• 专利标题:   Preparation of conductive adhesive for high-power light-emitting-diode package, involves adding epoxy resin and toughening agent to mixing chamber, dispersing mixture, adding functional graphene material and stirring mixture.
  • 专利号:   CN107513359-A
  • 发明人:   LI N, LI F, HE G, ZHANG L
  • 专利权人:   YANTAI SEAYU NEW MATERIALS CO LTD
  • 国际专利分类:   C09J011/04, C09J011/08, C09J163/00, C09J009/02
  • 专利详细信息:   CN107513359-A 26 Dec 2017 C09J-163/00 201813 Pages: 11 Chinese
  • 申请详细信息:   CN107513359-A CN10917074 30 Sep 2017
  • 优先权号:   CN10917074

▎ 摘  要

NOVELTY - 30-50 pts. wt. Epoxy resin and 2-10 pts. wt. toughening agent are sequentially added to twin planetary power mixing chamber, stirred at 15-25 rpm and high-speed dispersed at 15-30 degrees C and 800-1500 rpm for 1 hour. 5-10 pts. wt. Self-made functional graphene material is added to mixture and stirred for 1 hour. 30-70 pts. wt. Conductive silver is added to mixture and stirred for 30 minutes. 5-20 pts. wt. Latent curing agent is added to mixture and stirred for 1 hour. Fumed silica is added to mixture and stirred for 1 hour, to obtain high-thermal-conductivity conductive adhesive. USE - Preparation of high-thermal-conductivity conductive adhesive used for high-power light-emitting-diode package. ADVANTAGE - The method enables preparation of conductive adhesive with high thermal conductivity by simple and economical method. The light-emitting-diode package formed using the conductive adhesive has excellent strength, high-temperature resistance and heat conducting characteristics, and low shrinkage. DETAILED DESCRIPTION - 30-50 pts. wt. Epoxy resin and 2-10 pts. wt. toughening agent are sequentially added to twin planetary power mixing chamber, stirred at 15-25 rpm and high-speed dispersed at 15-30 degrees C and 800-1500 rpm for 1 hour. 5-10 pts. wt. Self-made functional graphene material is added to mixture and stirred for 1 hour. 30-70 pts. wt. Conductive silver is added to mixture and stirred for 30 minutes. 5-20 pts. wt. Latent curing agent is added to mixture and stirred for 1 hour. 0-2 pts. wt. Fumed silica is added to mixture and stirred for 1 hour. The vacuum pump is opened and vacuum pressure of 0.01-0.098 MPa is maintained for 1 hour, to obtain high-thermal-conductivity conductive adhesive. The epoxy resin comprises 3,4-epoxycyclohexylmethyl-3',4'-epoxycyclohexane carboxylate, 4,5-epoxycyclohexane-1,2-diglycidyl diglycidyl ester, bisphenol-A epoxy resin, bisphenol-F epoxy resin and/or phenol resin. The toughening agent comprises nitrile rubber, core shell toughening agent comprising Kane Ace MX-125 (RTM: bisphenol A liquid epoxy resin), Initialcreate ICAM-8627 (RTM: core-shell rubber) and/or S-2001-type toughening agent. The latent curing agent comprises dicyandiamide, Addison EH-4360S (RTM: low-chlorine epoxy resin), EH-4357S (RTM: low-chlorine epoxy resin), Ajinomoto PN-H (RTM: epoxy resin), Ajinomoto PN-23 (RTM: epoxy resin) and/or 1020-type latent curing agent. The fumed silica comprises CAB-O-SIL TS-720 (RTM: fumed silica), CAB-O-SIL EH-5 (RTM: fumed silica), Aerosil R202 (RTM: fumed silica) and/or AEROSIL A200 (RTM: fumed silica). The self-made functionalized graphene material is prepared by preparing scale graphene solution by adding 105.8 g concentrated sulfuric acid to dry 500 ml round-bottomed flask, adding mixture to ice water bath at 2-8 degrees C, adding 1.25 g sodium nitrate and 2.5 g scale graphene and stirring mixture for 1 hour to obtain solution (s1), adding 1.25 g potassium permanganate to solution (s1), stirring mixture in ice-water bath at 2-8 degrees C for 2 hours, heating mixture at 30-40 degrees C for 4 hours, dripping 115 ml deionized water, heating mixture at 98 degrees C, reacting mixture for 30 minutes, adding 0.35 L water and 6.25 ml 30% hydrogen peroxide solution until the color of dispersion is changed from brown to bright yellow, filtering mixture, washing precipitate with 0.5-0.75 L hydrochloric acid, loading precipitate to dialysis bag, dialyzing precipitate in deionized water until neutral, adding 0.26 g precipitate to 100 ml deionized water and ultrasonically processing mixture at 200 W for 3 hours to obtain graphene oxide dispersion, preparing functionalized graphene solution by weighing and dissolving 2.35 g benzidine in 30 ml absolute ethanol, mixing mixture with graphene oxide dispersion, adding mixture to conical flask, refluxing mixture at 90 degrees C for 10 hours, adding 0.5 ml hydrazine hydrate, continuously refluxing mixture for 10 hours, filtering mixture with polypropylene filter membrane having pore size of 0.22 mu m, washing residue with absolute ethanol for three times and drying residue.