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WO2012113877A1 - Procédé et dispositif de transport d'éléments métalliques en phase gazeuse - Google Patents

Procédé et dispositif de transport d'éléments métalliques en phase gazeuse Download PDF

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Publication number
WO2012113877A1
WO2012113877A1 PCT/EP2012/053090 EP2012053090W WO2012113877A1 WO 2012113877 A1 WO2012113877 A1 WO 2012113877A1 EP 2012053090 W EP2012053090 W EP 2012053090W WO 2012113877 A1 WO2012113877 A1 WO 2012113877A1
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WIPO (PCT)
Prior art keywords
metal elements
carrier gas
target
gas
synthesis chamber
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.)
Ceased
Application number
PCT/EP2012/053090
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German (de)
English (en)
Other versions
WO2012113877A8 (fr
Inventor
Christoph DÜLLMANN
Jan Dvorak
Matthias SCHÄDEL
Andreas TÜRLER
Julia EVEN
Jens Volker KRATZ
Lorenz NIEWISCH
Norbert WIEHL
Alexander Yakushev
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Scherrer Paul Institut
Johannes Gutenberg Universitaet Mainz
Technische Universitaet Muenchen
GSI Helmholtzzentrum fuer Schwerionenforschung GmbH
Original Assignee
Scherrer Paul Institut
Johannes Gutenberg Universitaet Mainz
Technische Universitaet Muenchen
GSI Helmholtzzentrum fuer Schwerionenforschung GmbH
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Scherrer Paul Institut, Johannes Gutenberg Universitaet Mainz, Technische Universitaet Muenchen, GSI Helmholtzzentrum fuer Schwerionenforschung GmbH filed Critical Scherrer Paul Institut
Priority to EP12708099.2A priority Critical patent/EP2678273A1/fr
Publication of WO2012113877A1 publication Critical patent/WO2012113877A1/fr
Publication of WO2012113877A8 publication Critical patent/WO2012113877A8/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G1/00—Methods of preparing compounds of metals not covered by subclasses C01B, C01C, C01D, or C01F, in general
    • C01G1/04—Carbonyls

Definitions

  • the invention relates to a method and a device for transporting metal elements in gaseous phase.
  • Transactinoids and other elements of the periodic table such as transition metals and elements of the d and p groups, it is usually not possible to use a macroscopic
  • Solid or liquid body to observe, but one observes the behavior of individual atoms and molecules under certain circumstances.
  • the target material is selected and exposed to the radiation, by nuclear reactions finally the desired elements arise.
  • thermal energy for example, thermal energy
  • Used neutrons and a neutron-induced Nuclear fission are caused, as for example on
  • Synchrotrons such as the heavy ion beam of the GSI, or a cyclotron are shot at a selected target.
  • Origin can be removed.
  • it may be of interest to refractory
  • Metal elements are generated, or at one
  • a cluster Gasj et is used, wherein an inert gas aerosol cluster of solid or liquid materials such as
  • Yield from the cluster gas et can be ensured. This may be due to the fact that during operation, the aerosol particles accumulate in some places in the system and thereby the system properties can be adversely affected. For another use would be a separation of the refractory elements from the clusters necessary. This is difficult, energy intensive and
  • fission zircon can be generated in the induced nuclear fission of uranium-235.
  • UF 3 is used as target material
  • the invention therefore has the task of providing a method which makes it possible
  • Metal elements can be used elsewhere.
  • the object of the invention is solved by the subject matters of the independent claims.
  • Advantageous developments of the invention are defined in the subclaims. According to the invention metal elements by means of the synthesis of metal element carbonyl complexes in a
  • the transport of the metal elements in the gaseous phase proves to be particularly advantageous.
  • this process does not require a phase transition to another, for example solid, phase for the transport, so that the metal elements are not complicated from the other phase into the gaseous phase for a first
  • Carbonyl formation ensures that the metal elements are essentially not attached to physical objects on the body
  • the carrier gas contains carbon monoxide.
  • the carrier gas is preferably combined with the metal elements in a reaction volume, wherein the
  • Metal element carbonyl complexes are Complex compounds of metal elements with
  • Carbon monoxide ligand The complex compounds have the general structure d m (C0) n . Under the term
  • Carbonyl complex will be referred to hereinafter as well
  • the metal elements are directly synthesized in the gaseous phase to metal element carbonyl complexes and are thereby stably transportable in the gaseous phase.
  • the metal element carbonyl complexes themselves are gaseous.
  • Molybdenum-104 preferably with six
  • a metal element ruthenium-108 may preferably react with five carbon monoxide molecules to form a trigonal bipyramidal Ru (CO) 5 carbonyl complex compound
  • a metal element can with charge number X with n carbon monoxide molecules
  • the synthesized metal element carbonyl complex may be in the form x dm (CO) ", where x is the mass number of the respective isotope, m is the number of the respective isotopes
  • Metal element atoms (d) in the metal element carbonyl complex and n represents the number of carbon monoxide ligands (CO) in the metal element carbonyl complex.
  • the number m of the respective metal element atoms and the number n of the carbon monoxide ligands may each be any natural number including "one".
  • a polynuclear metal element carbonyl complex is present.
  • metal elements which typically preferentially form polynuclear metal element carbonyl complexes are in particular
  • rhenium preferably 2 rhenium nuclei with 10 carbon monoxide molecules synthesize a 188 Re 2 (CO) 10, with two square-pyramidal 188 Re (CO) 5 sub-nuclei joined together via a metal-metal compound.
  • CO 188 Re 2
  • CO square-pyramidal 188 Re
  • Technetiums synthesize preferably 2 technetium nuclei and 10 carbon monoxide ligands to 99 ⁇ 2 (00) ⁇ , with a similar to the rhenium geometric design.
  • metal elements of the 6. and 8. Group of the Periodic Table preferably mononuclear Metal element carbonyl complexes, whereas metal elements of the 7th group have an odd number
  • Valence electrons preferably form polynuclear metal element carbonyl complexes.
  • the number of cores (metal elements) per metal element carbonyl complex which is preferred for a respective element usually results in compliance with the 18-electron rule for the respective metal element.
  • the synthesized metal element carbonyl complexes for example, do not adhere or only briefly adhere to surfaces, and therefore have a high volatility.
  • the metal element carbonyl complexes are suitable for transport and can also be used over greater distances, e.g. by
  • Synthesis of the metal element carbonyl complexes directly from molecular carbon monoxide gas and the metal elements can proceed successfully at moderate conditions without intermediate reaction.
  • the method can be carried out at a temperature in the interval between 50 and 600 K and at one pressure
  • the process can be carried out at a pressure in the interval between 0.005 to 20 bar and more preferably at a pressure in the interval between 0.1 to 10 bar.
  • the carbonyl complex synthesis can also take place in ordinary room conditions, ie at a Temperature of about 290 K ⁇ 10K and at one
  • the carrier gas can be next to the
  • Carbon monoxide contain a non-reactive and thus inert gas component.
  • the proportion of non-reactive gas may vary depending on the structure of a device used.
  • the inert gas may vary depending on the structure of a device used.
  • the non-reactive gas constituent serves for moderation of the metal elements to be transported in the reaction volume of the synthesis apparatus.
  • Metal element carbonyl complexes are increased. This allows the emitted from a target
  • Metal elements are moderated by the carrier gas particles.
  • the efficiency of moderation depends in particular on the mass ratio of the particles involved. In this case, by selecting the carrier gas particles, the proportion of carbon monoxide to the carrier gas, the
  • the carrier gas may also consist entirely or at least substantially of carbon monoxide.
  • thermalizing is meant that the energy of the metal elements of the kinetic energy of the
  • Carrier gas particles substantially corresponds. But it is also possible a high proportion of carbon monoxide with, for example, a minimum proportion of preferably 95%,
  • carbon monoxide Depending on the geometry chosen, the ion beam, the energy of the repulsive nuclei, and the nature of the other gases in the carrier gas, a lesser amount of carbon monoxide may be sufficient to form the complexes.
  • the proportion of carbon monoxide here can be well below 50%.
  • the carbon monoxide-containing carrier gas may be in addition to
  • Carbon monoxide also has another reactive
  • Metal elements, carbon monoxide and constituents of the further reactive gas may optionally be added
  • the further reactive gas component may preferably the
  • Moderation and / or the selectivity of the carbonyl complex synthesis can be influenced.
  • the reaction volume can be in the synthesis chamber
  • the synthesis chamber can allow a targeted gas flow of the carrier gas.
  • a supply line so for example a hose made of polyethylene or a pipe made of copper, can the gas into the synthesis chamber and that in it
  • Lead also a transport line to a
  • Outlet opening in particular a gas outlet of the
  • the carrier gas can flow out. With the carrier gas can
  • metal element carbonyl complexes leave the synthesis or reaction chamber and by means of a gas transport line connected to the reaction chamber to a location remote from the place of production of the metal elements
  • the metal elements in carbonyl complex form
  • Metal element carbonyl complexes have achieved yield.
  • gas transport line There are generally a variety of simple materials for use as a gas transport line conceivable.
  • simple plastics such as polyethylene (PE) or polytetrafluoroethylene (PTFE) can be used as a material for a gas transport line.
  • PE polyethylene
  • PTFE polytetrafluoroethylene
  • the choice of the material of the gas transport line can be dependent on the radiation resistance of the respective material, since it can be guided at least partially in a region in which a greatly increased
  • Radiation exposure may be present.
  • the generated elements in particular the radioactive
  • the length of the gas transport line may therefore preferably be just selected in such a way by a
  • Radiation shielding device for example, a sufficiently thick concrete wall to be able to be passed through.
  • the gas flow through the respective lines can be adjusted by various settings.
  • the delivery rate of the carrier gas may be the
  • Carrier gas components can be adjusted individually at each gas source.
  • a gas source for each component of the carrier gas may typically serve a compressed gas cylinder to which a pressure reducer may be connected. This can be an individual mass flow control guarantee.
  • the adjustment of the flow rate can be adapted to the structural geometry, such as the diameter or the length of the installed cables, on the one hand. On the other hand, the flow rate adjustment can also be adapted to the average life of the metal elements. This can be radioactive in terms of their
  • the flow rate can be set in a range between 1 ml / min and 10 1 / min in order to adjust the gas flow to these conditions.
  • an object called Target from a
  • Radiation source irradiated, thereby activated and in a reaction, in particular a nuclear reaction, the
  • a nuclear reaction can be, for example, a nuclear fission, a nuclear fusion process or a nuclear decay.
  • nuclear fission this can be induced in particular by neutrons.
  • the neutrons can be generated in a nuclear reactor.
  • thermal neutrons can preferably be used. These conditions may be, for example, on Research Reactor TRIGA Mainz at the Johannes Gutenberg University in Mainz.
  • the metal elements may be fused by using particle beams, in particular a
  • a particle accelerator is especially one
  • Linear accelerator a synchrotron or a cyclotron.
  • the particle or ion beams for example, in facilities such as the GSI Helmholtz Center for
  • Lead metal elements are known per se.
  • the target is thus with, for example, hadron-containing
  • hadrons themselves (e.g., neutrons) or hadrons-containing particles (e.g., ions).
  • hadrons themselves (e.g., neutrons) or hadrons-containing particles (e.g., ions).
  • photons it is also possible to use photons or
  • the material of the target is preferably selected according to which metal elements are to be produced.
  • a material for example, actinides, in particular the
  • fissile elements such as uranium, plutonium or Californium or objects containing these materials can be used.
  • the materials uranium, plutonium or Californium, and objects containing these materials can be used.
  • the materials uranium, plutonium, Californium, and objects containing these materials can be used.
  • molybdenum for example, molybdenum, technetium, rhenium, rhodium or
  • Object with high probability can adhere directly to this, so they can not be picked up and / or transported by a carrier gas.
  • the target can be lapped directly by the carrier gas, in order to avoid contact of the elements produced, in particular the refractory metal elements, for example, with the outer skin of the synthesis chamber, before this with the
  • Carbon monoxide molecules can be synthesized to metal element carbonyl complexes. This can be the
  • the range of the metal elements produced can be any metal elements produced.
  • Composition of the carrier gas can be influenced.
  • the conditions in particular gas type, gas mixture, temperature, pressure and / or size of the
  • Metal elements influenced such that at least 98% of the metal elements in the synthesis chamber by means of Carrier gases can be moderated to allow the highest possible yield for the subsequent transport of the metal elements. Preference is given to the production of metal elements which are for the most part short-lived, and those which are extremely short-lived, for example from the group of transactinoids.
  • Half-lives of the short-lived refractory metal elements are typically less than 10 minutes, those of the extremely short-lived in the range below 100 milliseconds.
  • the metal elements decay, they emit radioactive radiation.
  • This radioactive radiation of the radioactively decomposing metal elements can be measured by means of a radiation detector in a detection device. If the detector is connected downstream to the transport line connected to the synthesis chamber, the existence of the metal elements, in particular in the form of the metal element carbonyl complexes at the point of decomposition, can prove beyond doubt the transport location by means of the carrier gas.
  • the metal elements are preferably radioactive
  • applications for the metal element transport according to the invention can be found, for example, in tribology, in radiochemistry and in nuclear medicine.
  • the place of use may then be, for example, a room in which people can stay, for example a treatment or therapy room.
  • the metal elements can then be in the room or the therapy room of her
  • radioactive materials for example, in the field of nuclear medicine, for example in a scintigraphic examination, for example of the skeleton, lung, thyroid, kidneys, heart and tumors, it may be of considerable advantage to use as short-lived radioactive materials as so-called
  • Carbonyl complex formation are brought over the Gastransportiertung in the vicinity of the patient, the lowest possible radiation exposure of the patient can be achieved. It can therefore be used exactly to the purpose of the investigation tuned radioactive isotopes.
  • metal elements in particular refractory metal elements by means of the above-described
  • the metal elements to be transported are preferably elements from the Maugrup s, ie the d groups of
  • Periodic Table may also be metal elements from the range of the main groups of the periodic table, which can be transported in the gaseous phase by means of the described method. This can be, for example Indium, tallium or germanium. Furthermore, the elements of the actinides and lanthanides can be transported by the described method. Refractory metal elements from the d-groups of the Periodic Table may in particular be ruthenium, iridium, rhodium, osmium, rhenium, molybdenum, tungsten or technetium, in particular radioactively decomposing isotopes of these elements.
  • the method shown preferably operates selectively.
  • the selection of a particular metal element from a number of generated or existing metal elements is done depending on various process parameters. For example, by setting the
  • Delivery rate of the carrier gas can the selectivity of the
  • Transport process can be influenced. Furthermore, the particle number resulting from the probability of generation of the chosen target material can also have an influence on the selectivity of the metal element carbonyl complex synthesis. This can already prefer the emergence of a selected metal element with the right choice.
  • reaction volume For generating and providing metal elements in gaseous phase, a reaction volume is defined in which the metal elements with the carbon monoxide of the carrier gas to metal element carbonyl complexes
  • Metal element can be achieved a special stability. These interactions make electrons of the filled sigma orbital of carbon monoxide in
  • the structure of the synthesized metal-element carbonyl complex is predicted primarily by the VSEPR model and the 18-electron rule. Carbonyl complexes with several or even different metal elements are due to the density of the metal element particles in the
  • complex symmetry may be tetrahedral, trigonal-bipyramidal,
  • metal element particles in a metal element carbonyl complex may also have symmetry, for example
  • the 6th group preferably form hexacarbonyl complex compounds, those of the 8th group, due to the 18-electron rule
  • the molybdenum metal element of the 6th group forms, for example, a high probability of hexacarbonyl complex compound in the form of 104 Mo (CO). 6
  • 104 Mo carbon monoxide molecules synthesize with a 104 Mo to form a metal element-carbonyl complex in
  • the reaction volume can be accommodated in a device in a synthesis chamber, which also has a supply line for providing and initiating the
  • Radiation pollution may accompany the removal of the metal elements from the place of origin to a
  • the reaction volume is in particular always with
  • Flow can be generated with which the metal element carbonyl complexes can be carried.
  • the entire reaction volume can be continuously rinsed with the fresh incoming carrier gas in order to avoid stationary flow areas.
  • the production of the metal elements is done in particular by a target of fissile material, which is irradiated by a radiation source and activated.
  • the metal elements can therefore be directly in the process
  • Nuclear fission reactions can give rise to many different core fragments and thus, and through their further decay processes, an additional nuclear fragment
  • Synthesis chamber to install The target can also be attached outside the synthesis chamber.
  • Core fragments that do not correspond to the desired metal element may preferably have a target
  • Metal elements can be penetrated without too much loss of yield.
  • the target coverage can be selected so that it can retain heavier fission fragments than the metal elements. Accordingly, through
  • Selecting the target cover material and / or adjusting the thickness of the target cover increases the selectivity of the target cover penetrating metal elements from the resulting core fragments.
  • the synthesis chamber can be provided with an entrance window.
  • This can be constructed in such a way that the respectively used radiation directed to the target, in particular thermal neutrons or accelerated ions, can pass.
  • the entrance window can be a Mylar film, which in particular only a few
  • Microns has thickness.
  • the detection device can
  • a catcher for filtering and collecting the metal element carbonyl complexes from the
  • the detection device may comprise a detector which detects the decay of the
  • Metal element carbonyl complexes also by a
  • a per se known gas chromatograph comprises a gas chromatography column through which the gas stream is passed with the metal elements.
  • the gas chromatography column may further include a
  • FIG. 1 a basic structure of a schematic
  • Fig. 2 shows another exemplary construction of a
  • FIG. 3 shows a further device structure with
  • FIG. 6 shows an exemplary construction of a synthesis chamber for synthesizing the metal element carbonyl complexes
  • Fig. 7 is a flow chart for the inventive
  • Fig. 8 is a gas flow diagram with a closed
  • Gas loop; 9 shows a relative transport yield of refractory metal elements as a function of
  • Fig. 10 shows a relative transport yield of refractory
  • FIG. 1 shows an embodiment of a synthesis chamber 14.
  • the synthesis chamber 14 has two inlet openings 46 which can each be connected to a supply line 10.
  • the carrier gas may consist of those not shown in FIG.
  • Compressed gas cylinders 2, 4 are mixed and is connected via the with the inlet 46 of the synthesis chamber 14
  • reaction volume 58 in which the carrier gas and metal elements 55 are combined to facilitate the synthesis of the metal element carbonyl complexes
  • the carbon monoxide gas is in the
  • the synthesis chamber 14 comprises a target 54.
  • the target 54 preferably contains fissile material, in particular uranium, plutonium or californium, in order to produce metal elements 55 during a nuclear reaction, for example an induced nuclear fission.
  • fissile material in particular uranium, plutonium or californium
  • Synthesis chamber 14 and in particular the target 54 are irradiated with a radiation 60.
  • a radiation 60 In the shown
  • the target 54 is placed in the synthesis chamber 14.
  • the radiation 60 penetrates the wall 52 of the synthesis chamber 14 at a location provided for this purpose, the inlet window 53.
  • the flow path of the carrier gas at the inlet 46 is symbolized by the arrow 40.
  • the arrow 42 shows the
  • the synthesis of the metal elements is briefly described below.
  • the metal elements generated and emitted by the target 54 are defined by the components of the
  • Carrier gas in the synthesis chamber 14 thermalizes, which increases the likelihood of synthesizing
  • Metal elements synthesize in reaction volume 58 with the carrier gas to metal element carbonyl complexes.
  • the synthesized metal element carbonyl complexes are entrained to the outlet 48 by the gas flow of the carrier gas, appearing in the direction shown by the arrow 42
  • a pressure sensor 51 is attached to the synthesis chamber 14 for measuring the pressure in the reaction volume.
  • FIG. 2 shows a further embodiment of a
  • Reaction volume 58 The further construction of the apparatus is in accordance with the synthesis chamber 14 described with reference to FIG.
  • FIG. 3 shows a further embodiment of a
  • the target 54 is arranged as in the structure described with Figure 2 outside the synthesis chamber 14 and can be irradiated with the radiation 60, in particular particle radiation.
  • Ablenkmagnete 61 act on the location of the target 54 with a deflecting force.
  • Particles moving in the magnetic field of the deflecting magnets 61 are deflected by their deflecting force depending on various particle parameters such as mass and charge number.
  • the target 54 is irradiated, wherein the radiation 60 at least partially penetrates the target 54.
  • This penetrating radiation is shown as "primary radiation” 60 with a little curved arrow in Figure 3.
  • This radiation 60 is little influenced by the deflection magnets 61 in their direction, it does not strike the synthesis chamber 14.
  • the metal elements 55 produced in the target 54 on the other hand, become is deflected by means of the magnetic field in the direction of the synthesis chamber 14.
  • the magnetic field of the deflection magnets 61 is preferably matched to the desired metal elements 55
  • FIG. 4 schematically shows an exemplary structure of a device for generating, providing, transporting and measuring refractory metal elements. This is at a nuclear reactor 18, in this example the
  • the reactor core 16 generates and thermalises the neutrons, which are then made available to four different measurement sites 64, in the case shown.
  • the synthesis chamber 14 shown in more detail in FIG. 4 is installed at one of the four measuring stations 64.
  • a carrier gas is in the case shown by a
  • the carrier gas source comprises a carbon monoxide gas bottle 2 and a
  • Inert gas cylinder 4 N 2 gas as an inert gas As an inert gas.
  • Synthesis chamber 14 is explained in more detail in particular with reference to FIG 4. Optionally, depending on the requirement in the
  • Carbon monoxide gas cylinder 2 or so a mixture of carbon monoxide gas and inert gas from the
  • Carbon monoxide gas cylinder 2 and the inert gas cylinder 4 are fed into the supply line 10. About one with an outlet 48 of the synthesis chamber 14th
  • connected transport line 12 may be the carrier gas which contains the synthesized in the synthesis chamber 14 Metallelement- Carbonyl complexes containing a remote from the place of production of the metal elements in the synthesis chamber 14 structure 15 in the form of a detection or measuring device to the side facing away from the synthesis chamber 14 end 13 of
  • Transport line 12 are supplied.
  • Synthesis chamber 14 remote end 13 of the transport line 12 is connected.
  • a filter 34 is arranged, by means of the filter 34, the metal element carbonyl complexes produced are filtered from the carrier gas stream.
  • the filter 34 consists for example of a simple
  • a detector 20 is in this embodiment above the
  • the detector 20 may be a germanium gamma detector. By means of the detector, the
  • Decay frequency can be obtained.
  • the transport yield can be determined.
  • a gas pump 30 is in the flow direction of the
  • Gas Chromatograph 21 connected. This comprises a gas chromatography column 22 with a cooling device 24 and a coolant reservoir 26.
  • Gas chromatograph connected furnace 32 allows a more accurate setting of a temperature gradient along the gas chromatography column 22.
  • a detector 20 ' is arranged longitudinally displaceable on the gas chromatography column 22.
  • the detector 20 ' may be, for example, a germanium gamma detector. In principle, any detector that detects a radioactive radiation is suitable.
  • the detector 20 ' measures the decay frequency distribution of the radioactive metal element decays along the gas chromatography column
  • Coolant reservoir 2 6 connected.
  • thermochromatography column 22 forms during operation of the gas chromatograph 21, a temperature gradient from. This corresponds to a thermochromatography apparatus.
  • the structure 15 ' viewed in the direction of flow of the carrier gas behind the structure 15', in particular the
  • both structures 15, 15 'can also be constructed serially, by referring to the aforementioned
  • Detection device 15 from Figure 1 connects. If a plurality of detectors 20, 20 'is used, those in the gas chromatography column 22 may not
  • the structures 15, 15 'shown in FIGS. 4 and 5 in the form of detection or measuring devices are exemplary. It may there also a different kind used as evidence or measuring apparatus used construction or apparatus for further use of the metal elements produced or be integrated and connected to the end 13 of the transport line 12 to the
  • FIG. 6 shows a further embodiment of the
  • Synthesis chamber 14 in a cross section The reference numbers used correspond to those of the previous ones
  • Embodiments match.
  • Carrier gas arranged which the carrier gas around the target 54 distributed around in the synthesis chamber 14 admits.
  • the flow path of the carrier gas at the inlet 46 is symbolized by the arrow 40.
  • the arrows 44 symbolize a rotationally symmetrical distribution of the carrier gas around the synthesis chamber 14 and the entry of the carrier gas in the reaction volume 58th
  • Target cover 56 attached.
  • the target cover 56 may comprise further, in particular heavier, fission products, which may be formed in the target 54 in the case of nuclear reactions such as induced nuclear fission, from the reaction volume 58
  • the material of which the target cover 56 consists, or which has the target cover 56, will be based on the target material and the desired
  • Target cover 56 made of aluminum.
  • a pressure sensor 51 is connected to a port 50 in this embodiment. The pressure sensor 51 allows the adjustment of the gas pressure in the synthesis chamber 14. Also, the synthesis chamber 14 shown in Fig. 6 can be
  • the synthesis chamber 14 has an inlet 46 which is connected to a supply line 10 and with a
  • Carrier gas source 3 can be connected.
  • the carrier gas may be introduced via the inlet 46 into the synthesis chamber.
  • the synthesis chamber 14 also has a reaction volume 58 in which the carrier gas and the metal elements in
  • the synthesis chamber 14 likewise comprises a target 54.
  • the target 54 is in the synthesis chamber 14 in the example shown
  • the flow path of the carrier gas is symbolized by arrows, wherein at the inlet 46 of the arrow 40
  • the target 54 may be irradiated with the radiation 60.
  • the process parameters of the device preferably allow the release of the metal elements to take place directly in the gaseous phase.
  • a target cover 56 is attached on the target 54 of the embodiment shown in Figure 6, a target cover 56 is attached.
  • the target 54 may also be configured such that the target cover 56 is included in the target 54. Also, use of the entrance window 53 as
  • Target cover 56 especially in the case of a
  • FIG. 7 shows a flow chart for the method according to the invention for providing and transporting
  • FIG. 8 shows a flow chart of the gas flow. In the embodiment shown, this is a closed circuit, so that the carrier gas circulates between feed line 10, the synthesis chamber 14 and transport line 12.
  • the carrier gas taken from the carrier gas bottles 2, 4 and adjusted by means of the mass flow controllers 6, 8 is supplied to the circuit in order to fill the circuit and / or to compensate for gas loss.
  • the mass flow controller 7 the mass flow is measured with the pressure regulator 9, the pressure in the circuit and / or adjusted.
  • the carrier gas is therefore recirculated.
  • valves 29 the desired gas flow path is adjustable.
  • the carrier gas can be sucked and / or the supply and transport lines 10, 12 before
  • the gas pump 30 can be separated from the gas flow path by means of the valve 29. It is also possible in the supply line by means of a valve 29 further, possibly other carrier gas supplied to the gas flow path.
  • FIG. 9 shows that with the one shown in FIG.
  • Total delivery gives the proportionate mixture size of the carbon monoxide gas.
  • the ordinate shows a corresponding transport of metal elements normalized to such a corresponding metal element transport by potassium chloride.
  • the yield obtained is a multiple of the yield obtained when using
  • FIG. 9 shows the results for four refractory metal elements with two measurement series each. Two each for technetium, molybdenum, ruthenium and rhodium.
  • FIG. 10 shows the yield of metal element transport as a function of the delivery rate of the carrier gas. Again, a structure has been used which corresponds to that shown in Figure 4.
  • the detector 20, 20 'and the mass flow controllers 6, 8 are recorded and the data are evaluated by the evaluation device 62.
  • the abscissa here shows the carrier gas flow in ml / min, the ordinate on a transport with potassium chloride
  • FIG. 10 shows the results for four refractory metal elements technetium, molybdenum, ruthenium and rhodium.
  • FIG. 11 shows the yield of the metal element transport as a function of the set pressure of the carrier gas in the range from 1000 to 1500 mbar. The ordinate is again normalized to a conventional transport with
  • Refractory metal elements technetium, molybdenum, ruthenium and rhodium shown.
  • radiation e.g., neutrons, ions

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Particle Accelerators (AREA)
  • Chemical Vapour Deposition (AREA)

Abstract

L'invention concerne un dispositif et un procédé pour produire, mettre à disposition et transporter des éléments métalliques en phase gazeuse. Le gaz porteur contient du monoxyde de carbone, le gaz porteur et les éléments métalliques sont combinés sous la forme d'un volume réactionnel et les éléments métalliques et le monoxyde de carbone sont synthétisés sous forme de complexes éléments métalliques-carbonyle.
PCT/EP2012/053090 2011-02-24 2012-02-23 Procédé et dispositif de transport d'éléments métalliques en phase gazeuse Ceased WO2012113877A1 (fr)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0960856A2 (fr) * 1998-05-12 1999-12-01 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Génération de standards de carnoyle metallique pour la calibration de systèmes spectroscopiques
US20040109810A1 (en) * 2002-12-04 2004-06-10 Khozan Kamram M Process for producing nickel carbonyl, nickel powder and use thereof
WO2007112394A2 (fr) * 2006-03-29 2007-10-04 Tokyo Electron Limited Procédé et système intégré de purification et de distribution d'un précurseur de carbonyle métallique

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0960856A2 (fr) * 1998-05-12 1999-12-01 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Génération de standards de carnoyle metallique pour la calibration de systèmes spectroscopiques
US20040109810A1 (en) * 2002-12-04 2004-06-10 Khozan Kamram M Process for producing nickel carbonyl, nickel powder and use thereof
WO2007112394A2 (fr) * 2006-03-29 2007-10-04 Tokyo Electron Limited Procédé et système intégré de purification et de distribution d'un précurseur de carbonyle métallique

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EP2678273A1 (fr) 2014-01-01
WO2012113877A8 (fr) 2012-10-26
DE102011000908B4 (de) 2013-08-01

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