CN103936009A - Device and method for producing nanoscale high-purity silicon powder by thermal decomposition of silane - Google Patents
Device and method for producing nanoscale high-purity silicon powder by thermal decomposition of silane Download PDFInfo
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Abstract
The invention discloses a device and a method for producing nanoscale high-purity silicon powder by thermal decomposition of silane. The device comprises a silane thermal decomposition system, a silicon powder filtering and collecting system and a tail gas recovery treatment system, wherein the silane thermal decomposition system comprises a reaction gas silane pipeline, a reaction gas hydrogen pipeline, a proportion buffer tank, a silane tubular reactor and a tail gas cooler; the silicon powder filtering and collecting system comprises a hydrogen blowback filter pipeline, a first-stage silicon powder filter, a second-stage silicon powder filter, a first-stage silicon powder collecting bin, a second-stage silicon powder collecting bin, a vacuum pump, a first-stage silicon powder outlet pipeline and a second-stage silicon powder outlet pipeline; the tail gas recovery treatment system comprises a tail gas deep freezer, a compressor, an adsorber, a gas-liquid separation tank, a gas-liquid separation tank liquid silane outlet pipeline and a gas-liquid separation tank hydrogen outlet pipeline. The device is applicable to production of industrial nanoscale high-purity silicon powder, the silicon powder of which the grain size is over 30nm can be effectively collected, all tail gas can be recycled, and the device has the advantages of being free of pollution discharge, less in investment, low in cost and the like.
Description
Technical field
The present invention relates to a kind of thermal decomposition of silane and produce the device and method of nano level high-purity silicon powder.
Background technology
Nano silica fume is a kind of brown color powder, of many uses.Can be used as charged lithium cells negative material, improve lithium battery capacity and charge and discharge cycles number of times, also can be used in fire-resistant coating and refractory materials, have huge potential application foreground in fields such as stupalith, matrix material, catalytic material, photoelectric material and biomaterials simultaneously.
Conventional nano silica fume production technique has electrostatic spray assistant chemical deposition (ES-CVD) at present, hot-wire chemical gas-phase deposition (HWCVD), induced with laser chemical vapour deposition (LICVD) etc., but these methods are high to equipment requirements, energy consumption is large, and is difficult to realize industrialization production.
Summary of the invention
The object of the invention is to overcome that existing nano level high-purity silicon powder production technique cost is high, the deficiency such as the large and industrialization of energy consumption, provide that a kind of equipment is simple, the thermal decomposition of silane of operational safety is produced the device and method of nano level high-purity silicon powder, can realize closed cycle produces continuously, cost is low, and production capacity is high.
The device that a kind of thermal decomposition of silane is produced nano level high-purity silicon powder comprises thermal decomposition of silane system, silica flour filters gathering system and tail gas recycle treatment system, and described silane decomposing system comprises reaction gas silane pipeline, reaction gas hydrogen gas lines, proportioning surge tank, silane tubular reactor, exhaust gas cooler, reaction gas silane pipeline, reaction gas hydrogen gas lines is connected with proportioning surge tank, proportioning surge tank, silane tubular reactor, exhaust gas cooler is connected in turn, and silica flour filters gathering system and comprises hydrogen power back-blowing filter pipeline, one-level silica flour strainer, secondary silica flour strainer, one-level silica flour collecting bin, secondary silica flour collecting bin, vacuum pump, one-level silica flour outlet line, secondary silica flour outlet line, hydrogen power back-blowing filter pipeline one end is connected with reaction gas hydrogen gas lines, the hydrogen power back-blowing filter pipeline the other end respectively with one-level silica flour strainer, secondary silica flour strainer is connected, exhaust gas cooler, one-level silica flour strainer, secondary silica flour strainer is connected in turn, one-level silica flour strainer, one-level silica flour collecting bin, one-level silica flour outlet line is connected in turn, secondary silica flour strainer, secondary silica flour collecting bin, secondary silica flour outlet line is connected in turn, one-level silica flour collecting bin, secondary silica flour collecting bin is connected with vacuum pump respectively, and tail gas recycle treatment system comprises tail gas cryogenic device, compressor, adsorption tower, knockout drum, the liquid silane outlet line of knockout drum, knockout drum hydrogen outlet pipeline, secondary silica flour strainer, tail gas cryogenic device, compressor, adsorption tower, knockout drum, the liquid silane outlet line of knockout drum is connected in turn, and knockout drum is connected with proportioning surge tank by knockout drum hydrogen outlet pipeline.
The method that nano level high-purity silicon powder is produced in described device thermolysis comprises the steps:
1) high purity silane and high-purity hydrogen enter proportioning surge tank and carry out mixing match, obtain gas mixture;
2) gas mixture enters silane tubular reactor, in silane tubular reactor, and silane thermal degradation granulate silica flour and hydrogen, the outlet of silane tubular reactor obtains gas powder gas mixture;
3) reacted gas powder gas mixture is after exhaust gas cooler is cooling, and temperature is down to below 100 DEG C, enters one-level silica flour strainer, and silica flour is leached, and is collected in one-level silica flour filter bottom;
4) be adsorbed on the high-purity hydrogen that the silica flour of filter membrane outside uses hydrogen power back-blowing filter pipeline to provide and carry out reverse blowing disposal;
5) when one-level silica flour strainer reaches after the silica flour of specified quantity, close one-level silica flour strainer, open secondary silica flour strainer, allow the cooled gas powder of exhaust gas cooler gas mixture enter secondary silica flour strainer and continue to produce;
6) displacement one-level silica flour strainer: with vacuum pump, one-level silica flour is collected to feed bin and vacuumize processing, be communicated with one-level silica flour strainer and one-level silica flour and collect feed bin, silica flour is put into one-level silica flour and collect feed bin,
7) when secondary silica flour strainer reaches after the silica flour of specified quantity, enable the one-level silica flour strainer after displacement, and secondary silica flour strainer is carried out to replacement operator, realize one-level silica flour strainer and secondary silica flour strainer and switch use, make reaction there is continuity; Described carries out replacement operator for secondary silica flour strainer is vacuumized to processing with vacuum pump to secondary silica flour strainer, is communicated with secondary silica flour strainer and secondary silica flour and collects feed bin, silica flour is put into secondary silica flour and collect feed bin;
8) tail gas after one-level silica flour strainer or the filtration of secondary silica flour strainer enters tail gas recycle treatment system, after, compressor compresses cooling through tail gas cryogenic device, adsorption tower absorption, at knockout drum by silane and Hydrogen Separation, separating obtained hydrogen fills into proportioning surge tank by knockout drum hydrogen outlet pipeline, and separating obtained silane is purified.
Described high purity silane and the purity of high-purity hydrogen are greater than 99.9999%.
In described gas mixture, the volumetric molar concentration of silane is 5% ~ 20%, and the pressure of gas mixture maintains 0.3Mpa, and the flow control that enters reactor after silane and hydrogen proportioning is at 80-100kg/h.
The thermal degradation temperature of described silane is controlled at 500 DEG C ~ 900 DEG C.Further the thermal degradation temperature of described silane is controlled at 500 DEG C ~ 600 DEG C.
Described silane tubular reactor is provided with one section of constant temperature hot-zone, can make Heating temperature constant in 0 ~ 1200 DEG C.
Described exhaust gas cooler uses circulating cooling water cooling, can make reacted gas powder mixture temperature be down to below 100 DEG C.
Described hydrogen power back-blowing filter pipeline gos deep into one-level silica flour strainer and secondary silica flour filter center, the silica flour of the outer absorption of reverse blow strainer.
Described tail gas recycle treatment system adopts cryogenic liquid refrigerated separation silane and hydrogen, and described cryogenic liquid is liquid nitrogen.
The present invention is applicable to the production of industrial nano grade high-purity silicon powder, and tail gas is all recycled, and non-pollution discharge has less investment, low cost and other advantages.
Brief description of the drawings
Fig. 1 is the structural representation that thermal decomposition of silane is produced nano level high-purity silicon powder device;
Fig. 2 is that temperature of reaction is at the SEM of the silica flour of 880 DEG C of productions photo;
Fig. 3 is that temperature of reaction is at the SEM of the silica flour of 500 DEG C of productions photo;
Fig. 4 is that temperature of reaction is at the SEM of the silica flour of 750 DEG C of productions photo;
Fig. 5 is that temperature of reaction is at the SEM of the silica flour of 600 DEG C of productions photo;
In figure, should gas silane pipeline 1, reaction gas hydrogen gas lines 2, proportioning surge tank 3, silane tubular reactor 4, exhaust gas cooler 5, hydrogen power back-blowing filter pipeline 6, one-level silica flour strainer 7, secondary silica flour strainer 8, one-level silica flour collecting bin 9, secondary silica flour collecting bin 10, vacuum pump 11, one-level silica flour outlet line 12, secondary silica flour outlet line 13, tail gas cryogenic device 14, compressor 15, adsorption tower 16, knockout drum 17, the liquid silane outlet line 18 of knockout drum, knockout drum hydrogen outlet pipeline 19.
Embodiment
As shown in Figure 1, a kind of device of thermal decomposition of silane production nano level high-purity silicon powder comprises thermal decomposition of silane system, silica flour filters gathering system and tail gas recycle treatment system, and described silane decomposing system comprises reaction gas silane pipeline 1, reaction gas hydrogen gas lines 2, proportioning surge tank 3, silane tubular reactor 4, exhaust gas cooler 5, reaction gas silane pipeline 1, reaction gas hydrogen gas lines 2 is connected with proportioning surge tank 3, proportioning surge tank 3, silane tubular reactor 4, exhaust gas cooler 5 is connected in turn, and silica flour filters gathering system and comprises hydrogen power back-blowing filter pipeline 6, one-level silica flour strainer 7, secondary silica flour strainer 8, one-level silica flour collecting bin 9, secondary silica flour collecting bin 10, vacuum pump 11, one-level silica flour outlet line 12, secondary silica flour outlet line 13, hydrogen power back-blowing filter pipeline 6 one end are connected with reaction gas hydrogen gas lines 2, hydrogen power back-blowing filter pipeline 6 the other ends respectively with one-level silica flour strainer 7, secondary silica flour strainer 8 is connected, exhaust gas cooler 5, one-level silica flour strainer 7, secondary silica flour strainer 8 is connected in turn, one-level silica flour strainer 7, one-level silica flour collecting bin 9, one-level silica flour outlet line 12 is connected in turn, secondary silica flour strainer 8, secondary silica flour collecting bin 10, secondary silica flour outlet line 13 is connected in turn, one-level silica flour collecting bin 9, secondary silica flour collecting bin 10 is connected with vacuum pump 11 respectively, and tail gas recycle treatment system comprises tail gas cryogenic device 14, compressor 15, adsorption tower 16, knockout drum 17, the liquid silane outlet line 18 of knockout drum, knockout drum hydrogen outlet pipeline 19, secondary silica flour strainer 8, tail gas cryogenic device 14, compressor 15, adsorption tower 16, knockout drum 17, the liquid silane outlet line 18 of knockout drum is connected in turn, and knockout drum 17 is connected with proportioning surge tank 3 by knockout drum hydrogen outlet pipeline 19.
Described silane tubular reactor 4 has one section of constant temperature hot-zone, can make Heating temperature constant between 0 ~ 1200 DEG C arbitrary temperature.
Described exhaust gas cooler 5 uses circulating cooling water cooling, can make reacted gas powder mixture temperature be down to below 100 DEG C.
Described hydrogen power back-blowing filter pipeline 6 gos deep into one-level silica flour strainer 7 and secondary silica flour strainer 8 centers, the silica flour of the outer absorption of reverse blow strainer.
Described tail gas recycle treatment system adopts cryogenic liquid refrigerated separation silane and hydrogen, and described cryogenic liquid is liquid nitrogen.
The silica flour storing in one-level silica flour collecting bin 9, secondary silica flour collecting bin 10 can be respectively by one-level silica flour outlet line 12,13 dischargings of secondary silica flour outlet line.
embodiment 1:
The high purity silane 500kg that is 6N purity evenly mixes with the ratio that the high-purity hydrogen of 6N is 20% according to volumetric molar concentration, and enter into 880 DEG C according to mixed total amount 100kg/h, pressure is the silane tubular reactor thermal degradation of 0.30Mpa, generate microgranular silica flour and unreacted tail gas through overcooling laggard enter to silica flour strainer, after filtering, tail gas enters tail gas recycle treatment system, through overcooling, compression, after absorption, by silane and Hydrogen Separation, separating obtained hydrogen fills into proportioning surge tank, separating obtained silane comes back to silane scavenging tower and purifies in order to re-using.The silica flour of producing, after one-level silica flour collecting bin and the collection of secondary silica flour collecting bin, obtains the silica flour 314kg of 150nm ~ 350nm, and a transformation efficiency of silane is 71.78%, and the SEM photo obtaining is as Fig. 2.
embodiment 2:
The high purity silane 500kg that is 6N purity evenly mixes with the ratio that the high-purity hydrogen of 6N is 5% according to volumetric molar concentration, and enter into 500 DEG C according to mixed total amount 80kg/h, pressure is the silane tubular reactor thermal degradation of 0.30Mpa, generate microgranular silica flour and unreacted tail gas through overcooling laggard enter to silica flour strainer, after filtering, tail gas enters tail gas recycle treatment system, through overcooling, compression, after absorption, by silane and Hydrogen Separation, separating obtained hydrogen fills into proportioning surge tank, separating obtained silane comes back to silane scavenging tower and purifies in order to re-using.The silica flour of producing, after one-level silica flour collecting bin and the collection of secondary silica flour collecting bin, obtains the silica flour 178kg of 30nm ~ 90nm, and a transformation efficiency of silane is 40.69%, and the SEM photo obtaining is as Fig. 3.
embodiment 3:
The high purity silane 500kg that is 6N purity evenly mixes with the ratio that the high-purity hydrogen of 6N is 15% according to volumetric molar concentration, and enter into 750 DEG C according to mixed total amount 80kg/h, pressure is the silane tubular reactor thermal degradation of 0.30Mpa, generate microgranular silica flour and unreacted tail gas through overcooling laggard enter to silica flour strainer, after filtering, tail gas enters tail gas recycle treatment system, through overcooling, compression, after absorption, by silane and Hydrogen Separation, separating obtained hydrogen fills into proportioning surge tank, separating obtained silane comes back to silane scavenging tower and purifies in order to re-using.The silica flour of producing, after one-level silica flour collecting bin and the collection of secondary silica flour collecting bin, obtains the silica flour 262kg of 50nm ~ 250nm, and a transformation efficiency of silane is 59.89%, and the SEM photo obtaining is as Fig. 4.
embodiment 4:
The high purity silane 500kg that is 6N purity evenly mixes with the ratio that the high-purity hydrogen of 6N is 10% according to volumetric molar concentration, and enter into 600 DEG C according to mixed total amount 90kg/h, pressure is the silane tubular reactor thermal degradation of 0.30Mpa, generate microgranular silica flour and unreacted tail gas through overcooling laggard enter to silica flour strainer, after filtering, tail gas enters tail gas recycle treatment system, through overcooling, compression, after absorption, by silane and Hydrogen Separation, separating obtained hydrogen fills into proportioning surge tank, separating obtained silane comes back to silane scavenging tower and purifies in order to re-using.The silica flour of producing, after one-level silica flour collecting bin and the collection of secondary silica flour collecting bin, obtains the silica flour 231kg of 30nm ~ 120nm, and a transformation efficiency of silane is 52.80%, and the SEM photo obtaining is as Fig. 5.
Claims (10)
1. thermal decomposition of silane is produced a device for nano level high-purity silicon powder, it is characterized in that, comprises thermal decomposition of silane system, silica flour filters gathering system and tail gas recycle treatment system, and described silane decomposing system comprises reaction gas silane pipeline (1), reaction gas hydrogen gas lines (2), proportioning surge tank (3), silane tubular reactor (4), exhaust gas cooler (5), reaction gas silane pipeline (1), reaction gas hydrogen gas lines (2) is connected with proportioning surge tank (3), proportioning surge tank (3), silane tubular reactor (4), exhaust gas cooler (5) is connected in turn, and silica flour filters gathering system and comprises hydrogen power back-blowing filter pipeline (6), one-level silica flour strainer (7), secondary silica flour strainer (8), one-level silica flour collecting bin (9), secondary silica flour collecting bin (10), vacuum pump (11), one-level silica flour outlet line (12), secondary silica flour outlet line (13), hydrogen power back-blowing filter pipeline (6) one end is connected with reaction gas hydrogen gas lines (2), hydrogen power back-blowing filter pipeline (6) the other end respectively with one-level silica flour strainer (7), secondary silica flour strainer (8) is connected, exhaust gas cooler (5), one-level silica flour strainer (7), secondary silica flour strainer (8) is connected in turn, one-level silica flour strainer (7), one-level silica flour collecting bin (9), one-level silica flour outlet line (12) is connected in turn, secondary silica flour strainer (8), secondary silica flour collecting bin (10), secondary silica flour outlet line (13) is connected in turn, one-level silica flour collecting bin (9), secondary silica flour collecting bin (10) is connected with vacuum pump (11) respectively, and tail gas recycle treatment system comprises tail gas cryogenic device (14), compressor (15), adsorption tower (16), knockout drum (17), the liquid silane outlet line of knockout drum (18), knockout drum hydrogen outlet pipeline (19), secondary silica flour strainer (8), tail gas cryogenic device (14), compressor (15), adsorption tower (16), knockout drum (17), the liquid silane outlet line of knockout drum (18) is connected in turn, and knockout drum (17) is connected with proportioning surge tank (3) by knockout drum hydrogen outlet pipeline (19).
2. a method for thermolysis production nano level high-purity silicon powder is installed in enforcement as claimed in claim 1, it is characterized in that comprising the steps:
1) high purity silane and high-purity hydrogen enter proportioning surge tank (3) and carry out mixing match, obtain gas mixture;
2) gas mixture enters silane tubular reactor (4), in silane tubular reactor (4), and silane thermal degradation granulate silica flour and hydrogen, the outlet of silane tubular reactor (4) obtains gas powder gas mixture;
3) reacted gas powder gas mixture is after exhaust gas cooler (5) is cooling, and temperature is down to below 100 DEG C, enters one-level silica flour strainer (7), and silica flour is leached, and is collected in one-level silica flour strainer (7) bottom;
4) silica flour that is adsorbed on filter membrane outside uses the high-purity hydrogen that provides of hydrogen power back-blowing filter pipeline (6) to carry out reverse blowing disposal;
5) when one-level silica flour strainer (7) reaches after the silica flour of specified quantity, close one-level silica flour strainer (7), open secondary silica flour strainer (8), allow the cooled gas powder of exhaust gas cooler (5) gas mixture enter secondary silica flour strainer (8) and continue to produce;
6) displacement one-level silica flour strainer (7): with vacuum pump (11), one-level silica flour is collected to feed bin (9) and vacuumize processing, be communicated with one-level silica flour strainer (7) and collect feed bin (9) with one-level silica flour, silica flour is put into one-level silica flour and collect feed bin (9);
7) when secondary silica flour strainer (8) reaches after the silica flour of specified quantity, enable the one-level silica flour strainer (7) after displacement, and secondary silica flour strainer (8) is carried out to replacement operator, realize one-level silica flour strainer (7) and secondary silica flour strainer (8) and switch use, make reaction there is continuity; Described carries out replacement operator for secondary silica flour strainer (8) is vacuumized to processing with vacuum pump (11) to secondary silica flour strainer (8), be communicated with secondary silica flour strainer (8) and collect feed bin (10) with secondary silica flour, silica flour is put into secondary silica flour and collect feed bin (10);
8) tail gas after one-level silica flour strainer (7) or secondary silica flour strainer (8) filtration enters tail gas recycle treatment system, after, compressor (15) cooling through tail gas cryogenic device (14) compression, adsorption tower (16) absorption, at knockout drum (17) by silane and Hydrogen Separation, separating obtained hydrogen fills into proportioning surge tank (3) by knockout drum hydrogen outlet pipeline (19), and separating obtained silane is purified.
3. produce the method for nano level high-purity silicon powder according to the thermal decomposition of silane described in right 2, it is characterized in that described high purity silane and the purity of high-purity hydrogen are greater than 99.9999%.
4. produce the method for nano level high-purity silicon powder according to the thermal decomposition of silane described in right 2, the volumetric molar concentration that it is characterized in that silane in described gas mixture is 5% ~ 20%, the pressure of gas mixture maintains 0.3Mpa, and the flow control that enters reactor after silane and hydrogen proportioning is at 80-100kg/h.
5. produce the method for nano level high-purity silicon powder according to the thermal decomposition of silane described in right 2, it is characterized in that the thermal degradation temperature of described silane is controlled at 500 DEG C ~ 900 DEG C.
6. produce the method for nano level high-purity silicon powder according to the thermal decomposition of silane described in right 2, it is characterized in that the thermal degradation temperature of described silane is controlled at 500 DEG C ~ 600 DEG C.
7. produce the method for nano level high-purity silicon powder according to the thermal decomposition of silane described in right 2, it is characterized in that described silane tubular reactor (4) is provided with one section of constant temperature hot-zone, can make Heating temperature constant in 0 ~ 1200 DEG C.
8. produce the method for nano level high-purity silicon powder according to the thermal decomposition of silane described in right 2, it is characterized in that described exhaust gas cooler (5) uses circulating cooling water cooling, can make reacted gas powder mixture temperature be down to below 100 DEG C.
9. produce the method for nano level high-purity silicon powder according to the thermal decomposition of silane described in right 2, it is characterized in that described hydrogen power back-blowing filter pipeline (6) gos deep into one-level silica flour strainer (7) and secondary silica flour strainer (8) center, the silica flour of the outer absorption of reverse blow strainer.
10. produce the method for nano level high-purity silicon powder according to the thermal decomposition of silane described in right 2, it is characterized in that described tail gas recycle treatment system adopts cryogenic liquid refrigerated separation silane and hydrogen, described cryogenic liquid is liquid nitrogen.
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| CN201410159327.3A CN103936009B (en) | 2014-04-21 | 2014-04-21 | A kind of thermal decomposition of silane produces the device and method of nano level high-purity silicon powder |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109607545A (en) * | 2019-01-02 | 2019-04-12 | 河南硅烷科技发展股份有限公司 | A kind of high purity silane CVD method continuously prepares the industrial method of nano silica fume |
| WO2023115762A1 (en) * | 2021-12-22 | 2023-06-29 | 中国有色桂林矿产地质研究院有限公司 | Method for preparing nano silicon powder by means of pyrolysis of silane with inductive plasma |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102046529A (en) * | 2008-03-31 | 2011-05-04 | 施米德硅晶片科技有限责任公司 | Method and system for the production of pure silicon |
| WO2013025707A1 (en) * | 2011-08-15 | 2013-02-21 | Dow Corning Corporation | Electrode composition comprising a silicon powder and method of controlling the crystallinity of a silicon powder |
| CN203794640U (en) * | 2014-04-21 | 2014-08-27 | 浙江中宁硅业有限公司 | Device for producing nanoscale high-purity silicon powder through silane thermal decomposition |
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2014
- 2014-04-21 CN CN201410159327.3A patent/CN103936009B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102046529A (en) * | 2008-03-31 | 2011-05-04 | 施米德硅晶片科技有限责任公司 | Method and system for the production of pure silicon |
| WO2013025707A1 (en) * | 2011-08-15 | 2013-02-21 | Dow Corning Corporation | Electrode composition comprising a silicon powder and method of controlling the crystallinity of a silicon powder |
| CN203794640U (en) * | 2014-04-21 | 2014-08-27 | 浙江中宁硅业有限公司 | Device for producing nanoscale high-purity silicon powder through silane thermal decomposition |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109607545A (en) * | 2019-01-02 | 2019-04-12 | 河南硅烷科技发展股份有限公司 | A kind of high purity silane CVD method continuously prepares the industrial method of nano silica fume |
| WO2023115762A1 (en) * | 2021-12-22 | 2023-06-29 | 中国有色桂林矿产地质研究院有限公司 | Method for preparing nano silicon powder by means of pyrolysis of silane with inductive plasma |
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