Condensation recovery device and purification equipment

Abstract

The utility model relates to a condensation recovery device and purification equipment, the condensation recovery device comprises: a first condensation assembly, the first condensation assembly comprises a first condensation pipe, a first cooling cavity surrounding the first condensation pipe and a condensation coil pipe arranged in the first condensation pipe, the first condensation pipe is provided with an air inlet and a discharge port, and the discharge port is provided with a discharge port; the first cooling cavity and the condensing coil are used for cooling gas in the first condensing pipe together; the second condensation assembly communicates with the upper portion of the first condensation assembly and comprises a second condensation pipe, a second cooling cavity surrounding the second condensation pipe and a scraping mechanism arranged in the second condensation pipe, and the scraping mechanism comprises a rotating shaft and a scraping plate; the second cooling cavity is used for cooling gas in the second condensation pipe, and the scraper blade can scrape off condensation materials adhering to the second condensation pipe when rotating along with the rotating shaft. The condensation recovery device disclosed by the utility model is good in heat exchange effect, capable of improving the product yield and convenient to clean.

Description

Technical Field

[0001] The utility model relates to the technical field of condensation devices, in particular to a condensation recovery device and a purification device. Background Art

[0002] Precursors are important raw materials in the semiconductor industry, mainly used for semiconductor thin film deposition, including chemical vapor deposition (CVD), physical vapor deposition (PVD), atomic layer vapor deposition (ALD) and other deposition techniques derived therefrom. To achieve vapor deposition, high-purity precursor materials are required. Generally, the purity of solid precursors used for vapor deposition needs to reach 99.99999%, so purification treatment of solid precursors is required.

[0003] The sublimation condensation recovery device is one of the commonly used purification devices. First, the solid precursor is heated and sublimated, and then the sublimated gas is cooled and recovered by the condensation recovery device to obtain high-purity precursor powder. In the existing condensation recovery device, the heat exchange efficiency is poor, resulting in a low recovery rate of the precursor. In addition, after multiple condensations, the inner wall of the device is adhered with materials, which is not easy to clean and affects the recovery rate. Summary of the Utility Model

[0004] Based on the above defects in the prior art, the purpose of the present utility model is to provide a condensation recovery device with good heat exchange effect, which can improve the product yield and is easy to clean.

[0005] For this reason, the present utility model provides the following technical solutions.

[0006] The present utility model provides a condensation recovery device, which includes:

[0007] A first condensation component, which includes a first condensation tube, a first cooling cavity surrounding the first condensation tube, and a condensation coil disposed in the first condensation tube. The first condensation tube is provided with an air inlet and a discharge port, and the first cooling cavity and the condensation coil jointly cool the gas in the first condensation tube;

[0008] A second condensation component, which is connected above the first condensation component and includes a second condensation tube, a second cooling cavity surrounding the second condensation tube, and a scraping mechanism disposed in the second condensation tube. The scraping mechanism includes a rotating shaft and a scraping plate; the second cooling cavity is used to cool the gas in the second condensation tube, and when the scraping plate rotates with the rotating shaft, it can scrape the condensed material adhered to the second condensation tube.

[0009] Optionally, the condensation recovery device includes a transfer pipe, which is respectively connected to the first condensation tube and the second condensation tube;

[0010] The condensing coil is provided with a first refrigerant inlet and a first refrigerant outlet, and the first refrigerant inlet and the first refrigerant outlet are respectively connected to the transfer tube.

[0011] Optionally, the first condenser pipe is connected to the transfer pipe via a first flange, and the second condenser pipe is connected to the transfer pipe via a second flange.

[0012] Optionally, the first condenser tube, the second condenser tube and the transfer tube are all made of Hastelloy alloy.

[0013] Optionally, an oxide protective film layer is formed on the inner walls of the first condenser tube, the second condenser tube and the transfer tube.

[0014] Optionally, one end of the second condenser tube away from the first condenser tube is connected to a motor via a third flange, and a driving end of the motor is coaxially connected to the rotating shaft.

[0015] Optionally, the first condensing assembly includes a first cooling jacket, which is sleeved on the outer periphery of the first condensing tube to form the first cooling cavity therebetween;

[0016] The second condensing assembly includes a second cooling jacket, which is sleeved on the outer periphery of the second condensing tube to form the second cooling cavity therebetween.

[0017] Optionally, the first cooling chamber is used to accommodate a refrigerant at a temperature of 5-15°C, the condensing coil is used to accommodate a refrigerant at a temperature of 5-15°C, and the second cooling chamber is used to accommodate a refrigerant at a temperature of 0-10°C.

[0018] Optionally, a funnel section is provided at the bottom of the first condenser tube, and the discharge port is connected to the bottom of the funnel section;

[0019] And / or, a sight glass is provided at the lower part of the first condenser tube for observing the condensation condition in the first condenser tube;

[0020] And / or, the second condenser is provided with a pressure sensor interface, a temperature sensor interface, a vacuum interface and a cleaning interface.

[0021] The utility model also provides a purification device, which comprises:

[0022] A condensate recovery device as described above;

[0023] The sublimation device comprises a gas outlet, wherein the gas outlet is communicated with the gas inlet.

[0024] The utility model has the following technical effects:

[0025] The present utility model provides a condensation recovery device. During the upward flow of the sublimated gas, it is successively cooled by a first condensation component and a second condensation component. Moreover, the first condensation component cools through a first cooling cavity and a condensation coil together, improving the heat exchange effect, and thus the yield can be increased. In addition, part of the sublimated gas is condensed within the first condensation component, and the condensed material falls and drops from the discharge port into the collection tank. The remaining sublimated gas continues to flow upward into the second condensation component, where it is condensed into a condensed material and falls. A small amount of the condensed material adheres to the inner wall of the second condensation pipe and is scraped off by a scraping mechanism, improving the yield and facilitating subsequent cleaning. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] Figure 1 is a structural sectional view of the condensation recovery device of the present utility model;

[0027] Figure 2 is Figure 1 the enlarged view at A in

[0028] Figure 3 is Figure 2 the enlarged view at B in

[0029] Figure 4 is the top view of the condensation recovery device of the present utility model.

[0030] DESCRIPTION OF THE REFERENCE NUMERALS

[0031] 100, condensation recovery device;

[0032] 1, first condensation component; 11, first condensation pipe; 111, air inlet; 112, discharge port; 113, funnel section; 114, sight glass; 12, first cooling cavity; 13, condensation coil; 131, first refrigerant inlet; 132, first refrigerant outlet; 14, first cooling jacket; 141, second refrigerant inlet; 142, second refrigerant outlet;

[0033] 2, second condensation component; 21, second condensation pipe; 211, pressure sensor interface; 212, temperature sensor interface; 213, vacuum interface; 214, cleaning interface; 22, second cooling cavity; 23, scraping mechanism; 231, rotating shaft; 232, scraping plate; 24, second cooling jacket; 241, third refrigerant inlet; 242, third refrigerant outlet;

[0034] 3, adapter pipe; 4, first flange; 5, second flange; 6, third flange; 7, motor; 81, first seal; 82, second seal; 83, third seal. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0035] To make the technical solutions and beneficial effects of the present utility model more obvious and understandable, the following will be described in detail by way of specific examples. Unless otherwise defined, the technical and scientific terms used herein have the same meanings as those in the technical field to which this application belongs.

[0036] In the description of the present utility model, unless otherwise clearly defined, the orientation or positional relationship indicated by terms such as "center", "longitudinal", "transverse", "length", "width", "thickness", "height", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", etc. is based on the orientation or positional relationship shown in the drawings. It is only for the convenience of simplifying the description of the present utility model, rather than indicating that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, that is, it cannot be understood as a limitation to the present utility model.

[0037] In the present utility model, the terms "first" and "second" are only used for the purpose of clear description and cannot be understood as the relative importance of the indicated features or the number of the indicated technical features. Therefore, the features defined with "first" and "second" can clearly include at least one such feature. In the description of the present utility model, the meaning of "a plurality" is at least two; the meaning of "several" is at least one; unless otherwise clearly defined.

[0038] In the present utility model, unless otherwise clearly defined, terms such as "installation", "connection", "attachment", "fixation", "setting", etc. should be understood in a broad sense. For example, "connection" can be a fixed connection, a detachable connection or an integrally formed connection; it can be a mechanical connection or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium, and can also be the communication inside two elements or the interaction relationship between two elements. For those of ordinary skill in the art, the specific meanings of the above terms in the present utility model can be understood according to specific circumstances.

[0039] In the present utility model, unless otherwise clearly defined, the first feature being "on", "above", "over" and "upon" the second feature, or "under", "beneath", "below" or "underneath" the second feature can be that the first feature is in direct contact with the second feature, or the first feature and the second feature are in indirect contact through an intermediate medium. Moreover, the first feature being "above", "over" and "upon" the second feature can be that the first feature is directly above or obliquely above the second feature, or merely indicates that the horizontal height of the first feature is higher than the horizontal height of the second feature. The first feature being "under", "beneath", "below" and "underneath" the second feature can be that the first feature is directly below or obliquely below the second feature, or merely indicates that the horizontal height of the first feature is less than the horizontal height of the second feature.

[0040] The "upper" and "lower" mentioned in the present utility model are both based on Figure 1 the markings in

[0041] Next, according to Figures 1 to 4 the present utility model will be described in detail for the condensation recovery device.

[0042] In this embodiment, as Figures 1 to 3 shown, the condensation recovery device 100 includes a first condensation assembly 1 and a second condensation assembly 2. The first condensation assembly 1 includes a first condensation pipe 11, a first cooling chamber 12 surrounding the first condensation pipe 11, and a condensation coil 13 disposed inside the first condensation pipe 11. The first condensation pipe 11 is provided with an air inlet 111 and a discharge port 112, and the air inlet 111 is used to introduce the sublimated gas. The first cooling chamber 12 is used to accommodate the refrigerant, and the gas inside the first condensation pipe 11 is cooled jointly by the first cooling chamber 12 and the condensation coil 13. The second condensation assembly 2 is connected above the first condensation assembly 1. The second condensation assembly 2 includes a second condensation pipe 21, a second cooling chamber 22 sleeved on the outer periphery of the second condensation pipe 21, and a scraping mechanism 23 disposed inside the second condensation pipe 21. The scraping mechanism 23 includes a rotating shaft 231 and a scraping plate 232. The second cooling chamber 22 is used to accommodate the refrigerant, and thus can cool the gas inside the second condensation pipe 21. At the same time, when the rotating shaft 231 starts to rotate, the rotating shaft 231 drives the scraping plate 232 to rotate synchronously, and the scraping plate 232 can scrape the condensed material adhered to the second condensation pipe 21 during the rotation process.

[0043] By adopting the above technical solution, during the upward flow of the sublimated gas, it is successively cooled by the first condensation assembly 1 and the second condensation assembly 2 respectively. And the first condensation assembly 1 jointly implements cooling through the first cooling chamber 12 and the condensation coil 13, improving the heat exchange effect, and thus can improve the yield. In addition, part of the sublimated gas is condensed inside the first condensation assembly 1, and the condensed material falls and drops from the discharge port 112 into the collection tank. The remaining sublimated gas continues to flow upward into the second condensation assembly 2 and is condensed into condensed material and falls inside the second condensation assembly 2. A small part of the condensed material will adhere to the inner wall of the second condensation pipe 21 and is scraped by the scraping mechanism 23, improving the yield and facilitating subsequent cleaning. The condensation recovery device 100 of this solution can be used for the condensation recovery after sublimation of common solid precursors in the semiconductor industry, including but not limited to solid precursors such as aluminum trichloride, hafnium tetrachloride, trimethylindium, and pentakis(dimethylamino)tantalum.

[0044] In one embodiment, as Figure 1As shown in the figure, the condensation recovery device 100 includes a transfer pipe 3. The lower port of the transfer pipe 3 is connected to the first condenser pipe 11, and the upper port of the transfer pipe 3 is connected to the second condenser pipe 21. The condensation coil 13 is provided with a first refrigerant inlet 131 and a first refrigerant outlet 132, and the first refrigerant inlet 131 and the first refrigerant outlet 132 are respectively inserted through the transfer pipe 3.

[0045] Furthermore, as Figure 1 and Figure 2 shown in the figure, the first condenser pipe 11 and the transfer pipe 3 are connected by a first flange 4, and the assembly gap between the first condenser pipe 11, the transfer pipe 3 and the first flange 4 is sealed by a first seal 81. The second condenser pipe 21 and the transfer pipe 3 are connected by a second flange 5, and the assembly gap between the second condenser pipe 21, the transfer pipe 3 and the second flange 5 is sealed by a second seal 82. For the condensation recovery device 100 of this solution, the first condenser pipe 11 can be detached from the transfer pipe 3 for cleaning. Also, after detaching the second condensation assembly 2 from the transfer pipe 3 first, the second condenser pipe 21 and the scraping mechanism 23 can be separated and cleaned respectively, where the condensation coil 13 is cleaned together with the transfer pipe 3.

[0046] In one embodiment, the first condenser pipe 11, the second condenser pipe 21 and the transfer pipe 3 are all Hastelloy parts. The sublimation temperature of the solid precursor is generally 150 - 350°C. The existing condensation recovery devices use 316 stainless steel, which is prone to corrosion under the long-term action of corrosive steam at 150 - 350°C. However, the Hastelloy of this solution has good corrosion resistance to acidic gases at 150 - 350°C.

[0047] In one embodiment, oxide protective film layers are formed on the inner walls of the first condenser pipe 11, the second condenser pipe 21 and the transfer pipe 3. In a specific embodiment, the first condenser pipe 11, the second condenser pipe 21 and the transfer pipe 3 are all made of Hastelloy into seamless pipe structures, and then mechanical polishing and electro-chemical polishing treatments are successively performed on the inner walls of the pipes, so that the surface roughness of the corresponding inner walls of the pipes ≤ 0.25μm, and a dense oxide protective film layer can also be formed on the corresponding inner walls of the pipes, effectively preventing the first condenser pipe 11, the second condenser pipe 21 and the transfer pipe 3 from contaminating the condensed material due to ion precipitation.

[0048] In one embodiment, as Figure 1 shown in the figure, the number of the scraping plates 232 is at least two, and all the scraping plates 232 are arranged in a circumferential array to increase the scraping force.

[0049] In one embodiment, a plurality of protrusions (not shown in the figure) and a plurality of grooves (not shown in the figure) are provided on the side wall of the scraping plate 232 facing away from the rotating shaft 231, and the protrusions and the grooves are alternately arranged in the axial direction of the rotating shaft 231; when the scraping plate 232 rotates, the protrusions are used to scrape the condensed material adhered to the second condensing pipe 21, and the grooves are used to disperse the scraped condensed material, playing the role of scraping and dispersing. Specifically, the scraping mechanism 23 is located inside the second condensing pipe 21. Since the inner space of the second condensing pipe 21 is limited, by providing the protrusions and the grooves alternately arranged on the side wall of the scraping plate 232, the occupied space is small.

[0050] In one embodiment, as Figure 1 and Figure 2 shown, the first condensing assembly 1 includes a first cooling jacket 14, the first cooling jacket 14 is sleeved on the outer periphery of the first condensing pipe 11, a first cooling cavity 12 is formed between the first cooling jacket 14 and the first condensing pipe 11, the first cooling jacket 14 is provided with a second refrigerant inlet 141 and a second refrigerant outlet 142, and the second refrigerant inlet 141 is used for introducing refrigerant. As Figure 1 and Figure 3 shown, the second condensing assembly 2 includes a second cooling jacket 24, the second cooling jacket 24 is sleeved on the outer periphery of the second condensing pipe 21, a second cooling cavity 22 is formed between the second cooling jacket 24 and the second condensing pipe 21, the second cooling jacket 24 is provided with a third refrigerant inlet 241 and a third refrigerant outlet 242, and the third refrigerant inlet 241 is used for introducing refrigerant.

[0051] In one embodiment, the first cooling cavity 12 is used to accommodate refrigerant at 5 - 15 °C, the condensing coil 13 is used to accommodate refrigerant at 5 - 15 °C, the second cooling cavity 22 is used to accommodate refrigerant at 0 - 10 °C. This solution uses a two-stage different refrigerant to condense and sublimate the gas, improving the refrigerant utilization rate, and thus can improve the product yield.

[0052] In one embodiment, as Figure 1 and Figure 3 shown, one end of the second condensing pipe 21 facing away from the first condensing pipe 11 is connected to the motor 7 through a third flange 6, the driving end of the motor 7 is coaxially connected to the rotating shaft 231, and the assembly gaps of the second condensing pipe 21, the third flange 6 and the motor 7 are sealed by a third seal 83. When it is necessary to clean the second condensing pipe 21 and the scraping mechanism 23, the motor 7 needs to be removed first, and then the scraping mechanism 23 is taken out to clean the second condensing pipe 21 and the scraping mechanism 23 respectively.

[0053] In one embodiment, as Figure 1 shown, the bottom of the first condensing pipe 11 is provided with a funnel section 113, the discharge port 112 communicates with the bottom of the funnel section 113, and the pipe wall of the funnel section 113 gradually narrows from top to bottom to guide the falling condensed material to the discharge port 112.

[0054] In one embodiment, as Figure 1 and Figure 4 shown, the second condenser 21 is provided with a pressure sensor interface 211, a temperature sensor interface 212, a vacuum interface 213 and a cleaning interface 214. The pressure sensor interface 211 is used to install a pressure sensor to obtain the pressure value inside the second condenser 21 through the pressure sensor; the temperature sensor interface 212 is used to install a temperature sensor to obtain the temperature value inside the second condenser 21 through the temperature sensor; the vacuum interface 213 is used to connect to a vacuum pump to evacuate the second condenser 21, the adapter tube 3 and the first condenser 11 through the vacuum pump; the cleaning interface 214 is used to connect to a cleaning device to introduce a cleaning liquid.

[0055] In one embodiment, as Figure 1 shown, a sight glass 114 is provided at the lower part of the first condenser 11. The sight glass 114 is located below the condensing coil 13 and the first cooling chamber 12 to observe the condensation condition inside the first condenser 11.

[0056] The present utility model also provides a purification device. The purification device includes a condensation recovery device 100 and a sublimation device (not shown in the figure). The sublimation device includes an air outlet, and the air outlet is communicated with the air inlet 111. The material to be purified is first heated and sublimated into a gas by the sublimation device, and the sublimated gas enters the first condenser 11 through the air inlet 111, and then is condensed by the condensation recovery device 100 to obtain a powdered material.

[0057] The specific use steps of the condensation recovery device 100 in this solution are as follows: Before the condensation starts, coolants at 5 - 15°C are respectively introduced into the first coolant inlet 131 and the second coolant inlet 141, and a coolant at 0 - 10°C is introduced into the third coolant inlet 241. When the temperature inside the condensation recovery device 100 cools down to a preset temperature, the motor 7 is started. The sublimated gas enters the first condenser 11 from the air inlet 111. Part of the sublimated gas is condensed by the first condensation assembly 1 to form a condensed material, and the condensed material falls and is discharged through the discharge port 112. The remaining sublimated gas continues to flow upward and enters the second condenser 21, where it is cooled by the second condensation assembly 2 to form a condensed material. Moreover, the material adhered to the inner wall of the second condenser 21 is scraped off by the scraper 232 of the scraping mechanism 23.

[0058] It should be understood that the above embodiments are all exemplary and do not cover all possible implementation manners included in the claims. Without departing from the scope of the present disclosure, various deformations and changes can also be made on the basis of the above embodiments. Similarly, various technical features of the above embodiments can also be arbitrarily combined to form additional embodiments of the present utility model that may not be clearly described. Therefore, the above embodiments only represent several implementation manners of the present utility model and do not limit the protection scope of the patent of the present utility model.

Claims

1. A condensation recovery device, characterized in that: The condensation recovery device (100) comprises: A first condensation component (1), comprising a first condensation tube (11), a first cooling chamber (12) surrounding the first condensation tube (11), and a condensation coil (13) arranged in the first condensation tube (11), the first condensation tube (11) being provided with an air inlet (111) and a discharge port (112), the first cooling chamber (12) and the condensation coil (13) jointly cooling the gas in the first condensation tube (11); The second condensation component (2) is connected to the top of the first condensation component (1), and includes a second condensation tube (21), a second cooling chamber (22) surrounding the second condensation tube (21), and a scraping mechanism (23) arranged in the second condensation tube (21), and the scraping mechanism (23) includes a rotating shaft (231) and a scraper (232); the second cooling chamber (22) is used to cool the gas in the second condensation tube (21), and the scraper (232) can scrape off the condensed material adhered to the second condensation tube (21) when rotating with the rotating shaft (231).

2. The condensation recovery device according to claim 1, characterized in that: The condensation recovery device (100) comprises a transfer tube (3) which is respectively connected to the first condensation tube (11) and the second condensation tube (21); The condensing coil (13) is provided with a first refrigerant inlet (131) and a first refrigerant outlet (132), and the first refrigerant inlet (131) and the first refrigerant outlet (132) are respectively connected to the transfer tube (3).

3. The condensation recovery device according to claim 2, characterized in that: The first condenser pipe (11) is connected to the transfer pipe (3) via a first flange (4), and the second condenser pipe (21) is connected to the transfer pipe (3) via a second flange (5).

4. The condensation recovery device according to claim 2, characterized in that: The first condenser tube (11), the second condenser tube (21) and the transfer tube (3) are all Hastelloy alloy parts.

5. The condensation recovery device according to claim 2, characterized in that: The inner walls of the first condenser tube (11), the second condenser tube (21) and the transfer tube (3) are all formed with an oxide protective film layer.

6. The condensation recovery device according to any one of claims 1 to 5, characterized in that: One end of the second condenser tube (21) facing away from the first condenser tube (11) is connected to the motor (7) via a third flange (6), and the driving end of the motor (7) is coaxially connected to the rotating shaft (231).

7. The condensation recovery device according to any one of claims 1 to 5, characterized in that: The first condensing assembly (1) comprises a first cooling jacket (14), which is sleeved on the outer circumference of the first condensing tube (11) and forms the first cooling chamber (12) therebetween; The second condensing component (2) comprises a second cooling jacket (24), which is sleeved on the outer circumference of the second condensing tube (21) and forms the second cooling chamber (22) therebetween.

8. The condensation recovery device according to any one of claims 1 to 5, characterized in that: The first cooling chamber (12) is used to accommodate a refrigerant at a temperature of 5-15°C, the condensing coil (13) is used to accommodate a refrigerant at a temperature of 5-15°C, and the second cooling chamber (22) is used to accommodate a refrigerant at a temperature of 0-10°C.

9. The condensation recovery device according to any one of claims 1 to 5, characterized in that: A funnel section (113) is provided at the bottom of the first condenser tube (11), and the discharge port (112) is connected to the bottom of the funnel section (113); And / or, a sight glass (114) is provided at the lower part of the first condenser tube (11) for observing the condensation condition in the first condenser tube (11); And / or, the second condenser (21) is provided with a pressure sensor interface (211), a temperature sensor interface (212), a vacuum interface (213) and a cleaning interface (214).

10. A purification device, characterized in that: The purification equipment comprises: The condensation recovery device according to any one of claims 1 to 9; A sublimation device comprises a gas outlet, wherein the gas outlet is connected to the gas inlet (111).

Images