Up-down opening tubular furnace vacuum equipment system and application thereof
Through the design of upper and lower open tube furnaces and flexible connectors, combined with electrical refrigeration and liquid nitrogen refrigeration, the problem of slow heat dissipation of quartz tubes is solved, rapid cooling and efficient production are achieved, and material purity and equipment life are improved.
Patent Information
- Application Number
- CN202510808930.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-06-17
- Publication Date
- 2025-08-15
AI Technical Summary
The heat dissipation efficiency of quartz tubes in existing tube furnace vacuum equipment is low and the cooling speed is slow, resulting in low production efficiency and difficult to ensure material purity.
It adopts an upper and lower open tube furnace, and slideable sealed doors are installed at both ends of the quartz tube, which are connected to the filter system through flexible connectors. Combined with electric refrigeration, the copper sheet with holes and liquid nitrogen refrigeration can achieve rapid cooling of the quartz tube, and is equipped with an independently controlled temperature zone and fan system.
It significantly shortens the cooling time of quartz tubes, improves the purity and production efficiency of materials, and extends the service life of the vacuum pump.
Smart Images
Figure CN120488713A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to vacuum machinery and chemical equipment, and in particular to a tube furnace vacuum equipment system used for purification, thermal property testing and preparation of organic or inorganic materials. Background Art
[0002] When organic / inorganic compounds are used as semiconductor materials or organic semiconductor materials, their purity greatly affects their performance. This is especially true for organic optoelectronic materials, such as organic electroluminescent devices (OLEDs), organic solar cells (OPVs), and composite materials for batteries. These materials require very high purity to exclude encapsulated solvents and impurities. Tubular vacuum equipment systems are commonly used purification equipment and can also be used for sintering materials such as ceramics, perovskites, and phosphors, as well as for thermal properties testing of materials.
[0003] The vacuum sublimation instrument of organic materials in the prior art also belongs to the tubular vacuum equipment system, and there have been relevant patent applications and production, but the existing equipment generally has the following characteristics: the tubular furnace adopts a side semi-open type (attached to the instruction manual) Figure 2 a) and upward half-opening type (attached to the instruction manual) Figure 2 b), and all temperature zones are turned on at the same time. If a sublimator has 5 to 8 temperature zones, all temperature zones are turned on at the same time when it is turned on. Due to gravity, the sublimated or sintered materials are often deposited at the bottom of the quartz tube. The quartz tube is under high vacuum, and the heat transfer inside the system is poor. The bottom of the quartz tube is in contact with the heating furnace, resulting in unsatisfactory heat dissipation. It generally takes 2-4 hours for the internal material to cool from 250 degrees to room temperature (25 degrees). The existing technology adds a cooling fan next to the temperature zone, but it still takes 1 to 2 hours to cool down, and the production efficiency is low.
[0004] In order to solve the above shortcomings of low heat dissipation efficiency and slow cooling speed of the quartz tube in the vacuum tube furnace, an efficient tube furnace vacuum equipment system is needed. Summary of the Invention
[0005] The present invention provides a tubular vacuum equipment system, comprising a tubular furnace (1) (2) with upper and lower openings, a filtering system (3), a vacuum system (4) and a control system (5) (such as Figure 1 As shown); wherein, the upper and lower open tube furnace (2) can be controlled to move up and down independently, and when it is fully opened, Figure 3 As shown; a quartz tube is installed in the tube furnace, and a sliding sealing door device is installed at both ends of the quartz tube. A vacuum gauge is fixed at both ends to detect the vacuum degree of the system. One end connected to the filtration system (3) is connected through a flexible connector such as a metal bellows (5). The connectors (7) on both sides of the quartz tube are controlled to move up and down. When fully opened, Figure 3As shown; the filtration system (3) is a liquid nitrogen tank or an electric refrigeration plate and a combination thereof; the vacuum system includes a vacuum gauge, a vacuum valve, a low vacuum front pump and a high vacuum secondary pump, and connecting pipelines; the control system includes a host, a monitoring and control program, a display screen, temperature control and display, etc.
[0006] In particular, the upper and lower opening type tubular furnace (1) (2) can be composed of 3-8 furnace chambers that can be independently controlled to open and close, each furnace chamber is composed of 1-3 zones that can be independently heated and temperature controlled, and each furnace chamber is equipped with 1-2 fans that can be independently turned on and off.
[0007] Particularly preferably, when the upper and lower opening type tube furnace (2) is opened by moving the tube furnace up and down, the quartz tube can also move up and down, and finally when it is fully opened, Figure 3 way.
[0008] In particular, one side of the filtration system (3) is connected to the quartz tube via a flexible connector, and the other side is connected to the vacuum system; the side connected to the quartz tube is equipped with a perforated copper sheet or filter for electric heating or cooling, and the side connected to the vacuum system is equipped with a tank that can hold liquid nitrogen.
[0009] Preferably, the high vacuum secondary pump of the vacuum system (4) is a diffusion pump, a molecular pump or a cold pump, or a combination thereof.
[0010] Preferably, the high vacuum secondary pump of the vacuum system (4) can be installed on the horizontal side of the filtering system (3), or installed above its box.
[0011] Preferably, the control system (5) independently heats and controls the temperature of each tube furnace; controls the on / off of each fan; and displays and records data such as the vacuum degree and temperature during system operation.
[0012] As can be seen from the above technical solutions, the tubular furnace provided by the present invention has a rapid cooling effect, which improves work efficiency. It is also equipped with a combination of an electrically refrigerated perforated copper sheet or filter with high adsorption performance and anti-oil return from the mechanical pump and liquid nitrogen refrigeration. The added benefit of this combined tubular furnace vacuum system is that it can increase the cooling rate inside the quartz tube by 1-2 times; at the same time, it can improve the quality of the material and reduce the content of impurities; the new adsorption system can not only efficiently adsorb dust, but also prevent oil return by adsorbing organic solvents at low temperatures. At the same time, the cold perforated copper sheet or filter is easy to disassemble, clean, and replace, and the operation is simple, which can more effectively prevent dust from entering the vacuum pump system and extend the service life of the vacuum pump.
[0013] The present invention and the conventional existing solution are opened in the same manner as shown in the figure, which can significantly shorten the cooling time and improve the material quality.
[0014] Compared with the method in which the tubular furnaces (1) and (2) can be raised and lowered simultaneously but the quartz tube does not move, the technical solution of the present invention solves the technical problems that the quartz tube is placed on the tubular furnace (1) part by its own gravity, and the tubular furnace (2) is closed with the tubular furnace (1) after it is lowered, thereby solving the technical problems that the tubular furnace (1) part is damaged by the inability to raise and lower the part to a certain position, or the tubular furnace (2) is not tightly closed with the tubular furnace (1). BRIEF DESCRIPTION OF THE DRAWINGS
[0015] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, a brief introduction is given to the drawings required for the prior art and the technical solutions of the present invention.
[0016] Figure 1 It is a structural schematic diagram of the tubular furnace vacuum equipment system of the present invention.
[0017] Figure 2 Cross-section of a traditional semi-open a) or upward-open b) tube furnace
[0018] Figure 3 Cross-sectional view of the tubular furnace of the present invention when fully opened. DETAILED DESCRIPTION
[0019] The tube furnace vacuum system of the present invention is used as a vacuum sublimator for organic / inorganic materials. The general specific steps are as follows:
[0020] The present invention's vacuum tube furnace system operates by first opening the sealed door at one end of the quartz tube, pushing the material and collection tube into the tube, and then starting the vacuum system to evacuate the chamber. Once the far end of the tube (away from the vacuum system) reaches a preset vacuum level, heating the chamber begins and continues until it reaches the set temperature. After a predetermined holding time, the chamber is opened and closed to cool. Once the temperature drops to room temperature, nitrogen is introduced through the gas inlet to release the vacuum. The corresponding loading and collection tubes are removed, and the material is scraped off before conducting the necessary analysis and testing.
[0021] Example 1
[0022] A quartz tube with a diameter of 200 mm is equipped with 7 independently heated and temperature-controlled furnaces. The organic material LC-065 (1 kg, 99.97% purity by high performance liquid chromatography) is placed at the far end of the quartz tube from the vacuum system, and collecting tubes are placed in the middle of the quartz and the near end of the quartz tube respectively. The refrigeration system is turned on to cool the copper sheet or copper mesh of the filtration system, and liquid nitrogen is added to the liquid nitrogen tank. After the refrigeration sheet reaches the set temperature, the vacuum system is turned on and the vacuum operation is performed until the vacuum degree indicated by the far end vacuum gauge drops below the set vacuum degree. The LC-065 is vacuum sublimated according to conventional operations and kept sublimated at the set temperature for 8 hours. After the sublimation is completed, the tubular furnace (2) and the quartz tube are raised at the same time to reach the following temperature: Figure 3The furnace was maintained in the indicated state and the cooling fan on the side of the tube furnace was turned on until the outside of the bottom of the quartz tube indicated a temperature of ≤30°C. The cooling time was recorded. After closing the vacuum system, nitrogen was introduced to break the vacuum and raise the pressure within the system to atmospheric pressure. The material in each temperature zone was scraped off and analyzed by high-performance liquid chromatography.
[0023] Example 2
[0024] A quartz tube with a diameter of 100 mm is equipped with 5 independently heated and temperature-controlled furnaces. A red phosphorescent material LCRD-003 (10G, 99.7% purity by high performance liquid chromatography) is placed at the far end of the quartz tube from the vacuum system, and collection tubes are placed in the middle of the quartz and the near end of the quartz tube respectively. The refrigeration system is turned on to cool the copper sheet or copper mesh of the filtration system, and liquid nitrogen is added to the liquid nitrogen tank. After the refrigeration sheet reaches the set temperature, the vacuum system is turned on and the vacuum operation is performed until the vacuum degree indicated by the far end vacuum gauge drops below the set vacuum degree. The LCRD-003 is sublimated according to conventional operations and kept sublimated at the set temperature for 2 hours. After the sublimation is completed, the tubular furnace (2) and the quartz tube are raised at the same time to reach the following temperature: Figure 3 The furnace was maintained in the indicated state and the cooling fan on the side of the tube furnace was turned on until the outside of the bottom of the quartz tube indicated a temperature of ≤30°C. The cooling time was recorded. After closing the vacuum system, nitrogen was introduced to break the vacuum and raise the pressure within the system to atmospheric pressure. The material in each temperature zone was scraped off and analyzed by high-performance liquid chromatography.
[0025] Example 3
[0026] A quartz tube with a diameter of 100 mm is equipped with 5 independently heated and temperature-controlled furnaces. A green phosphorescent material LCGD-003 (10G, 99.6% purity by high performance liquid chromatography) is placed at the far end of the quartz tube from the vacuum system, and collection tubes are placed in the middle of the quartz and the near end of the quartz tube respectively. The refrigeration system is turned on to cool the copper sheet or copper mesh of the filtration system, and liquid nitrogen is added to the liquid nitrogen tank. After the refrigeration sheet reaches the set temperature, the vacuum system is turned on and the vacuum operation is performed until the vacuum degree indicated by the far end vacuum gauge drops below the set vacuum degree. The LCRD-003 is sublimated according to conventional operations and kept sublimated at the set temperature for 2 hours. After the sublimation is completed, the tubular furnace (2) and the quartz tube are raised at the same time to reach the following temperature: Figure 3 The furnace was maintained in the indicated state and the cooling fan on the side of the tube furnace was turned on until the outside of the bottom of the quartz tube indicated a temperature of ≤30°C. The cooling time was recorded. After closing the vacuum system, nitrogen was introduced to break the vacuum and raise the pressure within the system to atmospheric pressure. The material in each temperature zone was scraped off and analyzed by high-performance liquid chromatography.
[0027] Comparative Example 1
[0028] A quartz tube with a diameter of 200 mm is equipped with an integral furnace, which is opened as follows: Figure 2 a) Place the organic material LC-065 (1 kg, HPLC purity of 99.97%) at the far end of the quartz tube, and place collection tubes in the middle of the quartz tube and the near end of the quartz tube respectively. Add liquid nitrogen to the liquid nitrogen tank, wait for the refrigeration plate to reach the set temperature, turn on the vacuum system, and perform the vacuum operation until the vacuum degree indicated by the far end vacuum gauge drops below the set vacuum degree. Sublimate the LC-065 according to the conventional operation and keep it sublimated at the set temperature for 8 hours. After the sublimation is completed, open the tube furnace to reach the following temperature: Figure 2 The cooling fan on the side of the tube furnace was turned on until the outside of the bottom of the quartz tube showed ≤30°C and the cooling time was recorded. After closing the vacuum system, nitrogen was introduced to break the vacuum and raise the pressure in the system to atmospheric pressure. The material in each temperature zone was scraped off and analyzed by high-performance liquid chromatography.
[0029] Comparative Example 2
[0030] A quartz tube with a diameter of 100 mm was equipped with five independently heated and temperature-controlled furnaces. Red phosphorescent material LCRD-003 (10G, 99.7% purity by HPLC) was placed at the far end of the tube and sublimated in the same manner as in Comparative Example 1. After sublimation, the time and purity of the test material were recorded.
[0031] Comparative Example 3
[0032] A quartz tube with a diameter of 100 mm was equipped with five independently heated and temperature-controlled furnaces. Red phosphorescent material LCGD-003 (10G, 99.6% purity by HPLC) was placed at the far end of the tube and sublimated in the same manner as in Comparative Example 1. After sublimation, the time and purity of the test material were recorded.
[0033] Table 1
[0034] Implementation Method Collection area cooling time Purity of collection area materials The materials in the collection area are mainly simple and mixed Example 1 26 minutes 99.99％ 50ppm Example 2 18 minutes 99.82％ 120ppm Example 3 20 minutes 99.8％ 105ppm Comparative Example 1 90 minutes 99.98％ 250ppm Comparative Example 2 43 minutes 99.75％ 307ppm Comparative Example 3 42 minutes 99.73％ 407ppm
[0035] Compared with the previously disclosed tubular furnace sublimator, the present invention is characterized in that the quartz tube and the upper part (2) of the tubular furnace can be independently raised and lowered, and the tubular furnace (2) and (1) can be tightly fitted. Compared with the method in which the tubular furnace (2) and the quartz tube can be raised and lowered simultaneously, and the quartz tube is stationary, the quartz tube of the present invention is placed on the tubular furnace (1) by its own gravity, and the tubular furnace (2) is closed with the tubular furnace (1) after it is lowered, thereby solving the technical problems of damage to the fixed quartz tube caused by the tubular furnace (1) not being raised and lowered properly, or the tubular furnace (2) not being tightly closed with the tubular furnace (1).
[0036] The above description is only an exemplary embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any technician familiar with the technical field can obtain other drawings through the drawings without creative work. Within the technical scope disclosed by the present invention, the technical solution and inventive concept of the present invention are equivalently replaced or changed, which should be covered by the scope of protection of the present invention.
Claims
1. A tubular furnace vacuum equipment system, characterized in that: The equipment system includes an upper and lower open tube furnace (1) (2), a filtering system (3), a vacuum system (4) and a control system (5); the upper and lower open tube furnace (2) moves up and down and can be closed with (1); a quartz tube is installed in the tube furnace, and sliding sealing door devices are installed at both ends of the quartz tube. Vacuum gauges are fixed at both ends and are connected to the filtering system (3) through metal bellows (5) and move up and down through connectors (7) on both sides; the filtering system (3) is a liquid nitrogen tank or an electric refrigeration plate and a combination thereof; the vacuum system includes a vacuum gauge, a vacuum valve, a low vacuum front pump and a high vacuum secondary pump, and connecting pipelines; the control system includes a host, a monitoring and control program, a display screen, temperature control and display, etc.
2. The tube furnace vacuum equipment system according to claim 1, characterized in that: The upper and lower opening tubular furnace is equipped with 3 to 8 independent upper and lower opening heating furnaces; each heating furnace is composed of 1-3 heating zones with independent temperature control, and each heating furnace is equipped with 1-2 independently controlled cooling fans.
3. The tube furnace vacuum equipment system according to claim 1 or 2, characterized in that: One side of the filtering system (3) is connected to the quartz tube via a flexible connector, and the other side is connected to the vacuum system.
4. The tube furnace vacuum equipment system according to claim 1 or 2, characterized in that: The filtering system (3) is provided with a perforated copper sheet or filter screen for electric heating or cooling on one side connected to the quartz tube; and a liquid nitrogen cooling tank on the other side connected to the vacuum system.
5. The tube furnace vacuum equipment system according to claim 1 or 2, characterized in that: The high vacuum secondary pump of the vacuum system (4) is a diffusion pump, a molecular pump or a cold pump, or a combination thereof.
6. The tube furnace vacuum equipment system according to claim 1 or 2, characterized in that: The high vacuum secondary pump of the vacuum system (4) is installed above or on the side of the filter system (3) box.
7. The tube furnace vacuum equipment system according to claim 1 or 2, characterized in that: This equipment is used for vacuum purification of organic / inorganic materials, heat resistance testing and material preparation.