EP4027081A2 - Vorrichtung und verfahren zur kryogenfreien kühlung - Google Patents

Vorrichtung und verfahren zur kryogenfreien kühlung Download PDF

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Publication number
EP4027081A2
EP4027081A2 EP22154522.1A EP22154522A EP4027081A2 EP 4027081 A2 EP4027081 A2 EP 4027081A2 EP 22154522 A EP22154522 A EP 22154522A EP 4027081 A2 EP4027081 A2 EP 4027081A2
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EP
European Patent Office
Prior art keywords
holding device
sample holding
sample
vacuum chamber
radiation shield
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.)
Granted
Application number
EP22154522.1A
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English (en)
French (fr)
Other versions
EP4027081B1 (de
EP4027081A3 (de
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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Publication date
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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/de
Publication of EP4027081A2 publication Critical patent/EP4027081A2/de
Publication of EP4027081A3 publication Critical patent/EP4027081A3/de
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Classifications

    • 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

  • 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.
  • a method of loading a sample into the working region of cryogen free cooling apparatus comprises:
  • cryostat any cold surface coupled to the cooling stage of the cooling system or to an intermediate stage of a sub 4K cooler such as a still of a dilution refrigerator, it is most convenient to utilize the heat radiation shield already present.
  • the cold body is a body held at the lowest temperature within the cooling apparatus in which case the thermal connector allows a weak thermal connection initially to the cold body for precooling following which the connection to the cold body is strengthened so the sample cools to the desired final temperature.
  • more than one heat radiation shield could be provided within the vacuum chamber. One or more of these could therefore be used further to precool the sample.
  • the apparatus further comprises a second heat radiation shield located inside the first radiation shield and surrounding the working region, the cryogen free cooling system having a second cooling stage, colder than the first cooling stage, coupled to the second heat radiation shield, the second radiation shield having an aperture aligned with the apertures of the first heat radiation shield and vacuum chamber wall so as to allow the sample holding device to pass therethrough, whereby the sample holding device can be releasably coupled for heat conduction to the second heat radiation shield.
  • 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.
  • sample loading apparatus just described, particularly the releasable nature of the sample holding device, is considered inventive in its own right and separate from the concept of pre-cooling the sample as defined in the first and second aspects of the invention.
  • 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 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.
  • 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).
  • 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.
  • 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 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.
  • the sample and carrier may optionally be precooled by making a weaker thermal contact to a colder temperature body, such as the coldest body.
  • the relative warming of the cryostat and cooling of the sample and carrier can be controlled by design of the thermal contact.
  • 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)
EP22154522.1A 2009-03-16 2010-03-15 Vorrichtung und verfahren zur kryogenfreien kühlung Active EP4027081B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP22205298.7A EP4148353B1 (de) 2009-03-16 2010-03-15 Kryogenfreie kühlvorrichtung und verfahren

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
GBGB0904500.6A GB0904500D0 (en) 2009-03-16 2009-03-16 Cryofree cooling apparatus and method
PCT/GB2010/000454 WO2010106309A2 (en) 2009-03-16 2010-03-15 Cryogen free cooling apparatus and method
EP19187223.3A EP3620732B2 (de) 2009-03-16 2010-03-15 Vorrichtung und verfahren zur kryogenfreien kühlung
EP10710389.7A EP2409096B2 (de) 2009-03-16 2010-03-15 Kryogenfreie kühlvorrichtung und verfahren

Related Parent Applications (4)

Application Number Title Priority Date Filing Date
EP10710389.7A Division EP2409096B2 (de) 2009-03-16 2010-03-15 Kryogenfreie kühlvorrichtung und verfahren
EP10710389.7A Division-Into EP2409096B2 (de) 2009-03-16 2010-03-15 Kryogenfreie kühlvorrichtung und verfahren
EP19187223.3A Division EP3620732B2 (de) 2009-03-16 2010-03-15 Vorrichtung und verfahren zur kryogenfreien kühlung
EP19187223.3A Division-Into EP3620732B2 (de) 2009-03-16 2010-03-15 Vorrichtung und verfahren zur kryogenfreien kühlung

Related Child Applications (2)

Application Number Title Priority Date Filing Date
EP22205298.7A Division-Into EP4148353B1 (de) 2009-03-16 2010-03-15 Kryogenfreie kühlvorrichtung und verfahren
EP22205298.7A Division EP4148353B1 (de) 2009-03-16 2010-03-15 Kryogenfreie kühlvorrichtung und verfahren

Publications (3)

Publication Number Publication Date
EP4027081A2 true EP4027081A2 (de) 2022-07-13
EP4027081A3 EP4027081A3 (de) 2022-08-31
EP4027081B1 EP4027081B1 (de) 2022-12-21

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ID=40637422

Family Applications (4)

Application Number Title Priority Date Filing Date
EP22205298.7A Active EP4148353B1 (de) 2009-03-16 2010-03-15 Kryogenfreie kühlvorrichtung und verfahren
EP19187223.3A Active EP3620732B2 (de) 2009-03-16 2010-03-15 Vorrichtung und verfahren zur kryogenfreien kühlung
EP10710389.7A Active EP2409096B2 (de) 2009-03-16 2010-03-15 Kryogenfreie kühlvorrichtung und verfahren
EP22154522.1A Active EP4027081B1 (de) 2009-03-16 2010-03-15 Vorrichtung und verfahren zur kryogenfreien kühlung

Family Applications Before (3)

Application Number Title Priority Date Filing Date
EP22205298.7A Active EP4148353B1 (de) 2009-03-16 2010-03-15 Kryogenfreie kühlvorrichtung und verfahren
EP19187223.3A Active EP3620732B2 (de) 2009-03-16 2010-03-15 Vorrichtung und verfahren zur kryogenfreien kühlung
EP10710389.7A Active EP2409096B2 (de) 2009-03-16 2010-03-15 Kryogenfreie kühlvorrichtung und verfahren

Country Status (7)

Country Link
US (1) US20120102975A1 (de)
EP (4) EP4148353B1 (de)
JP (1) JP2012520987A (de)
ES (2) ES2935698T3 (de)
FI (3) FI4027081T3 (de)
GB (1) GB0904500D0 (de)
WO (1) WO2010106309A2 (de)

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GB2493553B (en) * 2011-08-11 2017-09-13 Oxford Instr Nanotechnology Tools Ltd Cryogenic cooling apparatus and method
CN102967834B (zh) * 2012-11-23 2014-10-15 中国科学院武汉物理与数学研究所 一种磁共振引擎装置及方法
CN104884969A (zh) * 2012-12-27 2015-09-02 皇家飞利浦有限公司 用于对无低温超导磁体的失超保护的系统和方法
DE102015215919B4 (de) 2015-08-20 2017-06-22 Bruker Biospin Gmbh Verfahren und Vorrichtung zur Vorkühlung eines Kryostaten
EP3163222B1 (de) 2015-10-28 2018-07-18 Technische Universität München Kältemittelfreie kühlvorrichtung
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
DE102019203341A1 (de) * 2019-03-12 2020-09-17 Pressure Wave Systems Gmbh Kryostat
EP3734303B1 (de) * 2019-05-03 2024-04-03 Afore Oy Kryogener wafertester mit beladevorrichtung
GB2592415A (en) * 2020-02-27 2021-09-01 Oxford Instruments Nanotechnology Tools Ltd Insert for a cryogenic cooling system
FI129268B (fi) 2020-05-13 2021-10-29 Bluefors Oy Laite ja menetelmä lämpöä johtavan kytkennän tekemiseksi
US11360140B1 (en) 2020-12-18 2022-06-14 Microsoft Technology Licensing, Llc RF functional probe

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US4446702A (en) 1983-02-14 1984-05-08 Helix Technology Corporation Multiport cryopump
US4577465A (en) 1984-05-11 1986-03-25 Helix Technology Corporation Oil free vacuum system
US5077523A (en) 1989-11-03 1991-12-31 John H. Blanz Company, Inc. Cryogenic probe station having movable chuck accomodating variable thickness probe cards
US5834938A (en) 1995-08-18 1998-11-10 Seiko Instruments Inc. Nondestructive inspection apparatus with superconducting magnetic sensor
US5727392A (en) 1996-12-19 1998-03-17 Helix Technology Corporation Convection-shielded cryopump
US5806319A (en) 1997-03-13 1998-09-15 Wary; John Method and apparatus for cryogenically cooling a deposition chamber
US20070234751A1 (en) 2006-04-06 2007-10-11 National Institute Of Advanced Industrial Science And Technology Sample cooling apparatus
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Also Published As

Publication number Publication date
ES2909009T3 (es) 2022-05-04
GB0904500D0 (en) 2009-04-29
ES2935698T3 (es) 2023-03-09
EP2409096B1 (de) 2019-08-21
EP2409096B2 (de) 2024-06-19
EP4027081B1 (de) 2022-12-21
EP4148353B1 (de) 2024-05-22
EP2409096A2 (de) 2012-01-25
EP3620732B1 (de) 2022-02-16
WO2010106309A8 (en) 2011-10-13
FI2409096T4 (fi) 2024-06-20
WO2010106309A2 (en) 2010-09-23
WO2010106309A3 (en) 2011-05-19
EP3620732A1 (de) 2020-03-11
FI4027081T3 (fi) 2023-01-13
US20120102975A1 (en) 2012-05-03
FI4148353T1 (fi) 2023-03-29
EP4148353A1 (de) 2023-03-15
EP3620732B2 (de) 2024-10-09
EP4027081A3 (de) 2022-08-31
JP2012520987A (ja) 2012-09-10
EP4148353C0 (de) 2024-05-22

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