Patent Publication Number: US-2022212196-A1

Title: Variable Temperature Analytical Instrument Assemblies, Components, and Methods for Providing Variable Temperatures

Description:
RELATED PATENT DATA 
     This application claims priority to U.S. Provisional Patent Application Ser. No. 62/840,101 filed Apr. 29, 2019, entitled “Variable Temperature Analytical Instrument Assemblies, Components, and Methods for Providing Variable Temperatures”, the disclosure of which is incorporated by reference herein. 
    
    
     TECHNICAL FIELD 
     The present disclosure relates to variable temperature analytical instrumentation and methods, more particularly, to variable temperature analytical methods that utilize low Kelvin temperatures, as well as sample support assemblies and methods. 
     BACKGROUND 
     It is increasingly important to be able to change the temperature of a sample being analyzed rapidly and to be able to move between different samples analyses rapidly. The state of the art provides sample analysis support systems that require lengthy times to change temperatures within the systems which can lead to lengthy times to perform analysis and accordingly lengthy times to provide analytical results. For example, where one is going to perform low Kelvin analyses, they are required to first provide the sample and then over hours of time reduce the temperature of the analyte in order to perform the analysis. The present disclosure addresses shortcomings of the prior art and provides variable temperature sample support and methods for use in variable temperature instrumentation. 
     SUMMARY 
     Variable temperature analytical assemblies are provided that can include a first mass configured to be maintained at variable temperatures and a second mass moveable between a first position and a second position. The first position can be thermally disengaged from the first mass and the second position can be thermally engaged to the first mass. 
     Methods for changing temperatures of a mass are provided with the methods including providing a first mass and moving a second mass between one of at least two positions to thermally engage the first mass. 
     Low thermal conductance components are also provided that can include a central hub and at least a pair of spokes extending from the central hub. The pair of spokes can support the central hub and have ends configured to mount to a support structure. 
     Low thermal conductance assemblies are also provided that can include a thermally adjustable mass coupled to a cold source as well as thermally insulated members coupled to the mass and thermally insulating the mass from the cold source. The assembly can include one or more flexure bodies defined within the mass and configured to couple with the thermally insulative members. 
     Methods for thermally isolating a mass from a support structure are provided with the methods including resting a thermally conductive mass upon a central hub supported by at least two spokes extending to a support structure. 
     Variable temperature analytical assemblies are also provided that can include a support structure about a first mass and a central hub supporting the first mass and at least a pair of spokes extending from the central hub to engage the support structure. 
     Variable temperature analytical assemblies are also provided that can include a first mass configured to be maintained at variable temperatures and a thermal link extending from a variable temperature assembly. 
    
    
     
       DRAWINGS 
       Embodiments of the disclosure are described below with reference to the following accompanying drawings. 
         FIG. 1  is a top view depiction of a variable temperature analytical assembly according to an embodiment of the disclosure. 
         FIG. 2  is variable temperature assembly according to an embodiment of the disclosure. 
         FIG. 3  is another variable temperature assembly according to an embodiment of the disclosure. 
         FIG. 4  is the variable temperature assembly of  FIG. 3  in one orientation according to an embodiment of the disclosure. 
         FIG. 5  is the variable temperature assembly of  FIG. 4  in another orientation according to an embodiment of the disclosure. 
         FIG. 6  is a view of a variable temperature assembly according to an embodiment of the disclosure. 
         FIG. 7  is at least one cross sectional view of the variable temperature assembly of  FIG. 6  according to an embodiment of the disclosure. 
         FIG. 8A  is a perspective view of internal components in alignment with the housing of the variable temperature assembly of  FIG. 6  according to an embodiment of the disclosure. 
         FIG. 8B  is a perspective view of the internal components of the variable temperature assembly of  FIG. 6  without the housing according to an embodiment of the disclosure. 
         FIG. 9A  is a partial cutaway view of the variable temperature assembly of  FIG. 6  according to an embodiment of the disclosure. 
         FIG. 9B  is another partial cutaway view of the variable temperature assembly of  FIG. 6  according to an embodiment of the disclosure. 
         FIG. 10  is a cross sectional view of another variable temperature assembly according to an embodiment of the disclosure. 
         FIG. 11  is a top view of a component of a variable temperature assembly according to an embodiment of the disclosure. 
         FIG. 12  is another view of the variable temperature assembly of  FIG. 11  according to an embodiment of the disclosure. 
         FIG. 13  is a cross sectional view of a component of a variable temperature assembly according to an embodiment of the disclosure. 
         FIG. 14  is a top view of a component of a variable temperature assembly according to an embodiment of the disclosure. 
         FIG. 15  is a depiction of a variable temperature assembly in thermal connection with an analytical component. 
         FIG. 16  depicts a variable temperature assembly in thermal connection with a sample analysis assembly according to an embodiment of the disclosure. 
         FIG. 17  depicts the assemblies of  FIG. 16  in one orientation according to an embodiment of the disclosure. 
         FIG. 18  depicts the assemblies of  FIG. 16  in another orientation according to an embodiment of the disclosure. 
         FIG. 19  depicts a cold source in relation to another mass according to an embodiment of the disclosure. 
         FIG. 20  depicts a cold source in relation to another mass according to an embodiment of the disclosure. 
         FIG. 21  depicts a cold source in relation to a mass in accordance with another embodiment of the disclosure. 
         FIG. 22  depicts a cold source in relation to a mass in accordance with another embodiment of the disclosure. 
         FIGS. 23A   1  through  23 A 21  depict different arrangements of an analytical component according to an embodiment of the disclosure. 
         FIGS. 24A   1  through  24 A 14  depict different arrangements of an analytical component according to an embodiment of the disclosure. 
         FIGS. 25A   1  through  25 A 4  depict different side elevations of an analytical component according to an embodiment of the disclosure. 
         FIG. 26  depicts a supported mass in relation to a temperature source according to an embodiment of the disclosure. 
         FIG. 27  is a more detailed view of a portion of the supported mass of  FIG. 26  according to an embodiment of the disclosure. 
     
    
    
     DESCRIPTION 
     The present disclosure will be described with reference to  FIGS. 1-27 . Referring first to  FIG. 1 , a conceptual embodiment of a variable temperature analytical assembly  10  is shown in  FIG. 1 . Component  10  can include a base  12 . This base can be thermally connected to a cold source. A cold source can include a mass or masses or a liquid or gas that holds an amount of heat that is less than the mass or masses or surroundings engaged with the cold source. For example, in certain configurations, a mass may be coupled to a nitrogen source or a helium source under vacuum, and under this vacuum in engagement the mass may have a temperature that is in the low Kelvin range up to and including the 4 Kelvin range. 
     Component  10  can also include a thermal standoff  14 . Thermal standoff  14  can be material that is a poorly thermal conducting material providing a thermal barrier to base or cold source  12 . Component  10  can also include another mass  16  that may be considered a sample mount but may be configured to have the temperature of the mass adjusted variably between ranges, for example, between 4 Kelvin and 1000 Kelvin in accordance with embodiments of the present disclosure. Thermal standoff  14  may support mass  16  or insulate mass  16  from base or mass  12 . 
     Referring next to  FIG. 2 , a variable temperature assembly  20  is depicted that includes a first mass  22  associated with a second mass  24 . First mass  22  can be configured to be maintained at variable temperatures and second mass  24  can be moveable between a first position and a second position with the first position being thermally disengaged from the first mass and the second position being thermally engaged to the first mass. Second mass  24  can be associated with a cold source  26  which may take the form of a mass as shown, or may be associated with a cold source  26  via a link  25 . 
     Referring next to  FIG. 3 , a variable temperature assembly  30  is shown. Component  30  can include a cold source or base  31  that can be maintained at very low temperatures and having very little heat. In relation to cold source  31  can be a first mass  33 . First mass  33  can be configured as a sample mount, for example. Also, first mass  33  can be configured to couple and link to other sample analysis components as desirable and described in more detail later. First mass can be constructed of copper, molybdenum, titanium, and/or aluminum for example. 
     As shown in  FIG. 3 , first mass  33  is represented as a block. 
     However, other configurations such as posts or even links or link couplings are contemplated. In relation to first mass  33  can be a second mass  36 . Second mass can be constructed of copper, molybdenum, titanium, and/or aluminum for example. Second mass  36  may be referred to as a toggling member. Second mass  36  is moveable in relation to first mass  33 . 
     In accordance with example implementations, first mass  33  may be coupled to an electrode  35   b  and cold source  31  may be coupled to an electrode  35   a . The electrodes may be constructed of gold coated sapphire and/or copper for example. Each of these electrodes may be set off from each of the masses via an electrical isolator or insulator  34 . The insulators may be constructed of sapphire, alumina, and/or mica for example. In accordance with example implementations, a flexure member  37  may extend from the second mass to a structure  38 . Structure  38  may be a part of cold source  31  or a supporting structure or housing structure about component  30 . 
     Flexure member  37  can be configured to allow second mass  36  to move between at least two positions; one in thermal connection with first mass  33  and another in thermally disconnection from first mass  33 . Member  37  can be constructed of copper and/or Titanium for example. Member  37  is shown extending to housing  38 . In alternative embodiments, member  37  can extend to standoffs or struts  32  as shown in  FIGS. 7-8B . In other embodiments, member  36  is moveable between the two positions without member  37 . For example, member  36  is aligned within a constraint such as a guide structure, not shown. 
     In accordance with example implementations, second mass  36  can include thermally conductive members  39  configured to thermally engage cold source  31  or first mass  33 . Members  39  can be constructed of gold coated sapphire for example. Supporting first mass  33  can be thermal standoffs  32 . Standoffs  32  can be constructed of Macor®, zirconia, and/or titanium for example. Supports, standoffs, or struts  32  can be tubular in construction and/or hollow as well. In this shown configuration, struts  32  support mass  33  while extending horizontally from cold source  31 . In  FIGS. 7-8B , this strut is shown engaging mass  33  at flexure bodies  64 . 
     Electrodes  35   b  and  35   a  and/or second mass  36  may have electrical potentials provided thereto. In accordance with example implementations, the electrical potentials can be varied, but they can also be sufficiently different to provide for the movement of mass  36  between at least one of two positions. Dielectric washers  40  can be provided about thermally conductive members  39  about member  36 . In accordance with example implementations these washers can be constructed of polyimide (Kapton), PTFE (Teflon), PEEK, sapphire, and/or MICA and can be configured to prevent high voltage arcing. 
     One of the two positions can be in thermal engagement as shown in  FIG. 4  and represented as variable temperature assembly  30   a  in the on or thermally engaged position, and the other of the two positions can be thermally disengaged as shown in the orientation of assembly  30   b  in  FIG. 5 . In the first position the spacing is sufficient to provide for thermal engagement of mass  36  to mass  33 . For purposes of description, while thermally engaged with mass  33 , mass  36  appears disengaged with source  31 , this is not necessarily the case as the thermal engagement between all three of these elements may be maintained when mass  36  is engaging mass  33 . However, as shown in  FIG. 5 , when mass  36  is disengaged with mass  33 , these masses are thermally disconnected. 
     Referring next to  FIG. 6 , a variable temperature assembly  60  is shown and will be further depicted via cross sections and cutouts in views as shown in  FIG. 7 through 9B . Assembly  60  can be configured to have a variable temperature sample support as first mass  33 , and this variable temperature sample support can be configured to be heated via irradiative exposure, solid state conductance, and/or charged particle bombardment. In this particular embodiment, the sample support or first mass  33  can be heated via solid state conductance. Accordingly, mass  33  is configured to house a heater within a flexure body  62 . Mass  33  can also extend to be supported by standoffs  32  and connect with standoffs  32  via additional flexure bodies  64 . Coupled within metal electrode  35   b  can be wiring  51   b , and coupled within metal electrode  35   a  can be wiring  51   a . Coupled within mass  36  can be electrical wiring  51   c . Wiring  51   a ,  51   b , and/or  51   c  can be manipulated to provide different voltages between one or more of the electrodes  35   a ,  35   b , and mass  36  to facilitate the movement of mass  36  in relation to mass  33 . 
     Referring to  FIGS. 9A and 9B , heater  102  is shown operatively engaged with mass  33  and with a flexure body  62 . Temperature probe  104  is also shown operatively engaged within mass  33 . 
     Referring next to  FIG. 10 , a variable temperature assembly  110  is shown that provides additional detail to mass  36  having a flexure body supporting thermally conductive masses  39 . Additionally, component  110  provides an alternative member structure  37  representing a platform rather than the strutted flexure members of component  60 . 
     Referring next to  FIG. 11 , a more detailed view of mass  33  is provided to depict flexure body structures as well as openings for heater and/or temperature gauge elements. In accordance with example implementations and with reference to  FIGS. 11 and 12 , mass  33  can include additional structures such as supports  130  which can be operatively engaged with a standoff member, for example, and this operable engagement can extend via arm  132  to central body  134 . Within arm  132  or extension  130  can be flexure bodies  64 . These flexure bodies can be intentional recesses within arm  132  or member  130  that allows for the rapid expansion and contraction of mass  33  when moving between variable temperature ranges that include between 4 Kelvin and 1000 Kelvin. These recesses can extend from one edge of arm  132 , for example, to an opposing edge, and then provide a discrete opening within the arm, thus allowing for more surface area for expansion and contraction during heat shifts. Not unlike flexure member  64 , flexure member  62  can include buttresses  136  that are biased to support a heating element or temperature probe and allow for the conductance of the heating element to extend to mass  33  while allowing for the expansion and contraction of mass  33 . Accordingly, flexure body  62  can be configured as shown in a circular fashion with buttresses  136  about a cylindrical opening  138  that incudes surrounding recesses within mass  33 . 
     Referring next to  FIG. 13 , a more detailed view of an embodiment of mass  36  is shown in a cross section with flexure body  62  about a thermally conductive assembly that includes thermally conductive components  39  embracing a central portion of mass  36 . These flexure members also include buttresses  136  biases against a flexible portion residing between openings  137   a  and  137   b.    
     As shown in  FIG. 14 , conductive mass  33  is supported by members within mass  36  to allow for the rapid expansion and contraction of component  39  as it engages and disengages mass  33 . Because of the rapid temperature change, the flexure bodies can allow for the expansion and contraction of the mass without subsequently damaging the mass or component  39 . As shown, there are buttress portions to flexure body  62  that are also biasly engaged within recessed openings of mass  36 . 
     Referring next to  FIG. 15 , and in accordance with another example implementation, an analytical assembly  150  is provided that includes variable temperature assembly  152  operatively engaging a sample analysis component  154 . The operable engagement between these two components can be via a thermal link, for example; however, other operable thermal engagements are contemplated. 
     Referring next to  FIG. 16 , the assembly of  150  is shown in accordance with another embodiment of the disclosure. Referring to  FIG. 16 , assembly  150   a  can include a variable temperature assembly  152   a  that includes a first mass  33  in operable association with a second mass  36  as described herein. Second mass  36  may be in association with a cold source  31  via a link, for example, and/or via operable association as described herein. Standoffs  32  can provide the thermal disconnection between mass  33  and cold source  31 . Mass  33  may be thermodynamically coupled to sample analysis component  154   a  via a link  156 , for example. Analysis component  154   a  may include a first mass  163  that can be coupled to a heater component  172  and/or a sensor component  174 . Mass  163  can be thermally disassociated from a base portion  161  via thermal standoffs, supports, or struts  162 , and base  161  may also be configured to be a cold source as well. In accordance with example implementations, both  154   a  and  152   a  may include cold sources of different temperatures, thereby providing the ability to move between different lower temperatures at a more rapid rate. Accordingly, source  161  may be thermally linked to mass  163 , for example. 
     Referring to  FIGS. 17 and 18 , assembly  150   a  is shown in two different operable orientations, one where thermal engagement is provided in  FIG. 17 , and one where there is no thermal engagement as shown in  FIG. 18 . With particular reference to  FIGS. 17 and 18 , a thermal link is provided between member  36  and cold source  31 , for example. 
     Referring next to  FIGS. 19-22 , analytical component configurations are shown depicting various arrangements of first and second masses. Referring first to  FIG. 19 , a first mass  193  is shown in relation to a second mass  191 . In accordance with these embodiments, a second mass  191  can be a cold source mass and may be fixed in position, for example. Referring to  FIG. 20 , mass  193  can be supported by standoffs, supports, or struts  192   a  above cold source  191 . These standoffs, supports, or struts  192   a  can be tubular and/or hollow as well as ceramic, for example, and provide thermal insulation between cold source  191  and mass  193 . Referring next to  FIG. 21 , in accordance with an alternative embodiment, cold source  191  can support mass  193  via a hub and spoke construction  192   b . This hub and spoke construction will be described further later in the specification. As can be seen, mass  193  is thermally linked to cold source  191 . As shown, cold source  191  may extend up and provide a housing or support structure for hub and spoke structure  192   b  as well as mass  193 . It is not necessary that it extend and provide the housing or the structure; the structure can be independent and even insulated from cold source  191 , and the structure may form all or part of a housing for the analytical component as desired. Referring next to  FIG. 22 , a strut configuration  192   c  is used to support mass  193  in relation to cold source  191 . These struts can be laminate fiberglass struts such as G10 struts, for example. 
     Referring next to  FIGS. 23A   1 - 25 A 4 , various configurations of a hub and spoke support assembly are shown in different embodiments. In these embodiments, at least one hub  224  can exist in a circular fashion, for example, having spokes  223  extending therefrom. These spokes can extend and be configured to terminate to be coupled with a support structure, such as the support structures described herein. Hub  224  can be configured to support a mass such as a sample support mass or mass  33  as described herein. In accordance with example implementations, these sample analysis components can include a built frame  225  or may exist without a frame. In accordance with example implementations, various embodiments of this hub and spoke structure are depicted with reference to  FIGS. 23A   1  through  23 A 21 . In accordance with example configurations, multiple hubs may be provided and including additional concentric hubs about a central hub. 
     Referring next to  FIG. 24A   1  through  24 A 14 , additional alternative embodiments of the hub and spoke structure are provided where the spokes are not linearly aligned, but juxtaposed as in contrast to the structures shown in  FIGS. 23A   1  through  23 A 21 . With reference to  FIGS. 25A   1  through  25 A 4 , side views of the hub and spoke structure are shown to indicate that it may be desirable to have the spokes biased in a certain manner to allow for the hub to be above a horizontal plane in accordance with multiple implementations in  FIGS. 25A   1  through  25 A 4 . 
     Referring next to  FIGS. 26 and 27 , a standoff, support, or strut  262  is shown engaging a mass  33  at flexure body  62  providing within mass  33  about the engagement of mass  33  and strut  262 . Again strut  262  can be tubular or hollow and, in this configuration with the housing lateral of mass  33 , strut  262  can extend horizontally from the housing to engage mass  33 . A more detailed view of this configuration is shown in  FIG. 27  from a perspective cross section, demonstrating that strut  262  in a hollow configuration in some perspectives as well as can be supported by a housing or exterior support structure, but also engaging mass  33 .