CN109553089A - Multi-purpose material heat treatment apparatus - Google Patents
Multi-purpose material heat treatment apparatus Download PDFInfo
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- CN109553089A CN109553089A CN201811636010.9A CN201811636010A CN109553089A CN 109553089 A CN109553089 A CN 109553089A CN 201811636010 A CN201811636010 A CN 201811636010A CN 109553089 A CN109553089 A CN 109553089A
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- temperature resistant
- heat treatment
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- 239000000463 material Substances 0.000 title claims abstract description 27
- 238000010438 heat treatment Methods 0.000 title claims abstract description 18
- 238000005086 pumping Methods 0.000 claims abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 18
- 239000010453 quartz Substances 0.000 claims description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 17
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 14
- 238000000746 purification Methods 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- 229910052763 palladium Inorganic materials 0.000 claims description 7
- 229910000881 Cu alloy Inorganic materials 0.000 claims description 5
- SBYXRAKIOMOBFF-UHFFFAOYSA-N copper tungsten Chemical compound [Cu].[W] SBYXRAKIOMOBFF-UHFFFAOYSA-N 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- 238000012544 monitoring process Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims 1
- 239000003575 carbonaceous material Substances 0.000 abstract description 16
- 229910021392 nanocarbon Inorganic materials 0.000 abstract description 14
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000003913 materials processing Methods 0.000 abstract 1
- 239000002041 carbon nanotube Substances 0.000 description 14
- 229910021393 carbon nanotube Inorganic materials 0.000 description 14
- 239000007789 gas Substances 0.000 description 11
- 238000000034 method Methods 0.000 description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- KTWOOEGAPBSYNW-UHFFFAOYSA-N ferrocene Chemical compound [Fe+2].C=1C=C[CH-]C=1.C=1C=C[CH-]C=1 KTWOOEGAPBSYNW-UHFFFAOYSA-N 0.000 description 6
- 229910052786 argon Inorganic materials 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 239000002048 multi walled nanotube Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- HUKGIVMVTNTTRT-UHFFFAOYSA-J silicon(4+) tetraiodate Chemical compound I(=O)(=O)[O-].[Si+4].I(=O)(=O)[O-].I(=O)(=O)[O-].I(=O)(=O)[O-] HUKGIVMVTNTTRT-UHFFFAOYSA-J 0.000 description 3
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 238000005485 electric heating Methods 0.000 description 2
- 229910052740 iodine Inorganic materials 0.000 description 2
- 239000011630 iodine Substances 0.000 description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000003252 repetitive effect Effects 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- DTGKSKDOIYIVQL-WEDXCCLWSA-N (+)-borneol Chemical compound C1C[C@@]2(C)[C@@H](O)C[C@@H]1C2(C)C DTGKSKDOIYIVQL-WEDXCCLWSA-N 0.000 description 1
- REPVLJRCJUVQFA-UHFFFAOYSA-N (-)-isopinocampheol Natural products C1C(O)C(C)C2C(C)(C)C1C2 REPVLJRCJUVQFA-UHFFFAOYSA-N 0.000 description 1
- DSSYKIVIOFKYAU-XCBNKYQSSA-N (R)-camphor Chemical compound C1C[C@@]2(C)C(=O)C[C@@H]1C2(C)C DSSYKIVIOFKYAU-XCBNKYQSSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 241000723346 Cinnamomum camphora Species 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- CKDOCTFBFTVPSN-UHFFFAOYSA-N borneol Natural products C1CC2(C)C(C)CC1C2(C)C CKDOCTFBFTVPSN-UHFFFAOYSA-N 0.000 description 1
- 229940116229 borneol Drugs 0.000 description 1
- 229930008380 camphor Natural products 0.000 description 1
- 229960000846 camphor Drugs 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 230000005492 condensed matter physics Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000000112 cooling gas Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- DTGKSKDOIYIVQL-UHFFFAOYSA-N dl-isoborneol Natural products C1CC2(C)C(O)CC1C2(C)C DTGKSKDOIYIVQL-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000005543 nano-size silicon particle Substances 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/168—After-treatment
- C01B32/17—Purification
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/168—After-treatment
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F17/00—Metallocenes
- C07F17/02—Metallocenes of metals of Groups 8, 9 or 10 of the Periodic System
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/20—Nanotubes characterized by their properties
- C01B2202/30—Purity
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
A kind of multi-purpose material heat treatment apparatus in materials processing technology field, comprising: inorganic non-metallic high-temperature resistant container, for placing the conductive exothermal element for containing material to be processed;Container is equipped with air inlet and air outlet;The pulse power, power supply positive and negative electrode are connected separately with a high temperature resistant electrode;Two high temperature resistant electrodes connect conduction with conductive exothermal element;Vacuum evacuation device is connected, to container vacuum-pumping with the gas outlet of inorganic non-metallic high-temperature resistant container.The present invention is widely used, can complete fast purifying and the plated film of nano-carbon material in the same apparatus, be conducive to the industrialized production of nano-carbon material and its derived product.
Description
Technical field
The present invention relates to a kind of technology of field of material processing, specifically a kind of multi-purpose material heat treatment is set
It is standby.
Background technique
There is unique structure and special physico by the novel nano carbon material of representative of nanotube and nano particle
Property is learned, before showing wide application in fields such as Condensed Matter Physics, material science, chemistry and nanoelectronic components
Scape.
Industrial production nano-carbon material mainly uses arc process and Floating catalyst method at present, these methods, which facilitate, to be received
The acquisition of rice carbon material is provided convenience for the research and practical application of nano-carbon material.However receiving of preparing of the above method
Rice carbon material is frequently accompanied by a considerable amount of impurity, and the presence of these impurity greatly hinders the physical property research of nano-carbon material
And practical application, therefore more and more attention have been obtained to the purifying research of nano-carbon material.The technical pure of nano-carbon material
Change processing method and mainly uses traditional physics, chemical purification methods, such as extraction, thermal decomposition method, oxidation-reduction method, however this
The purification efficiency of a little conventional methods is low, and purification quality is not also high;The wherein equipment relative maturity that thermal decomposition method uses, but still
There are operating difficulties, the defects of heating time is long, and security risk is big.
Summary of the invention
The present invention In view of the above shortcomings of the prior art, proposes a kind of multi-purpose material heat treatment apparatus, uses
Way extensively, fast purifying and the plated film of nano-carbon material can be completed in the same apparatus, be conducive to nano-carbon material and its
The industrialized production of derived product, and can be realized the purification of 500 DEG C or less volatizable materials.
The present invention is achieved by the following technical solutions:
The present invention includes:
Inorganic non-metallic high-temperature resistant container, for placing the conductive exothermal element for containing material to be processed;Container be equipped with into
Port and gas outlet;
The pulse power, power supply positive and negative electrode are connected separately with a high temperature resistant electrode;Two high temperature resistant electrodes and conductive exothermal element
Connection is conductive;
Vacuum evacuation device is connected, to container vacuum-pumping with the gas outlet of inorganic non-metallic high-temperature resistant container.
The conductive exothermal element containing material to be processed is obtained through compacting.
Preferably, the inorganic non-metallic high-temperature resistant container is made of quartz.
The high temperature resistant electrode needs can choose different types of conductive electrode according to processing, for example, graphite electrode, gold
Belong to palladium electrode, tungsten-copper alloy electrode.
The inorganic non-metallic high-temperature resistant container is equipped with temperature-measuring port, and the temperature-measuring port is equipped with non-contact temperature measuring device, uses
In the temperature of monitoring conductive exothermal element;Preferably, the non-contact temperature measuring device uses optics temperature measurer.
The gas outlet of the inorganic non-metallic high-temperature resistant container is connected with cryotrap, the cooling gas object collected after purification
Material.
Technical effect
Compared with prior art, the configuration of the present invention is simple, it is widely used;Based on the good heating conduction of nano-carbon material,
Efficient self-heating (the Q=I of nano-carbon material can be realized using pulse current2Rt), the purifying of nano-carbon material is rapidly completed,
And can after coating material is added Quick-gasifying coating material, thus nano-carbon material surface carry out plated film processing;And
The present invention can also purify the chemical substance of 500 DEG C or less gasifiable (evaporation or distillations) after increasing cryotrap,
Such as ferrocene, elemental iodine, sulphur, camphor, borneol, material purity is not less than 99.8% after purification.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of embodiment 1 and embodiment 2;
Fig. 2 is the structural schematic diagram of embodiment 3;
Fig. 3 is the SEM photograph of crystal whisker-shaped multi-walled carbon nanotube in the embodiment of the present invention;
In figure: quartz container 1, conductive exothermal element 2, the pulse power 3, high temperature resistant electrode 4, vacuum evacuation device 5, optics are surveyed
Warm instrument 6, cryotrap 7.
Specific embodiment
With reference to the accompanying drawing and specific embodiment the present invention will be described in detail.
Embodiment 1
As shown in Figure 1, the present embodiment is related to a kind of purifier apparatus of carbon nanotube, comprising:
Quartz container 1, for placing the conductive exothermal element 2 for containing material to be processed;Quartz container 1 be equipped with air inlet and
Gas outlet;
The pulse power 3, power supply positive and negative electrode are connected separately with a high temperature resistant electrode 4, and high temperature resistant electrode 4 is using Metal Palladium electricity
Pole;Two metal palladium electrodes are arranged in quartz container 1;
Vacuum evacuation device 5 is connected with the gas outlet of quartz container 1, vacuumizes to quartz container 1.
The quartz container 1 is equipped with temperature-measuring port, and the temperature-measuring port is equipped with optics temperature measurer 6, for monitoring conductive exothermal member
The temperature of part 2.
The present embodiment is used for the purifying of carbon nanotube, specific operation process to be as follows:
S1, conductive exothermal element is made in the compacting of 500g carbon nanotube;Carbon nanotube selects the first element of Suzhou nanometer skill
Long 5-10 μm of art Co., Ltd, diameter 50-90nm, purity 90% crystal whisker-shaped multi-walled carbon nanotube, as shown in Figure 3;
S2, conductive exothermal element is placed in quartz container 1, is connect with two metal palladium electrodes;
S3, vacuumize, logical argon gas, repetitive operation 3 times, thoroughly exclude air;It vacuumizes again, makes the vacuum degree of quartz container
It is maintained at 9.0 × 10-8mbar;
S4, using pulse Electric heating, it is passed through electric current 1A, current impulse generates joule by metal palladium electrode in 1s
Thermal shock, the temperature of carbon nanotube are sharply increased to 500 DEG C, are passed through chlorine at this time, by the iron simple substance and oxygen of carbon nano tube surface
Change iron and is oxidized to ferric trichloride, ferric trichloride (315 DEG C of boiling point) gasification discharge;
S5, then lead to nitrogen and foreign gas is discharged, metals content impurity, which is obtained, less than 20ppm, purity is greater than 99.9%
High-purity carbon nanotube.
Embodiment 2
The present embodiment and embodiment 1 use identical device, carry out plated film to carbon nanotube;The only material of high temperature resistant electrode
It is varied, for the present embodiment using graphite electrode as high temperature resistant electrode, concrete operations are as follows:
S1, crystal whisker-shaped multi-walled carbon nanotube (the first element of Suzhou is weighed respectively in the ratio of carbon silicon mol ratio 1:0.5-2.0
Nanosolutions GmbH, 5-10 μm long, diameter 50-90nm, purity 99%) it is uniformly mixed and is compacted with iodate silicon, it is made and leads
Electrical heating element;
S2, conductive exothermal element is placed in quartz container, is connect with two graphite electrodes, then is successively vacuumized, logical argon
Gas, repetitive operation 3 times excludes air to thorough, then vacuumizes, and the vacuum degree of quartz container 1 is made to be maintained at 9.0 × 10-8mbar;
S3, it is passed through pulse current, size of current 1A, the current impulse time is 2s, and heating carbon nanotube and iodate silicon are mixed
Object is closed to 1100 DEG C, the pyrolysis of iodate silicon forms silicon nanocrystal in carbon nano tube surface, and generates iodine vapor;
S4, there is the carbon nanotube of nano-silicon to be cooled within the scope of 110-200 DEG C coating surface, and logical argon gas purging excludes
Plating silicon-carbon nanotube is made in iodine vapor.
Embodiment 3
The present embodiment connects cryotrap 7 on the basis of embodiment 1, in the gas outlet of quartz container 1, while using tungsten
Copper alloy electrode replaces metal palladium electrode as high temperature resistant electrode, and for the purification of ferrocene, concrete operations are as follows:
S1, 310g ferrocene (Henan Jie Sen chemical products Co., Ltd, purity 90%) is received with 20g crystal whisker-shaped multi wall carbon
Mitron (Suzhou the first element Nanosolutions GmbH, 5-10 μm long, diameter 50-90nm, purity 99%) is uniformly mixed and presses
It is real, conductive exothermal element 2 is made;
S2, conductive exothermal element 2 is placed in quartz container 1, is connect with two tungsten-copper alloy electrodes 4;Then vacuumize,
Logical argon gas repeats this operation 3 times, thoroughly excludes air, then vacuumize, the vacuum degree of quartz container is made to be maintained at 9.0 × 10- 8mbar;
S3, using pulse electric heating mode, it is passed through electric current 1A, current impulse is generated in 0.2s by tungsten-copper alloy electrode
The temperature of joule thermal shock, carbon nanotube and ferrocene mixture is sharply increased to 120 DEG C, ferrocene distillation discharge, in low temperature
Condensation-crystallization in cold-trap obtains purity greater than 99.9% high-purity ferrocene, and impurity free iron is deposited in quartz container.
Carbon nanotube can Reusability in the present embodiment.
It is emphasized that: the above is only presently preferred embodiments of the present invention, not make in any form to the present invention
Limitation, any simple modification, equivalent change and modification to the above embodiments according to the technical essence of the invention,
All of which are still within the scope of the technical scheme of the invention.
Claims (7)
1. a kind of multi-purpose material heat treatment apparatus characterized by comprising
Inorganic non-metallic high-temperature resistant container, for placing the conductive exothermal element for containing material to be processed;Container is equipped with air inlet
The gas outlet and;
The pulse power, power supply positive and negative electrode are connected separately with a high temperature resistant electrode;Two high temperature resistant electrodes are connect with conductive exothermal element
It is conductive;
Vacuum evacuation device is connected, to container vacuum-pumping with the gas outlet of inorganic non-metallic high-temperature resistant container.
2. multi-purpose material heat treatment apparatus according to claim 1, characterized in that the leading containing material to be processed
Electrical heating element is obtained through compacting.
3. multi-purpose material heat treatment apparatus according to claim 1, characterized in that the inorganic non-metallic high temperature resistant is held
Device is equipped with temperature-measuring port, and the temperature-measuring port is equipped with non-contact temperature measuring device, for monitoring the temperature of conductive exothermal element.
4. multi-purpose material heat treatment apparatus according to claim 3, characterized in that the non-contact temperature measuring device is adopted
With optics temperature measurer.
5. multi-purpose material heat treatment apparatus according to claim 1, characterized in that the inorganic non-metallic high temperature resistant is held
The gas outlet of device is connected with cryotrap, the gas material after cooling purification.
6. multi-purpose material heat treatment apparatus according to claim 1, characterized in that the inorganic non-metallic high temperature resistant is held
Device is made of quartz.
7. multi-purpose material heat treatment apparatus according to claim 1, characterized in that the high temperature resistant electrode includes graphite
One of electrode, metal palladium electrode, tungsten-copper alloy electrode.
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Cited By (1)
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CN110228804A (en) * | 2019-07-19 | 2019-09-13 | 陕西延长石油(集团)有限责任公司 | A kind of carbon nanotube sulphur modification and purification integral method |
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CN113443617A (en) * | 2021-08-19 | 2021-09-28 | 陕西六元碳晶股份有限公司 | Continuous carbon nanotube purifying device and process |
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