# US 7,611,548 B2 · Vertical sublimation apparatus

> Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt

- Number: US 7,611,548 B2
- Document ID: US7611548B2
- Status: Granted
- Kind: B2
- Application number: 10/660,715
- Filed: 2003-09-12
- Published: 2005-03-03
- Granted: 2009-11-03
- Earliest claimed: 2003-08-28
- Assignees: Industrial Technology Research Institute
- Inventors: Shyue-Ming Jang; Sheng Yang; Bang-I Liou; Jun-Yi Chen; Long-Shuenn Jean; Chun-Te Tsai; Chiu-Tung Huang
- Web page: https://patentgrep.com/patent/US7611548B2

## CPC

- B01D 7/00: Sublimation (B01D8/00 takes precedence; freeze-drying F26)
- B01D: SEPARATION (separating solids from solids by wet methods B03B, B03D; by pneumatic jigs or tables B03B; by other dry methods B07; magnetic or electrostatic separation of solid materials from solid materials or fluids, separation by high-voltage electric fields B03C; centrifuges, vortex apparatus B04; presses per se for squeezing-out liquid from liquid-containing material B30B9/02; treatment of water C02F, e.g. softening by ion-exchange C02F1/42; {arrangements of air intake cleaners in gas turbine plants F02C7/05} ; arrangements or mounting of filters in air-conditioning, air-humidification or ventilation F24F13/28)

## Abstract

A vertical and a horizontal vacuum sublimation apparatus with high efficiency and processes thereof are provided, especially for the materials with high melting point and low vapor pressure. The vertical sublimation purification apparatus comprises a sublimation channel body, a material rack, a heating evaporation device, a condensation device, an incubating device, and a product scratching device. The horizontal sublimation purification apparatus comprises a sublimation channel body, a material carrier, a heating evaporation device, and two end pipes. The apparatuses of the present invention can be applied to the mass production of high purity chemicals, and are capable of sublimating and purifying OLED illumination layer materials including Alq3, NPB and CuPc, which have high melting temperature and low vapor pressure.

## Claims

### Claim 1

A vertical sublimation apparatus, comprising:
a sublimation channel body;
a material rack for storing materials that will be evaporated;
a heating evaporation device surrounding an evaporation pipe to control heating temperatures according to different materials for evaporating said materials;
a vapor channel for transporting said evaporated materials into said sublimation channel body;
a vapor channel incubating device surrounding said vapor channel for maintaining the temperature of said vapor channel;
a condensation device surrounding the upper part of said sublimation channel body for controlling condensation temperatures required by different evaporated materials;
a product incubating device for maintaining the temperature of end products;
and
a product scratching device;
wherein said heating evaporation device, said vapor channel, said condensation device, said vapor channel incubating device and said product incubating device are individually configured.

### Claim 2 (depends on 1)

The vertical sublimation apparatus as claimed in claim 1, wherein the structure of said material rack comprises a plurality of rails and fixed rings, and said rails are fixed by two fixed rings and located in said evaporation pipe for storing materials ready to be evaporated.

### Claim 3 (depends on 1)

The vertical sublimation apparatus as claimed in claim 1, wherein said vapor channel incubating device surrounds an outlet port of said vapor channel to maintain the temperature of the sublimated vapor and transports said sublimated vapor continuously into said sublimation channel body.

### Claim 4 (depends on 3)

The vertical sublimation apparatus as claimed in claim 3, wherein said product incubating device surrounds the lower part of said sublimation channel body to avoid accumulation of said sublimated vapor.

### Claim 5 (depends on 1)

The vertical sublimation apparatus as claimed in claim 1, wherein said product scratching device comprises a central axis for shifting up and down and/or rotating said product scratching device, fixed rings, central support and sawtooth.

### Claim 6 (depends on 5)

The vertical sublimation apparatus as claimed in claim 5, wherein said sawtooth is located near said fixed rings beneath said central support for scratching off condensed products from the wall of said sublimation channel body.

### Claim 7 (depends on 1)

The vertical sublimation apparatus as claimed in claim 1, wherein said lower part of said sublimation channel body is formed as a product storage tank for collecting said condensed products falling therein after being scratched off by said scratching device.

### Claim 8 (depends on 1)

The vertical sublimation apparatus as claimed in claim 1, further comprising heat shield devices made of quartz wool and located at two ends of said sublimation channel body with one end of said evaporation pipe being further away from said sublimation channel body for maintaining a certain temperature inside said sublimation apparatus.

### Claim 9 (depends on 1)

The vertical sublimation apparatus as claimed in claim 1, further comprising sealing caps located at each end of said channels with heat shield devices placed therein and locked by O-rings to prevent leakage.

### Claim 10 (depends on 1)

A vacuum sublimation purification process applied to said vertical sublimation apparatus of claim 1, comprising the following steps:
placing materials on said material rack;
turning on said vacuum extraction device to vacuum;
turning on said heating evaporation device to achieve the required sublimation temperature of materials;
turning on all incubating devices to maintain the condensation temperature;
scratching and collecting products at a regular time interval during the evaporation process; and
cooling down the temperature after evaporation is completed and taking out products from said product storage tank, said steps being applied to the vertical sublimation apparatus of claim 1.

### Claim 11 (depends on 10)

The vacuum sublimation purification process as claimed in claim 10, wherein conditions of sublimation required for purifying Alq3 are: evaporation temperature being 350˜450° C., condensation temperature being 250˜350° C., evaporation temperature being 50˜100° C. higher than condensation temperature, and system pressure being 1˜1 10−6 mbar.

### Claim 12 (depends on 10)

The vacuum sublimation purification process as claimed in claim 10, wherein conditions of sublimation for purifying NPB are: evaporation temperature being 250˜350° C., condensation temperature being 150˜250° C., evaporation temperature being 30˜80° C. higher than condensation temperature, and system pressure being 0.1˜1 10−6 mbar.

### Claim 13 (depends on 10)

The vacuum sublimation purification process as claimed in claim 10, wherein conditions of sublimation for purifying CuPc are: evaporation temperature being 500˜650° C., condensation temperature being 400˜500° C., evaporation temperature being 50˜100° C. higher than condensation temperature, and system pressure being 0.1˜1 10−6 mbar.

### Claim 14 (depends on 11)

The vacuum sublimation purification process as claimed in claim 11, wherein conditions of sublimation for purifying NPB are: evaporation temperature being 250˜350° C., condensation temperature being 150˜250° C., evaporation temperature being 30˜80° C. higher than condensation temperature, and system pressure being 0.1˜1 10−6 mbar.

### Claim 15 (depends on 11)

The vacuum sublimation purification process as claimed in claim 11, wherein conditions of sublimation for purifying CuPc are: evaporation temperature being 500˜650° C., condensation temperature being 400˜500° C., evaporation temperature being 50˜100° C. higher than condensation temperature, and system pressure being 0.1˜1 10−6 mbar.