ALD solid precursor production device

Abstract

The utility model discloses an ALD (atomic layer deposition) solid precursor production device which comprises a liquid raw material pretreatment unit, a reaction unit, a filtration unit and a distillation unit, and the liquid raw material pretreatment unit comprises one or more treatment steps of liquid raw material deoxidization, water removal and cracking purification. Wherein the liquid raw material cracking and purifying treatment adopts a commercially available molecular distillation device or wiped film evaporation device, the filtering unit adopts a commercially available cylinder-cone type filtering, washing and drying three-in-one filtering machine, a helical ribbon type stirring paddle is adopted in the filtering unit, the distillation unit adopts a cylinder-cone type distillation kettle, and the distillation unit adopts a double-screw type stirring paddle. A helical ribbon type stirring paddle is adopted in the cylinder cone type distillation still, and when the ALD solid precursor production device is used for producing an ALD solid precursor, the production process is safe and efficient, and the automation degree is high.

Description

Technical Field

[0001] The utility model relates to the technical field of ALD precursor production devices, and more specifically, it relates to an ALD solid precursor production device. Background Technique

[0002] ALD precursors are key materials used in the thin film deposition process in advanced integrated circuit manufacturing. ALD precursors can be classified into gaseous, liquid, and solid precursors according to their precursor states. Most ALD precursors will undergo violent chemical reactions when exposed to water or oxygen at normal temperature and pressure, releasing heat and even catching fire. At the same time, even if ALD precursors come into contact with trace amounts of water or oxygen, it will cause the precursors to deteriorate, and thus cannot meet the requirements of integrated circuit manufacturing for precursor materials. Therefore, the production process of ALD precursor products requires anhydrous and anoxic conditions throughout. Due to the precursor state, gaseous and liquid ALD precursors are easy to transport and produce during the production process. However, there are few reports on the preparation devices or production devices for solid ALD precursors. The patent publication number CN214915953U discloses a synthesis system for ALD precursors, which uses a specially designed annular reactor. This system device is a customized product and is not easy to obtain. Therefore, the present utility model proposes an ALD solid precursor production device, which is composed of commercially available conventional kettles, tanks, etc. combined and integrated. The device is easy to build and is easy to achieve the airtight continuous, safe and efficient production of ALD solid precursors. Summary of the Utility Model

[0003] (I) Technical Problems to be Solved

[0004] In view of the problems existing in the prior art, the present utility model provides an ALD solid precursor production device to solve the technical problems mentioned in the background technique.

[0005] (II) Technical Solutions

[0006] To achieve the above object, the present utility model provides the following technical solution: An ALD solid precursor production device, comprising a first liquid raw material tank, a second liquid raw material tank, a solid raw material feeder, a cracking and purification device, a reaction kettle, a cylinder-cone type filtration, washing, and drying three-in-one filter, a cylinder-cone type distillation kettle, a distillation kettle heat exchanger, a first liquid raw material recovery tank, a second liquid raw material recovery tank, a first valve, a second valve, a third valve, a fourth valve, a fifth valve, a sixth valve, a seventh valve, an eighth valve, a ninth valve, a tenth valve, an eleventh valve, a twelfth valve, a thirteenth valve, a fourteenth valve, a fifteenth valve, a seventeenth valve, an eighteenth valve, a nineteenth valve, a twentieth valve, a twenty-first valve, a twenty-second valve, a twenty-third valve, a twenty-fourth valve, a twenty-fifth valve, a twenty-sixth valve, a twenty-seventh valve, a twenty-eighth valve, a twenty-ninth valve, a thirtieth valve, a thirty-first valve, a thirty-second valve, a thirty-fourth valve, a thirty-fifth valve, a first pipeline sight glass, a second pipeline sight glass, a first stirring motor, a second stirring motor, a third stirring motor, a fourth stirring motor, a fifth stirring motor. Multiple components are connected by pipelines.

[0007] The present utility model is further configured such that the first liquid raw material tank is connected to the reaction kettle through the fourth valve, the seventh valve, and a pipeline, realizing the function of transporting the liquid raw material from the first liquid raw material tank to the reaction kettle.

[0008] The present utility model is further configured such that the cracking and purification device is connected to the reaction kettle through the eighth valve and a pipeline, realizing the function of transporting the liquid raw material from the cracking and purification device to the reaction kettle.

[0009] The present utility model is further configured such that the solid raw material feeder is connected to the reaction kettle through the ninth valve and a pipeline, realizing the function of transporting the solid raw material from the solid raw material feeder to the reaction kettle.

[0010] The present utility model is further configured such that the reaction kettle is connected to the cylinder-cone type filtration, washing, and drying three-in-one filter through the eleventh valve, the thirteenth valve, and a pipeline, realizing the function of transporting the solid-liquid mixture from the reaction kettle to the cylinder-cone type filtration, washing, and drying three-in-one filter for filtration unit operation.

[0011] The present utility model is further configured such that the cylinder-cone type filtration, washing, and drying three-in-one filter is connected to the cylinder-cone type distillation kettle and the reaction kettle through the fifteenth valve, the first pipeline sight glass, the seventeenth valve, the eighteenth valve, and the tenth valve respectively, realizing the function of transporting the turbid material from the cylinder-cone type filtration, washing, and drying three-in-one filter to the reaction kettle and transporting the clear filtrate from the cylinder-cone type filtration, washing, and drying three-in-one filter to the cylinder-cone type distillation kettle.

[0012] The present utility model is further configured such that the cylinder-cone type distillation kettle is connected to the first liquid raw material recovery tank and the second liquid raw material recovery tank through the nineteenth valve, the distillation kettle heat exchanger, the thirty-first valve, the thirty-second valve, the second pipeline sight glass and pipelines, so as to realize that the raw material steam distilled from the cylinder-cone type distillation kettle is heat-exchanged and condensed into liquid and then flows to the first liquid raw material recovery tank or the second liquid raw material recovery tank for collection.

[0013] The present utility model is further configured such that the second liquid raw material tank is connected to the cylinder-cone type distillation kettle through the twentieth valve and the twenty-fifth valve, so as to realize the function of conveying the liquid raw material from the second liquid raw material tank to the cylinder-cone type distillation kettle.

[0014] The present utility model is further configured such that the first liquid raw material recovery tank is connected to the first liquid raw material tank through the thirtieth valve, the first valve and pipelines, so as to realize the function of conveying the recovered liquid raw material from the first liquid raw material recovery tank to the first liquid raw material tank.

[0015] The present utility model is further configured such that the second liquid raw material recovery tank is connected to the second liquid raw material tank through the twenty-ninth valve, the twenty-sixth valve and pipelines, so as to realize the function of conveying the recovered liquid raw material from the second liquid raw material recovery tank to the second liquid raw material tank; the cylinder-cone type distillation kettle is connected to the reaction kettle and the cylinder-cone type filtration, washing and drying three-in-one filter through the twenty-first valve, the twenty-second valve, the twenty-third valve, the sixth valve, the twenty-fourth valve, the twelfth valve and pipelines, so as to realize the function of conveying the material from the cylinder-cone type distillation kettle to the reaction kettle or the cylinder-cone type filtration, washing and drying three-in-one filter.

[0016] The present utility model is further configured such that through the connection of the twenty-first valve, the thirty-fifth valve and pipelines and the spiral ribbon type stirring paddle inside the cylinder-cone type distillation kettle, the function of closed continuous conveying of the solid precursor crude product is realized.

[0017] (III) Beneficial effects

[0018] Compared with the prior art, the present utility model provides an ALD solid precursor production device, which has the following beneficial effects:

[0019] 1. The liquid raw material distilled from the cylinder-cone type distillation kettle R03 enters the first liquid raw material recovery tank or the second liquid raw material recovery tank after being heat-exchanged by the distillation kettle heat exchanger, and then returns to the first liquid raw material tank or the second liquid raw material tank, and the liquid raw material can be recycled.

[0020] 2. When using the device of the present utility model to produce the ALD solid precursor crude product, the ALD solid precursor crude product can realize closed continuous discharging, with high automation degree, and the production process is safe and efficient. Description of the drawings

[0021] Figure 1 It is a schematic flow diagram of an ALD solid precursor production device.

[0022] In the figure: 101, reaction kettle; 102, cracking and purification device; 103, cylinder-cone type distillation kettle; 201, cylinder-cone type filter, washing and drying three-in-one filter; 301, first liquid raw material tank; 302, solid raw material feeder; 303, second liquid raw material tank; 304, first liquid raw material recovery tank; 305, second liquid raw material recovery tank; 401, first stirring motor; 402, second stirring motor; 403, third stirring motor; 404, fourth stirring motor; 405, fifth stirring motor; 501, distillation kettle heat exchanger; 61, first valve; 62, second valve; 63, third valve; 64, fourth valve; 65, fifth valve; 66, sixth valve; 67, seventh valve; 68, eighth valve; 69, ninth valve; 610, tenth valve; 611, eleventh valve; 612, twelfth valve; 613, thirteenth valve; 614, fourteenth valve; 615, fifteenth valve; 616, first pipeline sight glass; 617, seventeenth valve; 618, eighteenth valve; 619, nineteenth valve; 620, twentieth valve; 621, twenty-first valve; 622, twenty-second valve; 623, twenty-third valve; 624, twenty-fourth valve; 625, twenty-fifth valve; 626, twenty-sixth valve; 627, twenty-seventh valve; 628, twenty-eighth valve; 629, twenty-ninth valve; 630, thirtieth valve; 631, thirty-first valve; 632, thirty-second valve; 633, second pipeline sight glass; 634, thirty-fourth valve; 635, thirty-fifth valve. Specific embodiments

[0023] It should be noted that, without conflict, the embodiments in this application and the features in the embodiments can be combined with each other. The present invention will be described in detail below with reference to the drawings and in combination with the embodiments.

[0024] It should be pointed out that unless otherwise specified, all technical and scientific terms used in this application have the same meaning as commonly understood by those of ordinary skill in the technical field to which this application belongs.

[0025] In the present invention, unless otherwise stated, the orientations such as "up, down" are usually in the directions shown in the drawings, or in the vertical, perpendicular or gravitational directions; similarly, for ease of understanding and description, "left, right" are usually in the left and right shown in the drawings; "inside, outside" refer to the inside and outside relative to the contours of each component itself, but the above orientation terms do not limit the present invention.

[0026] Please refer toFigure 1 , an ALD solid precursor production device, including a first liquid raw material tank 301, a second liquid raw material tank 303, a solid raw material feeder 302, a cracking and purification device 102, a reaction kettle 101, a cylinder-cone type filtration, washing, and drying three-in-one filter 201, a cylinder-cone type distillation kettle 103, a distillation kettle heat exchanger 501, a first liquid raw material recovery tank 304, a second liquid raw material recovery tank 305, a first valve 61, a second valve 62, a third valve 63, a fourth valve 64, a fifth valve 65, a sixth valve 66, a seventh valve 67, an eighth valve 68, a ninth valve 69, a tenth valve 610, an eleventh valve 611, a twelfth valve 612, a thirteenth valve 613, a fourteenth valve 614, a fifteenth valve 615, a seventeenth valve 617, an eighteenth valve 618, a nineteenth valve 619, a twentieth valve 620, a twenty-first valve 621, a twenty-second valve 622, a twenty-third valve 623, a twenty-fourth valve 624, a twenty-fifth valve 625, a twenty-sixth valve 626, a twenty-seventh valve 627, a twenty-eighth valve 628, a twenty-ninth valve 629, a thirtieth valve 630, a thirty-first valve 631, a thirty-second valve 632, a thirty-fourth valve 634, a thirty-fifth valve 635, a first pipeline sight glass 616, a second pipeline sight glass 633, a first stirring motor 401, a second stirring motor 402, a third stirring motor 403, a fourth stirring motor 404, a fifth stirring motor 405, and multiple components are connected by pipelines.

[0027] In this embodiment, the deoxygenation and dehydration of the liquid raw materials in the liquid raw material pretreatment unit are carried out in the first liquid raw material tank 301 and the second liquid raw material tank 303. On the premise that the first stirring motor 401 and the fifth stirring motor 405 are turned on, the first liquid raw material tank 301 and the second liquid raw material tank 303 are first evacuated to a low vacuum until the gauge pressure reaches -10 to -30 Kpa, and then filled with an inert gas until the gauge pressure reaches 0 kpa. This operation is repeated 30 to 300 times to remove the oxygen in the liquid raw materials. The inert gas can be one of high-purity nitrogen, high-purity argon, high-purity helium, high-purity neon, and high-purity xenon, preferably high-purity nitrogen and high-purity argon.

[0028] More specifically, the method for dehydrating the liquid raw materials is to put 3A molecular sieves activated at 5% to 50% of the mass of the liquid raw materials into the first liquid raw material tank 301 and the second liquid raw material tank 303 and soak them for 12 to 48 hours to adsorb and remove the moisture in the liquid raw materials. The tanks of the first liquid raw material tank 301 and the second liquid raw material tank 303 for dehydrating the liquid raw materials are of a lower cone type, and a spiral ribbon type stirring paddle is used inside, which is convenient for discharging after the 3A molecular sieves are saturated with adsorption.

[0029] In summary, the overall equipment is used as follows:

[0030] The cracking and purification of the liquid raw material is carried out by using a commercially available molecular distillation device or a wiped film evaporation device cracking purifier 102 to crack and purify the liquid raw material. The filtration unit uses a commercially available cylindrical-conical type filtration, washing, and drying three-in-one filter 201. The distillation unit uses a commercially available cylindrical-conical type distillation kettle 103. The inside of the cylindrical-conical type distillation kettle 103 is equipped with a spiral ribbon type stirring paddle. The liquid raw material distilled from the cylindrical-conical type distillation kettle 103 enters the first liquid raw material recovery tank 304 or the second liquid raw material recovery tank 305 after being heat-exchanged by the distillation kettle heat exchanger 501, and then returns to the first liquid raw material tank 301 and the second liquid raw material tank 303, and the liquid raw material can be recycled.

[0031] First, tetrahydrofuran and toluene raw materials are respectively fed into the first liquid raw material tank 301 and the second liquid raw material tank 303. Then, activated 3A molecular sieves accounting for 25% of the mass of the liquid raw materials are respectively added into the first liquid raw material tank 301 and the second liquid raw material tank 303. The first stirring motor 401 and the fifth stirring motor 405 are started to stir the tetrahydrofuran and toluene in the first liquid raw material tank 301. Then, the first liquid raw material tank 301 and the second liquid raw material tank 303 are first evacuated to a gauge pressure of -20 Kpa and then filled with nitrogen until the gauge pressure is normal pressure. This operation is repeated 200 times to remove the oxygen in the raw materials of tetrahydrofuran and toluene. Then, the first stirring motor 401 and the fifth stirring motor 405 are turned off, and left standing for 24 hours to allow the 3A molecular sieve to adsorb and remove the moisture in the raw materials of tetrahydrofuran and toluene. The fourth valve 64 and the seventh valve 67 are opened to transfer the tetrahydrofuran raw material in the first liquid raw material tank 301 into the reaction kettle 101. The ninth valve 69 is opened, and sodium hydride solid is added into the reaction kettle 101 through the solid feeder 302. The eighth valve 68 is opened to drop the methylcyclopentadiene cracked and purified by the cracking purifier 102 into the reaction kettle 101 for chemical reaction to generate sodium methylcyclopentadienyl. Then, the eleventh valve 611 and the thirteenth valve 613 are opened to transfer the solid-liquid mixture in the reaction kettle 101 into the cone-cylinder type filter, washer, and dryer integrated filter 201 for filtration. The fifteenth valve 615, the seventeenth valve 617, and the tenth valve 610 are opened, and the filtrate flows back to the reaction kettle 101. Until the filtrate is observed to be clear through the first pipeline sight glass 616, the eighteenth valve 618 is opened, the seventeenth valve 617 and the tenth valve 610 are closed, and the clear filtrate flows to the cone-cylinder type distillation kettle 103. After filtration is completed, the twentieth valve 621, the twenty-second valve 622, the twenty-third valve 623, and the sixth valve 66 are opened to transfer the filtrate into the reaction kettle 101. The ninth valve 69 is opened, and yttrium trichloride solid is added into the reaction kettle 101 through the solid feeder 302 for chemical reaction to generate tris(methylcyclopentadienyl)yttrium. Then, the eleventh valve 611 and the thirteenth valve 613 are opened to transfer the solid-liquid mixture in the reaction kettle 101 into the cone-cylinder type filter, washer, and dryer integrated filter 201 for filtration. The fifteenth valve 615, the seventeenth valve 617, and the tenth valve 610 are opened, and the filtrate flows back to the reaction kettle 101. Until the filtrate is observed to be clear through the first pipeline sight glass 616, the eighteenth valve 618 is opened, the seventeenth valve 617 and the tenth valve 610 are closed, and the clear filtrate flows to the cone-cylinder type distillation kettle 103. After filtration is completed, the nineteenth valve 619, the thirty-second valve 632, and the thirty-fourth valve 634 are opened, and the fourth stirring motor 404 is started to stir the cone-cylinder type distillation kettle 103. The tetrahydrofuran in the cone-cylinder type distillation kettle 103 is vacuum distilled by vacuum until it is heat exchanged and condensed into a liquid state by the distillation kettle heat exchanger 501 and then flows into the first liquid raw material recovery tank 304.Open the 30th valve 630 and the 1st valve 61 to transport the recycled tetrahydrofuran raw material in the first liquid raw material recovery tank 304 to the first liquid raw material tank 301 for use in the next batch of production. Open the 25th valve 625 and the 20th valve 620 to transport the toluene raw material in the second liquid raw material tank 303 to the cylinder-cone type distillation kettle 103 to dissolve the yttrium tris(trimethylcyclopentadienyl) in the cylinder-cone type distillation kettle 103. Then open the 21st valve 621, the 22nd valve 622, the 20th valve 624, and the 12th valve 612 to transport the materials in the cylinder-cone type distillation kettle 103 to the cylinder-cone type filtration, washing, and drying three-in-one filter 201 for filtration. Open the 15th valve 615, the 17th valve 617, and the 10th valve 610, and the filtrate flows back to the reaction kettle 101. After observing that the filtrate is clear through the first pipeline sight glass 616, open the 18th valve 618, close the 17th valve 617 and the 10th valve 610, and the clear filtrate flows to the cylinder-cone type distillation kettle 103. After filtration is completed, open the 19th valve 619, the 31st valve 631, and the 34th valve 634, start the fourth stirring motor 404 to start stirring the cylinder-cone type distillation kettle 103, and vacuum distill the toluene in the cylinder-cone type distillation kettle 103 to the distillation kettle heat exchanger 501 for heat exchange and condensation into a liquid state and then flow into the second liquid raw material recovery tank 305. Open the 29th valve 629 and the 26th valve 626 to transport the recycled toluene raw material in the second liquid raw material recovery tank 305 to the second liquid raw material tank 303 for use in the next batch of production. The ALD solid precursor crude product is obtained in the cylinder-cone type distillation kettle 103. Open the 21st valve 621 and the 35th valve 635, and the ribbon agitator in the cylinder-cone type distillation kettle 103 can continuously transport the ALD solid precursor crude product under the drive of the fourth stirring motor 404.,

[0032] In all the above-mentioned solutions, for the connection between two components, welding, connection with bolts and nuts, connection with bolts or screws, or other well-known connection methods can be selected according to the actual situation, which will not be elaborated here one by one. For those involving fixed connection in the above text, welding is preferably considered. Although the embodiments of the present invention have been shown and described, for those of ordinary skill in the art, it can be understood that various changes, modifications, substitutions, and variations can be made to these embodiments without departing from the principle and spirit of the present invention. The scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. An ALD solid precursor production device, comprising a reaction kettle (101), a cracking and purification device (102), a cylinder-cone type distillation kettle (103), a cylinder-cone type filter, washer, and dryer three-in-one filter (201), a first liquid raw material tank (301), a solid raw material feeder (302), a second liquid raw material tank (303), a first liquid raw material recovery tank (304), a second liquid raw material recovery tank (305), and a distillation kettle heat exchanger (501), characterized in that: The reactor (101), pyrolysis purifier (102), cylinder-cone distillation kettle (103), cylinder-cone filtration, washing, and drying three-in-one filter (201), first liquid raw material tank (301), solid raw material feeder (302), second liquid raw material tank (303), first liquid raw material recovery tank (304), second liquid raw material recovery tank (305), and distillation kettle heat exchanger (501) are connected by pipelines. A first stirring motor (401) is provided on the first liquid raw material tank (301), a second stirring motor (402) is provided on the reactor (101), a third stirring motor (403) is provided on the cylinder-cone filtration, washing, and drying three-in-one filter (201), a fourth stirring motor (404) is provided on the cylinder-cone distillation kettle (103), and a fifth stirring motor (405) is provided on the second liquid raw material tank (303).

2. The ALD solid precursor production device according to claim 1, characterized in that: The first liquid raw material tank (301) is connected to the reactor (101) through a fourth valve (64), a seventh valve (67), and a pipeline.

3. The ALD solid precursor production device according to claim 1, wherein: The pyrolysis purifier (102) is connected to the reactor (101) through an eighth valve (68) and a pipeline.

4. The ALD solid precursor production device according to claim 1, characterized in that: The solid raw material feeder (302) is connected to the reactor (101) through a ninth valve (69) and a pipeline.

5. The ALD solid precursor production device according to claim 1, characterized in that: The reactor (101) is connected to the cylinder-cone filtration, washing, and drying three-in-one filter (201) through an eleventh valve (611), a thirteenth valve (613), and a pipeline.

6. The ALD solid precursor production device according to claim 5, characterized in that: The cylinder-cone filtration, washing, and drying three-in-one filter (201) is connected to the cylinder-cone distillation kettle (103) and the reactor (101) through a fifteenth valve (615), a first pipeline sight glass (616), a seventeenth valve (617), an eighteenth valve (618), and a tenth valve (610) respectively.

7. An ALD solid precursor production device according to claim 1, characterized in that: The cylinder-cone distillation kettle (103) is connected to the first liquid raw material recovery tank (304) and the second liquid raw material recovery tank (305) through a nineteenth valve (619), a distillation kettle heat exchanger (501), a thirty-first valve (631), a thirty-second valve (632), a second pipeline sight glass (633), and a pipeline respectively.

8. The ALD solid precursor production device according to claim 1, characterized in that: The second liquid raw material tank (303) is connected to the cylinder-cone distillation kettle (103) through a twentieth valve (620) and a twenty-fifth valve (625).

9. An ALD solid precursor production device according to claim 1, characterized in that: The first liquid raw material recovery tank (304) is connected to the first liquid raw material tank (301) through a thirtieth valve (630), a first valve (61), and a pipeline.

10. The ALD solid precursor production device according to claim 1, characterized in that: The second liquid raw material recovery tank (305) is connected to the second liquid raw material tank (303) through a twenty-ninth valve (629) and a twenty-sixth valve (626).

11. The ALD solid precursor production device according to claim 1, characterized in that: The cylinder-conical distillation kettle (103) is connected to the reaction kettle (101) and the cylinder-conical filtration, washing and drying three-in-one filter (201) respectively through the twenty-first valve (621), the twenty-second valve (622), the twenty-third valve (623), the sixth valve (66), the twenty-fourth valve (624), the twelfth valve (612) and pipelines.

12. The ALD solid precursor production device according to claim 11, characterized in that: The cylinder-conical distillation kettle (103) is connected to the twenty-first valve (621), the thirty-fifth valve (635), pipelines and the spiral ribbon agitator inside the cylinder-conical distillation kettle (103).

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