CN112808174A - Carbon tetrafluoride pyrolysis device and control method thereof - Google Patents
Carbon tetrafluoride pyrolysis device and control method thereof Download PDFInfo
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- CN112808174A CN112808174A CN202110165427.7A CN202110165427A CN112808174A CN 112808174 A CN112808174 A CN 112808174A CN 202110165427 A CN202110165427 A CN 202110165427A CN 112808174 A CN112808174 A CN 112808174A
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- 238000000197 pyrolysis Methods 0.000 title claims abstract description 123
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 238000000034 method Methods 0.000 title claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims description 44
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 28
- 229910052742 iron Inorganic materials 0.000 claims description 14
- 239000000428 dust Substances 0.000 claims description 9
- 238000004140 cleaning Methods 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 3
- 238000004804 winding Methods 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 15
- 238000013021 overheating Methods 0.000 abstract description 4
- 239000012535 impurity Substances 0.000 description 14
- 230000001590 oxidative effect Effects 0.000 description 10
- 230000006872 improvement Effects 0.000 description 9
- 238000001514 detection method Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- 235000015842 Hesperis Nutrition 0.000 description 1
- 235000012633 Iberis amara Nutrition 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- 239000010962 carbon steel Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005674 electromagnetic induction Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000005360 phosphosilicate glass Substances 0.000 description 1
- 238000001020 plasma etching Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002277 temperature effect Effects 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J6/00—Heat treatments such as Calcining; Fusing ; Pyrolysis
- B01J6/008—Pyrolysis reactions
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention provides a carbon tetrafluoride pyrolysis device and a control method thereof. The device and the method can make the temperature of the tower body of the pyrolysis tower uniform, avoid the condition that the pyrolysis effect is influenced due to local overheating or unavailable local temperature, and avoid the influence on the product quality due to the rupture of the pyrolysis tower.
Description
Technical Field
The invention relates to a carbon tetrafluoride pyrolysis device and a control method thereof, and belongs to the technical field of carbon tetrafluoride production.
Background
Carbon tetrafluoride (CF)4) Is that at presentThe plasma etching gas with the largest amount in the microelectronic industry is widely used for etching thin film materials such as silicon, silicon dioxide, silicon nitride, phosphosilicate glass, tungsten and the like, and also has a large number of applications in the aspects of cleaning the surfaces of electronic devices, producing solar batteries, laser technology, low-temperature refrigeration, gas insulation, leakage detection agents, controlling the attitudes of space rockets, detergents in printed circuit production, lubricants, brake fluids and the like. CF due to its extremely strong chemical stability4It can also be used in metal smelting and plastics industries.
At present, the production method of carbon tetrafluoride is mainly fluorocarbon synthesis. Because of the advantages of easily available raw materials, controllable process and the like, the method is widely adopted. In the process of preparing carbon tetrafluoride by the fluorocarbon synthesis method, some oxidizing impurities are generated, the existence of the oxidizing impurities affects the use effect of the carbon tetrafluoride, and therefore the oxidizing impurities must be removed. At present, the most commonly used method for removing the oxidative impurities in the carbon tetrafluoride product is to pyrolyze the oxidative impurities at high temperature, specifically: the high temperature effect is realized around the pyrolysis tower around the heating plate block, and in addition, only one temperature measurement is arranged on the pyrolysis tower, and the interlocking heating plate is used for heating.
However, the method easily causes local overheating of the pyrolysis tower, and the pyrolysis tower is cracked due to the fact that the temperature of the pyrolysis tower exceeds the carbon steel tolerance temperature, so that air enters a product system, and the product quality is affected; meanwhile, partial overheating causes pyrolysis transition of one part of gas and insufficient pyrolysis of the other part of gas, so that the pyrolysis effect is not ideal; in addition, because the pyrolysis tower needs to keep warm, need wrap the heat preservation of one deck in the pyrolysis tower periphery, so be difficult for discovering the crack under this service condition, influence follow-up production, reduced production efficiency.
Disclosure of Invention
The invention provides a carbon tetrafluoride pyrolysis device and a control method thereof, which can effectively solve the problems.
The invention is realized by the following steps:
the utility model provides a carbon tetrafluoride pyrolysis device, includes the pyrolysis tower, still includes high frequency heating device, high frequency heating device's coil winding is in the body of the tower periphery of pyrolysis tower, pack the iron ball in the pyrolysis tower.
As a further improvement, the coil of the high-frequency heating apparatus is divided into a plurality of heating sections.
As a further improvement, the number of heating sections is 4.
As a further improvement, a sieve plate is arranged at the bottom of the interior of the pyrolysis tower.
As a further improvement, the sieve plate is movably connected with the bottom of the interior of the pyrolysis tower.
As a further improvement, the pyrolysis tower is multiple and is arranged in series with each other.
A control method of a carbon tetrafluoride pyrolysis device is applied to the carbon tetrafluoride pyrolysis device, and the specific steps include:
s1, introducing the carbon tetrafluoride crude gas into a pyrolysis tower;
s2, setting a temperature threshold value of the high-frequency heating device, if the temperature of the coil is higher than the temperature threshold value, the high-frequency heating device is not started, and if the temperature of the coil is lower than the temperature threshold value, the high-frequency heating device starts heating;
and S3, heating for a period of time, discharging the pyrolyzed carbon tetrafluoride gas from the pyrolysis tower, and recovering the carbon tetrafluoride gas.
As a further refinement, the temperature threshold of a plurality of pyrolysis towers arranged in series is set to a gradient temperature.
As a further improvement, the temperature gradient is that the temperature of the first-stage pyrolysis tower is 265-270 ℃, the temperature of the second-stage pyrolysis tower is 275-280 ℃, the temperature of the third-stage pyrolysis tower is 280-285 ℃, the temperature of the fourth-stage pyrolysis tower is 285-290 ℃, and the temperature of the fifth-stage pyrolysis tower is 290-295 ℃.
As a further improvement, the method also comprises a step S4 of periodically cleaning the dust on the sieve plate.
The invention has the beneficial effects that:
according to the carbon tetrafluoride pyrolysis device, the coil of the high-frequency heating device is wound on the periphery of the tower body of the pyrolysis tower, so that the temperature of the tower body of the pyrolysis tower is uniform, the condition that the pyrolysis effect is influenced due to local overheating or unavailable local temperature is avoided, and the influence on the product quality due to the cracking of the pyrolysis tower is avoided.
The pyrolysis tower of the carbon tetrafluoride pyrolysis device is filled with the iron balls, and the iron balls can reach a set temperature value due to the adoption of a high-frequency heating mode, so that a better effect of pyrolyzing the oxidative impurities can be achieved through the iron balls, and meanwhile, the iron balls can also achieve a dust removal effect.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
Fig. 1 is a schematic structural diagram of a carbon tetrafluoride pyrolysis apparatus according to an embodiment of the present invention.
Reference numerals:
the device comprises a pyrolysis tower 1, a sieve plate 11, an air inlet 12, an air outlet 13 and a connecting port 14;
a high-frequency heating device 2 and a coil 21.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings of the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention. Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
In the description of the present invention, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implying any number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
Example 1
Referring to fig. 1, an embodiment of the present invention provides a carbon tetrafluoride pyrolysis apparatus, including a pyrolysis tower 1, and further including a high-frequency heating apparatus 2, where a coil 21 of the high-frequency heating apparatus 2 is uniformly wound around a periphery of a tower body 1 of the pyrolysis tower, the coil 21 is a metal coil, and an iron ball (not shown in the figure) is filled in the pyrolysis tower 1.
When using this carbon tetrafluoride pyrolysis device to carry out pyrolysis to carbon tetrafluoride thick other and get rid of oxidizing property impurity, open high frequency heating device 2 utilizes electromagnetic induction to produce eddy current in metal coil, causes metal coil's joule heating because of the resistance, and metal coil evenly twines in the periphery of pyrolysis tower 1, can be so that 1 body of the tower temperature of pyrolysis tower is even, can not appear local overheat or local temperature and can not reach and influence the condition of pyrolysis effect, avoids causing pyrolysis tower 1 to break and influences product quality. Meanwhile, the high-frequency heating mode is adopted, so that the iron ball can reach a set temperature value, a better effect of pyrolyzing the oxidative impurities can be achieved through the iron ball, and the dust removal effect can also be achieved through the iron ball.
The coil 21 of the high-frequency heating device 2 is divided into a plurality of heating sections, and each heating section is provided with a temperature measuring instrument, so that the whole pyrolysis tower 1 can be subjected to more accurate temperature control, and the heating is uniform. Preferably, the number of heating segments is 4.
The bottom of the inside of the pyrolysis tower 1 is provided with a sieve plate 11. The dust removed by the iron balls falls on the sieve plate 11, so that the dust is convenient to clean. Preferably, the sieve plate 11 is movably connected with the bottom of the inner part of the pyrolysis tower 1, such as by a flange. Therefore, the sieve plate 11 can be taken down and then cleaned of dust, and the operation is convenient.
The pyrolysis tower 1 is provided in plurality and in series with each other (not shown in the figure), and preferably 5. Each stage of the pyrolysis tower can be independently pyrolyzed. The temperature threshold of the high-frequency heating device 2 corresponding to the pyrolysis tower of different stages can be set in a gradient manner according to the analysis data of the discharged carbon tetrafluoride of the pyrolysis tower 1, so that the pyrolysis effect is further improved.
The bottom of the pyrolysis tower 1 is provided with an air inlet 12, and the top is provided with an air outlet 13 and a connecting port 14. The connection port 14 of the upper stage pyrolysis tower 1 is connected to the gas inlet 12 of the lower stage pyrolysis tower 1, so that a plurality of pyrolysis towers 1 are connected in series. The gas inlet 12 of each stage of the pyrolysis tower 1 is used for carbon tetrafluoride gas inlet, and the gas outlet 12 is used for carbon tetrafluoride gas outlet. Air is admitted from the bottom of pyrolysis tower 1 and is passed the iron ball, gives vent to anger from the top of pyrolysis tower again, and the iron ball can adsorb the dust like this, improves gaseous purification effect.
Example 2
The embodiment of the invention also provides a control method of the carbon tetrafluoride pyrolysis device, which is applied to the carbon tetrafluoride pyrolysis device in the embodiment 1, and comprises the following specific steps:
s1, introducing the carbon tetrafluoride raw gas into the pyrolysis tower 1 through the gas inlet 12.
S2, a temperature threshold value of the high-frequency heating device 2 is set, and if the temperature of the coil 21 is higher than the temperature threshold value, the high-frequency heating device 2 is not started, and if the temperature of the coil 21 is lower than the temperature threshold value, the high-frequency heating device 2 starts heating. Coil 21 even winding is in the periphery of pyrolysis tower 1 to divide into a plurality of heating sections, can carry out the even heating to the pyrolysis tower, local overheat or local temperature can not appear and can not reach and influence the condition of pyrolysis effect, avoid causing pyrolysis tower 1 to break and influence product quality.
And S3, heating for a period of time, discharging the pyrolyzed carbon tetrafluoride gas from a gas outlet 13 of the pyrolysis tower 1, and recovering the carbon tetrafluoride gas.
As a further refinement, the temperature threshold of a plurality of pyrolysis towers arranged in series is set to a gradient temperature.
As a further improvement, the temperature gradient is that the temperature of the first-stage pyrolysis tower is 265-270 ℃, the temperature of the second-stage pyrolysis tower is 275-280 ℃, the temperature of the third-stage pyrolysis tower is 280-285 ℃, the temperature of the fourth-stage pyrolysis tower is 285-290 ℃, and the temperature of the fifth-stage pyrolysis tower is 290-295 ℃. In this embodiment, preferably, the temperature gradient is that the temperature of the first-stage pyrolysis tower is 270 ℃, the temperature of the second-stage pyrolysis tower is 275 ℃, the temperature of the third-stage pyrolysis tower is 280 ℃, the temperature of the fourth-stage pyrolysis tower is 285 ℃, and the temperature of the fifth-stage pyrolysis tower is 290 ℃. The temperature gradient is very critical to the pyrolysis effect, and the pyrolysis effect can be greatly improved.
S4, the dust on the sieve plate 11 is cleaned periodically, and the sieve plate 11 can be removed for cleaning after the pyrolysis is stopped.
The flow velocity of the carbon tetrafluoride crude gas is 0.4-1.2m3and/S. This flow rate is critical if the flow rate is less than 0.4m3And S, the gas in the same batch stays in the pyrolysis tower for too long time, the pyrolysis is transited, and impurities in the carbon tetrafluoride can decompose more impurities, but the subsequent separation of the impurities is not facilitated. If the flow velocity is greater than 1.2m3S, the gas of the same batch stays in the pyrolysis tower for too short a time, pyrolysis is insufficient, and oxidative impurities are difficult to remove. In this embodiment, 0.8m is preferable3/S。
The gas obtained by pyrolyzing the crude carbon tetrafluoride gas by the method is further subjected to alkali washing or rectification to remove other impurities produced by pyrolyzing the oxidative impurities. And finally, measuring the content of the carbon tetrafluoride in the carbon tetrafluoride gas by adopting a gas chromatography.
Through detection, the content of carbon tetrafluoride in the carbon tetrafluoride gas is 99.9995%, which is far higher than the requirement of the electronic industry, and the pyrolysis effect of the device is very ideal.
Comparative example 1
There was no pyrolysis temperature gradient, and the pyrolysis temperature was 275 deg.C, and the other operations were the same as in example 2. Through detection, the content of carbon tetrafluoride in the carbon tetrafluoride gas is 95.98%.
Comparative example 2
The pyrolysis tower was not filled with iron balls, and the other operations were the same as in example 2. Through detection, the content of carbon tetrafluoride in the carbon tetrafluoride gas is 94.66%.
Comparative example 3
The flow velocity of the carbon tetrafluoride crude gas is 0.3m3(S), other operations were the same as in example 2. Through detection, the content of carbon tetrafluoride in the carbon tetrafluoride gas is 91.32%.
Comparative example 4
The flow rate of the carbon tetrafluoride crude gas is 1.5m3(S), other operations were the same as in example 2. Through detection, the content of carbon tetrafluoride in the carbon tetrafluoride gas is 89.56%.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The utility model provides a carbon tetrafluoride pyrolysis device, includes the pyrolysis tower, its characterized in that still includes high frequency heating device, high frequency heating device's coil winding is in the body of the tower periphery of pyrolysis tower, pack the iron ball in the pyrolysis tower.
2. The carbon tetrafluoride pyrolysis apparatus of claim 1, wherein the coil of the high-frequency heating apparatus is divided into a plurality of heating sections.
3. The carbon tetrafluoride pyrolysis apparatus according to claim 2, wherein the number of the heating sections is 4.
4. The carbon tetrafluoride pyrolysis apparatus of claim 1, wherein a screen plate is provided at a bottom of an inside of the pyrolysis tower.
5. The carbon tetrafluoride pyrolysis apparatus of claim 5, wherein the screen deck is movably connected to a bottom of an interior of the pyrolysis tower.
6. The carbon tetrafluoride pyrolysis apparatus of claim 1, wherein the pyrolysis tower is a plurality of towers arranged in parallel and in series with each other.
7. A control method of a carbon tetrafluoride pyrolysis apparatus, which is characterized by applying the carbon tetrafluoride pyrolysis apparatus according to any one of claims 1 to 6, and comprises the following specific steps:
s1, introducing the carbon tetrafluoride crude gas into a pyrolysis tower;
s2, setting a temperature threshold value of the high-frequency heating device, if the temperature of the coil is higher than the temperature threshold value, the high-frequency heating device is not started, and if the temperature of the coil is lower than the temperature threshold value, the high-frequency heating device starts heating;
and S3, heating for a period of time, discharging the pyrolyzed carbon tetrafluoride gas from the pyrolysis tower, and recovering the carbon tetrafluoride gas.
8. The method for controlling a carbon tetrafluoride pyrolysis apparatus according to claim 7, wherein the temperature threshold values of the plurality of pyrolysis towers arranged in series are set to a gradient temperature.
9. The method as claimed in claim 8, wherein the temperature gradient is that the temperature of the first-stage pyrolysis tower is 265-270 ℃, the temperature of the second-stage pyrolysis tower is 275-280 ℃, the temperature of the third-stage pyrolysis tower is 280-285 ℃, the temperature of the fourth-stage pyrolysis tower is 285-290 ℃, and the temperature of the fifth-stage pyrolysis tower is 290-295 ℃.
10. The method for controlling a carbon tetrafluoride pyrolysis apparatus according to claim 7, further comprising step S4 of periodically cleaning dust on the sieve plate.
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| US20050240067A1 (en) * | 2002-12-16 | 2005-10-27 | 3M Innovative Properties Company | Process for manufacturing fluoroolefins |
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2021
- 2021-02-06 CN CN202110165427.7A patent/CN112808174A/en active Pending
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| CN101462348A (en) * | 2008-10-27 | 2009-06-24 | 黄旭峰 | Electromagnetic heating system of injection mould machine |
| CN203408697U (en) * | 2013-06-09 | 2014-01-29 | 如皋市众昌化工有限公司 | Boron trifluoride oxidizing tower heating device |
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| CN207382618U (en) * | 2017-06-24 | 2018-05-18 | 衡水毅美新材料科技有限公司 | A kind of electromagnetism section heating type screw rod cracking apparatus |
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