EP3620732B1 - Appareil et procédé de refroidissement exempts de cryogène - Google Patents

Appareil et procédé de refroidissement exempts de cryogène Download PDF

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Publication number
EP3620732B1
EP3620732B1 EP19187223.3A EP19187223A EP3620732B1 EP 3620732 B1 EP3620732 B1 EP 3620732B1 EP 19187223 A EP19187223 A EP 19187223A EP 3620732 B1 EP3620732 B1 EP 3620732B1
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European Patent Office
Prior art keywords
holding device
sample
sample holding
radiation shield
heat radiation
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EP19187223.3A
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German (de)
English (en)
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EP3620732A1 (fr
EP3620732B2 (fr
Inventor
John Garside
Simon Kingley
Gavin Crowther
Matthias Buehler
Doreen Wernicke
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Oxford Instruments Nanotechnology Tools Ltd
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Oxford Instruments Nanotechnology Tools Ltd
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Application filed by Oxford Instruments Nanotechnology Tools Ltd filed Critical Oxford Instruments Nanotechnology Tools Ltd
Priority to EP22205298.7A priority Critical patent/EP4148353B1/fr
Priority to EP22154522.1A priority patent/EP4027081B1/fr
Publication of EP3620732A1 publication Critical patent/EP3620732A1/fr
Publication of EP3620732B1 publication Critical patent/EP3620732B1/fr
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25D—REFRIGERATORS; COLD ROOMS; ICE-BOXES; COOLING OR FREEZING APPARATUS NOT OTHERWISE PROVIDED FOR
    • F25D19/00—Arrangement or mounting of refrigeration units with respect to devices or objects to be refrigerated, e.g. infrared detectors
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25B—REFRIGERATION MACHINES, PLANTS OR SYSTEMS; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS
    • F25B9/00—Compression machines, plants or systems, in which the refrigerant is air or other gas of low boiling point
    • F25B9/14—Compression machines, plants or systems, in which the refrigerant is air or other gas of low boiling point characterised by the cycle used, e.g. Stirling cycle
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25B—REFRIGERATION MACHINES, PLANTS OR SYSTEMS; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS
    • F25B9/00—Compression machines, plants or systems, in which the refrigerant is air or other gas of low boiling point
    • F25B9/14—Compression machines, plants or systems, in which the refrigerant is air or other gas of low boiling point characterised by the cycle used, e.g. Stirling cycle
    • F25B9/145—Compression machines, plants or systems, in which the refrigerant is air or other gas of low boiling point characterised by the cycle used, e.g. Stirling cycle pulse-tube cycle

Definitions

  • the invention relates to a cryogen free cooling apparatus and a method for using such an apparatus.
  • a key challenge with these systems is that the sample is entered into the equipment at room temperature, typically around 300K and then moved to another position where thermal contact is made with a body at a much lower temperature which in some systems can be lower than 1K.
  • the sample and associated mounting and connection equipment is usually pre-cooled either by passing it through cold cryogen gas on its way in to the system or by passing cold cryogen gas or liquid through the sample transfer mechanism, this reduces the thermal shock both on the sample and on the equipment.
  • cryogenic systems that do not require the addition of liquid cryogens or that only require liquid nitrogen during initial cool down have been developed. These are generally known as cryogen free (or "cryofree") systems. These systems use a mechanical cooler such as a GM cooler, Stirling cooler or a pulse tube to provide the cooling power. Because the cooling power of commercially available coolers is somewhat lower than the cooling power available from a reservoir of liquid cryogen, these systems can typically take longer to warm up, change the sample and cool down. There is therefore a considerable need for a method of changing samples in cryogen free systems without the need to warm up the entire system.
  • cryogen free systems there are a number of technical challenges when attempting to load a warm sample in to a cold cryostat. Firstly, the internals of the system are usually contained within a sealed vacuum vessel to reduce heat load. Secondly, within that sealed vacuum vessel, the sample space is usually enclosed by one or more radiation shields to further reduce the heat load. Thirdly, there are no liquid cryogens available to pre-cool the sample as it moves from room temperature to the cold mounting body. Also, electrical contacts need to be remotely made to the sample when it is loaded in the cryostat. This invention seeks to provide solutions to these problems.
  • US-A-5611207 discloses a cryogenic cooling apparatus comprising a vacuum chamber enclosing: a mechanical cooler having first and second heat stations, the second heat station being colder than the first heat station, a cylindrical radiation shield thermally secured to the first heat station and provided with circular access opening, and a heat switch thermally secured to the second heat station.
  • a shutter is rotated to thermally couple a measurement insert to the radiation shield and pre-cool the insert. After pre-cooling the insert, the shutter is again rotated and the insert is thermally coupled to the second heat station.
  • US-A-5611207 discloses a cryogen free cooling apparatus according to the preamble of claim 1.
  • a cryogen free cooling apparatus and a method of loading a sample into the working region of a cryogen free cooling apparatus according to the present invention is defined in claim 1 and claim 13, respectively.
  • the sample loading apparatus further includes a vacuum vessel in which the sample holding device and elongate probe are movably mounted, the vacuum vessel being connectable to the aperture of the vacuum chamber wall.
  • the first heat radiation shield will be held at a temperature of between 45K and 90K while the second radiation shield (if provided) will be held at a temperature of less than 6K or even less than 4.2K.
  • the heat radiation shield apertures may be left open but in order to reduce heat transfer, preferably each aperture is closable by a respective closure system.
  • An example of a suitable closure system comprises one or more flexible flaps, or hinged and sprung flaps.
  • the sample loading apparatus comprises two elongate probes, each coupled to the sample holding device, but in other embodiments a single elongate probe could be used. In both cases, preferably the or each probe is rotatable about its axis relative to the sample holding device. Of course, more than two probes could be used.
  • the connector is conveniently formed by providing a screw thread at one end of the or each rod, the first connector cooperating with a screw thread on the first or second heat radiation shield to achieve thermal connection therebetween.
  • the thermal connection can be achieved using a spring connection where the sample holding device is fitted with a or a plurality of thermally conductive springs which engage on an inner surface of the aperture of the radiation shield. That inner surface may be extended, for example by addition of a tube assembly or a thicker plate assembly to allow for engagement.
  • the spring connectors could also be fixed on the heat or radiation shield and the sample holding device pushed on to them.
  • the thermal connection could be via springs at the higher temperature shields and via screw contact at the lower temperature shields or any combination thereof.
  • the connector could be defined by cone or wedge-shaped mating parts to amplify the contact pressure from the mounting mechanism. This significantly improves performance.
  • the or each probe is releasably coupled to the sample holding device whereby a first operation of the probe(s) causes the sample holding device to be connected to a support at the working region, and a second operation enables the probe(s) to be released from the sample holding device and retracted.
  • a first operation of the probe(s) causes the sample holding device to be connected to a support at the working region
  • a second operation enables the probe(s) to be released from the sample holding device and retracted.
  • This enables the probe(s) to be removed from the vacuum chamber of the cryostat so as to reduce heat flow into the cryostat. Actuators to allow this could be provided on the probe or cold body.
  • the cryogen free cooling apparatus can be used for a variety of purposes such as DNP, NMR etc. and typically a magnet will be located within the cryostat surrounding the working region.
  • FIG. 1 A first embodiment of the current invention is shown in more detail in Figures 1 to 5 .
  • a sample 1 is mounted on a sample carrier or sample loading device 2 supported on thermally conductive rods of two rod or probe assemblies 3.
  • the sample carrier 2 has space for a number of electrical and/or optical connectors (not shown) to allow connection to connectors on the primary cold body in the cryostat. This allows multiple push fit connectors to be used which gives high flexibility and the wiring to go through the cryostat rather than down the probe tube, which has significant thermal benefits.
  • the ends of the two rod assemblies 3 are free to rotate within the carrier.
  • a tube and flange assembly forms a vacuum vessel 6 surrounding the rod assemblies 3 and which is open at one end, this end being sealed against the bottom of a gate valve 5 when assembled to a cryostat 50.
  • the rod assemblies pass through a pair of o-ring seals 7.
  • the cryostat 50 comprises an outer vacuum vessel 4 which is closed except for a port 52 covered by a large diameter gate valve 5. Within the vacuum chamber 4 is located a first radiation shield 54 having an aperture 56 aligned with the aperture 52 of the vacuum chamber, and within the first radiation shield 54 is located a second radiation shield 10 having an aperture 58 aligned with the apertures 52,56.
  • the radiation shields 10,54 surround a working region 20 at which is located a cold mounting body 15.
  • the shields 10,54 are cooled by a conventional mechanical cooler such as a GM cooler, Stirling cooler, or pulse tube device. This is not shown in the drawings for reasons of clarity.
  • a first stage of the mechanical cooler is thermally coupled to the shield 54 and a second, colder stage to the shield 10.
  • the first shield 54 is cooled to a temperature of about 77K and the second shield 10 to a temperature of 6K or less, for example about 4.2K.
  • the second shield is held at a temperature higher than 6K.
  • each of the shields as well as the cold mounting body 15 held at the lowest temperature can be considered as "cold bodies".
  • the aperture 56 of the shield 54 is defined by a plate 12 with a cut-out 17.
  • the aperture 58 of the shield 10 is defined by another plate 12 and cut-out 17.
  • the apertures 56,58 can be closed by a suitable closure mechanism.
  • Figure 5 shows a close up cross-sectional view of one possible embodiment of such a mechanism.
  • a or a plurality of flaps 25 are connected to the radiation shield 10 via a sprung hinge arrangement 26. When the rod assembly 3 passes through the flap assembly, the flap or plurality thereof 25 open.
  • the flap or plurality thereof 25 may optionally be shaped or fitted with guide mechanisms to prevent the sample carrier, baffles or rod assemblies from catching on the flaps as the rod assembly and/or carrier is retracted.
  • a sample 1 is loaded on to the sample carrier 2 and electrical or optical connections are made.
  • the sample carrier 2 is then mounted on the end of the rod assemblies 3.
  • the rod assemblies 3 are then retracted through the sliding o-ring seals 7 until the sample carrier is fully within the vacuum vessel 6.
  • the vacuum vessel 6 is then attached to the gate valve 5 and air is pumped out of the vacuum vessel 6 through ports 8A,8B and valves 8.
  • the gate valve is opened.
  • the rod assemblies 3 are then pushed to move the sample carrier through the gate valve and to the first pre-cool position.
  • Figure 2 shows the sample carrier 2 approaching the plate 12 of the shield 54 to thermally connect the sample carrier to a radiation shield pre-cool position defining a first cold body.
  • the rod assemblies 3 have a key 22 ( Figure 4 ) on the end which, when engaged, turns a screw thread 18.
  • the screw threads 18 are aligned with mating screw threads 19 on the plate 12 allowing the sample carrier 2 to be screwed to the plate 12 on the radiation shield 54, thereby making thermal contact.
  • An optional thermometer (not shown) is provided on the sample carrier or rod assembly to allow the temperature of the sample carrier to be monitored during cool down. When the sample carrier 2 is sufficiently cold, the rod assemblies 3 are again rotated to separate the two screw threads.
  • the entire rod and carrier assembly is then rotated by means of a rotating seal on the vacuum vessel 6 or gate valve 5, to allow the carrier 2 to pass through the cut-out 17.
  • the carrier is then optionally connected in a similar manner to a or a plurality of optional additional radiation shields, such as the shield 10 (forming additional cold bodies).
  • the rod assemblies 3 are pushed to their final position to allow connection of the sample carrier 2 to the cold body 15 which could by way of example be connected to the mixing chamber of a dilution refrigerator or a sample plate of a cryostat.
  • Figure 3 shows the sample carrier 2 contacting the cold plate 15.
  • the screw threads 18 are engaged in mating screw threads (not shown) on the cold plate 15.
  • a number of optional push fit electrical and optional optical connections can be made between the sample carrier 2 and the cold body 15. These connectors are not shown on this diagram. In this view, two baffle assemblies 14 are also visible.
  • baffle assemblies are free to slide on the rod assemblies 3 and are pushed or pulled towards the sample carrier by spring assemblies 21.
  • baffle assemblies 14 are shown here in a retracted position, in reality they will be forced by the spring assemblies to contact the plates on the radiation shield, thereby closing the cut-outs 17 and making thermal contact.
  • the baffle assemblies are also optionally connected to the rod assemblies using sliding thermal connections such as thermally conductive spring assemblies, thus allowing the heat passing down the rods from room temperature to be intercepted.
  • Figure 4 shows a close up cross sectional view of the sample carrier and rod assemblies.
  • the key 22 that inserts into a matching connection on the screw thread 18.
  • On the key and rod assembly there is a screw thread 23 and on the sample carrier there is a matching screw thread 24.
  • This arrangement means that if the rod assemblies are retracted, the screw threads 23,24 will clash and the sample carrier will therefore also be retracted.
  • the rod assemblies can then be partially retracted to remove the key from the back of the screw thread 18 and reduce heat flow to the sample. However, this is not essential and the sample could remain connected to the probe.
  • the rod assembly can then be rotated to allow the screw threads to pass through each other and then either be partially retracted from the cryostat, leaving the baffles in contact with the radiation shields, or be fully retracted from the cryostat in order to further reduce heat load.
  • the optional mechanism 11 can be fitted to close the cut outs in the radiation shields.
  • FIG. 6 A second embodiment of the current invention is shown in Figure 6 .
  • a single rod assembly 3 is used with a single large diameter screw thread 18.
  • an adapter 27 which connects the rod assembly to the sample carrier assembly 2.
  • an adapter 27 On the adapter there are a or a plurality of protrusions 28 that engage in slots or recesses 29 formed on the means 12 to allow the carrier to be thermally connected to the radiation shields.
  • the sample is loaded into the carrier and entered through the gate valve 5 as per the first embodiment.
  • the rod assembly is rotated to engage the protrusions 28 in the slots or recesses 28 and the rod assembly is then pushed towards the cryostat until the protrusions 28 meet an obstruction 30.
  • Thermal connection is then optionally made through the protrusions or through optional spring contacts 31.
  • the slot and obstruction are optional and serve to prevent the sample carrier from being accidentally pushed past the radiation shield prior to pre-cooling.
  • the sample rod When the sample is cooled adequately, the sample rod is optionally retracted slightly and rotated to allow the protrusions 28 to move past the obstruction 30. The rod assembly can then be further inserted to allow it to be thermally connected to the next radiation shield if so required.
  • the optional baffles 13 fitted with optional spring thermal contacts 14 engage in the assembly 12 so as to both close the port in the radiation shield and optionally to make thermal contact between the radiation shield and the rod assembly to intercept heat.
  • a similar optional process for pre-cooling on subsequent radiation shield(s) can then be included before moving the sample to the cold body.
  • Figure 7 shows a cross sectional view of the sample carrier assembly of the second embodiment engaged on the cold body.
  • the sample carrier 2 is enclosed in a tube 32 with a screw thread 18 on one end.
  • a means 33 of connecting the tube to the adapter on the end of the rod assembly is provided at the opposite end of the tube. This allows the tube to be inserted and retracted and to be rotated by the rod assembly.
  • the sample carrier is free to rotate inside the tube and is thermally connected to the adapter at the end of the rod assembly using a spring thermal contact 34.
  • the rod assembly is then rotated to pull the sample carrier on to the mating part, making the thermal contact and optional electrical and optical connections.
  • the rod assembly can then be retracted from the cryostat, disconnecting at the means of connecting the tube to the adapter on the end of the rod assembly.
  • Optional baffles can be fitted to close the ports in the radiation shields if the rod assembly is to be completely removed. Removal of the sample is essentially the reverse of the insertion process, with the exception that it is not usually necessary to leave the sample carrier at the radiation shields to warm up when retracting the sample.
  • the mechanism for connection to the radiation shields from being a screw connection to being a spring connection
  • the sample carrier is fitted with a or a plurality of thermally conductive springs which engage on an inner surface of the cut-out on the radiation shield. That inner surface may be extended, for example by addition of a tube assembly or a thicker plate assembly to allow for engagement.
  • the thermal connection could be via springs at the higher temperature shields and via screw contact at the lower temperature shields or any combination thereof.
  • Cone or wedge-shaped mating parts on either side of the releasable coupling could be used to amplify the contact pressure from the mounting mechanism. Pneumatic or piezo or other forms of releasable contact could also be used.
  • connection to the or each cold body can optionally be via thermally conductive spring contacts rather than screw connection.
  • connection to the radiation shields can optionally be via thermally conductive spring contacts or screw contacts.
  • thermal connection is or could be made to a radiation shield or shield
  • this thermal connection could alternatively be made to any other suitable cold surface.
  • thermally conductive spring contacts these can be made from a single material, such as Berillium Copper, or may be made from a laminate or composite of different materials to provide both a good spring force and a high thermal conductivity.
  • Dissimilar materials are preferred so as to reduce eddy currents and quench forces when used with a magnet. Examples of dissimilar materials could be copper for high thermal conductivity and stainless steel for high strength and lower electrical conductivity to reduce induced eddy currents.
  • Other possibilities could include titanium and copper or brass and copper or alumium alloy and copper. Generically, it is one material of high thermal conductivity and one of high strength and higher resistance.
  • the second material could also be a plastic or a composite.
  • an additional port or plurality thereof can be added to the second vacuum vessel to allow the sample and optionally the sample carrier to be removed without removal of the second vacuum vessel from the main vacuum vessel.
  • connection to the radiation shields it is possible to change the connection to the radiation shields to a screw thread on the outside of the rotating tube assembly. It is also possible to change the screw thread connection to the cold body to be an external thread, meaning the same thread can be used to connect to the radiation shields for pre-cooling and then to the cold body.
  • the tube assembly with the thread may optionally have a split in it to allow the diameter to change to compensate for thermal expansion and contraction.
  • a superconducting magnet could be located in the cryostat 50 as is known conventionally for dynamic nuclear polarisation and nuclear magnetic resonance and other cryogenic magnetic field applications.
  • the rods form actuators for connecting and disconnecting to the cold bodies and are demountable from the cryostat.
  • the rods (or other actuators) could form part of the cryostat and the sample carrier could be carried on a probe independent of the rods (or other actuators), the rods (or other actuators) being manipulated to engage the screw threads (or other connection mechanism) as before.

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Combustion & Propulsion (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Separation By Low-Temperature Treatments (AREA)

Claims (14)

  1. Un appareil de refroidissement sans cryogène comprenant :
    une chambre sous vide (4) ;
    un premier bouclier anti-rayonnement thermique (54) entourant une zone de travail (20) et situé dans la chambre sous vide ;
    un système de refroidissement sans cryogène comportant un premier étage de refroidissement raccordé au premier bouclier anti-rayonnement thermique (54) et un deuxième étage de refroidissement, plus froid que le premier étage de refroidissement ;
    des orifices alignés (52, 56) dans le premier bouclier anti-rayonnement thermique (54) et la paroi de la chambre sous vide ;
    un appareil de chargement de l'échantillon possédant une ou plusieurs sondes allongées (3) et un dispositif porte-échantillon (2) fixé sur la ou les sondes allongées (3), cette ou ces sondes allongées est ou sont conçue(s) pour l'insertion du dispositif porte-échantillon au travers des orifices alignés (52, 56), jusqu'à la zone de travail (20) ; et
    un ou plusieurs connecteurs thermiques (18), le dispositif porte-échantillon étant configuré pour une connexion amovible pour assurer une conduction thermique par le biais dudit ou desdits connecteur(s) thermique(s) au niveau du premier bouclier anti-rayonnement thermique (54) de façon à pré-refroidir un échantillon (1) sur ou dans le dispositif porte-échantillon avant l'insertion du dispositif porte-échantillon dans la zone de travail (20) ;
    caractérisé par un deuxième bouclier anti-rayonnement thermique (10) implanté à l'intérieur du premier bouclier anti-rayonnement thermique (54) et entourant la zone de travail (20), et ce deuxième bouclier anti-rayonnement thermique est raccordé au deuxième étage de refroidissement et a un orifice (58) aligné sur les orifices (52, 56) du premier bouclier anti-rayonnement thermique et de la paroi de la chambre sous-vide de façon à permettre le passage au travers du dispositif porte-échantillon (2), et ce dispositif porte-échantillon peut être raccordé, de façon amovible, pour assurer une conduction thermique par le biais dudit ou desdits connecteur(s) thermique(s) (18) au deuxième bouclier de rayonnement thermique de façon à assurer un pré-refroidissement supplémentaire d'un échantillon (1) sur ou dans le dispositif porte-échantillon avant que ce dispositif porte-échantillon ne soit inséré dans la zone de travail (20).
  2. L'appareil que décrit la revendication 1, si ce n'est que l'orifice aligné (52) dans la paroi de la chambre sous vide comporte un système de fermeture (5), comme, par exemple, une soupape à vide.
  3. L'appareil que décrit la revendication 1 ou 2, si ce n'est que les orifices alignés (56, 58) dans les premier et deuxième boucliers anti-rayonnement thermique (54, 10) comportent des systèmes respectifs de fermeture (25).
  4. L'appareil que décrit la revendication 3, si ce n'est que les systèmes respectifs de fermeture pour les premier et deuxième boucliers anti-rayonnement thermique (54, 10) comportent un ou plusieurs volets flexibles ou volets à charnières et à ressort.
  5. L'appareil que décrit l'une ou l'autre des revendications précédentes, si ce n'est que l'appareil de chargement de l'échantillon comporte au moins deux sondes allongées (3), et chacune de ces sondes est raccordée au dispositif porte-échantillon (2).
  6. L'appareil que décrit la revendication 5, si ce n'est que la ou les sondes (3) peuvent tourner autour de leur axe par rapport au dispositif porte-échantillon (2).
  7. L'appareil que décrit la revendication 5 ou 6, si ce n"est que la ou les sondes (3) est ou sont filetée(s) à un bout afin de définir un dit connecteur thermique (18), le connecteur coopérant avec un filet sur le premier bouclier anti-rayonnement thermique (54) afin de réaliser une connexion thermique entre eux.
  8. L'appareil que décrit l'une ou l'autre des revendications 1 à 5, si ce n'est qu'au moins un des connecteurs thermiques comporte un ou plusieurs ressorts thermo-conducteurs (31) implantés de manière à réaliser un contact thermique entre le premier bouclier anti-rayonnement thermique (54) et le dispositif porte-échantillon (2).
  9. L'appareil que décrit la revendication 8, si ce n'est que les ressorts conducteurs (31) se composent d'un matériau composite à forte thermoconductivité et à force élevée de ressort.
  10. L'appareil que décrit l'une ou l'autre des revendications précédentes, si ce n'est que l'appareil de chargement de l'échantillon peut tourner par rapport à la chambre sous vide (4) et aux boucliers anti-rayonnement thermique (54, 10) de façon à s'aligner de manière sélective sur le ou les connecteurs thermiques ou sur l'orifice respectif afin d'y permettre le passage du dispositif porte-échantillon (2).
  11. L'appareil que décrit l'une ou l'autre des revendications précédentes, si ce n'est que cet appareil est configuré de telle sorte que la ou les sondes (3) est ou sont raccordée(s), de manière amovible, au dispositif porte-échantillon (2) de telle sorte qu'un premier fonctionnement de cette ou ces sondes entraîne le raccordement de ce dispositif porte-échantillon à un support (15) au niveau de la zone de travail (20) et qu'un deuxième fonctionnement et des fonctionnements ultérieurs permettent à cette ou ces sondes de s'écarter de ce dispositif porte-échantillons et de prendre la position escamotée.
  12. L'appareil que décrit l'une ou l'autre des revendications précédentes, si ce n'est que l'appareil de chargement de l'échantillon comporte, en outre, un récipient sous vide (6) dans lequel le dispositif porte-échantillon (2) et la ou les sondes allongées (3) sont montés, de façon amovible, et ce récipient sous vide peut se raccorder à l'orifice (52) de la paroi de la chambre sous vide.
  13. Une méthode de chargement d'un échantillon (1) dans la zone de travail (20) de l'appareil de refroidissement sans cryogène que décrit la revendication 12, et cette méthode comporte les éléments suivants :
    le placement d'un échantillon (1) dans ou sur le dispositif porte-échantillon (2) ;
    la fixation du récipient sous vide (6) de l'appareil de chargement de l'échantillon sur la chambre sous vide (4) et son alignement sur l'orifice (52) de la chambre sous vide ;
    l'évacuation du récipient sous vide (6) ;
    l'ouverture de l'orifice (52) de la chambre sous vide (4) et l'actionnement de la ou des sondes allongées (3) pour insérer le dispositif porte-échantillon (2) dans l'orifice ouvert de manière à raccorder thermiquement ce dispositif porte-échantillon au premier bouclier anti-rayonnement thermique (54);
    le refroidissement de l'échantillon (1) dans ou sur le dispositif porte-échantillon sous l'effet de la conduction thermique, jusqu'au bouclier anti-rayonnement thermique (54) ;
    la déconnexion du dispositif porte-échantillon (2) depuis le premier bouclier anti-rayonnement thermique (54) ; et
    l'actionnement de la ou des sondes allongées (3) pour insérer le dispositif porte-échantillon dans la zone de travail (20).
  14. La méthode que décrit la revendication 13, si ce n'est, avant d'atteindre la zone de travail (20), que le dispositif porte-échantillon (2) est raccordé thermiquement au deuxième bouclier anti-rayonnement thermique (10), est refroidi en permettant à la chaleur de circuler jusqu'au deuxième bouclier anti-rayonnement, est déconnecté du deuxième bouclier anti-rayonnement et le dispositif porte-échantillon est ensuite inséré dans la zone de travail (20).
EP19187223.3A 2009-03-16 2010-03-15 Appareil et procédé de refroidissement exempts de cryogène Active EP3620732B2 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
EP22205298.7A EP4148353B1 (fr) 2009-03-16 2010-03-15 Appareil et procédé de refroidissement sans cryogène
EP22154522.1A EP4027081B1 (fr) 2009-03-16 2010-03-15 Appareil et procédé de refroidissement exempts de cryogène

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DE102015215919B4 (de) 2015-08-20 2017-06-22 Bruker Biospin Gmbh Verfahren und Vorrichtung zur Vorkühlung eines Kryostaten
EP3163222B1 (fr) 2015-10-28 2018-07-18 Technische Universität München Appareil de refroidissement sans cryogène
CN109488720B (zh) * 2018-12-27 2024-04-26 仪晟科学仪器(嘉兴)有限公司 闭循环液氦制冷机的机械隔离式震动屏蔽系统
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ES2909009T3 (es) 2022-05-04
GB0904500D0 (en) 2009-04-29
EP4027081A2 (fr) 2022-07-13
ES2935698T3 (es) 2023-03-09
EP2409096B1 (fr) 2019-08-21
EP2409096B2 (fr) 2024-06-19
EP4027081B1 (fr) 2022-12-21
EP4148353B1 (fr) 2024-05-22
EP2409096A2 (fr) 2012-01-25
WO2010106309A8 (fr) 2011-10-13
FI2409096T4 (fi) 2024-06-20
WO2010106309A2 (fr) 2010-09-23
WO2010106309A3 (fr) 2011-05-19
EP3620732A1 (fr) 2020-03-11
FI4027081T3 (fi) 2023-01-13
US20120102975A1 (en) 2012-05-03
FI4148353T1 (fi) 2023-03-29
EP4148353A1 (fr) 2023-03-15
EP3620732B2 (fr) 2024-10-09
EP4027081A3 (fr) 2022-08-31
JP2012520987A (ja) 2012-09-10
EP4148353C0 (fr) 2024-05-22

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