CN213100901U

CN213100901U - Sublimation purification device for organic semiconductor material

Info

Publication number: CN213100901U
Application number: CN202020526663.8U
Authority: CN
Inventors: 孟鸿; 刘铭; 张泽伟; 吴雨亭; 闫丽佳
Original assignee: Peking University Shenzhen Graduate School
Current assignee: Peking University Shenzhen Graduate School
Priority date: 2020-04-08
Filing date: 2020-04-08
Publication date: 2021-05-04
Anticipated expiration: 2030-04-08

Abstract

The utility model discloses a sublimation purification device of organic semiconductor material. The sublimation purification device comprises a plurality of inner pipes which are connected in sequence, wherein a mesh screen is arranged between every two adjacent inner pipes, and the mesh screen has the functions of rectifying tower plates, adsorbing impurities and ventilating and conducting heat. The utility model discloses a sublimation purification device comprises a horizontal type and a vertical type, a heat conduction mesh screen is arranged between two adjacent inner pipes, and the mesh screen has the function of rectification components and can be suitable for high-efficiency purification of various materials; meanwhile, the mesh screen has good thermal conductivity and high thermal stability, the density of the ventilation hole channel can be adjusted, purified substances can be prevented from being separated out, and subsequent impurity cleaning is facilitated; the adsorbing substances fixed on the mesh screen have the functions of further adsorbing impurities and purifying products, and can be replaced according to the properties of the purification components to achieve a better purification effect.

Description

Sublimation purification device for organic semiconductor material

Technical Field

The utility model relates to a sublimation purification stove technical field especially relates to organic semiconductor material's sublimation purification device.

Background

Organic electronic devices have attracted much attention at home and abroad because of their advantages of active light emission, short response time, wide viewing angle, full color, low power consumption, and the like. The purity of the organic semiconductor material directly affects the operating characteristics and stability of the organic electronic device. Impurities in the organic light-emitting layer can form a trap to block the diffusion movement of excitons and capture part of excitons, so that the quenching of the excitons is caused, and the light-emitting efficiency of the organic electroluminescent device can be reduced; the impurities on the carrier transmission layer can capture carriers, so that the transmission efficiency of the carriers is reduced; an internal electric field is formed after the impurities capture carriers to block the injection of subsequent charges, so that the open-circuit voltage of the device is increased, and the current density is reduced; in addition, the instability of the impurities is prone to decomposition, which affects the lifetime of the device. It is therefore of great importance to improve the purity of the organic semiconductor material.

The purification method commonly used at home and abroad is gradient sublimation purification, a certain temperature gradient is formed on a glass tube by setting the temperatures of different temperature zones, and a material to be purified is placed in a high-temperature heating zone to sublimate the material. The sublimated material is diffused to the low-temperature area for deposition, generally, the high-purity material is deposited in a short distance close to the sublimation area, and the deposition area of the impurities is far away from the sublimation area, so that the purpose of separating the impurities is achieved. However, in the gradient sublimation purification method, the temperature gradient formed is the only driving force for separating the materials, and thus careful temperature control is required during sublimation. Moreover, the requirement of purity cannot be met by one-time heating sublimation, and the material needs to be sublimated for two times or even more times to achieve sufficient purity.

In the sublimation purification method of organic small molecules disclosed in patent CN102924207A published by the company, akagye photoelectric materials, guangdong, the obstacle is disposed in the sublimation heating tube to change the sublimation purification path, but the existence of the obstacle makes the airflow pass through the opening, which increases the airflow velocity, so that the deposition of the material on the subsequent obstacle is reduced, most of the material is deposited in the first baffle area, and the deposition of the material on the subsequent obstacle is very little, therefore, the effective recovery quality of the existence of the obstacle is not improved, and even the recovery quality is reduced.

In addition, the conventional sublimation purifying apparatus is designed in a horizontal structure. In this structure, as the purification apparatus chamber and the heating region are horizontally arranged, the raw material is diffusion-separated in the horizontal direction. In this type of device, the material produces differences in the temperature distribution of the upper and lower parts of the instrument under the influence of gravity and vertical thermal convection, resulting in differences in the purification effect of the upper and lower parts of the same horizontal position within the furnace, which in turn results in reduced purification efficiency.

SUMMERY OF THE UTILITY MODEL

In view of the above-mentioned prior art not enough, the utility model aims at providing an organic semiconductor material's sublimation purification device aims at solving the problem that current sublimation purification stove purification inefficiency.

The technical scheme of the utility model as follows:

the sublimation purification device for the organic semiconductor material comprises a plurality of inner pipes which are sequentially connected, wherein a mesh screen is arranged between every two adjacent inner pipes, and the mesh screen has the functions of rectifying tower plates, adsorbing impurities and ventilating and conducting heat.

The utility model discloses an inside mesh screen that sets up comes the rectification purification component, adsorbs impurity to reach the separation of main material and impurity at sublimation in-process, product purity is higher, and air velocity is even. The mesh screen has the heat conductivity, makes the organic semiconductor material of purification gather in the collection area, increases output.

Further, the mesh screen comprises a support and an adsorbent material on the support. The support provides a support carrier for the adsorbed species, which is typically stainless steel, and may also be a metal with or without magnetic nanoparticles.

Further, the support is a hollow or net structure.

Further, the adsorption substance is one or more of activated carbon, carbon nanotubes, graphene, carbon fibers, silica gel, diatomite, porous ceramics, magnetic metal particles and the like. Particularly, the proper adsorption material can be selected according to the performance of the purification material

Still further, the adsorbent species may have an orientation.

Further, one or more mesh screens are arranged between two adjacent inner pipes.

Further, when a plurality of mesh screens are provided between adjacent two of the inner tubes, each mesh screen has magnetism, and a magnetic field is provided between the mesh screens.

Further, the mesh has a pore size of between 1 micron and 1 cm.

Further, the thickness of the mesh screen is between 10 microns and 10 centimeters.

Further, the sublimation purification device is of a horizontal structure or a vertical structure, and the inner pipes are connected in sequence in the horizontal direction or in sequence in the vertical direction.

The utility model discloses a sublimation purification device comprises a horizontal type and a vertical type, a heat conduction mesh screen is arranged between two adjacent inner pipes, and the mesh screen has the function of rectification components and can be suitable for high-efficiency purification of various materials; meanwhile, the mesh screen has good thermal conductivity and high thermal stability, the density of the ventilation hole channel can be adjusted, purified substances can be prevented from being separated out, and subsequent impurity cleaning is facilitated; the adsorbing substances fixed on the mesh screen have the functions of further adsorbing impurities and purifying products, and can be replaced according to the properties of the purification components to achieve a better purification effect.

Adopt sublimation purification method of organic semiconductor material's sublimation purification device, wherein, will treat the organic semiconductor material of purification through the heating, the mesh screen between the inner tube is passed through after the sublimation, and partial material is adsorbed, and impurity part is adsorbed in a large number, and the enrichment of main material is in the material collecting region, is favorable to improving the purity of main material.

The utility model discloses following beneficial effect has:

1. the mesh screen is arranged between the inner pipes and can adsorb impurity substances, so that the purity of the main substance is improved;

2. the mesh screen is made of a material with an adsorption function, and a proper adsorption material can be selected according to the performance of the purification material;

3. the mesh screen is a good conductor of heat, which can avoid the material from condensing on the mesh screen;

4. a magnetic field can be generated among the multiple layers of magnetic mesh screens, and the magnetic field reduces the entropy value of a separation material by changing the stress condition among the molecules in a sublimation substance, thereby achieving the purposes of improving the separation efficiency and saving the energy consumption;

5. the utility model provides a purification device of vertical structure has reduced convection current and gravity to the influence of purification effect, makes the material component more homogeneous on the same diffusion length in the device. In addition, the semiconductor thin films required for OLED devices are typically made in a vertical orientation. The purification instrument with a vertical structure is used, so that the sublimation directions of purification and device preparation are kept consistent, and the device is closer to a use scene.

Drawings

FIG. 1 is a schematic structural view of a horizontal sublimation purification apparatus of the present invention;

FIG. 2 is a schematic view of the internal structure of the horizontal sublimation purification apparatus of the present invention;

fig. 3 is a schematic view of the structure of the mesh screen of the present invention;

FIG. 4 is a schematic view of the internal and external structure of the vertical sublimation purification apparatus of the present invention;

in the figure: 1 is an inner tube, 2 is an adsorbent membrane, 3 is a mesh screen, 4 is an adsorbent (carbon nano tube) and 5 is a crude material.

Detailed Description

The utility model provides a sublimation purification device of organic semiconductor material, for making the utility model discloses a purpose, technical scheme and effect are clearer, more clear and definite, it is following right the utility model discloses further detailed description. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.

The overall design of the purification device is shown in fig. 1. The purification furnace (outer tube) is a high-purity quartz tube with the length of 1.0m and the inner diameter of 5cm, and is heated by winding an electric heating wire. The heating can be to 400 c above the sublimation point of all known OLED materials at low pressure. The winding of the electric heating wire is completed by a program-controlled movable winder. The winding is provided with a horizontal motor, a winding motor and related sensors, and the repeatability control of the number distribution of the heating belt turns is realized through program control. The winder is detachable structure, is convenient for with the heating tape separation, heating tape high temperature harm winder during the prevention experiment. Both ends of the heating cavity are provided with a pipeline and a door part made of 316 stainless steel materials. The cabin door component is divided into an inner layer and an outer layer. The inner layer can drive the hearth outer tube to rotate, and the outer layer is fixed on the purification furnace structural support. The inner layer and the outer layer are sealed by magnetic fluid, so that the hearth can integrally rotate in the purification process, and high vacuum in the hearth is ensured.

The inlet part of the cabin door is provided with an external air pipe and a corresponding valve, and inert gases such as nitrogen, argon and the like can be introduced to be used as carrier gas or protective gas. In the embodiment, a pretreatment system (an automatic reaction kettle, a polymer rectification device and the like) of the material is combined with the sublimation purification device, so that an external interface is reserved at an inlet port of the purification device and connected with equipment used for pretreatment. The hatch door leaves the interface in addition and inserts the thermocouple directly in the purification cavity, can monitor the accurate temperature of each position in the cavity, conveniently knows the sublimation nature of material to realize the accurate control to the inside temperature gradient of device. The outlet of the purification cavity is connected with a vacuum system, which is composed of a mechanical pump and a molecular pump, and is provided with a corresponding control valve, so that the vacuum degree in the purification cavity can reach 10^-4Pa. The instrument is provided with a video monitoring and data analysis system. The temperature and pressure of each part of the instrument are controlled by a control program and a monitoring systemThe functions of controlling, reading, archiving and analyzing in situ of key parameters such as force, tower plate position and the like are convenient for optimizing experimental parameters.

Referring to fig. 2-3 (in the figure, 1 is an inner tube, 2 is an adsorbent membrane, 3 is a mesh screen, 4 is a carbon nanotube, and 5 is a crude material), the sublimation purification apparatus includes 6 inner tubes, and a mesh screen, three mesh screens are provided between adjacent inner tubes from the heating zone. The mesh screen is formed by weaving carbon nanotubes (or other carbon nanotubes) into a mesh structure to be tightly attached to a steel grid; the organic semiconductor material is placed in a heating area for heating, and after sublimation, the organic semiconductor material passes through a mesh screen (tower plate) between inner pipes, and an additional separation effect is introduced, so that the problem of poor gradient sublimation effect is solved. First, the trays can function in the device like liquid fractionation trays, forming multiple sublimation-desublimation balances within the device, increasing the efficiency of a single sublimation. Secondly, the column plate has the function of impurity adsorption besides the function of fractionation. Because the quantity of impurity molecules is far less than that of the molecules of the required material, the adsorption proportion of the impurity molecules (the adsorption proportion of the adsorption molecules to all the molecules of the component) is far greater than that of the molecules of the required material, thereby realizing the aim of removing impurities. Wherein the impurities and the main substance are adsorbed, the adsorption ratio of the impurities is large, and the main substance containing a small amount of impurities passes through a further mesh screen for further purification until the high-purity main substance is obtained in the material collecting region.

The vertical configuration is as shown in fig. 4, and the components are the same as the horizontal device except that the components are arranged in a vertical configuration.

The novel device is used for purifying materials, and the purity of the materials purified in one time is over 99.9 percent and the purity of the materials purified in two times is over 99.99 percent through detection by means of GC, HPLC and the like. Compared with the purification effect of the purchased MBRAUN material purification device, the purity of the MBRAUN material purification device is equal to or higher than that of the imported material purification device under the same condition.

It is to be understood that the invention is not limited to the above-described embodiments, and that modifications and variations may be made by those skilled in the art in light of the above teachings, and all such modifications and variations are intended to be included within the scope of the invention as defined in the appended claims.

Claims

1. The sublimation purification device for the organic semiconductor material comprises a plurality of inner pipes and a plurality of outer pipes which are connected in sequence, and is characterized in that a mesh screen is arranged between every two adjacent inner pipes, and the mesh screen has the functions of rectifying tower plates, adsorbing impurities and ventilating and conducting heat; the outer tube is wound with an electric heating wire, and the electric heating wire is wound by a program-controlled movable winder; the winder is provided with a horizontal motor, a winding motor and related sensors, and the repeatability control of the distribution of the number of turns of the heating belt is realized through program control; the winder is of a detachable structure;

the sublimation purification device also comprises a cabin door component which is divided into an inner layer and an outer layer;

when a plurality of mesh screens are arranged between two adjacent inner pipes, each mesh screen has magnetism, and a magnetic field is arranged between the mesh screens;

the thickness of the mesh screen is between 10 microns and 10 centimeters;

the sublimation purification device is of a vertical structure, and the inner pipes are sequentially connected in the vertical direction.

2. The sublimation purification apparatus of claim 1, wherein the mesh screen comprises a support and an adsorbent material on the support.

3. Sublimation purification apparatus according to claim 2, wherein the support is of hollow or mesh structure.

4. The sublimation purification apparatus of claim 2, wherein the adsorptive substance is one or more of activated carbon, carbon nanotubes, graphene, carbon fibers, silica gel, diatomaceous earth, porous ceramics, and magnetic metal particles.

5. The sublimation purification apparatus of claim 1, wherein one or more mesh screens are provided between adjacent two of the inner tubes.

6. The sublimation purification apparatus of claim 1, wherein the mesh screen has a pore size of between 1 micron and 1 cm.