有機(jī)硅微球的制備與折射率調(diào)控及其光散射性能的研究
發(fā)布時(shí)間：2018-09-13 10:50
【摘要】：LED照明節(jié)能、高效、體積小、長壽、環(huán)保等。同樣亮度下,LED照明能耗僅為白熾燈照明的1/10,熒光燈照明的1/4。LED照明取代白熾燈及熒光燈照明優(yōu)勢明顯。然而,LED發(fā)光強(qiáng)度高,光線較為集中,需要一個(gè)良好光擴(kuò)散性能的燈罩使其光線發(fā)散均勻。因此,研究制備高性能的光散射材料并應(yīng)用于大功率LED照明系統(tǒng)中,具有重要的實(shí)用價(jià)值。有機(jī)硅微球由于熱穩(wěn)定性好,尺寸穩(wěn)定性佳,粒徑和折射率可以通過化學(xué)反應(yīng)來調(diào)控的特點(diǎn),作為光擴(kuò)散粒子應(yīng)用于光擴(kuò)散材料具有十分廣闊的應(yīng)用前景。本文以甲基三甲氧基硅烷(MTMS)、苯基三甲氧基硅烷(PTMS)為原料,采用水解-縮聚法成功制備了分散性優(yōu)異的PMTMS和PPTMS有機(jī)硅微球。對(duì)反應(yīng)體系中反應(yīng)參數(shù):如單體濃度、氨水用量、溫度和攪拌速度等條件對(duì)微球形貌及粒徑分布的影響進(jìn)行了研究。采用掃描電子顯微鏡(SEM)、熱重分析儀(TGA)、傅里葉變換紅外光譜(FT-IR)等方法對(duì)微球進(jìn)行表征。進(jìn)一步,本文以MTMS和PTMS共聚制備了折射率從1.3851到1.5081可調(diào)的有機(jī)硅微球。并將得到的微球與環(huán)氧樹脂E51及聚碳酸酯(PC)復(fù)合,制備了2mm厚的光擴(kuò)散材料。所得結(jié)果如下:(1)影響微球形貌的主要因素是單體濃度和氨水濃度。隨著反應(yīng)體系中單體濃度的增加,微球的平均粒徑逐漸增大,單體濃度較高時(shí),微球容易發(fā)生團(tuán)聚;氨水用量增加,催化反應(yīng)速率較快,成核數(shù)增多,最終形成微球的平均粒徑減小。當(dāng)氨水濃度較低的情況下,硅氧烷單體水解不完全,縮聚程度不高,不易形成微球。當(dāng)反應(yīng)體系的pH為8～11時(shí),能夠得到分散性良好的有機(jī)硅微球。采用種子法研究了 PPTMS微球的生長過程,發(fā)現(xiàn),硅氧烷在瞬間大量成核,接著核繼續(xù)生長,向反應(yīng)體系中補(bǔ)加單體后,并沒有出現(xiàn)新核的形成。(2)對(duì)環(huán)氧樹脂光擴(kuò)散材料的透光率和霧度結(jié)果進(jìn)行分析,得出:隨著微球折射率的減小及摻雜濃度的增加,環(huán)氧樹脂復(fù)合光擴(kuò)散材料霧度增高,透光率降低。當(dāng)采用微球粒徑為1.05 μm,摻雜濃度為0.1 phr時(shí),2 mm厚的光擴(kuò)散片的透光率為83.6%,霧度為95.5%。(3)對(duì)PC光擴(kuò)散材料的光擴(kuò)散性能進(jìn)行了研究,并對(duì)實(shí)驗(yàn)數(shù)據(jù)與理論模擬結(jié)果進(jìn)行了對(duì)比分析,發(fā)現(xiàn):當(dāng)微球相對(duì)于PC的折射率為0.91～0.93時(shí),有機(jī)硅微球與PC折射率匹配較好,能有效地解決透光率與霧度之間的矛盾,此時(shí),能夠制備出高透光率與高霧度的光擴(kuò)散材料。當(dāng)微球粒徑為1.7 μm,折射率為1.458(相對(duì)折射率為0.92),填充濃度為0.4 phr時(shí),厚度為2 mm的光擴(kuò)射材料總透光率為87.9%,霧度為98.5%。
[Abstract]:LED lighting energy saving, high efficiency, small size, longevity, environmental protection and so on. Under the same brightness, the energy consumption of 1/4.LED lighting is only 1 / 10 of that of incandescent lighting, and the 1/4.LED lighting of fluorescent lighting has obvious advantages in replacing incandescent and fluorescent lighting. However, the light intensity of LED is high and the light is concentrated, so it needs a lampshade with good light diffusivity to spread the light evenly. Therefore, it is of great practical value to study the preparation of high performance light scattering materials and their application in high power LED lighting systems. Because of its good thermal stability and good dimensional stability, the size and refractive index of organosilicon microspheres can be controlled by chemical reaction. In this paper, PMTMS and PPTMS organosilicon microspheres with excellent dispersity were prepared by hydrolysis-condensation method from methyl trimethoxy silane (MTMS), phenyl trimethoxy silane (PTMS). The effects of reaction parameters, such as monomer concentration, amount of ammonia water, temperature and stirring speed, on the morphology and particle size distribution of microspheres were studied. The microspheres were characterized by scanning electron microscope (SEM) (SEM), thermogravimetric analyzer (TGA),) Fourier transform infrared spectroscopy (FT-IR). Furthermore, organosilicon microspheres with adjustable refractive index from 1.3851 to 1.5081 were prepared by MTMS and PTMS copolymerization. The obtained microspheres were compounded with epoxy resin E51 and polycarbonate (PC) to prepare 2mm thick photodiffusion materials. The results are as follows: (1) the main factors affecting the morphology of the microspheres are monomer concentration and ammonia concentration. With the increase of monomer concentration in the reaction system, the average particle size of the microspheres gradually increased. When the monomer concentration was higher, the microspheres were easy to agglomerate, and the amount of ammonia increased, the catalytic reaction rate was faster, and the nucleation number increased. The average particle size of the resulting microspheres was reduced. When the concentration of ammonia is low, the hydrolysis of siloxane monomer is not complete, the degree of condensation is not high, and it is not easy to form microspheres. When the pH of the reaction system is 8 ~ 11:00, the organosilicon microspheres with good dispersion can be obtained. The growth process of PPTMS microspheres was studied by means of seed method. It was found that the nucleation of siloxane was in a large quantity in the instant, then the nucleus continued to grow, and the monomer was added to the reaction system. (2) the results of light transmittance and haze of epoxy resin photodiffusion materials are analyzed. It is concluded that with the decrease of refractive index of epoxy resin and the increase of doping concentration, the fog of epoxy resin composite photodiffusion materials increases. The transmittance decreases. When the diameter of microspheres is 1.05 渭 m and the concentration of doping is 0.1 phr, the transmittance of the photodiffuser with 2 mm thickness is 83.6 and the fog is 95.55.3.The photodiffusion properties of PC photodiffusion materials are studied, and the experimental data and theoretical simulation results are compared and analyzed. It is found that when the refractive index of microspheres relative to PC is 0.91-0.93, the refractive index of organosilicon microspheres and PC is better matched, and the contradiction between transmittance and haze can be effectively solved. In this case, the optically diffused materials with high transmittance and high fog can be prepared. When the diameter of microspheres is 1.7 渭 m, the refractive index is 1.458 (relative refractive index is 0.92) and the filling concentration is 0.4 phr, the total transmittance of the diffused materials with thickness of 2 mm is 87.9 and the fog is 98.5.
【學(xué)位授予單位】：深圳大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類號(hào)】：O634.41
本文編號(hào)：2240964
[Abstract]:LED lighting energy saving, high efficiency, small size, longevity, environmental protection and so on. Under the same brightness, the energy consumption of 1/4.LED lighting is only 1 / 10 of that of incandescent lighting, and the 1/4.LED lighting of fluorescent lighting has obvious advantages in replacing incandescent and fluorescent lighting. However, the light intensity of LED is high and the light is concentrated, so it needs a lampshade with good light diffusivity to spread the light evenly. Therefore, it is of great practical value to study the preparation of high performance light scattering materials and their application in high power LED lighting systems. Because of its good thermal stability and good dimensional stability, the size and refractive index of organosilicon microspheres can be controlled by chemical reaction. In this paper, PMTMS and PPTMS organosilicon microspheres with excellent dispersity were prepared by hydrolysis-condensation method from methyl trimethoxy silane (MTMS), phenyl trimethoxy silane (PTMS). The effects of reaction parameters, such as monomer concentration, amount of ammonia water, temperature and stirring speed, on the morphology and particle size distribution of microspheres were studied. The microspheres were characterized by scanning electron microscope (SEM) (SEM), thermogravimetric analyzer (TGA),) Fourier transform infrared spectroscopy (FT-IR). Furthermore, organosilicon microspheres with adjustable refractive index from 1.3851 to 1.5081 were prepared by MTMS and PTMS copolymerization. The obtained microspheres were compounded with epoxy resin E51 and polycarbonate (PC) to prepare 2mm thick photodiffusion materials. The results are as follows: (1) the main factors affecting the morphology of the microspheres are monomer concentration and ammonia concentration. With the increase of monomer concentration in the reaction system, the average particle size of the microspheres gradually increased. When the monomer concentration was higher, the microspheres were easy to agglomerate, and the amount of ammonia increased, the catalytic reaction rate was faster, and the nucleation number increased. The average particle size of the resulting microspheres was reduced. When the concentration of ammonia is low, the hydrolysis of siloxane monomer is not complete, the degree of condensation is not high, and it is not easy to form microspheres. When the pH of the reaction system is 8 ~ 11:00, the organosilicon microspheres with good dispersion can be obtained. The growth process of PPTMS microspheres was studied by means of seed method. It was found that the nucleation of siloxane was in a large quantity in the instant, then the nucleus continued to grow, and the monomer was added to the reaction system. (2) the results of light transmittance and haze of epoxy resin photodiffusion materials are analyzed. It is concluded that with the decrease of refractive index of epoxy resin and the increase of doping concentration, the fog of epoxy resin composite photodiffusion materials increases. The transmittance decreases. When the diameter of microspheres is 1.05 渭 m and the concentration of doping is 0.1 phr, the transmittance of the photodiffuser with 2 mm thickness is 83.6 and the fog is 95.55.3.The photodiffusion properties of PC photodiffusion materials are studied, and the experimental data and theoretical simulation results are compared and analyzed. It is found that when the refractive index of microspheres relative to PC is 0.91-0.93, the refractive index of organosilicon microspheres and PC is better matched, and the contradiction between transmittance and haze can be effectively solved. In this case, the optically diffused materials with high transmittance and high fog can be prepared. When the diameter of microspheres is 1.7 渭 m, the refractive index is 1.458 (relative refractive index is 0.92) and the filling concentration is 0.4 phr, the total transmittance of the diffused materials with thickness of 2 mm is 87.9 and the fog is 98.5.
【學(xué)位授予單位】：深圳大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類號(hào)】：O634.41
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