2SiO1/2)基团为封端基团。5. The heat-and-humidity-resistant LED packaging silica gel according to claim 3, characterized in that, in the methylphenyl hydrogen-containing silicone resin, 0.2<a<0.45, 0.1<b<0.25, 0.1<C<0.35, And the (HMe 2 SiO 1/2 ) group is a capping group. 6.根据权利要求3所述的耐湿热的LED封装硅胶,其特征在于,所述甲基苯基乙烯基硅树脂的折射率不小于1.54,25℃时粘度为5000cps-100000cps;,分子量为200-1500,多分散性指数小于1.3,且分子量小于500的分子摩尔百分含量小于1%;6. The heat-and-humidity resistant LED packaging silica gel according to claim 3, characterized in that the refractive index of the methylphenyl vinyl silicone resin is not less than 1.54, the viscosity at 25°C is 5000cps-100000cps; and the molecular weight is 200 -1500, the polydispersity index is less than 1.3, and the mole percentage of molecules with molecular weight less than 500 is less than 1%; 所述甲基苯基含氢硅树脂的折射率为不小于1.54,25℃时粘度为200cps-5000cps,分子量为500-1000,H的质量分数为0.1%-0.6%。The refractive index of the methylphenyl hydrogen-containing silicone resin is not less than 1.54, the viscosity at 25°C is 200cps-5000cps, the molecular weight is 500-1000, and the mass fraction of H is 0.1%-0.6%. 7.根据权利要求1或2所述的耐湿热的LED封装硅胶,其特征在于,所述铂金催化剂选自:1,3-二乙烯基-1,1,3,3-四甲基二硅氧烷铂(0),1,3-二乙烯基-1,1,3,3-四甲基二硅氧烷铂(0),六氯合铂氢酸中的至少一种7. The heat-and-humidity-resistant LED packaging silica gel according to claim 1 or 2, wherein the platinum catalyst is selected from the group consisting of: 1,3-divinyl-1,1,3,3-tetramethyldisilica At least one of oxane platinum(0), 1,3-divinyl-1,1,3,3-tetramethyldisiloxane platinum(0), hexachloroplatinum hydride 所述反应抑制剂选自:乙炔基环己醇、多乙烯基化合物、硅烷改性炔醇中的至少一种。The reaction inhibitor is selected from at least one of ethynyl cyclohexanol, polyvinyl compounds, and silane-modified acetylenic alcohols. 8.权利要求1-7任一项所述的耐湿热的LED封装硅胶的制备方法,其特征在于,包括以下步骤:8. The preparation method of the heat-and-humidity-resistant LED encapsulation silica gel described in any one of claims 1-7, is characterized in that, comprises the following steps: 制备A组分:将A组分的各原料混合均匀,即得;Preparation of component A: Mix the raw materials of component A evenly to obtain; 制备B组分:将B组分的各原料混合均匀,即得。Preparation of component B: Mix all the ingredients of component B evenly to get ready. 9.根据权利要求8所述的耐湿热的LED封装硅胶的制备方法,其特征在于,9. the preparation method of the heat-and-humidity-resistant LED packaging silica gel according to claim 8, is characterized in that, 所述制备A组分步骤中,将各原料分别加入搅拌机中,在常温下搅拌均匀,抽真空去除起泡,即得;In the step of preparing component A, add each raw material into a blender, stir evenly at room temperature, vacuumize to remove foaming, and obtain; 所述制备B组分步骤中,将各原料分别加入搅拌机中,在常温下搅拌均匀,抽真空去除起泡,即得。In the step of preparing component B, add each raw material into a blender, stir evenly at room temperature, and vacuumize to remove foaming. 10.权利要求1-7任一项所述的耐湿热的LED封装硅胶在用于封装LED中的应用。10. The application of the heat-and-moisture-resistant LED encapsulating silica gel described in any one of claims 1-7 in encapsulating LEDs.
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