KR100781241B1 - refining method for organic matter - Google Patents

Abstract

The present invention is to provide a method for purifying impurities contained in the purified organic matter effectively, and also to obtain an organic matter purification method in which the obtained organic matter is grown in a crystalline state. Maintaining the inside of the glass tube in a vacuum state, cooling between the heater and the heater of the plurality of heaters to give a temperature deviation, and recovering the amorphous sample and obtaining a crystal sample.

Organics Purification

Description

Refining method for organic matter

1 is a block diagram showing an organic material purification method using a sublimation method according to the prior art

2 is a block diagram showing a method for purifying organic matter using the sublimation method according to the present invention.

Figure 3 shows in detail the copper tube portion according to the present invention;

The present invention relates to a method for purifying organic matter.

Although the organic EL display element has superior characteristics compared to the inorganic EL element in low driving voltage, low power consumption, light weight and color, it has been a big problem in practical use because of its short lifetime.

There are many reasons for determining the lifetime of this device, but important causes include impurities in organic materials, interfaces between organic materials and electrodes, low crystallization temperature (Tg) of organic materials, oxidation of devices by oxygen and moisture, etc. There is a number.

Among them, the purity of organic matter is very important.

When impurities are contained in organic materials used in organic electroluminescent devices, impurities reduce their lifetimes, and act as trap sites for the excitons formed to dissipate excitons into non-luminescent transitions. Will be

As a result, the stability of the device is greatly reduced.

The existing CaPC, Alq ₃ , NPD and Dopant already contain various impurities which are unavoidable in the synthesis step.

Therefore, various methods of purification have been used so far, but the widely used method is the sublimation method devised by Hans J. Wagner et al. (Journal of Materials Science 17 (1982) 2781-2791).

1 is a block diagram showing an organic material purification apparatus using a sublimation method according to the prior art.

Referring to FIG. 1, a glass tube 1 through which a sample moves, a plurality of heaters 2-a and 2-b for applying different heat to the glass tube 1, and the glass tube 1 And a copper tube 3 positioned between the plurality of heaters 2-a and 2-b to conduct heat generated from the heater to the glass tube 1 and a temperature for sensing a temperature of the copper tube 3. A sensor (5), a flow meter (6) for reading the flow rate of the inert gas for moving the organic substance sublimated by heat, a cooling section (9) for providing water cooling by providing a cooling line at the end of the copper pipe (3), It comprises a rotary pump (8) for maintaining the inside of the glass tube (1) in a vacuum state.
And, it further comprises a protective cap (not shown) for protecting the purification device, and a trap (10) to prevent the sample moved from the glass tube (1) to enter the rotary pump (8).

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The operation principle will be described in detail with reference to FIG. 1 as follows.

After placing the sample in the glass tube 1 and placing it near the first heater 2-a, the inside of the glass tube 1 was vacuumed using the rotary pump 8, and then N2, which is an inert gas, was used. Or Ar is flowed by the flowmeter 6 so that the flow volume may be about 1 torr.

Then, the temperature of the first heater 2-a is raised to a temperature near the sublimation point of the sample, and the temperature deviation is adjusted so that the other second heater 2-b has a lower temperature than the first heater 2-a. In this case, the sample is conveyed to the rotary pump 8 by an inert gas and formed in the vicinity of a plurality of heaters 2-a and 2-b having different temperature values in the glass tube 1.

In this case, the pure material is formed near the second heater, which is a region close to the first heater, and impurities of less mass fly further away, and impurities of large mass do not fly and remain in place.

After removing the glass tube, the organic substance can be obtained by recovering the amorphous substance formed near the heater according to the characteristics of the organic substance.

However, the purification method of the organic material purification apparatus according to the prior art described above has the following problems.

The sample is difficult to obtain in a crystalline state in a glass tube. In particular, materials susceptible to moisture and air, such as Alq3, are not obtained in a crystalline state but in an amorphous state.

In this way, when the organic material is obtained in an amorphous state, an area that can be contacted with air after purification becomes large, causing a problem of rapid contamination.

In addition, the amorphous state occupies a large volume with the same mass, so that it is impossible to put a large amount at a time when loading a sample to make a device.

Accordingly, an object of the present invention is to provide a method for purifying organic matter, which can be obtained to solve the above problems and to obtain a purified organic matter in a crystalline state through a purification apparatus.

Another object of the present invention is to provide an organic material purification method for effectively removing impurities in the purified organic material.

The organic purification method according to the present invention for achieving the above object is a glass tube to which a sample is moved, a plurality of heaters (heaters) for applying different heat to each of the glass tube, surrounding the glass tube, the plurality of cooling holes The organic substance purification using the sublimation method in the organic substance stabilization apparatus which consists of the copper tube formed, the flowmeter which reads the flow volume of the inert gas which moves the material sublimated by the said conducted heat, and the rotary pump which keeps the inside of the glass tube in a vacuum state. As a method,
Putting the sample in a glass tube and maintaining the inside of the glass tube in a vacuum state using a rotary pump, cooling the heater and the heater among the plurality of heaters to give a temperature deviation, and recovering the amorphous sample and obtaining a crystal sample; It is characterized by including.
The step of generating the temperature deviation may include a plurality of cooling holes having a diameter of 1 mm or more, forming a cooling hole for facilitating heat conduction from the heater to the glass tube and a cooling hole for facilitating the cooling of the glass tube. Create
In the obtaining of the crystal sample, due to the temperature variation, the amorphous sample formed in the low temperature region is removed, and the crystal sample formed at the high temperature is generated.
In addition, the organic purification method is air-cooled through a plurality of cooling holes.

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Other objects, features and advantages of the invention will become apparent from the following detailed description of embodiments taken in conjunction with the accompanying drawings.

Preferred embodiments of the organic matter purifying apparatus according to the present invention will be described with reference to the accompanying drawings.

2 is a block diagram showing an organic material purification apparatus using a sublimation method.

Referring to FIG. 2, a glass tube 1 through which a sample moves and a plurality of heaters 2-a, 2-b, 2-c, and 2-d applying different heat to the glass tube 1, respectively. And a plurality of cooling holes are formed between the glass tube 1 and the plurality of heaters 2-a, 2-b, 2-c, and 2-d to surround the glass tube 1 and form a plurality of cooling holes. A plurality of heaters to apply different heat to sense the temperature of the tube (3), a flow meter (6) for reading the flow rate of the inert gas to move the material sublimated by the conducted heat, and in the glass tube (1) It characterized in that it comprises a rotary pump (8) for maintaining the vacuum state.
And, it further comprises a protective cap (not shown) for protecting the purification device, and a trap (10) to prevent the sample moved from the glass tube (1) to enter the rotary pump (8).
Looking at the operation of the purification method, after placing the sample on the glass tube (1), the temperature different in each of the glass tube (1) through a plurality of heaters (2-a, 2-b, 2-c, 2-d) A value is applied to sublimate the sample.

At this time, different heat applied from the plurality of heaters 2-a, 2-b, 2-c, 2-d is conducted to the glass tube through a copper tube formed with a plurality of holes between the glass tube and the plurality of heaters. .

And the sublimed material is controlled through the flow meter (6) is carried toward the rotary pump (8) by an inert gas flowing into the glass tube (1), a plurality of heaters having different temperature values conducted to the glass tube (1) It forms in the vicinity of (2-a, 2-b, 2-c, 2-d), respectively.

At this time, the inside of the glass tube 1 is maintained in a vacuum state through the rotary pump 8 and is also cooled by air cooling through the cooling holes 4.

The hole (4) drilled in the copper tube acts in two ways. First, the heat generated from the heaters 2-a, 2-b, 2-c, and 2-d can directly reach the glass tube 1. The second helps to maintain the set temperatures of the first heater 2-a and the second heater 2-b.

For example, suppose that the first heater 2-a is set to 400 ° C and the second heater is set to 300 ° C (2-b).

At this time, if there is no intermediate cooling hole, the thermal conductivity of the copper pipe is high, so the temperature near the second heater 2-b is affected by the temperature of the first heater 2-b.

Therefore, the temperature of the second heater (2-b) is over 300 ℃, this will widen the area where the sublimed material is formed.

At this time, the organic matter formed in the low temperature region is not given enough crystallization energy to be in an amorphous state, and only the organic matter formed at high temperature is formed as some crystals.

Therefore, by forming a cooling tube between the heaters 2-a, 2-b, 2-c, and 2-d, the vicinity of the second heater 2-b has a set temperature value, and the intermediate temperature is It has an intermediate temperature value between the first heater 2-a and the second heater 2-b. Similarly, the intermediate temperature has an intermediate temperature value of the third heater 2-c and the fourth heater 2-d.

At this time, almost all pure organic matter is formed in this region, and by sufficient crystallization energy, most of the material grows to the crystalline state.

Figure 3 is a view showing in detail the copper pipe portion according to the present invention.

The hole 4 of the copper pipe 3 is composed of a plurality of diameters of 1 mm or more.

Accordingly, heat conduction from the heaters 2-a, 2-b, 2-c, and 2-d to the glass tube 1 is easily performed, and air is also introduced into the hole formed between the heater and the heater, so that the glass tube 1 Cooling becomes easy.

Most of the organic matter from which impurities have been removed by the cooling holes 4 is grown and obtained in the crystalline state near the cooling holes 4.

Organic matter purification method according to the present invention as described above has the following effects.

First, it is possible to precisely control the temperature range according to the organic material growth by lowering the thermal conductivity between the heater and the heater according to the cooling holes.

Secondly, since the obtained organic material is grown in a crystalline state, the area in contact with air is small, so it is less likely to be contaminated, and since it occupies a small volume with the same mass, a large amount can be added at a time when loading a sample.

Those skilled in the art will appreciate that various changes and modifications can be made without departing from the spirit of the present invention.

Therefore, the technical scope of the present invention should not be limited to the contents described in the embodiments, but should be defined by the claims.

Claims (3)

As a method for purifying organic matter using the sublimation method, Placing the sample in a glass tube and maintaining the inside of the glass tube in a vacuum state using a rotary pump; Cooling between the heater and the heater of the plurality of heaters to give a temperature deviation; And Recovering the amorphous sample and obtaining a crystal sample; organic material purification method using a sublimation method comprising a. The method of claim 1, wherein generating the temperature deviation, Using a sublimation method as a plurality of cooling holes having a diameter of 1mm or more, forming a cooling hole for facilitating heat conduction from the heater to the glass tube and a cooling hole for facilitating the cooling of the glass tube. Organic Purification Method. The method of claim 1, wherein the obtaining of the crystal sample, Due to the temperature deviation, the amorphous sample formed in the low temperature region is removed, and the organic substance purification method using the sublimation method, characterized by producing a crystalline sample formed at a high temperature.

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