Recent Advances in Encapsulation Materials for Light Emitting Diodes

1. Hamidnia M, Luo Y, Wang XD () Application of micro/nano technology for thermal management of high power LED packaging-a review. Appl Therm Eng 145:637–651

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2. Kalyani NT, Dhoble SJ () Organic light emitting diodes: energy saving lighting technology-a review. Renew Sust Energy Rev 16:–

3. Wu BS, Hitti Y, MacPherson S, Orsat V, Lefsrud MG () Comparison and perspective of conventional and LED lighting for photobiology and industry applications. Environ Exp Bot 171:

4. Alim MA, Abdullah MZ, Aziz MSA, Kamarudin R () Die attachment, wire bonding, and encapsulation process in LED packaging: a review. Sens Actuators A 329:

5. Deng Z, Wang M, Zhu C, Li C, Liu J, Tu M, Xie L, Gui D () Study on light aging of anhydride-cured epoxy resin used for RGB LED packaging material. Polym Test 80:

6. Zhan X, Zhang J, Wang X, Cheng J () Progress on silicone packaging materials for power LED. Procedia Eng 27:687–692

7. Chen Z, Liu Z, Shen G, Wen R, Lv J, Huo J, Yu Y () Effect of chain flexibility of epoxy encapsulants on the performance and reliability of light-emitting diodes. Ind Eng Chem Res 55:–

8. Tang B, Liu X, Zhao X, Zhang J () Highly efficient in situ toughening of epoxy thermosets with reactive hyperbranched polyurethane. J Appl Polym Sci 131:

9. Ma S, Liu W, Gao N, Yan Z, Zhao Y () Synthesis and properties of LED-packaging epoxy resin toughened by a novel polysiloxane from hydrolysis and condensation. Macromol Res 19:972–979

10. Liu Y, Luan X, Feng Y, Tan X, Han Y, Sun X () Self-adhesive epoxy modified silicone materials for light emitting diode encapsulation. Polym Adv Technol 28:–

11. Tong L, Feng Y, Sun X, Han Y, Jiao D, Tan X () High refractive index adamantane-based silicone resins for the encapsulation of light-emitting diodes. Polym Adv Technol 29:–

12. Kim Y, Kim S, Iqbal F, Yie H, Kim H () Effect of transmittance on luminescence properties of phosphor-in-glass for LED packaging. Opt Express 23:A43–A50

13. Ru Y, Zhang X, Wang L, Dai L, Yang W, Qiao J () Polymer composites with high haze and high transmittance. Polym Chem 6:–

14. Arik M, Becker CA, Weaver SE, Petroski J () Thermal management of LEDs: package to system. Proc SPIE :64–75

15. Yung KC, Liem H, Choy HS () Heat dissipation performance of a high-brightness LED package assembly using high-thermal conductivity filler. Appl Opt 52:–

16. Park BG, Myung WR, Lee CJ, Jung SB () Mechanical, electrical, and thermal reliability of Sn-58wt.% bi solder joints with ag-decorated MWCNT for LED package component during aging treatment. Composites Part B 182:

17. Zhao X, Hou Z, Wang B, Shen Q, Jia H, Zhang A, Liu X, Xu B () Synthesis, luminance and ultraviolet resistance of a copolymer phosphor of Eu-complex and siloxane in near UV-based LED. Res Chem Intermed 43:–

18. Wen R, Huo J, Lv J, Liu Z, Yu Y () Effect of silicone resin modification on the performance of epoxy materials for LED encapsulation. J Mater Sci Mater Electron 28:–

19. Chung PT, Yang CT, Wang SH, Chen CW, Chiang AST, Liu CY () ZrO2/epoxy nanocomposite for LED encapsulation. Mater Chem Phys 136:868–876

20. Gao N, Liu WQ, Ma SQ, Tang C, Yan Z () Cycloaliphatic epoxy resin modified by two kinds of oligo-fluorosiloxanes for potential application in light-emitting diode (LED) encapsulation. J Polym Res 19:1–10

21. Hsieh TH, Kinloch AJ, Taylor AC, Sprenger S () The effect of silica nanoparticles and carbon nanotubes on the toughness of a thermosetting epoxy polymer. J Appl Polym Sci 119:–

22. Ladani RB, Wu S, Kinloch AJ, Ghorbani K, Zhang J, Mouritz AP, Wang CH () Improving the toughness and electrical conductivity of epoxy nanocomposites by using aligned carbon nanofibres. Compos Sci Technol 117:146–158

23. Salom C, Prolongo MG, Toribio A, Martínez-Martínez AJ, de Cárcer IA, Prolongo SG () Mechanical properties and adhesive behavior of epoxy-graphene nanocomposites. Int J Adhes Adhes 84:119–125

24. Wu Z, Wang M, Wang Z () The gas phase SiO2/epoxy nanocomposites with enhanced mechanical and thermal properties. High Perform Polym 27:469–475

25. Sun Y, Liu W, Tan J, Wang H () Nano-and micro-structured random copolymer modified cycloaliphatic epoxy resins for use as light-emitting diode encapsulation. J Macromol Sci Part A 53:201–209

26. Gao N, Liu WQ, Ma SQ, Yan ZL, Zhao Y () Modification of epoxy resin with cycloaliphatic-epoxy oligosiloxane for light-emitting diode (LED) encapsulation application. J Macromol Sci Part B 51:–

27. Liu J, Ueda M () High refractive index polymers: fundamental research and practical applications. J Mater Chem 19:–

28. Higashihara T, Ueda M () Recent progress in high refractive index polymers. Macromolecules 48:–

29. Luo C, Zuo J, Zhao J () Synthesis and property of epoxy prepolymer and curing agent with high refractive index. High Perform Polym 25:986–991

30. Luo C, Zuo J, Wang F, Yuan Y, Lin F, Huang H, Zhao J () High refractive index and flame retardancy of epoxy thermoset cured by tris (2-mercaptoethyl) phosphate. Polym Degrad Stab 129:7–11

31. Chen G, Zhang Q, Hu Z, Wang S, Wu K, Shi J, Liang L, Lu M () Liquid crystalline epoxies bearing biphenyl ether and aromatic ester mesogenic units: synthesis and thermal properties. J Macromol Sci Part A 56:484–495

32. Zhang Q, Chen G, Wu K, Shi J, Liang L, Lu M () Biphenyl liquid crystal epoxy containing flexible chain: synthesis and thermal properties. J Appl Polym Sci 137:e

33. Yang X, Zhu J, Yang D, Zhang L, Guo Y, Zhong X, Kong J, Gu J () High-efficiency improvement of thermal conductivities for epoxy composites from synthesized liquid crystal epoxy followed by doping BN fillers. Composites Part B 185:

34. Islam AM, Lim H, You NH, Ahn S, Goh M, Hahn JR, Yeo H, Jang SG () Enhanced thermal conductivity of liquid crystalline epoxy resin using controlled linear polymerization. ACS Macro Lett 7:–

35. Anithambigai P, Chakravarthii MKD, Mutharasu D, Huong LH, Zahner T, Lacey D, Kamarulazizi I () Potential thermally conductive alumina filled epoxy composite for thermal management of high power LEDs. J Mater Sci Mater Electron 28:856–867

36. Chen Y, Hou X, Liao M, Dai W, Wang Z, Yan C, Li H, Lin C, Jiang N, Yu J () Constructing a “pea-pod-like” alumina-graphene binary architecture for enhancing thermal conductivity of epoxy composite. Chem Eng J 381:

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37. Chen X, Lim JSK, Yan W, Guo F, Liang YN, Chen H, Lambourne A, Hu X () Salt template assisted BN scaffold fabrication toward highly thermally conductive epoxy composites. ACS Appl Mater Interfaces 12:–

38. Lin CH, Whang WT, Chen CH et al () Novel siloxane-modified epoxy resins as promising encapsulant for LEDs. Polymers 12:21

39. Yurrita N, Aizpurua J, Cambarau W, Huang S, Chen K () Photovoltaic modules encapsulated in composite material modified with ultraviolet additives. Sol Energy Mater Sol Cells 230:

40. Gan Y, Jiang X, Yin J () Thiol-ene photo-curable hybrid silicone resin for LED encapsulation: enhancement of light extraction efficiency by facile self-keeping hemisphere coating. J Mater Chem C 2:–

41. Kim JS, Yang SC, Kwak SY, Choi YW, Paik KW, Bae BS () High performance encapsulant for light-emitting diodes (LEDs) by a sol-gel derived hydrogen siloxane hybrid. J Mater Chem 22:–

42. He Q, Li A, Zhang Y, Liu S, Guo Y, Kong L () A study on mechanical and tribological properties of silicone rubber reinforced with white carbon black. Tribol-Mater Surf Interfaces 12:9–16

43. Li Y, Chen Z, Li X, Zeng H () A new surface modification method to improve the dispersity of nano-silica in organic solvents. J Sol-Gel Sci Technol 58:290–295

44. Di M, He S, Li R, Yang D () Radiation effect of 150 keV protons on methyl silicone rubber reinforced with MQ silicone resin. Nucl Instr Meth Phys Res B 248:31–36

45. Pradhan B, Srivastava SK () Layered double hydroxide/multiwalled carbon nanotube hybrids as reinforcing filler in silicone rubber. Composites Part A 56:290–299

46. Ma W, Li J, Deng B, Lin X, Zhao X () Properties of functionalized graphene/room temperature vulcanized silicone rubber composites prepared by an in-situ reduction method. J Wuhan Univ Technol Mater Sci Ed 28:127–131

47. Hu H, Ma J, Li X, Yin Q, Fan L, Wei X, Peng Q, Yang J () Benzocyclobutene-functional double-decker silsesquioxane: self-assembled hybrid resin for high-performance dielectrics and LED encapsulants. Polym Chem 10:–

48. Lee S, Hong JY, Jang J () Multifunctional graphene sheets embedded in silicone encapsulant for superior performance of light-emitting diodes. ACS Nano 7:–

49. Zhang H, Lin Y, Zhang D, Wang W, Xing Y, Lin J, Hong H, Li C () Graphene nanosheet/silicone composite with enhanced thermal conductivity and its application in heat dissipation of high-power light-emitting diodes. Curr Appl Phys 16:–

50. Gao J, Bao F, Wu Q, Ma R, Han X, Jin D, Chen K, He J, Guo Z, Yan C () Multifunctional graphene filled silicone encapsulant for high-performance light-emitting diodes. Mater Today Commun 7:149–154

51. Gui D, Yu S, Xiong W, Cai X, Liu C, Liu J () Liquid crystal functionalization of graphene nanoplatelets for improved thermal and mechanical properties of silicone resin composites. RSC Adv 6:–

52. Zhao X, Zang C, Ma Q, Wen Y, Jiao Q () Thermal and electrical properties of composites based on (3-mercaptopropyl) trimethoxysilane-and cu-coated carbon fiber and silicone rubber. J Mater Sci 51:–

53. Yang D, Huang S, Ruan M, Li S, Yang J, Wu Y, Guo W, Zhang L () Mussel inspired modification for aluminum oxide/silicone elastomer composites with largely improved thermal conductivity and low dielectric constant. Ind Eng Chem Res 57:–

54. Xu S, Gao Q, Zhou C, Li J, Shen L, Lin H () Improved thermal stability and heat-aging resistance of silicone rubber via incorporation of UiO-66-NH2. Mater Chem Phys 274:

55. Wu S, Xiong Q, Li X, Chen D, Liu B () Properties of thermally conductive silicone rubbers filled with admicellar polymerized polypyrrole-coated Al2O3 particles. J Appl Polym Sci 138:

56. Pan Z, Zhu S, Huang B, Kang Y, Zhu L () Synthesis of high-refractive-index epoxy-modified vinyl methyl phenyl silicone resins for encapsulation of LEDs. J Electron Mater 48:–

57. Pan Z, Chen M, Zeng K, Kang Y () Synthesis of epoxy-modified methyl phenyl silicone resins for LED encapsulation. Silicon 14:–

58. Novak BM () Hybrid nanocomposite materials-between inorganic glasses and organic polymers. Adv Mater 5:422–433

59. Tao P, Li Y, Siegel RW, Schadler LS () Transparent dispensible high-refractive index ZrO2/epoxy nanocomposites for LED encapsulation. J Appl Polym Sci 130:–

60. Mont FW, Kim JK, Schubert MF, Schubert EF, Siegel RW () High-refractive-index TiO2-nanoparticle-loaded encapsulants for light-emitting diodes. J Appl Phys 103:

61. Ding KH, Wang GL, Zhang M () Preparation and optical properties of transparent epoxy composites containing ZnO nanoparticles. J Appl Polym Sci 126:734–739

62. Im H, Kim J () Thermal conductivity of a graphene oxide-carbon nanotube hybrid/epoxy composite. Carbon 50:–

63. Agrawal A, Satapathy A () Epoxy composites filled with micro-sized AlN particles for microelectronic applications. Part Sci Technol 33:2–7

64. Constantinescu DM, Apostol DA, Picu CR, Krawczyk K, Sieberer M () Mechanical properties of epoxy nanocomposites reinforced with functionalized silica nanoparticles. Procedia Struct Integr 5:647–652

65. Lai Y, Jin L, Hang J, Sun X, Shi L () Highly transparent thermal stable silicone/titania hybrids with high refractive index for LED encapsulation. J Coat Technol Res 12:–

66. Zhan X, Xing Q, Liu H, Zhang J, Cheng J, Lin X () A facile method for fabrication of titanium-doped hybrid materials with high refractive index. RSC Adv 4:–

67. Huang Y, Feng Y, Sun X, Han Y, Liu D, Tan X () Preparation of ZrO2/silicone hybrid materials for LED encapsulation via in situ sol-gel reaction. Polym Adv Technol 30:–

68. Kim YH, Bae JY, Jin J, Bae BS () Sol-gel derived transparent zirconium-phenyl siloxane hybrid for robust high refractive index LED encapsulant. ACS Appl Mater Interfaces 6:–

69. Yang Y, Li YQ, Shi HQ, Li WN, Xiao HM, Zhu LP, Luo YS, Fu SY, Liu TX () Fabrication and characterization of transparent ZnO-SiO2/silicone nanocomposites with tunable emission colors. Composites Part B 42:–

70. Trung NN, Luu QP, Son BT, Sinh LH, Bae JY () Preparation and characterization of silicone resin nanocomposite containing CdSe/ZnS quantum dots. Polym Compos 33:–

71. Cheng Y, Lu C, Yang B () A review on high refractive index nanocomposites for optical applications. Recent Pat Mater Sci 4:15–27

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Saabluster,

Nice work with encapsulating the XR-E emitters. I have been watching this in excitement to see what happens when a flashaholic has control over the emitter dome shape. BTW, how have these mods affected overall lumen output compared to before the mod? I personally lost domes off of two Rebel emitters and it seems like the phosphor was perfectly intact and the LED operational. The K2, and the Cree products still use bond wires that would be torn after removing the die. Hopefully, regardless of the emitter used, domes will not have to be removed in your experiments. Clean silicone domes of the XP-E, XP-G, and Rebel might disappear when you goop your silicone gel over top of it (so dome removal may be unnecessary).

So, I was just wondering why the encapsulated XR-E (dome removed) with the acrylic lens did better than the one without. Is it an issue with different indexes of refraction? Is it because the acrylic lens has a smoother surface?

You may have stumbled on something good for aspheric lens users, but I think before you should start selling these in large quantities, you should do more testing. I think that members would love to see comparisons between 3-4 new XR-E emitters from the same batch. Who knows, maybe your modded emitter without the lens degraded some, and if in better shape, could have perform the best. Having new emitters that perform the same from the start will help produce more conclusive tests in a more scientific fashion. (I understand the preliminary experiments with spare XR-Es). BTW, does the Deft use a high quality current regulator so even big changes in LED forward voltage will not affect output? I was just wondering.

Between the two modified XR-E emitters, I guess I do not understand why they are so different. Why not remove the ring and then re-encapsulate the emitter? Why not re-encapsulate a Rebel, XP-E or XP-G? I see that the consistency of the optical grade silicone gel causes your "dome" to sag before it cures, but why not let gravity aid you? I do not know its viscosity or its values for surface tension, but maybe when held upside down, a dome might form a geometric shape in your favor (parabolic, spherical, elliptical, or catenary). If you are going for flatness, then why not temporarily fix it to the center flat spot of an old brushless PC cooling fan and let centripetal forces level off the top of the dome some? If the viscosity is high enough and you make the fan spin slow enough, you may get a very flat surface. As you spin it faster it may begin forming a parabolic dip in the center (like what happens with those experimental spinning mercury mirrors). You have a lot of control over the shape of this dome; that is awesome.

If that acrylic lens is the ultimate solution, then why not take an old Cree XR-E metal ring (or a spacer with the same height) and fix it above a Rebel, XP-E, or even XP-G then fix on the acrylic lens? Maybe a modded XP-G would produce a projected beam (in the Deft) of the same size as an un-modded XR-E from your existing setup (I am being hopeful here).

I am just asking that you try different setups with other emitters. We all bow to you since you have the optical grade silicone gel and experience. I like the XR-E, but have always been doubtful to the metal ring from the optical standpoint (I understand the mechanical purposes). If you can make a new dome over the tiny Rebel, XP-E, and XP-G, you might be able to shape the dome to do the same thing that the glass dome on the XR-E did, or you may be able to shrink down the apparent die size (flatten the dome) without sacrificing the total lumen output.

I always found the tint shift interesting. I also worry that the tint shift, while being pleasant to the eyes, may be bad for efficiency or overall longevity. It seems like a major change happens when the tint shift occurs, and it could be a bad change. Does it mean that more blue light is internally reflected back to the phosphor coating to produce reds
(due to the change in index of refraction), or does it maybe affect how heat is removed from the top of the light which affects the efficiency of the phosphors?

You could theoretically can cut rebel emitters down (the ceramic substrate) without affecting the etched traces to position the four dies tightly together so they almost touch (electrically, they could touch if you plan on wiring the dies in parallel). Just re-encapsulate them (or not if you cut cleanly) and this could equate into a quad TFFC die emitter. Its not a practical mod (with the MC-E, P7, and SST-50 out there), but I dream that it could be done.

Cheers,
-Tony