VARIABLE GAP THERMAL CONDUCTIVITY APPARATUS AND METHOD

Abstract

An apparatus and a method for determining the thermal conductivity of a fluid specimen are provided. The apparatus and the method include determining thermal conductivity using a quasi-steady state variable gap axial flow technique. The fluid specimen is heated on one side by a heat source with a known power output and cooled on the other side. After reaching steady state, a resulting temperature drop through the fluid specimen exists. This temperature drop, the known fluid specimen thickness (or gap distance), and the known power output are used to calculate the thermal resistance of the fluid specimen. The thermal conductivity of the fluid specimen is then determined using a curve fit of thermal resistance with respect to gap distance.

Claims

1. An apparatus for measuring thermal conductivity of a fluid specimen, the apparatus comprising: a test chamber to be at least partially enclosed in a furnace that is maintained at a predetermined temperature, the test chamber having a solid base and a solid wall arranged to hold the fluid specimen on a flat surface of the base, wherein the base comprises: cooling channels disposed inside the base at a predetermined distance from the flat surface of the base, the cooling channels configured to cool a first side of the fluid specimen adjacent to the flat surface of the base, and a first set of one or more temperature sensors disposed inside the base and distributed between the flat surface of the base and the cooling channels, the temperature sensors of the first set configured to sense a temperature of the first side of the fluid specimen and configured to sense a temperature through the base; and a moveable head having a flat surface, the head disposed inside the test chamber such that the flat surface of the moveable head is parallel to and spaced apart by a controllable gap from the flat surface of the base, such that the fluid specimen fills the gap, the head comprising: a heater module disposed inside and adjacent to the flat surface of the head, the heater module configured to heat a second side of the fluid specimen, opposite of the first side of the fluid specimen, adjacent to the flat surface of the head, and a second set of one or more temperature sensors disposed inside the head and distributed along the flat surface of the head, the second set being configured to sense a temperature of the heated second side of the fluid specimen.

2. The apparatus of claim 1, further comprising: an actuator module mechanically coupled with the movable head to cause, during operation of the apparatus, the head to move relative to the flat surface of the base to modify the gap between flat surface of the head and the flat surface of the base; and a distance sensor configured to measure a size of the gap between the flat surface of the head and the flat surface of the base.

3. The apparatus of claim 2, wherein the actuator module is configured to modify the size of the gap over a range of 0.01 mm-25 mm.

4. The apparatus of claim 2, wherein the actuator module is configured to modify the size of the gap in increments of 5 μm to 10 μm.

5. The apparatus of claim 1, wherein the temperature sensors comprise one or more of thermocouples, fiber optic-based temperature sensors, RTDs, or pyrometers.

6. The apparatus of claim 1, wherein the heater module comprises one or more of: one or more loops of sheathed resistance wire; or one or more ceramic heaters.

7. The apparatus of claim 1, wherein the moveable head includes a radial guard heater contained therein.

8. The apparatus of claim 1, wherein the fluid specimen comprises molten salt, molten glass, molten ceramic, molten metal, or a molten metal alloy.

9. The apparatus of claim 1, wherein the test chamber is sealed from an ambient environment, wherein the fluid specimen is reactive with gas from the ambient environment.

10. The apparatus of claim 2, further comprising: a controller module communicatively coupled with the actuator module, a distance sensor, the heater module, and the first and second set of temperature sensors, the controller module configured to: a) determine a heater power (Q) based on a configuration of the heater module, b) instruct the actuator module to translate the movable head to set the gap between the flat surface of the head and the flat surface of the base to a sequence of different gap sizes, c) for each gap size from among the different gap sizes, obtain the gap size from the distance sensor and determine a temperature difference (dT) between the heated-side temperature obtained from the temperature sensors of the second set, and the cooled-side temperature obtained from the temperature sensors of the first set, and d) determine the thermal conductivity of the fluid specimen based on the determined temperature differences for the corresponding gap sizes.

11. The apparatus of claim 10, wherein, to determine the thermal conductivity of the fluid specimen, the controller module is configured to: determine thermal resistances (R) as the respective temperature differences multiplied by an area of the heater (A) is divided by the heated power (R=dT/Q/A), and fit the determined thermal resistances for the corresponding gap sizes using a least square fit, and estimate the thermal conductivity of the fluid specimen from the fit.

12. A system comprising: the apparatus of claim 10; and a furnace at least partially enclosing the apparatus, the furnace being maintained at the predetermined temperature.

13. The system of claim 12, wherein the controller module is configured to: set the predetermined temperature of the furnace enclosure to a sequence of different furnace-enclosure temperatures; and determine a steady-state thermal conductivity of the fluid specimen as a function of furnace-enclosure temperature by iterating operations a) through d) for each furnace-enclosure temperature from among the different furnace-enclosure temperatures.

14. The system of claim 12, wherein the controller module is configured to: cause a temperature transient to the furnace enclosure, and determine a transient-mode thermal conductivity of the fluid specimen by iterating operations a) through d) during the furnace enclosure temperature transient.

15. A method for measuring the thermal conductivity of a fluid specimen, the method comprising: providing the apparatus of claim 1; adjusting the gap between the flat surface of the head and the flat surface of the base through a plurality of gap distances; for each of the plurality of gap distances, determining a heat flux and a temperature difference across the fluid specimen; determining the thermal resistance of the fluid specimen based on the determined heat flux and the temperature difference for each of the plurality of gap distances; and determining the thermal conductivity of the fluid specimen based on the thermal resistance of the fluid specimen for each of the plurality of gap distances.

16. The method of claim 15, wherein determining the thermal conductivity of the fluid specimen includes using a curve fit of the thermal resistance with respect to gap distance.

17. The method of claim 15, wherein adjusting the gap through a plurality of gap distances includes adjusting the gap in intervals of between 5 μm to 10 μm.

18. The method of claim 15, wherein adjusting the gap through a plurality of gap distances is performed over a range of 0.01 mm-25 mm.

19. The method of claim 15, wherein the steps of determining the heat flux and the temperature difference, determining the thermal resistance, and determining the thermal conductivity are performed by a controller module in digital logic.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

[0011] FIG. 1 is a perspective view of test apparatus for determining the thermal conductivity of a fluid specimen.

[0012] FIG. 2 is a cross-sectional view of test apparatus of FIG. 1 for determining the thermal conductivity of a fluid specimen.

[0013] FIG. 3 is a close-up cross-sectional view of a moveable heater cell within the test apparatus illustrated in FIG. 2.

[0014] FIG. 4 is a close-up view of a variable gap between a movable head within a test chamber of the test apparatus of FIG. 1.

[0015] FIG. 5 is a graph of temperature drop versus time for five gap distances using the test apparatus of FIG. 1.

[0016] FIG. 6 is a graph of thermal resistance versus gap distance for eleven gap distances using the test apparatus of FIG. 1.

DETAILED DESCRIPTION OF THE CURRENT EMBODIMENTS

[0017] The current embodiments include an apparatus for determining the thermal conductivity of a fluid specimen using a variable gap axial flow technique. As discussed below, the fluid specimen is heated on one side by a heat source with a known power output and cooled on the opposite side. The power output, the temperature drop across the fluid specimen, and the fluid specimen thickness are used to calculate its thermal resistance. The thermal conductivity of the fluid specimen is then determined using a curve fit of thermal resistance with respect to gap distance. Though primarily described below in connection with molten salts, the apparatus is also well suited for measuring the thermal conductivity of other fluid specimens, including for example molten glass, molten metals, molten ceramics, and high temperature gases.

[0018] Referring first to FIGS. 1-3, an apparatus in accordance with one embodiment is illustrated and generally designated 10. The apparatus 10 includes a cylindrical outer housing 12 and an upper flange seal 14 that cooperate to define an enclosure for a movable stem 16. The moveable stem 16 includes, at its lowermost portion, a heater cell 18 comprising a disc-shaped head 30 with at least one internal heating element 20. The moveable stem 18 includes an upper portion 22 and a lower portion 24 that are coupled together at a flange joint 26, such that the lower portion 24 can be replaced without requiring replacement of the upper portion 22. The stem 18 is movable under control of an actuator module 23, for example a linear or rotary actuator. The actuator module 23 is secured to a retaining plate 25 that is bolted to the upper flange seal 14. The cylindrical housing 12 is surrounded by a furnace 28, for example a clamshell furnace, the furnace 28 elevating the temperature of the fluid specimen to greater than 500° C., for example at least 900° C.

[0019] As shown in FIG. 3, the heater cell 18 is contained within a test chamber 32. The test chamber 32 includes an annular sidewall 34 and a base 36. The inner-facing surface 38 of the sidewall 34 and the upward-facing surface 40 of the base 36 define an enclosure 42 for both the heater cell 18 and a fluid specimen. The inner diameter of the annular sidewall 34 is greater than the outer diameter of the heater cell 18, such that a clearance exists between the moveable head 30 and the annular sidewall 34. The downward-facing surface 44 of the heater cell 18 is spaced apart from the upward-facing surface 40 of the base 36 by a variable gap distance, also referred to herein as specimen thickness. The gap distance can be precisely controlled by raising and lowering the moveable stem 16 as set forth above, optionally in increments as little as 5 μm to 10 μm, allowing the gap distance of between 0.05 to 15 mm. The heater cell 18 further includes a first plurality of thermocouples 46 for measuring a steady-state temperature immediately above the fluid specimen. As further shown in FIG. 3, the heater cell 18 is removably joined to the stem 16 via a flange 48, such that the heater cell 18 can be detached between measurements. For example, measuring the thermal conductivity of a molten salt can require a different heater cell than for measuring the thermal conductivity of molten metal, e.g., a different heater arrangement and geometry. Though not required, a quartz rod 50 extends from the heater cell 18 to a digital variance indicator 52 for measuring the gap distance, however in other embodiments the gap distance can be measured from the vertical displacement of the exterior of the stem 16 without reliance on the quartz rod 50.

[0020] A further example of a heater cell 18 within a test chamber 32 is illustrated in FIG. 4. In this example, the heater cell 18 includes a disc-shaped head 30 having an axial guard heater 60, a radial guard heater 62, an insulator 64, and a primary heater 66. The radial guard heater 62 is self-contained within the heater cell 18, thereby reducing radial heat losses and ensuring an isothermal plate temperature of the fluid specimen 100. In other embodiments however the heater cell 18 includes fewer elements, dependent on the fluid specimen under evaluation. As also shown in FIG. 4, the heater cell 18 includes a first plurality of thermocouples 46. The thermocouples 46 are distributed along radial and axial directions within the heater cell 18 to determine heat loss corrections and to verify isothermal temperature at the bottom of the heater cell 18. Additional instrumentation such as fiber optics, pyrometers, or resistance temperature sensors (RTDs) can also be included in the heater cell 18. The test chamber 32 includes a second plurality of thermocouples 68 distributed along radial and axial directions within the base 36. At least two of the second plurality of thermocouples 68 are distributed radially, immediately below the upward-facing surface 40 of the base 36, and at least one of the second plurality of thermocouples 68 is distributed axially, being offset from the upward-facing surface 40 of the base 36 and nearer to a plurality of cooling channels 70. The cooling channels 70 are offset from the upward-facing surface 40 of the base 46. This offset allows for axial flow heat flux sensing by thermocouples, heat flux sensors, or fiber optics to measure the flux leaving the fluid specimen 100. The present invention also includes low-emissivity surfaces to ensure that the emissivity of material surrounding the fluid specimen 100 is minimized, which reduces radiative heat transfer uncertainties. For example, the upward-facing surface 40 of the base 36, the exterior of the heater cell 18, and the inner annular surface 38 of the sidewall 34 can comprise rhodium or platinum electroplating, electro-polishing, or conventional mechanical polishing.

[0021] Operation of the apparatus 10 for measuring the thermal conductance of a fluid specimen will now be described. The fluid specimen 100 is added to the test chamber 32, which is then enclosed via the flange seal 14. An inert gas can displace ambient air from within the test chamber 32, thereby minimizing corrosion and increasing the service life of the apparatus 10. The furnace 28 is set to a desired temperature (e.g., 900° C.) and the system is allowed to reach thermal equilibrium (e.g., negligible temperature change over 0.5 to 1.0 hours). The heater elements 60, 62, 66 within the heater cell 18 then provide a known power output. If the hot side of the fluid specimen 100 exhibits a non-isothermal temperature, the power output can be lowered to reduce the temperature differences to less than 1° C. The gap distance is set then incremented or decremented by a fixed distance, for example 5 μm to 10 μm, or other interval dependent upon the fluid under evaluation. The fluid specimen 100 is heated from the top with the heater cell 18 and is cooled from the bottom with cooling channels 70. Once equilibrium is reached at each gap distance, the temperature difference across the fluid specimen 100 is recorded at a controller module 80. This is plotted in FIG. 5, which depicts the temperature drop at each gap size based on the output of the first plurality of thermocouples 46 and the second plurality of thermocouples 68. The temperature difference, the known fluid specimen thickness (or gap distance), and the known power output are used to calculate the thermal resistance of the fluid specimen 100. In particular, the thermal resistance R is calculated by the controller module 80 according to the following equation (1), in which dT represents the temperature drop across the fluid specimen, Q represents the heated power, and A represents the area of heating surface 44 of the heater cell 18:

[00001]$\begin{array}{cc}R=\frac{\mathrm{dT}.Math.A}{Q}& \left(1\right)\end{array}$

The thermal resistance R is plotted in FIG. 6 as a function of the gap distance. The heat flux can be corrected for heat losses using radial or axial thermocouples, or directly calculated using a heat flux sensor below the fluid specimen. The thermal conductivity of the fluid specimen is then determined using a curve fit of thermal resistance with respect to gap distance. In particular, the controller module 80 determines the thermal conductivity k by a least square fit of equations (2) or (3) on resistance versus gap size, where k.sub.r is the apparent radiative conductivity and dx represents the gap size (as recorded on the digital variance indicator 52):

R=k.sup.−1.Math.dx+C  (2)

R=(k+k.sub.r).sup.−1.Math.dx+C  (3)

[0022] Repeating the foregoing at different temperatures (e.g., by changing the temperature settings of the furnace) can also yield temperature dependent thermal conductivities. The foregoing method provides advantages over existing techniques, including laser flash thermal techniques. For example, volatile fluid specimens cannot be contained in existing laser flash crucibles, as salts tend to wet the walls, biasing results. Without a fully sealed crucible, laser flash thermal conductivity is not feasible for measuring volatile salts and would be extremely costly to install in radiation environments such as hot cells. In addition, laser flash techniques are an indirect measure of thermal conductivity, requiring density and specific heat capacity of the fluid specimen. By contrast, the above method is uniquely suited to determine the thermal conductivity of motel salts without knowledge of their density or specific heat capacity, optionally for the design and optimization of molten salt reactors. In particular, the thin fluid layer eliminates the potential for convection errors and allows for a direct measurement of thermal conductivity. The gap variation removes the need for multi-layer heat transfer corrections that are required with all other steady state techniques having fixed gaps. Further, the apparatus 10 includes a modular construction, which is ideal when components require replacement due to corrosion, and is fully sealed and can provide a fully inert cover gas when analyzing reactive fluids.

[0023] The above description is that of current embodiments of the invention. Various alterations and changes can be made without departing from the spirit and broader aspects of the invention as defined in the appended claims, which are to be interpreted in accordance with the principles of patent law including the doctrine of equivalents. This disclosure is presented for illustrative purposes and should not be interpreted as an exhaustive description of all embodiments of the invention or to limit the scope of the claims to the specific elements illustrated or described in connection with these embodiments. For example, and without limitation, any individual element(s) of the described invention may be replaced by alternative elements that provide substantially similar functionality or otherwise provide adequate operation. This includes, for example, presently known alternative elements, such as those that might be currently known to one skilled in the art, and alternative elements that may be developed in the future, such as those that one skilled in the art might, upon development, recognize as an alternative. Further, the disclosed embodiments include a plurality of features that are described in concert and that might cooperatively provide a collection of benefits. The present invention is not limited to only those embodiments that include all of these features or that provide all of the stated benefits, except to the extent otherwise expressly set forth in the issued claims. Any reference to claim elements in the singular, for example, using the articles “a,” “an,” “the” or “said,” is not to be construed as limiting the element to the singular.