This invention relates to a cryogenic apparatus, that is to say an apparatus for low-temperature refrigeration. Such apparatus may enable a specimen to be cooled to ultra-low temperatures so that measurements may be made on the properties of the specimen at such low temperatures.
A number of different thermo-mechanical devices are known for achieving such low temperatures, for example using pressure cycling of helium gas. This may be achieved using, for example, a Gifford-McMahon cooler, wherein high-pressure helium, at a pressure typically between 10 and 30 bar, is used as the working fluid and a cylinder contains a displacer and regenerator. A mechanical valve connects the cylinder to the gas at low pressure and high pressure alternately, and the displacer is moved in synchronisation with the operation of the valve. Gas expansion takes in heat from the environment at one end of the cylinder, so one end of the cylinder may be referred to as the cold head, and is cooled to a low temperature. However, it is not always convenient to place the specimen directly in contact with the cold head of a thermo-mechanical cooler. Furthermore, a two-stage Gifford-McMahon cooler may be able to cool a specimen to a temperature as low as 4K, but it is advantageous for at least some applications to provide a further cooling stage to reach even lower temperatures relatively quickly.
WO 2018/172772 A1 describes a cryogenic apparatus in which a first stage of a two-stage Gifford-McMahon cooler is in thermal contact with a copper top plate of a cylindrical intermediate-temperature shield, which also has a base plate. The lower end of the second stage of the Gifford McMahon cooler is in thermal contact with a second, smaller copper top plate of a cylindrical low-temperature shield, which also has a base plate; the intermediate temperature shield being concentric and enclosed within (but spaced-apart from) an outer the low-temperature shield being concentric and enclosed within (but spaced-apart from) an outer cylindrical enclosure and the intermediate-temperature shield being enclosed within (but spaced-apart from) the intermediate-temperature shield. In use, the low-temperature shield is typically at about 4K. A gas flow duct extends coaxially through the low-temperature shield and leads to a concentric cylindrical vessel, enclosed within, but spaced-apart from, the low-temperature shield, and containing liquid helium (in use). The cylindrical vessel is in thermal contact with a copper (top) support plate of a cylindrical operating-temperature shield, which also has a base plate. The operating-temperature shield is typically at about 1K, in use. Perforations are provided in the top plates of the intermediate-, low- and operating-temperature shields, such that when the outer enclosure is evacuated so, too, are the above-mentioned temperature shields. In use, a specimen to be cooled is mounted within the operating-temperature shield, usually on the underside of the top support plate, and is cooled by heat conduction through the support plate to helium within the cylindrical vessel.
A specimen insertion tube or “probe” extends through the top plate of the enclosure to near the bottom of the enclosure. The specimen insertion tube has a removable lid from which extends a support rod (of poor thermal conductivity) having a specimen support plate at its bottom end, to which a specimen can be mounted.
The thermo-mechanical coolers will, in most cases, produce some vibration, whereas in many cases it is advantageous or necessary to inhibit vibration of the specimen, for example, if it is required to perform high-NA (Numerical Aperture) imaging. For this reason, the thermo-mechanical coolers may be mechanically linked to the rest of the apparatus by a vibration-suppressing linkage, such as an edge-welded bellows of stainless steel or bellows of flexible plastic material.
In the described arrangements, although the specimen does not need to be in direct contact with the cold head and additional cooling is provided to facilitate the 1K ‘pot’ or vessel, the 50K, 4K and 1K ‘stages’ are all concentric and arranged about a substantially vertical or upright axis (in use), and insertion of the specimen into the 1K pot is facilitated (from the bottom or the top, depending on the particular configuration of the apparatus) along the same axis. However, this is not always convenient, and it would be desirable to provide a cryogenic apparatus in which (at least) the operating-temperature vessel can be spaced-apart from the longitudinal axis of a cold head of a thermo-mechanical cooler, such that, for example, the operating-temperature vessel can be conveniently mounted, or otherwise supported, on a separate structure, such as an optical table, and the specimen can be mounted in the operating-vessel from the top, rather than the bottom. It would also be advantageous to provide a cryogenic apparatus wherein a specimen can be introduced into, or removed from, the operating-temperature region of a 1K pot, preferably from the top, whilst causing minimal temperature losses, thereby minimising delay and inefficiencies during use.
Aspects of the present invention seek to address at least one or more of these issues.
In accordance with an aspect of the present invention, there is provided a cryogenic apparatus comprising:
The vibration-suppression means may, for example, comprise bellows.
In an embodiment, the cryogenic apparatus may comprise an outer vacuum chamber arrangement comprising a first outer chamber housing said first enclosure with a first circumferential air gap therebetween, a rigid tubular bridge member surrounding said tubular link member with a second circumferential air gap therebetween, and a second outer chamber housing said second enclosure with a third air gap therebetween, wherein the first second and third air gaps together define a fluid flow path, and wherein said thermo-mechanical cooler extends into said first outer chamber which has an evacuation port therein and the apparatus further comprises means for sealing said second outer chamber such that, in use, when air is extracted from said outer vacuum chamber arrangement via said evacuation port and said fluid flow path, a vacuum is created in said first and second enclosures.
In this case, the tubular bridge member may be coupled, via first external vibration-suppressing means, to a first port provided in the first outer chamber; and, optionally, the first outer chamber may comprise a second port and a support arm coupled, at one end via second external vibration-suppressing means, to the second port and, at the other end, to said tubular bridge member at a location along its length.
In an embodiment, the liquid helium delivery assembly may comprise at least one conduit that extends from the thermo-mechanical cooler, through said tubular link member, to said liquid helium containing vessel in said second enclosure. In this case, the liquid helium delivery assembly may comprise two substantially parallel capillaries that extend from said thermo-mechanical cooler, through said tubular link member, to said liquid helium containing vessel; and the liquid helium delivery system may, optionally, comprise a needle valve assembly between each of said capillaries and said thermo-mechanical cooler.
In an embodiment, the cryogenic apparatus may further comprise a generally cylindrical end cap having an opening at one end and being coupled at the other end, via fourth vibration suppressing means, to a fourth port of said connecting device.
In an embodiment, the thermo-mechanical cooler may comprise a two-stage thermo-mechanical cooler, wherein the first enclosure is coupled to a first stage if the thermo-mechanical cooler and the liquid helium delivery assembly is coupled to a second stage of said thermo-mechanical cooler.
The first and second enclosures may beneficially define intermediate-temperature shields and a first plate may be provided over the liquid helium containing vessel to define an operating-temperature region for receiving a sample or specimen, in use.
In an embodiment, the cryogenic apparatus may further comprise a second plate thermally coupled to said second enclosure and proximate to said first plate. The apparatus may, optionally, further comprise a cover for removably covering said first and second plates, in use, and providing an air-tight seal with the second enclosure.
In an embodiment, the cryogenic apparatus may further comprise a removable probe assembly configured to be removably mounted over said second enclosure with an air-tight seal therebetween, the probe assembly comprising a housing configured at one end to provide said air-tight seal and provided, at the other end, with an opening for receiving a probe, in use, for introducing a sample into, or removing a sample from, an operating temperature region proximate to said liquid containing vessel.
In an embodiment, the housing may comprise an elongate, generally tubular member and the probe arrangement may further comprise a tubular duct that extends longitudinally through and along the length of the housing with an annular space defined between the tubular duct and the inner surface of the housing, the distal end of said tubular duct configured to be thermally coupled to said liquid helium containing vessel, in use. The apparatus may, optionally, comprise a first outer chamber within which said first enclosure is located, a second outer chamber within which said second enclosure is mounted and a rigid tubular bridge surrounding said tubular link member, the first and second outer chambers being coupled together by said rigid tubular bridge member and a fluid flow path being defined between said first and second outer chambers via an annular space between said tubular link member and the inner surface of the rigid tubular bridge, wherein, when said housing is mounted and sealed over said second outer chamber, said annular space is in fluid communication with said fluid flow path such that, in use, when air is extracted at the first outer chamber, the first and second outer chambers and the annular space between the tubular duct and the housing is evacuated.
In an embodiment, the apparatus may comprising an elongate probe configured to extend into said tubular duct through said opening, the probe comprising a plurality of spaced apart baffles of substantially equal diameter to the inner diameter of the tubular duct.
An isothermal shield may, beneficially, be provided around an end of the tubular duct nearest the end configured to provide said air-tight seal, the isothermal shield comprising a tubular sheath around said tubular duct and having a thermal link to said tubular duct at one end and being configured to be thermally coupled to said second enclosure, in use.
A gas curtain assembly may, optionally, be mounted around said opening, said gas curtain assembly being configured to introduce helium gas into said housing so as to prevent ingress of air to the sample space.
At least one viewing window may, beneficially, be provided in each of the isothermal shield and the tubular duct, near the second enclosure, when in use, the viewing windows being horizontally aligned when the apparatus is oriented for use, such that a specimen mounted on the probe within the tubular duct can be viewed.
In an embodiment, the probe may comprise a conductor housing at its distal end, the conductor housing including one or more wiring ports configured to enable diagnostic wiring to be connected thereto, in use.
These and other aspects of the invention will be apparent from the following Detailed Description.
Embodiments of the present invention will now be described, by way of examples only, and with reference to the accompanying drawings, in which:
Directional descriptors, such as upper, lower, left, right, clockwise, anti-clockwise, front, rear and other similar adjectives are used for clarity and refer to the orientation of the invention as illustrated in the drawings; however, it will be clear to those skilled in the art that the invention may not always be oriented as illustrated and the invention is not intended to be limited in this regard.
Referring to
Referring additionally to
A pair of parallel, spaced-apart link intermediate-temperature link plates 37 extend downward from the lower surface of the copper top plate 30 to a base plate 38. Thus, the link plates 37, which are thermally coupled to the top plate 30 that is in thermal contact with the first stage of the cryocooler 22, act as intermediate-temperature links between the first stage of the cryocooler 22 and an intermediate-temperature (copper) shield 512 within the bridge 504, as will be described in more detail hereinafter.
An intermediate wall 402 extends between the intermediate-temperature link plates 37 (parallel to, and longitudinally spaced apart from, the base plate 38) to define an upper region 403 and a lower region 404. Referring also to
A first vibration-suppressing means (e.g. bellows) 408 is provided at the connection between the gas flow duct 40 to the intermediate wall 402 which forms the top plate of the lower region 404 between the intermediate-temperature link plates 37. A similar vibration-suppressing means (e.g. bellows 409 anchors the longitudinally (i.e. vertically) opposite port 405b of the cross fitting 405 to the base plate 38 at the base of the lower region 404 between the intermediate-temperature link plates 37.
One of the orthogonal ports 405c is coupled to a cylindrical end cap 79 (see
Referring additionally to
Referring back to
The second outlet port 502a of the enclosure 12 is coupled to one end of a rigid support arm 505 via a similar vibration-suppressing means (e.g. bellows) 506, the other end of the support arm 505 being bolted (or otherwise connected) to the rigid bridge 504.
Within the operating-temperature shield 45 there is provided a generally cylindrical vessel 42 comprising a cylindrical wall 46, extending ‘downward’ from the copper top plate 41, and a base plate 48. Thus, the thermally conductive top plate 41 of the operating-temperature assembly 24, which covers the operating-temperature shield 45 and the vessel 42, is thermally coupled to the intermediate-temperature (first) stage of the cryocooler assembly 11 via the thermally conductive tube 512 and washer 504a, the thermally-conductive tube 512 being thermally coupled, at one end, to an intermediate-temperature link plate 37 (of the cryocooler assembly 11) and, at the other end, via a thermally conductive washer 504a, to the copper top plate 41 of the operating temperature shield 45. The cylindrical vessel 42, in use, contains liquid helium.
Referring back, once again, to
This helium flow is brought about by a pump (not shown) which can extract helium gas from a return gas flow via the gas flow duct 40, and supply it to the reservoir. The pressure at the exit of the gas flow duct 40 may, for example, be less than 10 Pa (about 1 mbar) so that the liquid helium in the cylindrical vessel 42 evaporates below its normal boiling point, taking its latent heat from its surroundings, and in particular the copper support plate 41 (and hence from a specimen placed thereon or in close proximity thereto). The return helium gas flow is by way of the copper tube 512 to the gas flow duct 40.
Thus, as explained above, the cylindrical vessel 42 (containing liquid helium) is contained within a cylindrical operating temperature shield 45 which is typically about 1K, in use. The operating-temperature shield 45 and the vessel 42 are provided in a receptacle or ‘pot’ 43. The copper top plate 41 is an intermediate-temperature (e.g, ˜50K) plate. A second top plate 46a is provided over the cylindrical vessel 42 and is an operating-temperature (e.g. ˜1K) plate defining the surface or region by or on which a specimen or sample can be placed, in use. A removable cover (not shown) may be provided for covering the sample and receptacle 43 in use, and the cover may have ‘windows’ or viewing ports in its side walls to allow for viewing or imaging of the specimen or sample situated in or on the operating-temperature region.
As described above, the cryocooler 22 in this embodiment may be a two-stage Gifford-McMahon cooler, which uses high pressure helium at a pressure typically between 10 bar and 30 bar as the working fluid, in a closed circuit. The working fluid is provided by one or more external compressors (not shown). Each stage of the cryocooler 22 includes a cylinder with a movable displacer and a rotary valve to connect the cylinder alternately to high pressure and low pressure, and a mechanism to move the displacer(s) in synchronisation with the movement of the valve. Such coolers are commercially available products (e.g. Sumitomo Heavy Industries) and their details are not the subject of the present invention. Since the cryocooler 22 includes moving parts which operate typically at a frequency of about 1 Hz, the components that are subject to oscillation are isolated from the rigid bridge 504 by the respective arrangements of vibration-suppressing bellows 503, 506 and 408, 409, 410, 411 at the outlet ports 502a, 502b of the enclosure 12 and the ports 405a, 405b, 405c, 405d of the cross fitting 405 in the lower region 404 between the intermediate-temperature link plates 37. In use, liquid helium from the second stage of the cryocooler 22 is fed (via the capillaries 76b, 77b) to the cylindrical vessel 42 within the operating-temperature shield 45 of the receptacle or ‘pot’ 43. The copper tube 512 running through the rigid bridge 504 is thermally linked to the intermediate-temperature (e.g. 50K) link plates 37 such that it acts as an intermediate-temperature shield within the bridge 504. The return helium gas flow (described above) is via the same copper tube 512, which acts to help to maintain the temperature of the shield provided by the copper tube 512 such that no additional cooling thereof is required. Any vibration from the pump (not shown) in the operating-temperature assembly 11 is suppressed at the vibration-suppressing means 411 between the copper tube 512 and the port 405d of the cross fitting 405. Helium gas thus returned can be fed back to the second stage (not directly) of the cryocooler 22, which cools the helium to about 4K (liquid helium) and it can be fed back through the needle valve assembly 50 and capillaries 76b, 77b to the cylindrical vessel 42 in the operating-temperature assembly 24. A superconducting magnet can be incorporated in the sample plate 46a in some embodiments.
In use, and with the cover removed from the 1K receptacle 43, a specimen or sample may be placed on or near the copper top plate 46a and the cover (not shown) replaced such that there is an air tight seal between the cover and the receptacle 43. Then, the apparatus can be commissioned; first, by evacuating the enclosure 12, thereby evacuating the intermediate-temperature shield 32 and the intermediate-temperature shield 45 (via the bridge 504) and then starting the cooling process described above using the two-stage cryocooler and the liquid helium delivery system. In order to remove the specimen or sample, the cooling is switched off and the system warmed up. The cover can then be removed (thereby breaking the vacuum) and the sample or specimen accessed.
Referring back to
The lower portion of the OVC 902 having a larger diameter includes viewing ports 924. Within the OVC 902, there is a tubular duct 904 that extends concentrically and longitudinally through the OVC 902 and is in thermal communication at its ‘bottom’ end with the operating temperature (˜1K) support plate 46a. An intermediate-temperature shield 922 is mounted around the ‘lower’ end of the duct 904, with the lower end 922a being of a diameter substantially equal to the intermediate-temperature (˜50K) plate 41 and being bolted (or otherwise affixed) thereto such that they are thermally coupled. The intermediate-temperature shield 922, which may, for example, be formed of thin copper, narrows along its length and terminates about half way up the length of the duct 904. The lower, larger diameter portion of the intermediate-temperature shield 922 has viewing ports 926, wherein the viewing ports 924 of the OVC 902 and the viewing ports 926 of the intermediate-temperature shield 922 are aligned with similar viewing ports in the duct 904 to provide a clear optical path such that viewing or imaging of a sample located in the 1K region is facilitated. There is a thermal link 907 between the upper edge portion of the tubular intermediate-temperature shield 922 and the adjacent outer surface of the duct 904. Helium gas can be pumped into the OVC 902 via the inlet port 918 of the gas curtain assembly 903 to lower the temperature therein. The intermediate-temperature shield 922 acts as a “thermal intercept” along the length of the probe arrangement 900 such that the temperature in the duct 904 is ˜300K at the ‘upper’ end (adjacent to the gas curtain arrangement 903) and ˜50K at the top of the intermediate-temperature shield 922. Then there is a temperature gradient along the length of the duct 904, within the intermediate-temperature shield 922, from 50K at the top of the intermediate-temperature shield 922 to ˜1K at the operating temperature support plate 46a. This is highly efficient, especially when inserting a specimen into, or removing a specimen from, the operating-temperature region of the 1K pot 43, as described below.
A probe 906 is provided with a series of concentric baffles 908, spaced apart long its length, and a sliding seal flange 910 is provided close to the top of the probe 906 (when oriented for use). A conductor housing 912 is provided at the proximal (top) end of the probe 906 and a specimen mounting plate 914 is provided at the opposing distal (bottom) end. The conductor housing may include a number of wiring ports 916 to enable diagnostic wiring (and the like) to be connected. The gas curtain arrangement 903 incorporates a gas relief valve 918 and, in use, when the enclosure 12 is evacuated, so too is the operating-temperature assembly (via the tubular bridge 504). In use, the gas relief valve 918 can be used to release the vacuum and allow the probe to be removed from and inserted into the housing 902 so as to mount or remove a specimen relative to the support plate 46a, without having to stop and warm up the entire apparatus every time.
Referring to
It will be apparent to a person skilled in the art, from the foregoing description, that modifications and variations can be made to the described embodiments without departing from the scope of the invention as defined by the appended claims. For example, the apparatus may include other components, for example, a superconducting electromagnet to enable the specimen to be subjected to a magnetic field. The apparatus may also include sensors for a variety of parameters such as temperature and pressure within the helium recirculation path; and sensors (e.g. via the probe) for properties of the specimen.
Number | Date | Country | Kind |
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2015839.0 | Oct 2020 | GB | national |
Filing Document | Filing Date | Country | Kind |
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PCT/GB2021/052565 | 10/5/2021 | WO |