CN217526802U - Purification and separation system for monosilane and disilane mixed gas - Google Patents
Purification and separation system for monosilane and disilane mixed gas Download PDFInfo
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- CN217526802U CN217526802U CN202220066064.1U CN202220066064U CN217526802U CN 217526802 U CN217526802 U CN 217526802U CN 202220066064 U CN202220066064 U CN 202220066064U CN 217526802 U CN217526802 U CN 217526802U
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Abstract
The utility model provides a purification piece-rate system of monosilane and disilane gas mixture utilizes this system can carry out effective separation and purification to the gas mixture that contains monosilane, disilane, hydrogen, ammonia etc. of silicon magnesium method small batch volume, intermittent production. The purification and separation system comprises a gas storage tank for storing the mixed gas, a filter tower, an ammonia adsorption tower, a condensing device, a silane collecting device and a vacuum pump; wherein the air inlet of the filter tower is connected with the air outlet of the air storage tank through a pipeline; the air inlet of the ammonia adsorption tower is connected with the air outlet of the filter tower through a pipeline; the air inlet of the condensing device is connected with the air outlet of the ammonia adsorption tower through a pipeline; the monosilane collecting device is connected with the condensing device through a pipeline; the vacuum pump is connected with the condensing device through a pipeline.
Description
Technical Field
The utility model relates to a purification and separation technique of monosilane gas mixture, in particular to purification piece-rate system of monosilane and disilane gas mixture.
Background
Monosilane is the most widely used silane electronic gas products in semiconductor integrated circuits, photovoltaics and optical fibers at present. Disilane plays an extremely important role in thin film transistor liquid crystal display and chip manufacturing, and in the production of crystalline silicon thin film solar cells. When used as a deposition source, disilane has the advantages of high deposition rate, low deposition temperature requirement and higher added value compared with monosilane having the same action.
In the traditional monosilane and disilane production and purification process, gas components are separated by adopting a rectification and condensation method, in intermittent production and experiments, the gas yield of a single batch reaction is small, so that the rectification stability is poor, the separation is not thorough, the separation effect is difficult to control, and meanwhile, the traditional condensation separation system is difficult to separate the gas to the sufficient purity.
SUMMERY OF THE UTILITY MODEL
In view of this, the utility model provides a purification piece-rate system of monosilane and disilane gas mixture utilizes this system can carry out effective separation and purification to the gas mixture that contains monosilane, disilane, hydrogen, ammonia etc. of silicon magnesium method small batch, intermittent type production.
The utility model discloses a reach its purpose, provide following technical scheme:
the utility model provides a purification and separation system for monosilane and disilane mixed gas, which comprises an air storage tank for storing the mixed gas, a filter tower, an ammonia adsorption tower, a condensing device, a monosilane collecting device and a vacuum pump; wherein,
the gas inlet of the filter tower is connected with the gas outlet of the gas storage tank through a pipeline and is used for filtering the mixed gas from the gas storage tank to remove solid particles;
the gas inlet of the ammonia adsorption tower is connected with the gas outlet of the filter tower through a pipeline and is used for removing ammonia from the mixed gas treated by the filter tower;
the gas inlet of the condensing device is connected with the gas outlet of the ammonia adsorption tower through a pipeline and is used for freezing the mixed gas treated by the ammonia adsorption tower and separating monosilane contained in the mixed gas;
the monosilane collecting device is connected with the condensing device through a pipeline and is used for collecting the monosilane separated by the condensing device;
the vacuum pump is connected with the condensing device through a pipeline and used for pumping out non-condensable gas generated in the condensing device.
Preferably, the condensing device comprises a primary condensing tower and a secondary condensing tower which are connected in series;
the one-level condensing tower is equipped with the first condensing coil who is used for circulating the liquid nitrogen, the second grade condensing tower is equipped with the second condensing coil who is used for circulating the liquid nitrogen, first condensing coil and first liquid nitrogen input pipeline are connected, the second condensing coil is connected with second liquid nitrogen input pipeline, first liquid nitrogen input pipeline with be equipped with liquid nitrogen flow control valve on the second liquid nitrogen input pipeline respectively.
Furthermore, the vacuum pump is connected with the gas outlets of the first-stage condensation tower and the second-stage condensation tower through pipelines.
Preferably, a pressure reducing valve is arranged on a pipeline connected between the ammonia adsorption tower and the filter tower and close to an air inlet of the ammonia adsorption tower.
Preferably, a flow regulating valve is arranged on a pipeline connected between the ammonia adsorption tower and the condensing device.
Preferably, the ammonia adsorption tower is provided with a refrigerant jacket for the circulation of a refrigerant.
Further, the monosilane collecting device comprises a cold trap and a gas cylinder arranged in an inner cavity of the cold trap, and an inlet of the gas cylinder is connected with a gas outlet of the secondary condensation tower through a pipeline.
Preferably, the filler filled in the filter tower is selected from a fiber material, a porous ceramic material or a metal sintered filter screen filler.
Preferably, the filler filled in the ammonia adsorption tower is selected from activated carbon, a 3A molecular sieve, a 4A molecular sieve, a 5A molecular sieve or a 13X molecular sieve.
The utility model provides a technical scheme has following beneficial effect:
the utility model provides a novel purification piece-rate system of monosilane and disilane gas mixture, based on this system, can make things convenient for the efficient to carry out the desorption to particulate matter, ammonia, hydrogen etc. noncondensable gas in monosilane and the disilane gas mixture, isolate monosilane and disilane simultaneously. The utility model discloses a purification piece-rate system specially adapted silicon magnesium method is small in batches, the mist that contains monosilane, disilane, hydrogen, ammonia etc. that intermittent production obtained carries out purification separation.
Drawings
FIG. 1 is a schematic diagram of a system for purifying and separating a monosilane and disilane mixed gas in one embodiment.
Detailed Description
In order to facilitate understanding of the present invention, the present invention will be described more fully with reference to the accompanying drawings. The preferred embodiments of the present invention are shown in the drawings. The invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is easily understood that according to the technical solutions of the present application, those skilled in the art can mutually replace various structural modes and implementation modes without changing the essential spirit of the present application. Therefore, the following detailed description and the accompanying drawings are merely illustrative of the technical solutions of the present application, and should not be construed as limiting or restricting the technical solutions of the present application in their entirety.
The terms of orientation of up, down, left, right, front, back, top, bottom, and the like referred to or may be referred to in this specification are defined relative to the configuration shown in the drawings, and are relative terms, and thus may be changed correspondingly according to the position and the use state of the device. Therefore, these and other directional terms should not be construed as limiting terms. Furthermore, the terms "first," "second," "third," and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
Referring to fig. 1, the utility model provides a purification piece-rate system of monosilane and disilane gas mixture, it mainly includes gas holder 1, filter tower 2, ammonia adsorption tower 3, condensing equipment 8, monosilane collection device 6 and vacuum pump 7.
The gas storage tank 1 is used for storing a monosilane and disilane mixed gas, specifically, the mixed gas can be monosilane mixed gas produced by a silicon-magnesium method in small batch and intermittent production, the mixed gas mainly contains monosilane and disilane, usually contains a small amount of hydrogen, ammonia and the like, and can also contain solid particles such as metal, nonmetal and the like.
The air inlet of the filter tower 2 is connected with the air outlet of the air storage tank 1 through a pipeline 14, and the filter tower 2 is filled with fillers, such as fiber materials (such as glass wool), porous ceramic materials or metal sintered filter screen fillers, and the fillers can adopt commercially available existing materials; the filter tower 2 receives the mixed gas from the gas storage tank 1 and is used for filtering the mixed gas from the gas storage tank 1 so as to remove solid particles entrained therein.
The gas inlet of the ammonia adsorption tower 3 is connected with the gas outlet of the filter tower 2 through a pipeline 15, and the ammonia adsorption tower 3 is filled with fillers such as activated carbon, a 3A molecular sieve, a 4A molecular sieve, a 5A molecular sieve or a 13X molecular sieve, and the fillers can adopt commercially available existing materials; the ammonia adsorption tower 3 receives the mixed gas which is output from the gas outlet of the filter tower 2 and is subjected to filtering treatment, and is used for carrying out ammonia adsorption and removal on the mixed gas which is treated by the filter tower 2. Preferably, a pressure reducing valve 11 is provided on a line 15 connecting the ammonia adsorption column 3 and the filtration column 2, adjacent to the gas inlet of the ammonia adsorption column 3, and the pressure reducing valve 11 is adjusted so that the ammonia adsorption column 3 can maintain a constant pressure, for example, a pressure of not less than 0.2MPa and not more than 0.6MPa, for example, a pressure of 0.2 MPa; furthermore, the ammonia adsorption tower 3 is provided with a cooling medium jacket (not shown) for the cooling medium to flow through, for example, cooling water, and the temperature can be conveniently controlled by the cooling medium jacket, for example, the temperature of the ammonia adsorption tower 3 is controlled between 5 ℃ and 10 ℃, for example, between 8 ℃ and 10 ℃. In a preferred embodiment, the ammonia adsorption column 3 can be operated at a constant temperature and a constant pressure by providing a pressure reducing valve 11 near the inlet of the ammonia adsorption column 3 and providing a refrigerant jacket in the ammonia adsorption column 3. Preferably, a flow rate regulating valve 12 is provided on a line 16 connecting between the ammonia adsorption tower 3 and the condensing device 8, and the flow rate regulating valve 12 is adjusted so that the mixture gas can pass through the ammonia adsorption tower 3 at a constant speed. The mixed gas passes through the constant-temperature and constant-pressure ammonia adsorption tower 3 at a constant speed, so that ammonia gas in the mixed gas is removed, efficient, thorough and stable ammonia removal is facilitated, and disilane loss is lower.
The air inlet of the condensing device 8 is connected with the air outlet of the ammonia adsorption tower 3 through a pipeline 16, and the condensing device 8 receives the mixed gas output from the air outlet of the ammonia adsorption tower 3 and is used for freezing the mixed gas after ammonia gas is removed by the ammonia adsorption tower 3 and separating monosilane contained in the mixed gas. In a preferred embodiment, the condensation device 8 comprises a primary condensation column 4 and a secondary condensation column 5 connected in series; the first-stage condensing tower 4 is provided with a first condensing coil (not shown in the figure), the second-stage condensing tower 5 is provided with a second condensing coil (not shown in the figure), and the first condensing coil and the second condensing coil are both used for circulating liquid nitrogen; the first condensing coil is connected with a first liquid nitrogen input pipeline (not shown in the figure), the second condensing coil is connected with a second liquid nitrogen input pipeline (not shown in the figure), and liquid nitrogen flow regulating valves (not shown in the figure) are respectively arranged on the first liquid nitrogen input pipeline and the second liquid nitrogen input pipeline; in the working process, the liquid nitrogen flow in the first condensation coil or the second condensation coil is adjusted by adjusting the liquid nitrogen flow adjusting valve, so that the temperature in the primary condensation tower 4 or the secondary condensation tower 5 can be adjusted and controlled; for example, when the mixed gas is subjected to freezing treatment, a liquid nitrogen flow regulating valve on a first liquid nitrogen input pipeline is regulated to keep the liquid nitrogen of a first condensing coil at a large flow rate, so that the temperature in the primary condensing tower 4 is kept at a temperature level (for example, about-190 ℃) capable of freezing monosilane and disilane in the mixed gas; when the monosilane is required to be separated from the frozen mixed gas, liquid nitrogen flow regulating valves on a first liquid nitrogen input pipeline and a second liquid nitrogen input pipeline are respectively regulated, so that the temperature of a primary condensation tower and a secondary condensation tower reaches the temperature capable of gasifying the monosilane but not gasifying the monosilane, for example, the temperature in the primary condensation tower 4 reaches about-130 ℃, and the temperature in the secondary condensation tower 5 reaches about-150 ℃, so that the monosilane frozen in the primary condensation tower 4 is gasified to form a monosilane gas flow, the monosilane is continuously kept in a frozen state, and the monosilane gas flows into the downstream secondary condensation tower 5; in the secondary condensation tower 5, a small amount of disilane carried in the monosilane gas flow is condensed again, so that monosilane and disilane are separated more thoroughly, and the high-purity monosilane gas flow is obtained. The first-stage condensing tower 4 and the second-stage condensing tower 5 are connected in series, the liquid nitrogen flow is adjusted through a liquid nitrogen flow adjusting valve, and double-stage separation in a constant temperature and constant pressure mode can be realized, so that the separation efficiency of monosilane and disilane is higher, the separation is more thorough, and the separation purity higher than that of liquefaction separation is realized. The obtained high-purity monosilane gas flow enters a monosilane collecting device 6 through a pipeline 17, specifically, the monosilane collecting device 6 comprises a cold trap 10 and a gas cylinder 9 arranged in an inner cavity of the cold trap 10, an inlet of the gas cylinder 9 is connected with a gas outlet of a secondary condensation tower 5 through the pipeline 17, and liquid nitrogen is contained in the cold trap 10.
Specifically, a flow rate control valve 12 is provided in a line 16 connecting the ammonia adsorption tower 3 and the first-stage condensation tower 4 of the condensation device 8.
The vacuum pump 7 is connected to the condensing means 8 through a line 18, and the vacuum pump 7 is used for pumping out the non-condensable gas generated in the condensing means 8. Specifically, the vacuum pump 7 is connected with the air outlet of the first-stage condensation tower 4 and the air outlet of the second-stage condensation tower 5 through pipelines, and a valve 13 is arranged on a pipeline 18; when the condensing device 8 freezes the mixed gas, the non-condensable gas such as hydrogen gas can be pumped out of the system by turning on the vacuum pump 7.
Based on the purification and separation system of the monosilane and disilane mixed gas provided by the utility model, the adsorption and removal of ammonia gas under constant temperature and constant pressure are easy to realize, the ammonia removal effect is good, and the disilane loss is low; meanwhile, through double-stage freezing separation, better separation purity than that of liquefaction separation can be realized, and more thorough single-batch separation can be realized for the monosilane gas mixture prepared by small-batch intermittent production.
For the convenience of understanding, the following is an exemplary illustration of the process of purifying and separating the mixture gas by using the system for purifying and separating the mixture gas of monosilane and disilane provided by the present invention:
introducing the monosilane-disilane mixed gas (or called monosilane mixed gas) containing the solid particles stored in the gas storage tank 1 into the filter tower 2 through a pipeline 14, and filtering to remove the solid particles in the filter tower 2; then the mixed gas further enters an ammonia adsorption tower 3 through a pipeline 15, and ammonia gas in the mixed gas is adsorbed and removed in the ammonia adsorption tower 3; then the mixed gas further enters a primary condensation tower 4 with the temperature of-190 ℃ through a pipeline 16, monosilane and disilane in the mixed gas in the primary condensation tower 4 are frozen, and non-condensable gas such as hydrogen is pumped out by starting a vacuum pump 7; and then liquid nitrogen flow regulating valves on the first liquid nitrogen input pipeline and the second liquid nitrogen input pipeline are regulated to ensure that the temperature of the primary condensation tower 4 reaches-130 ℃, the temperature of the secondary condensation tower 5 reaches-150 ℃, monosilane in the primary condensation tower 4 is gasified to form monosilane gas flow, the monosilane gas flow enters the secondary condensation tower 5, a small amount of disilane carried in the monosilane gas flow is continuously condensed to obtain high-purity monosilane gas flow, and the high-purity monosilane gas flow flows into a gas bottle 9 of the cold trap 10 through a pipeline 17.
The utility model discloses in the concrete device or the component that use, for example one-level condensing tower, second grade condensing tower, cold trap, filter tower and ammonia adsorption tower etc. all can adopt the device that can realize corresponding function that the field is current. Where not otherwise stated herein, it will be understood and appreciated by those skilled in the art that they may be readily available from the art to which it pertains and from the common general knowledge.
The following examples are provided to illustrate the application of the purification and separation system of the present invention. The purification and separation system used in the following examples is as shown in fig. 1, and the detailed structure and operation process thereof can be described with reference to the foregoing, and are not described in detail.
Example 1
In this case, the untreated monosilane mixed gas contains: solid particles, ammonia, hydrogen, monosilane, disilane, and the like.
(1) Solid particulate matter filtering of monosilane gas mixture
Filtering the monosilane gas mixture containing solid particles by a filter tower to reduce the concentration of the particles to 0.05mg/m 3 (ii) a The filler in the filter tower is glass wool.
(2) Ammonia removal of monosilane gas mixture
Passing the filtered monosilane gas mixture with ammonia content of 12% (volume) through an ammonia adsorption tower at a flow rate of 50L/min, the pressure of the ammonia adsorption tower being 0.2-0.3MPaA and the temperature being 5-10 deg.C; the ammonia gas content of the monosilane gas mixture flowing out of the air outlet of the ammonia adsorption tower is 16ppm; disilane loss 0.82%. The filler in the ammonia adsorption tower is a 3A molecular sieve.
(3) Dehydrogenation of mixed gas
The monosilane gas mixture treated by the ammonia adsorption tower passes through a primary condensing tower and a secondary condensing tower, the temperature of the primary condensing tower is-190 ℃ during freezing treatment, and the content of hydrogen in the monosilane gas mixture can be reduced to 100ppm by pumping out non-condensable gas such as hydrogen and the like through a vacuum pump during the freezing treatment. When the separation of monosilane is carried out after freezing, the temperature of the first-stage condensing tower and the temperature of the second-stage condensing tower are respectively controlled to be-130 ℃ and-150 ℃ by adjusting the liquid nitrogen flow regulating valve, and the purity of the monosilane obtained by separation reaches 99.994%. The purity of disilane was 99.3%. The separated monosilane was collected in the cylinder of the cold trap.
Example 2
In this case, the untreated monosilane mixed gas contains: solid particles, ammonia, hydrogen, monosilane, disilane, and the like.
(1) Solid particulate matter filtering of monosilane gas mixture
Filtering the monosilane gas mixture containing solid particles by a filter tower, wherein the concentration of the particles can be reduced to 0.06mg/m 3 (ii) a The filler in the filter tower is glass wool.
(2) Ammonia removal from monosilane gas mixture
Passing the filtered monosilane gas mixture with ammonia content of 13% (volume) through an ammonia adsorption tower at a flow rate of 50L/min, a pressure of 0.2-0.3MPaA and a temperature of 5-10 ℃; the content of the monosilane gas mixture ammonia flowing out of the outlet of the ammonia adsorption tower is 25ppm; disilane loss 0.85%. The filler in the ammonia adsorption tower is a 4A molecular sieve.
(3) Dehydrogenation of mixed gas
The monosilane gas mixture treated by the ammonia adsorption tower passes through a primary condensing tower and a secondary condensing tower, the temperature of the primary condensing tower is-190 ℃ during freezing treatment, and non-condensable gas such as hydrogen and the like is pumped out by a vacuum pump during the freezing treatment process, so that the hydrogen content in the monosilane can be reduced to 120ppm. When the separation of monosilane is carried out after freezing, the temperature of the first-stage condensing tower and the temperature of the second-stage condensing tower are respectively controlled to be-130 ℃ and-150 ℃ by adjusting the liquid nitrogen flow regulating valve, and the purity of the monosilane obtained by separation reaches 99.997 percent. The purity of disilane was 99.5%. The separated monosilane was collected in a gas cylinder of a cold trap.
Example 3
In this case, the untreated monosilane mixed gas contains: solid particles, ammonia, hydrogen, monosilane, disilane, and the like.
(1) Filtering solid particles in monosilane gas mixture
Filtering the monosilane gas mixture containing solid particles by a filter tower, wherein the concentration of the particles can be reduced to 0.04mg/m 3 The following; the filler in the filter tower is glass wool.
(2) Ammonia removal from monosilane gas mixture
Passing the filtered monosilane gas mixture with ammonia content of 10% (volume) through an ammonia adsorption tower at a flow rate of 50L/min, the pressure of the ammonia adsorption tower being 0.2-0.3MPaA and the temperature being 5-10 deg.C; the content of ammonia in the monosilane gas mixture flowing out of the outlet of the ammonia adsorption tower is 19ppm; disilane loss 0.75%. The filler in the ammonia adsorption tower is a 4A molecular sieve.
(3) Dehydrogenation of mixed gas
The monosilane gas mixture treated by the ammonia adsorption tower passes through a primary condensing tower and a secondary condensing tower, the temperature of the primary condensing tower is-190 ℃ during freezing treatment, and non-condensable gas such as hydrogen and the like is pumped out by a vacuum pump during the freezing treatment process, so that the hydrogen content in the monosilane can be reduced to 180ppm. When the separation of monosilane is carried out after freezing, the temperature of the first-stage condensing tower and the temperature of the second-stage condensing tower are respectively controlled to be minus 130 ℃ and minus 150 ℃ by adjusting a liquid nitrogen flow regulating valve, the purity of the monosilane obtained by separation reaches 99.991 percent, and the purity of the disilane is 99.1 percent. The separated monosilane was collected in the cylinder of the cold trap.
EXAMPLES 1-3 summary of the results after purification and isolation
What has been described above is merely the principles and preferred embodiments of the present application. It should be noted that, for those skilled in the art, the embodiments obtained by appropriately combining the technical solutions respectively disclosed in the different embodiments are also included in the technical scope of the present invention, and several other modifications may be made on the basis of the principle of the present invention, and should also be regarded as the protection scope of the present application.
Claims (9)
1. The system for purifying and separating the monosilane and disilane mixed gas is characterized by comprising a gas storage tank, a filter tower, an ammonia adsorption tower, a condensing device, a monosilane collecting device and a vacuum pump, wherein the gas storage tank is used for storing the mixed gas; wherein, the first and the second end of the pipe are connected with each other,
the gas inlet of the filter tower is connected with the gas outlet of the gas storage tank through a pipeline and is used for filtering the mixed gas from the gas storage tank to remove solid particles;
the gas inlet of the ammonia adsorption tower is connected with the gas outlet of the filter tower through a pipeline and is used for removing ammonia from the mixed gas treated by the filter tower;
the gas inlet of the condensing device is connected with the gas outlet of the ammonia adsorption tower through a pipeline and is used for freezing the mixed gas treated by the ammonia adsorption tower and separating monosilane contained in the mixed gas;
the monosilane collecting device is connected with the condensing device through a pipeline and is used for collecting the monosilane separated by the condensing device;
the vacuum pump is connected with the condensing device through a pipeline and used for pumping out non-condensable gas generated in the condensing device.
2. The system for purifying and separating the monosilane and disilane mixed gas according to claim 1, wherein the condensing device comprises a primary condensing tower and a secondary condensing tower which are connected in series;
the one-level condensing tower is equipped with the first condensing coil who is used for circulating the liquid nitrogen, the second grade condensing tower is equipped with the second condensing coil who is used for circulating the liquid nitrogen, first condensing coil and first liquid nitrogen input pipeline are connected, the second condensing coil is connected with second liquid nitrogen input pipeline, first liquid nitrogen input pipeline with be equipped with liquid nitrogen flow control valve on the second liquid nitrogen input pipeline respectively.
3. The system for purifying and separating the monosilane and disilane mixed gas according to claim 2, wherein the vacuum pump is connected with the gas outlets of the primary condensation tower and the secondary condensation tower through pipelines.
4. The system for purifying and separating the monosilane and disilane mixed gas according to claim 3, wherein a pressure reducing valve is arranged on a pipeline connected between the ammonia adsorption tower and the filter tower and adjacent to an air inlet of the ammonia adsorption tower.
5. The system for purifying and separating the monosilane and disilane mixed gas according to claim 4, wherein a flow control valve is arranged on a pipeline connected between the ammonia adsorption tower and the condensing device.
6. The system for purifying and separating a mixture of monosilane and disilane according to any one of claims 1 to 5, wherein the ammonia adsorption tower is provided with a cooling medium jacket through which a cooling medium flows.
7. The system for purifying and separating the mixed gas of the monosilane and the disilane as claimed in any one of claims 2 to 5, wherein the monosilane collecting device comprises a cold trap and a gas cylinder arranged in an inner cavity of the cold trap, and an inlet of the gas cylinder is connected with an outlet of the secondary condensation tower through a pipeline.
8. The system for purifying and separating the monosilane and disilane mixed gas according to any one of claims 1 to 5, wherein the filter tower is filled with a filler selected from a fibrous material, a porous ceramic material and a metal sintered screen filler.
9. The system for purifying and separating the mixed gas of monosilane and disilane according to any one of claims 1 to 5, wherein the ammonia adsorption tower is filled with a filler selected from activated carbon, a 3A molecular sieve, a 4A molecular sieve, a 5A molecular sieve and a 13X molecular sieve.
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