EP4392164A1 - Procédé et dispositif pour éliminer l'oxygène résiduel de gaz inertes par synthèse de nanoparticules métalliques - Google Patents
Procédé et dispositif pour éliminer l'oxygène résiduel de gaz inertes par synthèse de nanoparticules métalliquesInfo
- Publication number
- EP4392164A1 EP4392164A1 EP22768693.8A EP22768693A EP4392164A1 EP 4392164 A1 EP4392164 A1 EP 4392164A1 EP 22768693 A EP22768693 A EP 22768693A EP 4392164 A1 EP4392164 A1 EP 4392164A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- inert gas
- residual oxygen
- electrodes
- nanoparticles
- ppm
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 76
- 239000001301 oxygen Substances 0.000 title claims abstract description 76
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 76
- 239000011261 inert gas Substances 0.000 title claims abstract description 61
- 238000000034 method Methods 0.000 title claims description 30
- 239000002082 metal nanoparticle Substances 0.000 title description 5
- 230000002194 synthesizing effect Effects 0.000 title 1
- 239000007789 gas Substances 0.000 claims abstract description 47
- 239000002105 nanoparticle Substances 0.000 claims abstract description 43
- 229910052751 metal Inorganic materials 0.000 claims abstract description 26
- 239000002184 metal Substances 0.000 claims abstract description 26
- 230000001590 oxidative effect Effects 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims description 22
- 239000002245 particle Substances 0.000 claims description 17
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 14
- 239000000523 sample Substances 0.000 claims description 14
- 229910052782 aluminium Inorganic materials 0.000 claims description 10
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 10
- 229910052742 iron Inorganic materials 0.000 claims description 7
- 238000000926 separation method Methods 0.000 claims description 5
- 230000015572 biosynthetic process Effects 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 239000003990 capacitor Substances 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 4
- 229910052749 magnesium Inorganic materials 0.000 description 4
- 239000011777 magnesium Substances 0.000 description 4
- 150000002739 metals Chemical class 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 230000001419 dependent effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910052738 indium Inorganic materials 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- 239000011701 zinc Substances 0.000 description 3
- 229940123973 Oxygen scavenger Drugs 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- 239000011787 zinc oxide Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910000799 K alloy Inorganic materials 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 229910000573 alkali metal alloy Inorganic materials 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 229910003437 indium oxide Inorganic materials 0.000 description 1
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000000386 microscopy Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 229910052756 noble gas Inorganic materials 0.000 description 1
- 150000002835 noble gases Chemical class 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/32—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by electrical effects other than those provided for in group B01D61/00
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/10—Single element gases other than halogens
- B01D2257/104—Oxygen
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2259/00—Type of treatment
- B01D2259/80—Employing electric, magnetic, electromagnetic or wave energy, or particle radiation
- B01D2259/818—Employing electrical discharges or the generation of a plasma
Definitions
- the invention relates to a method and a device for removing residual oxygen from an inert gas.
- UHV ultra-high vacuum
- UHV systems are expensive to purchase and operate.
- the implementation of processes in UHV systems is time-consuming because the formation of an ultra-high vacuum requires a long pumping time that increases with falling residual pressure.
- materials with a low vapor pressure, for example cannot be processed in an ultra-high vacuum.
- Magnesium has an outstanding effect that can be used in particular for argon and other noble gases as inert gases. However, magnesium has no long-term stability under nitrogen due to nitride formation on electrode surfaces.
- metal is to be removed from the at least one electrode in a significantly more than stoichiometric amount in order to form a sufficient number of nanoparticles with a sufficiently large reactive surface area to remove the residual oxygen from the inert gas to the desired extent.
- 4 mol to 100 mol, preferably 8 mol to 40 mol, of the metal can be removed per 1 mol molecule of residual oxygen.
- metal in the order of 1 pg can be removed in order to form the nanoparticles from it.
- the oxidized nanoparticles are inert. Nevertheless, it is usually useful to filter the oxidized nanoparticles from the inert gas. This can easily be achieved with a series connection of particle filters with increasing degrees of separation.
- the series connection of two 99.5% particle filters and one 99.999% particle filter has proven itself to essentially completely remove the oxidized nanoparticles from the inert gas without the 99.999% particle filter having to be changed frequently because it becomes contaminated with the filtered nanoparticles added.
- the residual oxygen content can even be reduced to below 1 ⁇ 10′ 14 ppm. Concrete a residual oxygen content of 3.5 ⁇ 10′15 ppm was achieved when the process according to the invention was carried out twice.
- a filter device which is designed to filter the oxidized nanoparticles from the inert gas, is preferably arranged downstream of the reaction space.
- the filter device can have a series connection of particle filters with increasing degrees of separation, as has already been explained in connection with the method according to the invention.
- a Changing the particle filter is only seldom necessary during operation of the device according to the invention because the particle filters only clog very slowly if their degree of separation is designed appropriately due to the small absolute number of nanoparticles formed and correspondingly to be filtered off with the particle filters.
- the gas discharge 9 leads to a removal of metal from the electrodes 5 and 6, from which nanoparticles 12 form within the inert gas 8 in the reaction chamber 2.
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
Pour éliminer l'oxygène résiduel d'un gaz inerte (8), une tension est appliquée entre deux électrodes adjacentes au gaz inerte (8), cette tension provoquant une décharge gazeuse (9) directe dans le gaz inerte (8). Consécutivement à la décharge gazeuse (9), du métal est enlevé par au moins l'une des électrodes (5, 6). Le métal forme des nanoparticules (12) dans le gaz inerte (8) qui s'oxydent spontanément par consommation de l'oxygène résiduel.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE102021121928.0A DE102021121928A1 (de) | 2021-08-24 | 2021-08-24 | Verfahren und Vorrichtung zum Entfernen von Restsauerstoff aus Inertgasen mittels Synthese von Metallnanopartikeln |
PCT/EP2022/073308 WO2023025716A1 (fr) | 2021-08-24 | 2022-08-22 | Procédé et dispositif pour éliminer l'oxygène résiduel de gaz inertes par synthèse de nanoparticules métalliques |
Publications (1)
Publication Number | Publication Date |
---|---|
EP4392164A1 true EP4392164A1 (fr) | 2024-07-03 |
Family
ID=83280394
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP22768693.8A Pending EP4392164A1 (fr) | 2021-08-24 | 2022-08-22 | Procédé et dispositif pour éliminer l'oxygène résiduel de gaz inertes par synthèse de nanoparticules métalliques |
Country Status (3)
Country | Link |
---|---|
EP (1) | EP4392164A1 (fr) |
DE (1) | DE102021121928A1 (fr) |
WO (1) | WO2023025716A1 (fr) |
Family Cites Families (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5492678A (en) | 1993-07-23 | 1996-02-20 | Hokushin Industries, Inc. | Gas-cleaning equipment and its use |
CN111617714B (zh) * | 2020-05-27 | 2021-10-01 | 常州大学 | 一种催化反应装置及催化剂带电研究用仪器和使用方法 |
-
2021
- 2021-08-24 DE DE102021121928.0A patent/DE102021121928A1/de active Pending
-
2022
- 2022-08-22 WO PCT/EP2022/073308 patent/WO2023025716A1/fr active Application Filing
- 2022-08-22 EP EP22768693.8A patent/EP4392164A1/fr active Pending
Also Published As
Publication number | Publication date |
---|---|
WO2023025716A1 (fr) | 2023-03-02 |
DE102021121928A1 (de) | 2023-03-02 |
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Legal Events
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PUAI | Public reference made under article 153(3) epc to a published international application that has entered the european phase |
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17P | Request for examination filed |
Effective date: 20231213 |
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AK | Designated contracting states |
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