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Method and device for auxiliary sublimation and purification of inert solid particles

A solid particle, inert technology, applied in the field of inert solid particle assisted sublimation purification, can solve the problems of target product degradation, low thermal conductivity of organic materials, unfavorable heat conduction, etc. Effect

Inactive Publication Date: 2021-04-27
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Because the high vacuum inside the sublimation device is not conducive to heat conduction, and the thermal conductivity of organic materials is low, the heating of crude products is usually uneven
Excessive temperature may lead to degradation of the target product and generation of new impurities
Therefore, the uniformity of heating can only be ensured by reducing the amount of filler, which greatly reduces the efficiency of sublimation

Method used

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  • Method and device for auxiliary sublimation and purification of inert solid particles

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Experimental program
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Effect test

Embodiment 1

[0025] Inert solid particles assisted sublimation purification compound TCTA;

[0026] The sublimation instrument used in this method is Hangzhou Saiweisi SVC-60.

[0027] Concrete purification steps are as follows:

[0028] 5.00 g of 4,4', 4"-tris(carbazol-9-yl) triphenylamine crude product and 1.00 g of high-purity silica (Shanghai Aladdin Biochemical Technology Co., Ltd. AR, 3-10 mesh, 2-7mm ) to mix evenly; add it to the sublimation instrument, and set the sublimation instrument parameters to: the first section of sublimation temperature t 1 =240℃, the second stage t 2 =180℃, the third stage t 3 =110°C, the pressure is P=1.0*10 -6 Pa, sublimated for 12 hours. 1.32 g of pure product were obtained.

Embodiment 2

[0030] Preparation of organic light-emitting diodes;

[0031] Take the pre-made indium tin oxide (ITO) glass with a sheet resistance of 15Ω, clean it with acetone, detergent, deionized water and isopropanol in sequence, and treat it with plasma for 10 minutes. Then, in the vacuum evaporation equipment, 2,3,6,7,10,11-hexacyano-1,4,5,8,9,12-hexaazabenzo Phenanthrene (HATCN) as the hole injection layer, 40nm thick 4,4',4"-tris(carbazol-9-yl)triphenylamine (TCTA) as the exciton blocking layer, 20nm thick 9'-(1, 3-Phenyl)bis-9H-carbazole (mCP) and Ir(mPPy)3 (95:5 mass percent) mixed film as the light-emitting layer, 40nm thick 1,3,5-tris(1-phenyl- 1H-benzimidazol-2-yl)benzene (TPBi) is used as the electron transport layer, 1nm thick lithium fluoride (LiF) is used as the electron injection layer, and 100nm thick aluminum (Al) is used as the cathode. The device structure is: ITO / HATCN / TCTA / mCP:Ir(mPPy) 3=95:5 / TPBi / LiF / Al.The high-purity quartz sand of particle size 1-3mm is added ...

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Abstract

The invention discloses a method and a device for auxiliary sublimation and purification of inert solid particles. According to the invention, inert solid particles are mixed with a to-be-sublimated organic material, so that the effects of heat conduction and explosion boiling prevention are achieved in the sublimation process, steam can be stably generated, the situations of degradation and impurity evaporation caused by uneven heating in the sublimation process are effectively prevented, and a sublimation product with high purity can be obtained.

Description

technical field [0001] The invention belongs to the technical field of organic photoelectric materials, and in particular relates to a method and device for inert solid particle assisted sublimation purification. Background technique [0002] Organic light-emitting diodes (OLEDs) have attracted extensive attention due to their advantages of flexibility, active light emission, high efficiency, low-voltage drive, and easy fabrication of large-area devices. OLED-related research can be traced back to the 1960s. In 1963, Professor Pope of New York University discovered the electroluminescence phenomenon of organic molecular single crystal anthracene for the first time, and then some single crystal structure materials have electroluminescence properties. However, due to the high driving voltage of the device at that time, it failed to attract widespread attention. It was not until 1987 that Dr. Deng Qingyun and others from Kodak Company of the United States produced OLED devices...

Claims

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Application Information

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IPC IPC(8): B01D7/00
CPCB01D7/00
Inventor 应磊曹镛
Owner SOUTH CHINA UNIV OF TECH
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