Carbon deposition device for quartz tube

Abstract

The present application relates to material surface modification and chemical vapor deposition equipment technical field, and disclose a kind of quartz tube carbon plating device of carbon source blockage prevention.The quartz tube carbon plating device of carbon source blockage prevention includes hearth, heating device, liquid carbon source storage barrel, vacuum valve, hearth plug, gas storage tank, gas valve, gas flow meter, vacuum resistance gauge, cooling device.This device is externally fitted with water cooling jacket at hearth gas outlet, cooperate hearth plug, vacuum resistance gauge and vacuum pump valve, to the uncracked carbon source tail gas is forced to quench, avoid to generate oil dirt and carbon powder blockage pipeline.This device is accurately controlled by carbonizing process parameters, form uniform dense carbon film on the inner wall of quartz tube, while solving pipeline blockage pain point, reduce equipment maintenance cost, simple structure, convenient operation, applicable to the carbonizing treatment of CdTe crystal growth quartz tube, with higher practical value and popularization significance.

Description

Technical Field

[0001] This invention relates to the field of material surface modification and chemical vapor deposition equipment technology, specifically to a quartz tube carbon plating device that prevents carbon source blockage. Background Technology

[0002] In materials science and the semiconductor industry, carbon plating using quartz tubes (such as chemical vapor deposition) is widely used for material surface modification. Existing tube furnace carbon plating processes typically use liquid organic matter (such as acetone) as the carbon source, carrying carbon source vapor through a carrier gas (such as nitrogen) into a high-temperature furnace for pyrolysis, thereby depositing a carbon film on the substrate. However, in actual production or experimental processes, some carbon source gas often fails to completely pyrolyze in the heating zone. These unpyrolyzed carbon source gas mixtures, at high temperatures, are easily subjected to side reactions at the furnace outlet and in subsequent vacuum lines as their temperature slowly decreases during extraction by the vacuum pump. This generates viscous oil or deposits as solid carbon powder. With repeated use, this oil and carbon powder severely clogs the exhaust pipes, leading to decreased vacuum levels, reduced extraction efficiency, and even damage to the vacuum pump components. This significantly increases equipment maintenance and cleaning costs and directly affects the stability of the carbon plating process and product quality. Summary of the Invention

[0003] In order to solve the technical problems of unpyrolyzed carbon sources easily forming carbon powder and oil stains that clog pipes in the prior art, the present invention provides a quartz tube carbon plating device to prevent carbon source blockage.

[0004] To achieve the above objectives, the present invention designs a quartz tube carbon plating device to prevent carbon source blockage, comprising a furnace 1, a heating device 2, a liquid carbon source storage tank 3, a vacuum valve 4, a furnace plug 5, a gas storage tank 6, a gas valve 7, a gas flow meter 8, a vacuum resistance gauge 9, and a cooling device 10. The gas storage tank 6 is connected to the liquid carbon source storage tank 3 via a pipe. A gas valve 7 is provided on the connecting pipe between the gas storage tank 6 and the liquid carbon source storage tank 3. The liquid carbon source storage tank 3 is connected to the furnace 1 via a pipe. A gas flow meter 8 is provided on the connecting pipe between the liquid carbon source storage tank 3 and the furnace 1. A heating device 2 is provided on the outer wall of the furnace 1. A cooling device 10 is fitted on the outside of the gas outlet of the furnace 1. The tail of the furnace 1 is sealed and connected to the exhaust pipe via a furnace plug 5. A vacuum resistance gauge 9 and a vacuum valve 4 are provided in sequence on the exhaust pipe.

[0005] Preferably, the furnace chamber 1 is a silicon carbide furnace chamber, and a quartz table is provided inside, which is used to support the quartz tube to be carbonized.

[0006] Preferably, the furnace chamber 1 is provided with a quartz gas delivery rod, which is inserted from the plug of the furnace plug 5, and its gas outlet is located in the center of the quartz tube to be carbonized.

[0007] Preferably, the heating device 2 has a heating rate of 10℃ / min, which can heat the reaction zone of the furnace 1 to 800℃ and hold it for 1 hour, and then continue to heat it to 1000℃ and hold it for 1 hour.

[0008] Preferably, the heating device 2 is a resistance heating strip.

[0009] Preferably, the length of the cooling device 10 is 1 / 3 to 1 / 2 of the total length of the furnace 1, and it is installed at the tail end of the furnace 1 on the gas outlet side adjacent to the heating zone.

[0010] Preferably, the cooling device 10 is a water-cooled jacket, and circulating cooling water is circulated inside the water-cooled jacket.

[0011] Preferably, the heating device 2 is a resistance heating strip.

[0012] Preferably, the gas flow meter 8 stabilizes the airflow at 1 L / min.

[0013] Preferably, the gas storage tank 6 contains nitrogen gas, which bubbles the liquid in the liquid carbon source storage tank 3, carrying steam into the furnace 1.

[0014] Preferably, the liquid carbon source storage tank 3 contains acetone.

[0015] Compared with the prior art, the present invention has the following beneficial effects: The core of this invention lies in the innovative addition of a cooling device at the gas outlet of the silicon carbide furnace. Through the forced cooling effect of this device, excess carbon source gas that has not yet undergone pyrolysis rapidly cools down after leaving the high-temperature reaction zone (quenching effect). This rapid cooling effectively prevents the unpyrolyzed carbon source from polymerizing or coking at intermediate temperatures, thus avoiding its transformation into difficult-to-clean carbon powder and viscous oil. The cooled carbon source exhaust gas maintains good flowability, smoothly passing through the furnace plug 7 and subsequent pipelines, and is efficiently drawn away by the vacuum pump. This device completely solves the problem of easy blockage in the exhaust gas pipeline, extends the service life of the equipment, reduces maintenance frequency, and ensures the stability of the system vacuum. Attached Figure Description

[0016] Figure 1 This is a schematic diagram of the structure of a quartz tube carbon plating device for preventing carbon source blockage according to the present invention; The reference numerals in the figure are as follows: 1-furnace chamber; 2-heating device; 3-liquid carbon source storage tank; 4-vacuum valve; 5-furnace chamber plug; 6-gas storage tank; 7-gas valve; 8-gas flow meter; 9-vacuum resistance gauge; 10-cooling device.

[0017] Figure 2 This is a carbon-coated quartz tube successfully deposited using this device.

[0018] Figure 3 This is a SEM image of a carbon film successfully deposited on a carbon-coated quartz tube using this device.

[0019] Figure 4 The carbon source was blocked due to a clogged pipe in the charcoal furnace that was not equipped with a cooling device.

[0020] Figure 5 The carbon source was not blocked despite the installation of a cooling device to purify the carbon furnace pipes. Detailed Implementation

[0021] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0022] Example 1 like Figure 1 The aforementioned quartz tube carbon plating device for preventing carbon source blockage includes a furnace 1, a heating device 2, a liquid carbon source storage tank 3, a vacuum valve 4, a furnace plug 5, a gas storage tank 6, a gas valve 7, a gas flow meter 8, a vacuum resistance gauge 9, and a cooling device 10. The gas storage tank 6 is connected to the liquid carbon source storage tank 3 via a pipe. A gas valve 7 is provided on the connecting pipe between the gas storage tank 6 and the liquid carbon source storage tank 3. The liquid carbon source storage tank 3 is connected to the furnace 1 via a pipe. A gas flow meter 8 is provided on the connecting pipe between the liquid carbon source storage tank 3 and the furnace 1. A heating device 2 is provided on the outer wall of the furnace 1. A cooling device 10 is fitted on the outside of the gas outlet of the furnace 1. The tail of the furnace 1 is sealed and connected to the exhaust pipe via a furnace plug 5. A vacuum resistance gauge 9 and a vacuum valve 4 are provided in sequence on the exhaust pipe.

[0023] In this embodiment, the heating device 2 is a resistance heating belt, the furnace chamber 1 is a silicon carbide furnace chamber, the gas storage tank 6 is filled with nitrogen, the liquid carbon source storage tank 3 is filled with acetone, the cooling device 10 is a water cooling belt, and the vacuum valve 4 is connected to a vacuum pump.

[0024] Use as Figure 1 The method for preparing carbon-plated quartz tubes using the apparatus shown is described in detail below: (1) Place the cleaned and dried quartz tube on the quartz table inside the furnace chamber 1, and apply vacuum silicone grease to the furnace chamber plug 5 to seal the furnace chamber.

[0025] (2) Open the vacuum valve 4 to evacuate the entire pipeline and furnace 1, and monitor the vacuum level in the system in real time through the vacuum resistance gauge 9 to ensure that the system is in an oxygen-free state.

[0026] (3) When the entire system is in an oxygen-free state, turn the vacuum valve 4 angle valve to one turn, turn on the heating device 2, heat the furnace 1 to the set 800℃ at a heating rate of 10℃ / min and keep it at that temperature for 1 hour, then continue to heat it to 1000℃ to make the furnace 1 be filled with a uniform temperature field, heat the liquid carbon source storage tank 3 to 70℃ to make the acetone in the tank decompose at high temperature, turn on the gas valve 7 and turn on the gas flow meter 8 to make precise flow control, so that nitrogen is introduced into the high temperature furnace 1 at a uniform rate of 1L / min. The system is continuously ventilated for 1 hour. During this process, when the high-temperature exhaust gas carrying the unpyrolyzed acetone carbon source passes through the cooling device 10 area, the gas temperature is rapidly reduced. The rapid cooling effect causes the unpyrolyzed carbon source to lose the temperature conditions for generating polymer oil stains or carbon powder, thus maintaining its original state or existing in an extremely fine form. Subsequently, this cooled and safe exhaust gas passes through the furnace plug 5 used for sealing the end, passes through the vacuum resistance gauge 9 detection pipeline, and is finally smoothly extracted from the system by the vacuum pump through the vacuum valve 4 and safely discharged.

[0027] (8) After introducing nitrogen gas for 1 hour, stop heating device 2, stop heating liquid carbon source storage tank 3, close gas valve 7, fully open vacuum valve 4, so that the temperature of furnace 1 drops to room temperature, and take out carbon-plated quartz tube from furnace 1.

[0028] The results of scanning electron microscopy examination are as follows: Figure 3 As shown in (b), the carbon film thickness on the surface of the quartz tube is 0.8 micrometers, and there is no blockage in the tube. Figure 5 It can be used directly next time.

[0029] Example 2 The steps are the same as in Example 1, except that the process is changed during the ventilation stage, with nitrogen gas continuously purging for 0.5 hours, and then the ventilation is stopped.

[0030] The results of scanning electron microscopy examination are as follows: Figure 3 As shown in (c), the carbon film thickness on the surface of the quartz tube is 0.5 micrometers, and there is no blockage in the tube, so it can be used directly next time.

[0031] Example 3 The steps are the same as in Example 1, except that the process is changed during the ventilation phase, and ventilation is continued for 5 hours, after which ventilation is stopped.

[0032] The results of scanning electron microscopy examination are as follows: Figure 3 As shown in (a), the carbon film thickness on the surface of the quartz tube is 5 micrometers, and there is no blockage in the tube, so it can be used directly next time.

[0033] Comparative Example 3 In comparison, the device used in this comparative example differs from that used in Example 1 in that the furnace tube is not fitted with a water-cooling jacket. All other components and connection methods are the same as in Example 1. The quartz tube is carbonized in the same way as in Example 1. During the reaction, some of the acetone carbon source does not have time to be completely decomposed in the heating zone and moves to the tail with the gas flow.

[0034] In this comparative example, no water-cooling jacket was installed on the outside of the tail end of furnace 1. The high-temperature exhaust gas carrying the unpyrolyzed acetone carbon source passed directly through the furnace plug 5 used for sealing the end, and then through the detection pipeline where the vacuum resistance gauge 9 was located. Because the exhaust gas temperature was not rapidly reduced, the unpyrolyzed carbon source generated polymer oil and carbon powder at a suitable temperature, which gradually adhered to the inner wall of the pipeline, the interface of the vacuum resistance gauge, and the vacuum pump valve, causing pipeline blockage. Figure 4 As shown, the pipeline needs to be disassembled and cleaned before it can be used again.

[0035] In summary, this device features an ingenious structural design. By simply adding a cooling device at the gas outlet of the furnace, it perfectly solves the industry problem of carbon source condensation clogging the pipes in traditional chemical vapor deposition (CVD) carbon plating devices at extremely low modification costs, demonstrating its high practical value and significance for promotion.

[0036] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A quartz tube carbon plating device for preventing carbon source blockage, characterized in that: The quartz tube carbon plating device for preventing carbon source blockage includes a furnace (1), a heating device (2), a liquid carbon source storage tank (3), a vacuum valve (4), a furnace plug (5), a gas storage tank (6), a gas valve (7), a gas flow meter (8), a vacuum resistance gauge (9), and a cooling device (10). The gas storage tank (6) is connected to the liquid carbon source storage tank (3) through a pipe. A gas valve (7) is provided on the connecting pipe between the gas storage tank (6) and the liquid carbon source storage tank (3). The liquid carbon source storage tank (3) is connected to the furnace (1) through a pipe. A gas flow meter (8) is provided on the connecting pipe between the liquid carbon source storage tank (3) and the furnace (1). A heating device (2) is provided on the outer wall of the furnace (1). A cooling device (10) is provided on the outside of the gas outlet of the furnace (1). The tail of the furnace (1) is sealed and connected to the exhaust pipe through the furnace plug (5). A vacuum resistance gauge (9) and a vacuum valve (4) are provided in sequence on the exhaust pipe.

2. The quartz tube carbon plating device for preventing carbon source blockage according to claim 1, characterized in that: The furnace chamber (1) is a silicon carbide furnace chamber, and a quartz table is provided inside.

3. The quartz tube carbon plating device for preventing carbon source blockage according to claim 1, characterized in that: The furnace chamber (1) is equipped with a quartz gas delivery rod, which is inserted from the plug of the furnace plug (5) and its outlet is located in the center of the quartz tube to be carbonized.

4. The quartz tube carbon plating device for preventing carbon source blockage according to claim 1, characterized in that: The length of the cooling device (10) is 1 / 3 to 1 / 2 of the total length of the furnace (1).

5. The quartz tube carbon plating device for preventing carbon source blockage according to claim 1, characterized in that: The heating device (2) is a resistance heating strip.

6. The quartz tube carbon plating device for preventing carbon source blockage according to claim 1, characterized in that: The cooling device (10) is a water-cooled jacket, and circulating cooling water is circulated inside the water-cooled jacket.

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