TWI480285B - Method for manufacturing an encapsulating material and composition for manufacturing an encapsulating material - Google Patents
Method for manufacturing an encapsulating material and composition for manufacturing an encapsulating material Download PDFInfo
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Description
本發明係關於一種用以製備封裝膠材之材料組成物；特別關於一種可用以製備具有高耐熱性封裝膠材之材料組成物。 The present invention relates to a material composition for preparing an encapsulant; and more particularly to a material composition which can be used to prepare a package having a high heat resistance.
現今用以作為封裝膠材之材料組成物多為矽膠或樹脂，以藉矽膠或樹脂混合其他高分子材料、輔助溶劑等製成該封裝膠材，方得使用該封裝膠材於發光二極體模組，而將該發光二極體模組予以封裝。 Nowadays, the material composition used as the encapsulating material is mostly silicone or resin, and the encapsulating adhesive is used to make the encapsulating adhesive by mixing other polymer materials and auxiliary solvents, etc., and the encapsulating adhesive is used for the LED. The module is packaged and the LED module is packaged.
然而，傳統由矽膠構成的該封裝膠材通常會於實際使用過程中，因該發光二極體模組運作時可能產生之高溫，而導致該封裝膠材在高於180℃之高溫環境作用下，即明顯使該封裝膠材產生黃化現象；甚至，經長時間累加該發光二極體模組所發散之熱能，不僅會再使該封裝膠材於超過200℃的高溫環境下伴隨裂紋產生，嚴重還會導致該封裝膠材出現色座標飄移、流明損失等物理性劣化之現象。 However, the conventional encapsulant composed of silicone rubber is usually used in actual use, because the high temperature environment may occur when the LED module is operated, and the package rubber is subjected to a high temperature environment higher than 180 ° C. That is, the encapsulating adhesive material is obviously yellowed; even after a long time of accumulating the heat energy radiated by the LED module, the encapsulating rubber is not only accompanied by cracks in a high temperature environment exceeding 200 ° C. Seriously, the packaged adhesive material may exhibit physical deterioration such as color shift and lumen loss.
基於前述問題，多數業者多選擇另以聚矽氧樹脂取代傳統矽膠，藉由聚矽氧樹脂較一般有機樹脂所具有之較佳耐熱性、透明性、難以變色、難以物理性劣化等優異特性，來延長封裝膠材的使用壽命。惟，當以聚矽氧樹脂作為封裝材料時，其多數與發光二極體模組間的密著性皆不佳，反而容易使氣體通透而衍生新的問題。 Based on the above problems, most manufacturers choose to replace the traditional tannin extract with polyoxynoxy resin, which has better heat resistance, transparency, difficulty in discoloration, and difficulty in physical deterioration than the general organic resin. To extend the life of the package adhesive. However, when polyoxyxylene resin is used as the encapsulating material, most of the adhesion to the LED module is poor, and on the contrary, it is easy to make the gas permeate and introduce a new problem.
有鑑於此，確實有必要發展一種有別於傳統之材料組成物， 以就該材料組成物製成封裝膠材，進而解決如上所述之各種問題。 In view of this, it is indeed necessary to develop a material composition that is different from the traditional ones. The package material is made in terms of the material composition, thereby solving various problems as described above.
本發明主要目的乃改善上述問題，以提供一種用以製備封裝膠材之材料組成物，其係能夠使所製成之封裝膠材具有較佳緻密性及耐熱性，而不致因高溫環境產生黃化、裂解等現象，且亦可阻隔水氣者。 The main object of the present invention is to improve the above problems, and to provide a material composition for preparing a package adhesive material, which can make the packaged rubber material having better compactness and heat resistance without causing yellow color due to high temperature environment. It can also be used to block water and gas.
本發明次一目的係提供一種用以製備封裝膠材之材料組成物，其係能夠使所製成之封裝膠材具有較佳透光性者。 A second object of the present invention is to provide a material composition for preparing an encapsulant which is capable of imparting a light transmissive property to the encapsulant produced.
本發明又一目的係提供一種用以製備封裝膠材之材料組成物，其係能夠使所製成之封裝膠材具有較佳穩定度者。 Another object of the present invention is to provide a material composition for preparing an encapsulant which is capable of imparting better stability to the encapsulant produced.
為達前述發明目的，本發明封裝膠材之製備方法，包括：提供一材料組成物，包含以體積百分比計32.11%~36.84%之四乙氧基矽烷、33.3%~38.31%之第一輔溶劑、11.7%~22.2%之第二輔溶劑及10.7%~13.01%之甲醯胺，及0.03%~0.08%之酸液，其中，該第一輔溶劑為乙醇或甲醇，該第二輔溶劑為水；於室溫下混合該材料組成物，使該材料組成物形成一膠結物；於100℃下燒結該膠結物5小時，使該膠結物形成一固形封裝膠材；將該固形封裝膠材於200~800℃下進行高溫熱處理5小時；及將進行高溫熱處理後之固形封裝膠材於70~80℃下進行低溫熱處理10~50小時。 For the purpose of the foregoing invention, a method for preparing a packaged rubber of the present invention comprises: providing a material composition comprising 32.11% to 36.84% by volume of tetraethoxy decane, and 33.3% to 38.31% of the first auxiliary solvent. 11.7%~22.2% of the second auxiliary solvent and 10.7%~13.01% of the methotrexate, and 0.03%~0.08% of the acid solution, wherein the first auxiliary solvent is ethanol or methanol, and the second auxiliary solvent is Water; mixing the composition of the material at room temperature to form a cement; sintering the cement at 100 ° C for 5 hours to form the solidified encapsulant; the solid encapsulant The high temperature heat treatment is performed at 200 to 800 ° C for 5 hours; and the solid package rubber after high temperature heat treatment is subjected to low temperature heat treatment at 70 to 80 ° C for 10 to 50 hours.
其中，該材料組成物係於室溫下攪拌30分鐘，待產生膠結現象後，續於室溫下靜置24小時，以形成該膠結物。 Wherein, the material composition was stirred at room temperature for 30 minutes, and after being cemented, it was allowed to stand at room temperature for 24 hours to form the cement.
其中，該酸液為鹽酸、硫酸、磷酸或硝酸。 Wherein, the acid solution is hydrochloric acid, sulfuric acid, phosphoric acid or nitric acid.
其中，以體積百分比計，該四乙氧基矽烷為36.84%、乙醇為38.31%、水為11.79%、甲醯胺為13.01%及鹽酸為0.05%。 Among them, the tetraethoxy decane was 36.84%, the ethanol was 38.31%, the water was 11.79%, the formamide was 13.01%, and the hydrochloric acid was 0.05%.
為達前述發明目的，本發明另提供一種用以製備封裝膠材之材料組成物，包括：以體積百分比計8.568%~17.13%之甲基三乙氧基矽 烷、6.15%~20.5%之二甲基二乙氧基矽烷、55.8%~75.37%之第一輔溶劑、6.5%之第二輔溶劑及0.04%之氨水；其中，該第一輔溶劑為乙醇或甲醇，該第二輔溶劑為水。 In order to achieve the foregoing object, the present invention further provides a material composition for preparing an encapsulant comprising: 8.568% to 17.13% by volume of methyltriethoxyphosphonium. Alkane, 6.15%~20.5% dimethyldiethoxy decane, 55.8%~75.37% first auxiliary solvent, 6.5% second auxiliary solvent and 0.04% ammonia water; wherein the first auxiliary solvent is ethanol Or methanol, the second auxiliary solvent is water.
其中，另包含以體積百分比計0.03%之酸液。 Among them, an acid solution containing 0.03% by volume is further included.
其中，該酸液為鹽酸、硫酸、磷酸或硝酸。 Wherein, the acid solution is hydrochloric acid, sulfuric acid, phosphoric acid or nitric acid.
其中，以體積百分比計，該甲基三乙氧基矽烷為17.13%、二甲基二乙氧基矽烷為20.5%、乙醇為55.8%、水為6.5%、氨水為0.04%及鹽酸為0.03%。 Wherein, the methyltriethoxydecane is 17.13%, the dimethyldiethoxydecane is 20.5%, the ethanol is 55.8%, the water is 6.5%, the ammonia is 0.04%, and the hydrochloric acid is 0.03%. .
第1圖：係封裝膠材經熱處理前後之外觀示意圖一。 Figure 1 is a schematic view of the appearance of the packaged rubber before and after heat treatment.
第2圖：係封裝膠材經熱處理前後之外觀示意圖二。 Figure 2: The appearance of the package rubber before and after heat treatment.
第3圖：係封裝膠材應用於封裝發光二極體模組之示意圖。 Figure 3: Schematic diagram of the application of the package adhesive to the packaged LED module.
第4a~4b圖：係封裝膠材的穿透率比較圖。 Figures 4a~4b: Comparison of penetration rates of packaged adhesives.
第5a~5b圖：係封裝膠材的耐熱性示意圖。 Figure 5a~5b: Schematic diagram of the heat resistance of the package adhesive.
第6圖：係封裝膠材的耐熱性示意圖。 Figure 6: Schematic diagram of the heat resistance of the package adhesive.
為讓本發明之上述及其他目的、特徵及優點能更明顯易懂，下文特舉本發明之較佳實施例，並配合所附圖式，作詳細說明如下：本發明用以製備封裝膠材之材料組合物，其主要係以矽烷氧化物為製成該封裝膠材的反應物，且該矽烷氧化物可以選擇為二甲基二乙氧基矽烷、甲基三乙氧基矽烷、四乙氧基矽烷等，其各自與其他成分的混合比例係分別詳述於本發明如下之第一及第二較佳實施例。 The above and other objects, features and advantages of the present invention will become more <RTIgt; a material composition mainly comprising a decane oxide as a reactant for forming the encapsulant, and the decane oxide may be selected from the group consisting of dimethyldiethoxydecane, methyltriethoxydecane, and tetraethylidene. The mixing ratio of each of oxydecane and the like to the other components is described in detail in the first and second preferred embodiments of the present invention.
該第一較佳實施例之用以製備封裝膠材之材料組成物，其係包含以體積百分比計32.11%~36.84%之四乙氧基矽烷、33.3%~38.31%之 第一輔溶劑、11.7%~22.2%之第二輔溶劑及10.7%~13.01%之甲醯胺；其中，該第一輔溶劑為乙醇或甲醇，該第二輔溶劑為水。 The material composition for preparing the encapsulant of the first preferred embodiment comprises 32.11%~36.84% by volume of tetraethoxynonane, 33.3%~38.31%. The first auxiliary solvent, 11.7% to 22.2% of the second auxiliary solvent, and 10.7% to 13.01% of the methotrexate; wherein the first auxiliary solvent is ethanol or methanol, and the second auxiliary solvent is water.
詳言之，本發明第一較佳實施例所述用以製備封裝膠材之材料組成物，主要係藉由四乙氧基矽烷所具有之耐熱、高透光等特性，以與第一輔溶劑及第二輔溶劑的共同作用下產生結膠反應，並同時透過甲醯胺於結膠反應過程的協同作用，以更進一步降低所製成封裝膠材的材料毛細現象。藉此，如第1圖，可以看到本發明所製成之封裝膠材(a1：熱處理前)經過熱處理(a2：250℃熱處理)後，仍保持原有極佳之透光性；反之，可以看到傳統矽膠所製成之封裝膠材(b1：熱處理前)經過熱處理(b2：250℃熱處理)後，明顯產生黃化現象，故經本發明所製成之封裝膠材相較於傳統矽膠製成之封裝膠材不僅可以具有較佳耐熱、高透光等特性，還可以在該封裝膠材應用於發光二極體模組時，維持其結合緻密性，有效阻隔氧與水氣進入該發光二極體模組內而產生不良作用。 In detail, the material composition for preparing the encapsulant according to the first preferred embodiment of the present invention is mainly characterized by heat resistance and high light transmittance of tetraethoxy decane, and the first auxiliary The solvent and the second auxiliary solvent act together to produce a gelation reaction, and at the same time, through the synergistic action of the methotrexate in the gelation reaction process, the material capillary phenomenon of the encapsulated rubber material is further reduced. Therefore, as shown in FIG. 1, it can be seen that the encapsulating adhesive (a1: before heat treatment) prepared by the present invention maintains excellent light transmittance after heat treatment (a2: 250 ° C heat treatment); It can be seen that the encapsulating adhesive made of the traditional tannin extract (b1: before heat treatment) is subjected to heat treatment (b2: 250 ° C heat treatment), and yellowing phenomenon is apparent, so the encapsulant made by the present invention is compared with the traditional tannin extract. The prepared encapsulant can not only have better heat resistance, high light transmission and the like, but also can maintain the bonding density when the encapsulant is applied to the LED module, and effectively block oxygen and moisture from entering the package. The LED module has an adverse effect inside the LED module.
再者，本發明第一較佳實施例還可以另包含有以體積百分比計0.03~0.08%之酸液，以透過該酸液提升該材料組成物在製成該封裝膠材之效率，該酸液可以為鹽酸、硫酸、磷酸或硝酸等，以與水混合後，使其pH=2即可。 Furthermore, the first preferred embodiment of the present invention may further comprise an acid solution in a volume percentage of 0.03 to 0.08% to enhance the efficiency of the material composition in forming the encapsulating material through the acid solution. The liquid may be hydrochloric acid, sulfuric acid, phosphoric acid or nitric acid, etc., and after mixing with water, it may be made pH=2.
於該第一較佳實施例中，該第一輔溶劑可以選擇為乙醇，該第二輔溶劑則可以選擇為水，以藉該乙醇與水共混而為該四乙氧基矽烷的輔溶劑，致使該四乙氧基矽烷可以作用呈凝膠狀為佳；並且，藉由該第一較佳實施例所選擇之鹽酸更可加速該封裝膠材的成形效率。較佳者，該第一較佳實施例的該材料組成物係包含體積百分比計為36.84%之四乙氧基矽烷、38.31%之乙醇、11.79%之水、13.01%之甲醯胺及0.05%之鹽酸。 In the first preferred embodiment, the first auxiliary solvent may be selected as ethanol, and the second auxiliary solvent may be selected as water to be a co-solvent of the tetraethoxy decane by blending the ethanol with water. It is preferred that the tetraethoxy decane can function as a gel; and the hydrochloric acid selected by the first preferred embodiment can further accelerate the forming efficiency of the encapsulating material. Preferably, the material composition of the first preferred embodiment comprises 36.84% by volume of tetraethoxy decane, 38.31% of ethanol, 11.79% of water, 13.01% of methotrexate and 0.05% by volume. Hydrochloric acid.
基於前述第一實施例，本發明於實際製作該封裝膠材並將其用於封裝發光二極體模組之過程，係包含以下步驟： 第一步驟係混合四乙氧基矽烷、乙醇、水、鹽酸及甲醯胺，以共同形成一混合物；詳言之，本實施例係先混合鹽酸及水而形成pH值約為2之酸性水，且以該酸性水調配其他成份，致使各成份莫爾比為四乙氧基矽烷：乙醇：酸性水(水+鹽酸)：甲醯胺=1：4：4：2，並於各成份充分混合為該混合物後，較佳係於室溫下持續攪拌約30分鐘，以致使該混合物可以逐漸產生膠結現象。 Based on the foregoing first embodiment, the present invention actually processes the package adhesive and uses it to package the LED module, and includes the following steps: The first step is to mix tetraethoxy decane, ethanol, water, hydrochloric acid and formamide to form a mixture together; in detail, this embodiment first mixes hydrochloric acid and water to form acidic water having a pH of about 2. And the other components are mixed with the acidic water, so that the molar ratio of each component is tetraethoxy decane: ethanol: acidic water (water + hydrochloric acid): formamidine = 1:4:4:2, and is fully contained in each component. After mixing as the mixture, it is preferred to continue stirring at room temperature for about 30 minutes so that the mixture can gradually form a cementation phenomenon.
接續第一步驟，第二步驟係靜置該混合物，直至該混合物完全結膠，以形成一膠結物；較佳係於室溫下持續靜置約24小時，以經四乙氧基矽烷與乙醇、水產生膠結反應而使得該混合物結膠後呈現凝膠狀。 Following the first step, the second step is to leave the mixture until the mixture is completely gelled to form a cement; preferably, it is allowed to stand at room temperature for about 24 hours to pass tetraethoxy decane and ethanol. The water produces a cementation reaction which causes the mixture to gel and form a gel.
經該第二步驟生成該膠結物後，第三步驟係再將該膠結物作燒結，以形成固形之封裝膠材；較佳之燒結溫度為100℃，以於100℃下持續燒結約5小時，直至完全去除該膠結物中所含乙醇、水後，即可固形該膠結物而得該封裝膠材。 After the second step is to form the cement, the third step is to sinter the cement to form a solid encapsulated rubber; preferably, the sintering temperature is 100 ° C, and the sintering is continued at 100 ° C for about 5 hours. After the ethanol and water contained in the cement are completely removed, the cement can be solidified to obtain the encapsulated rubber.
較佳者，該封裝膠材還可以經第一道熱處理程序，以於第一道熱處理過程提升該封裝膠材的物理特性；其中，該第一道熱處理程序的處理溫度較佳為200℃~800℃，以持續作用約5小時。 Preferably, the encapsulating material is further subjected to a first heat treatment process to enhance the physical properties of the encapsulating material in the first heat treatment process; wherein the processing temperature of the first heat treatment process is preferably 200 ° C. At 800 ° C, for about 5 hours.
經前述第一道熱處理程序後，亦可以再選擇通過第二道熱處理程序，以致使該封裝膠材更具有較佳耐熱及穿透性；其中，該第二道熱處理程序的處理溫度較佳為70℃~80℃，以持續作用10~50小時。 After the first heat treatment process, the second heat treatment process may be further selected to make the package rubber more resistant to heat and penetration; wherein the second heat treatment process preferably has a processing temperature of 70 ° C ~ 80 ° C, for a sustained action of 10 to 50 hours.
如此，經上述所製成之封裝膠材遂可應用於封裝發光二極體模組，以由固形之封裝膠材覆蓋於該發光二極體模組，並透過傳統封裝手段予以完成；且以上熱處理程序乃視本領域技術人員於實際實施時之情況而定，本實施例僅係以二道熱處理程序，而致使該封裝膠材具有良好耐熱及穿透性為原則，並不再此設限亦容不贅述。 In this way, the packaged adhesive material prepared by the above can be applied to the packaged light-emitting diode module, and is covered by the solid-package adhesive material to the light-emitting diode module, and is completed by a conventional packaging method; The heat treatment process is determined by those skilled in the art in actual practice. This embodiment is only based on the two heat treatment procedures, so that the package rubber has good heat resistance and penetration, and the limit is no longer imposed. I will not repeat them.
此外，基於第一較佳實施例的基礎下，該第二較佳實施例之 用以製備封裝膠材之材料組成物，其係包含以體積百分比計8.568%~17.13%之甲基三乙氧基矽烷、6.15%~20.5%之二甲基二乙氧基矽烷、55.8%~75.37%之第一輔溶劑、6.5%之第二輔溶劑及0.04%之氨水；其中，該第一輔溶劑為乙醇或甲醇，該第二輔溶劑為水。 Further, based on the first preferred embodiment, the second preferred embodiment The material composition for preparing the encapsulant comprises 8.568%~17.13% by volume of methyltriethoxydecane, 6.15%~20.5% of dimethyldiethoxydecane, 55.8%~ 75.37% of the first co-solvent, 6.5% of the second co-solvent and 0.04% of the ammonia water; wherein the first co-solvent is ethanol or methanol, and the second co-solvent is water.
詳言之，本發明第二較佳實施例所述用以製備封裝膠材之材料組成物，主要仍係藉由同為矽烷氧化物之甲基三乙氧基矽烷及二甲基二乙氧基矽烷，與第一輔溶劑及第二輔溶劑的共同作用下產生結膠反應，並同時透過氨水於結膠反應過程的協同作用，以更進一步致使膠結所生成之封裝膠材可以具有高耐熱、高透光等之特性。詳如第2圖，可以看到本發明所製成之封裝膠材(a1：熱處理前)經過熱處理(a2：250℃熱處理；a3：300℃熱處理)後，仍保持原有極佳之透光性；反之，可以看到傳統矽膠所製成之封裝膠材(b1：熱處理前)經過熱處理(b2：250℃熱處理；b3：300℃熱處理)後，明顯產生黃化現象，故經本發明所致成之封裝膠材確實具有高耐熱、高透光等之特性；除此之外，經本發明第二實施例所製成之封裝膠材在應用於發光二極體模組時，可以與第一較佳實施例同樣具有較佳結合緻密性(參閱第3圖之a、b；a係以點膠方式封裝於發光二極體模組上、b則是添加螢光粉後，在以點膠方式封裝於發光二極體模組上)，有效阻隔氧與水氣之進入該發光二極體模組內而產生不良作用。 In detail, the material composition for preparing the encapsulant according to the second preferred embodiment of the present invention is mainly composed of methyl triethoxy decane and dimethyl diethoxy oxide which are the same as the decane oxide. The base decane reacts with the first auxiliary solvent and the second auxiliary solvent to produce a gelation reaction, and at the same time, the synergistic action of the ammonia water in the gelation reaction process, so as to further cause the encapsulation rubber formed by the cementation to have high heat resistance , high light transmission and other characteristics. As shown in Fig. 2, it can be seen that the encapsulating adhesive (a1: before heat treatment) made by the present invention is subjected to heat treatment (a2: 250 ° C heat treatment; a3: 300 ° C heat treatment), and still maintains excellent light transmission. On the contrary, it can be seen that the encapsulating adhesive made of traditional tannin (b1: before heat treatment) is subjected to heat treatment (b2: heat treatment at 250 ° C; heat treatment at b3: 300 ° C), which obviously causes yellowing, so it is caused by the invention. The packaged adhesive material has the characteristics of high heat resistance, high light transmission, etc.; in addition, the package adhesive material produced by the second embodiment of the present invention can be applied to the light emitting diode module. The preferred embodiment also has a better combination of compactness (see a, b in Fig. 3; a is encapsulated on the light emitting diode module in a dispensing manner, and b is dispensed after adding a fluorescent powder). The method is packaged on the LED module to effectively block the entry of oxygen and moisture into the LED module and cause adverse effects.
再者，本發明第二較佳實施例還可以另包含有以體積百分比計0.03%之酸液，以透過該酸液提升該材料組成物在製成該封裝膠材之效率，該酸液可以為鹽酸、硫酸、磷酸或硝酸等，以與水混合後，使其pH=2即可。 Furthermore, the second preferred embodiment of the present invention may further comprise an acid solution of 0.03% by volume to enhance the efficiency of the material composition in forming the encapsulating material through the acid solution, and the acid solution may It is hydrochloric acid, sulfuric acid, phosphoric acid, nitric acid, etc., and after mixing with water, it can make pH=2.
於該第二較佳實施例中，該第一輔溶劑與第一實施例相同可以選擇為乙醇，該第二輔溶劑亦與第一實施例相同可以選擇為水，以藉該乙醇與水共混而為該甲基三乙氧基矽烷及該二甲基二乙氧基矽烷的輔溶 劑，致使該甲基三乙氧基矽烷及該二甲基二乙氧基矽烷可以作用呈凝膠狀為佳；並且，藉由該第二較佳實施例所選擇之鹽酸更可加速該封裝膠材的成形效率。較佳者，該第二較佳實施例的該材料組成物係包含體積百分比計為17.13%之甲基三乙氧基矽烷、20.5%之二甲基二乙氧基矽烷、55.8%之乙醇、6.5%之水、0.04%之氨水及0.03%之鹽酸。 In the second preferred embodiment, the first auxiliary solvent may be selected as ethanol as in the first embodiment, and the second auxiliary solvent may also be selected as water in the same manner as the first embodiment, so as to share the water with the water. Mixed with the methyl triethoxy decane and the co-dissolved dimethyl diethoxy decane And the dimethyldimethoxy decane and the dimethyldiethoxy decane may preferably function as a gel; and the hydrochloric acid selected by the second preferred embodiment accelerates the package. The forming efficiency of the glue. Preferably, the material composition of the second preferred embodiment comprises 17.13% by volume of methyltriethoxydecane, 20.5% of dimethyldiethoxynonane, and 55.8% of ethanol. 6.5% water, 0.04% ammonia water and 0.03% hydrochloric acid.
基於前述第二實施例，本發明於實際製作該封裝膠材並將其用於封裝發光二極體模組之過程，係包含以下步驟：第一步驟係混合甲基三乙氧基矽烷、乙醇、水及鹽酸，以共同形成一第一混合物；詳言之，本實施例係將各成份置於一密閉容器中予以混合，並維持各成份莫爾比為甲基三乙氧基矽烷：乙醇：水：鹽酸=1：4：3：0.01；較佳者，係於室溫下持續攪拌約3~6小時，以充份混合。 Based on the foregoing second embodiment, the present invention actually processes the encapsulant and uses it for encapsulating the LED module, and comprises the following steps: the first step is to mix methyltriethoxydecane and ethanol. , water and hydrochloric acid to form a first mixture together; in detail, in this embodiment, the components are mixed in a closed container, and the molar ratio of each component is maintained to be methyltriethoxynonane:ethanol : Water: hydrochloric acid = 1:4:3:0.01; preferably, it is continuously stirred at room temperature for about 3 to 6 hours to be mixed thoroughly.
同第一步驟，另混合二甲基二乙氧基矽烷及乙醇，以共同形成一第二混合物；詳言之，本實施例另將各成份置於一密閉容器中予以混合，並維持各成份莫爾比為二甲基二乙基矽烷：乙醇=1：4；較佳者，係於室溫下持續攪拌約2~4小時，以充份混合。 In the same step as the first step, dimethyldiethoxydecane and ethanol are further mixed to form a second mixture; in detail, in this embodiment, the components are mixed in a closed container, and the components are maintained. The molar ratio is dimethyldiethyl decane:ethanol = 1:4; preferably, it is continuously stirred at room temperature for about 2 to 4 hours to be mixed thoroughly.
接續第一步驟而獲得該第一混合物及該第二混合物後，第二步驟遂混合該第一混合物與該第二混合物，且添加氨水與之相互作用，以形成一膠材混合液；詳言之，本實施例係將混合有該第一混合物及該第二混合物之溶液與氨水共同置於一開放容器中予以混合，並維持各成份莫爾比為第一混合物(甲基三乙氧基矽烷)+第二混合物(二甲基二乙基矽烷)：氨水=1：0.01；較佳者，係於室溫下持續攪拌約12~24小時，以充份混合，並逐漸於該開放容器周圍產生膠結現象。 After the first step is followed to obtain the first mixture and the second mixture, the second step is to mix the first mixture with the second mixture, and add ammonia water to interact with it to form a mixture of rubber; In this embodiment, the solution in which the first mixture and the second mixture are mixed is mixed with ammonia water in an open container, and the molar ratio of each component is maintained as a first mixture (methyltriethoxy group).矽 )) + second mixture (dimethyldiethyl decane): ammonia water = 1:0.01; preferably, it is continuously stirred at room temperature for about 12 to 24 hours, mixed thoroughly, and gradually in the open container There is a cementation around.
接續第二步驟，第三步驟係添加乾丙酮，以持續攪拌；較佳係於該開放容器內添加約10毫升之乾丙酮，並持續攪拌30~60分鐘。 Following the second step, the third step is to add dry acetone for continuous stirring; preferably about 10 ml of dry acetone is added to the open vessel and stirring is continued for 30 to 60 minutes.
之後，第四步驟係經熱處理程序，以去除該膠材混合液中所 含之醇類及水，形成一凝膠膠體。詳言之，本實施例遂以第一道熱處理程序去除醇類，熱處理溫度較佳約為70℃~80℃，以持續作用20~24小時，就此充份使該醇類得以自該膠材混合液中被蒸散；本實施例再以第二道熱處理程序去除水氣，並同時過濾該膠材混合液中所含微量氯化物，熱處理溫度較佳約為100℃~110℃，以持續作用24~36小時。 Thereafter, the fourth step is subjected to a heat treatment process to remove the mixture of the glue material Containing alcohol and water to form a gel colloid. In detail, in the present embodiment, the alcohol is removed by the first heat treatment process, and the heat treatment temperature is preferably about 70 ° C to 80 ° C for 20 to 24 hours, so that the alcohol can be sufficiently obtained from the rubber. The mixed solution is evaded; in this embodiment, the second heat treatment process is used to remove the water vapor, and at the same time, the trace chloride contained in the rubber mixture is filtered, and the heat treatment temperature is preferably about 100 ° C to 110 ° C for continuous action. 24~36 hours.
接續第四步驟所形成之凝膠膠體，第五步驟係再將該凝膠膠體作燒結，以形成固形之封裝膠材；較佳之燒結溫度為135℃~175℃，以於持續作用約24~36小時，直至完全去除該凝膠膠體中所含乙醇、水後，即可固形該凝膠膠體而得該封裝膠材。 Following the gel colloid formed in the fourth step, the fifth step is followed by sintering the gel colloid to form a solid encapsulated rubber; preferably, the sintering temperature is 135 ° C to 175 ° C for a sustained action of about 24~ After 36 hours, until the ethanol and water contained in the gel colloid are completely removed, the gel colloid can be solidified to obtain the encapsulated gel.
如此，經上述所製成之封裝膠材亦可應用於封裝發光二極體模組，以由固形之封裝膠材覆蓋於該發光二極體模組，並與第一實施例同樣透過傳統封裝手段予以完成；惟，經本發明第二實施例所製成之封裝膠材，係可選擇於未經燒結固化前，直接以凝膠狀態之凝膠膠體封裝該發光二極體模組，以提升封裝時之緻密性而可徹底隔絕水氣，此乃本領域技術人員於實際操作過程可加以選擇者，並不再此設限亦容不贅述。 Therefore, the packaged adhesive material prepared as described above can also be applied to the packaged light-emitting diode module to cover the light-emitting diode module by the solid package adhesive material, and is similar to the first embodiment through the conventional package. The method is completed; however, the encapsulating adhesive material prepared by the second embodiment of the present invention may be selected to directly encapsulate the light emitting diode module in a gel state in a gel state before being cured by sintering, thereby improving The tightness of the package can completely isolate the moisture, which can be selected by those skilled in the art in the actual operation process, and will not be further described herein.
為了證實本發明材料組成物用以製備成該封裝膠材，係可以使該封裝膠材具有緻密性及耐熱性，且不會因高溫環境而產生黃化、裂解等現象，且亦可阻隔水氣；是以，本發明係選擇將經由前述材料組成物所製成之封裝膠材用於封裝發光二極體模組，且進行以下實驗測試。 In order to prove that the material composition of the present invention is used for preparing the encapsulant, the encapsulant can be made dense and heat-resistant, and does not cause yellowing, cracking, etc. due to a high temperature environment, and can also block water. Therefore, in the present invention, the encapsulant made of the above material composition is selected for encapsulating the LED module, and the following experimental tests are performed.
請參閱第4a圖，其係為封裝膠材的穿透率比較圖。其中，a1為矽膠製成之封裝膠材，且其未經熱處理前、a2為矽膠製成之封裝膠材，且其經熱處理後；b1為本發明第一較佳實施例製成之封裝膠材，且其未經熱處理前、b2為本發明第一較佳實施例製成之封裝膠材，且其經熱處理後。由結果可知，當矽膠製成之封裝膠材經高溫長時間使用而出現黃化現象後，其穿透率明顯不佳；反之，本發明所製成之封裝膠材，其穿透率 皆係維持約為90%以上。 Please refer to Figure 4a, which is a comparison of the penetration ratio of the package adhesive. Wherein, a1 is a package adhesive made of silicone, and before it is not heat treated, a2 is a package adhesive made of silicone, and after heat treatment; b1 is an encapsulant made by the first preferred embodiment of the present invention; And before it is not subjected to heat treatment, b2 is an encapsulant made of the first preferred embodiment of the present invention, and after heat treatment. It can be seen from the results that when the encapsulant made of tannin is yellowed after being used for a long time at high temperature, the penetration rate is obviously not good; on the contrary, the encapsulation of the encapsulant made by the invention has a transmittance. Both are maintained at approximately 90%.
請參閱第4b圖，其係為封裝膠材的穿透率比較圖。其中，a1為矽膠製成之封裝膠材，且其未經熱處理前、a2為矽膠製成之封裝膠材，且其經250℃熱處理後、a3為矽膠製成之封裝膠材，且其經300℃熱處理後；b1為本發明第二較佳實施例製成之封裝膠材，且其未經熱處理前、b2為本發明第二較佳實施例製成之封裝膠材，且其經250℃熱處理後、a3為本發明第二較佳實施例製成之封裝膠材，且其經300℃熱處理後。由結果可知，當矽膠製成之封裝膠材經高溫長時間使用而出現黃化現象後，其穿透率明顯下降至75.2%與52.77%；反之，本發明所製成之封裝膠材，其經過熱處理後之穿透率仍皆維持約為90%以上。 Please refer to Figure 4b, which is a comparison of the penetration ratio of the package adhesive. Among them, a1 is a package adhesive made of tannin, and before it is not heat treated, a2 is a package adhesive made of tannin, and after heat treatment at 250 °C, a3 is a package adhesive made of tannin, and its After heat treatment at 300 ° C; b1 is a package adhesive made by the second preferred embodiment of the present invention, and before it is not heat treated, b2 is a package adhesive made of the second preferred embodiment of the present invention, and After the heat treatment at °C, a3 is a package adhesive made of the second preferred embodiment of the present invention, and after heat treatment at 300 °C. It can be seen from the results that when the encapsulant made of tannin has a yellowing phenomenon after being used for a long time at a high temperature, the transmittance is significantly reduced to 75.2% and 52.77%; otherwise, the encapsulant made by the present invention has The penetration rate after heat treatment is still maintained at about 90% or more.
請參閱第5a、5b圖，其係為經本發明第一較佳實施例所製成之封裝膠材的耐熱性示意圖。其中，第5a圖為各種溫度處理下的熱流示意圖；第5b圖為各種溫度處理下的材料熱重損失示意圖。由結果可知，當該封裝膠材作用參數為300℃、5小時，其熱重損失為27.2%；當該封裝膠材作用參數為800℃、5小時，其熱重損失為2.6%；當該封裝膠材作用參數為300℃、5小時候再經80℃、50小時，其熱重損失為7.4%。就此，係證實該封裝膠材確具有較佳耐熱性，而可應用於封裝發光二極體模組上，以長時間承受該發光二極體元件所發散之熱能，且不致劣化。 Please refer to Figures 5a and 5b, which are schematic diagrams showing the heat resistance of the encapsulant made by the first preferred embodiment of the present invention. Among them, Figure 5a is a schematic diagram of heat flow under various temperature treatments; Figure 5b is a schematic diagram of thermal weight loss of materials under various temperature treatments. It can be seen from the results that when the package rubber has a working parameter of 300 ° C for 5 hours, its thermogravimetric loss is 27.2%; when the package rubber has a working parameter of 800 ° C for 5 hours, its thermogravimetric loss is 2.6%; The package rubber has a working parameter of 300 ° C, and after 5 hours and then 80 ° C, 50 hours, its thermogravimetric loss is 7.4%. In this regard, it is confirmed that the encapsulating adhesive material has better heat resistance, and can be applied to the packaged LED module to withstand the heat energy radiated by the LED component for a long time without deterioration.
請參閱第6圖，其係為經本發明第一較佳實施例所製成之封裝膠材的耐熱性示意圖。其中，(a)為各種溫度處理下的DTA曲線；(b)為各種溫度處理下的材料熱重損失曲線。由結果可知，當該封裝膠材於300℃下進行熱處理時，其熱重損失約為99%，而在熱處理溫度提升至500℃時，該封裝膠材的熱重損失約在97%，相較下實際損失約1~3%。就此，經本發明第二較佳實施例所製成之封裝膠材與前述相同皆具有較佳耐熱性，而可應用於封裝發光二極體模組上，承受高溫而不致劣化。 Please refer to Fig. 6, which is a schematic view showing the heat resistance of the encapsulant made by the first preferred embodiment of the present invention. Among them, (a) is the DTA curve under various temperature treatments; (b) is the material thermogravimetric loss curve under various temperature treatments. It can be seen from the results that when the encapsulant is heat-treated at 300 ° C, the thermogravimetric loss is about 99%, and when the heat treatment temperature is raised to 500 ° C, the thermogravimetric loss of the encapsulant is about 97%. The actual loss is about 1 to 3%. In this regard, the encapsulant made by the second preferred embodiment of the present invention has the same heat resistance as the foregoing, and can be applied to the packaged LED module to withstand high temperature without deterioration.
綜上所述，本發明用以製備封裝膠材之材料組成物的主要特徵在於：藉由二甲基二乙氧基矽烷、甲基三乙氧基矽烷、四乙氧基矽烷等矽烷氧化物為製成該封裝膠材的反應物，遂可使製成之封裝膠材具有較佳耐熱及穿透性，並可透過甲醯胺、氨水等輔劑的共同作用，而致使成形後之封裝膠材能與發光二極體模組具有較佳結合緻密性，達到有效阻隔氧與水氣作用之功效。如此，本發明用以製備封裝膠材之材料組成物，不僅可以於低溫條件下利用中該材料組成物製成該封裝膠材，且該封裝膠材係能夠具有較佳耐熱性，以應用於封裝發光二極體模組，進一步承受該發光二極體元件所發散之熱能，避免該封裝膠材因高溫環境作用產生黃化、裂解等現象，達到延長封裝膠材使用壽命之功效；甚至，本發明還能夠透過該封裝膠材之緻密性，徹底阻隔水氣進入發光二極體模組內，以維持發光二極體元件的原有電性；並且，於長時間使用過程，仍可以維持該封裝膠材之較佳透光性，以提升該封裝膠材於應用上之穩定度。 In summary, the main feature of the material composition for preparing the encapsulating material of the present invention is that the decyl oxide is dimethyl decoxide, methyl triethoxy decane or tetraethoxy decane. In order to prepare the reaction material of the encapsulating material, the encapsulating adhesive prepared by the crucible can have better heat resistance and penetrability, and can cooperate with the auxiliary agent such as methotrexate and ammonia water to cause the package after forming. The rubber material can have better combination with the light-emitting diode module to achieve the effect of effectively blocking oxygen and water vapor. Thus, the present invention is used to prepare a material composition of the encapsulant, and the encapsulant can be made not only by using the material composition under low temperature conditions, but also the encapsulant can have better heat resistance for application. The packaged light-emitting diode module further receives the heat energy radiated by the light-emitting diode component, and avoids the yellowing and cracking of the packaged rubber material due to the high temperature environment, thereby achieving the effect of prolonging the service life of the package rubber; The invention can also completely block the moisture from entering the LED module through the compactness of the encapsulant, so as to maintain the original electrical properties of the LED component; and, during long-term use, the fiber can still be maintained. The encapsulating adhesive is preferably light transmissive to improve the stability of the encapsulating adhesive in application.
雖然本發明已利用上述較佳實施例揭示，然其並非用以限定本發明，任何熟習此技藝者在不脫離本發明之精神和範圍之內，相對上述實施例進行各種更動與修改仍屬本發明所保護之技術範疇，因此本發明之保護範圍當視後附之申請專利範圍所界定者為準。 While the invention has been described in connection with the preferred embodiments described above, it is not intended to limit the scope of the invention. The technical scope of the invention is protected, and therefore the scope of the invention is defined by the scope of the appended claims.
Claims (8)
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| DE102007057812A1 (en) * | 2007-11-30 | 2009-06-25 | Schott Ag | LED, has light converter comprising light conversion material for receiving output light and producing converted light, and sol gel glass, where light conversion material and filler are embedded in sol-gel glass |
| WO2012081411A1 (en) * | 2010-12-13 | 2012-06-21 | 東レ株式会社 | Phosphor sheet, led and light emitting device using same and method for producing led |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102007057812A1 (en) * | 2007-11-30 | 2009-06-25 | Schott Ag | LED, has light converter comprising light conversion material for receiving output light and producing converted light, and sol gel glass, where light conversion material and filler are embedded in sol-gel glass |
| WO2012081411A1 (en) * | 2010-12-13 | 2012-06-21 | 東レ株式会社 | Phosphor sheet, led and light emitting device using same and method for producing led |
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