Method and apparatus for purifying organic material using ionic liquid

Patent metadata

Field	Value
Publication number	US-2016193543-A1
Application number	US-201314653612-A
Country	US
Kind code	A1
Filing date	Dec 17, 2013
Priority date	Dec 18, 2012
Publication date	Jul 7, 2016
Grant date	—

Abstract

Disclosed is a simplified apparatus for purifying an organic material using an ionic liquid, including a sublimation unit for sublimating a raw organic material containing impurities for OLEDs by heating; a recrystallization unit for recrystallizing the sublimated gas of the organic material in the ionic liquid; and a control unit for controlling the operation of the sublimation unit and the recrystallization unit. Even when a very small amount of organic material is sublimated, the recrystallization thereof in the ionic liquid can be verified, thus easily checking the purification potential of the organic material using only a very small amount of organic material.

First claim

1 . A simplified method of purifying an organic material using an ionic liquid, which uses a simplified apparatus for purifying an organic material comprising a healing chamber in a vacuum atmosphere including a crucible for receiving a raw organic material containing impurities for an organic light emitting diode (OLED), and a substrate disposed in the heating chamber and coated with an ionic liquid, the simplified method comprising:
heating the crucible to a sublimation point of the raw organic material, thus generating a sublimated gas of the raw organic material; depositing the sublimated gas of the raw organic material on the ionic liquid; and recrystallizing the sublimated gas in the ionic liquid.

2 . The simplified method of claim 1 , further comprising separating the recrystallized organic material from the ionic liquid, after the recrystallizing.

3 . The simplified method of claim 1 , wherein, in the recrystallizing, a temperature of the ionic liquid is adjusted to control a solubility of the ionic liquid.

4 . The simplified method of claim 1 , wherein, in the recrystallizing, a temperature of the substrate is maintained in a range from room temperature to 200° C.

5 . A simplified apparatus for purifying an organic material using an ionic liquid, comprising:
a sublimation unit in a vacuum atmosphere for heating a raw organic material containing impurities for an organic light emitting diode (OLED) so as to be sublimated; a recrystallization unit in a vacuum atmosphere for depositing a sublimated gas of the organic material on a surface of the ionic liquid so as to be recrystallized in the ionic liquid; and a control unit for controlling operation of the sublimation unit and the recrystallization unit.

6 . The simplified apparatus of claim 5 , wherein the sublimation unit comprises a crucible for receiving the raw organic material, a heating chamber in which the crucible is disposed and which has a predetermined inner volume, a vacuum pump for evacuating an inside of the heating chamber, a first heater for heating the crucible, and a shutter for selectively opening or closing a top of the crucible.

7 . The simplified apparatus of claim 6 , wherein the shutter is provided to cover the top of the crucible, or is formed to cover the top of the crucible at a predetermined distance therefrom.

8 . The simplified apparatus of claim 6 , wherein the recrystallization unit comprises a substrate coated with the ionic liquid, a mask for supporting the substrate, a second heater fixed to an upper portion of the heating chamber, and a support member formed under the second heater to support the mask.

9 . The simplified apparatus of claim 8 , wherein the recrystallization unit further comprises a thermocouple provided to the support member to measure a temperature of the substrate, and
the control unit controls a temperature of the second heater using the temperature measured by the thermocouple.

10 . The simplified apparatus of claim 5 , wherein the ionic liquid is applied in droplet form on the substrate.

11 . The simplified apparatus of claim 5 , further comprising an analysis unit for analyzing a purified material recrystallized in the ionic liquid via photography.

12 . The simplified apparatus of claim 11 , wherein the analysis unit comprises a thickness monitor for measuring a thickness of the recrystallized purified material.

13 . A method of purifying an organic material using an ionic liquid, which uses an apparatus for purifying an organic material comprising a heating chamber in a vacuum atmosphere including a crucible for receiving a raw organic material containing impurities for an organic light emitting diode (OLED), and a storage tank containing the ionic liquid in a vacuum atmosphere, the method comprising:
heating the crucible to a sublimation point of the raw organic material, thus generating a sublimated gas of the raw organic material; inducing the sublimated gas of the raw organic material to flow into the ionic liquid of the storage tank; and dissolving and recrystallizing, in the ionic liquid, the sublimated gas incorporated into the ionic liquid.

14 . The method of claim 13 , wherein, in the inducing the sublimated gas of the raw organic material to flow, the sublimated gas is induced to flow into the ionic liquid using an inert gas that is supplied into the heating chamber.

15 . The method of claim 14 , further comprising discharging from the storage tank the inert gas that was not dissolved but was collected in an upper portion of the storage tank, after the dissolving.

16 . The method of claim 15 , further comprising recovering the recrystallized organic material from the ionic liquid, after the recrystallizing.

17 . The method of claim 15 , further comprising heating a gas mixture so as to maintain a temperature equal to or higher than the sublimation point, before incorporating the gas mixture into the ionic liquid.

18 . The method of claim 15 , wherein, in the recrystallizing, a temperature of the ionic liquid is adjusted to control a solubility of the ionic liquid.

19 . The method of claim 15 , wherein the inert gas discharged in the discharging is reused as the inert gas that is supplied in mixing.

20 . An apparatus for purifying an organic material using an ionic liquid, comprising:
a sublimation unit in a vacuum atmosphere for healing a raw organic material containing impurities for an organic light emitting diode (OLED) so as to be sublimated; a recrystallization unit in a vacuum atmosphere for incorporating a sublimated gas of the organic material into the ionic liquid so as to be recrystallized in the ionic liquid; and a control unit for controlling operation of the sublimation unit and the recrystallization unit.

21 . The apparatus of claim 20 , wherein the sublimation unit comprises a crucible for receiving the raw organic material, a heating chamber in which the crucible is disposed and which has a predetermined inner volume, a vacuum pump for evacuating an inside of the heating chamber, a first heater for heating the crucible, and an inert gas supply source connected to one side of the heating chamber to supply the inert gas.

22 . The apparatus of claim 21 , wherein the recrystallization unit comprises a storage tank containing the ionic liquid, a connection conduit, one side of which communicates with an inside of the heating chamber and the other side of which is immersed in the ionic liquid of the storage tank, a vacuum pump for evacuating an inside of the storage tank, and a discharge pump for discharging from the storage tank the gas accumulated on the ionic liquid of the storage tank.

23 . The apparatus of claim 22 , further comprising a second heater for heating a periphery of the connection conduit so as to maintain a sublimation point of the organic material.

24 . The apparatus of claim 22 , further comprising a third heater for heating a lower portion of the storage tank containing the ionic liquid to control a solubility of the organic material.

25 . The apparatus of claim 24 , further comprising an ionic liquid collector provided at an upper portion of the storage tank so that the ionic liquid used for purifying the organic material is collected so as to be reused through heating to a predetermined temperature or higher in a vacuum, evaporation, and separation from the impurities and the dissolved organic material.

Assignees

• Korea Ind Tech Inst

Inventors

• Kim Tae Won
• Lee Jong Ho
• Park Jae Cheol

Classifications

• B01D7/02 Primary

  Crystallisation directly from the vapour phase (into single crystals C30B23/00) · CPC title

• B01D7/00 Primary

  Sublimation (B01D8/00 takes precedence; freeze-drying F26) · CPC title

• H01L51/0025

  Electricity · mapped topic

• H01L51/5056

  Electricity · mapped topic

• H01L51/0059

  Electricity · mapped topic