Sensor assembly for differential scanning calorimeter

Abstract

To provide a sensing unit of a sensor assembly for a differential scanning calorimeter allowing for operation in both, the heat flux operating mode and in the power compensation operating mode, and having improved measurement characteristics.SOLUTION: A sensing unit for a differential scanning calorimeter includes a superposition of: layers 9, 10 of a thermoelectric arrangement; a layer 21 of an electrical heater arrangement; and a layer 27 of an absolute temperature measurement arrangement. The thermoelectric arrangements, the electrical heater arrangements and the absolute temperature measurement arrangements are symmetrically arranged on a sample-side and a reference-side of the sensor.SELECTED DRAWING: Figure 2

Description

[Technical field]

[0001] The present invention relates to a sensing unit and a sensor assembly including the sensing unit for a differential scanning calorimeter (DSC). [Background technology]

[0002] A commonly known differential scanning calorimeter includes a heat source, the temperature of which is controlled by a predetermined temperature program, and a sensor assembly is thermally coupled to the heat source to establish sample-side and reference-side flow paths for heat transfer to the sample and reference locations of the sensor assembly, respectively.

[0003] In a heat flux differential scanning calorimeter, the measurement signal corresponds to the temperature difference resulting from the rate of heat flow between a heat source and each of the sample and reference locations, whereas in a power compensated differential scanning calorimeter, the measurement signal corresponds to the power required to compensate for the heat flow to be measured. Summary of the Invention [Problem to be solved by the invention]

[0004] It is an object of the present invention to provide a sensing unit of a sensor assembly for a differential scanning calorimeter that allows operation in both heat flux and power compensated modes of operation and has improved measurement characteristics. [Means for solving the problem]

[0005] This object is achieved by a detection unit for a differential scanning calorimeter, which includes a disk-shaped substrate, which is suitable for being mounted in a thermally conductive contact with a temperature-controlled heat source of the differential scanning calorimeter. In addition, the detection unit includes a sample-side pan support area adapted to receive a lower part of a sample pan on the sample-side pan support area in a thermally conductive contact with the sample-side pan support area, and a reference-side pan support area adapted to receive a lower part of a reference pan on the reference-side pan support area in a thermally conductive contact with the reference-side pan support area. The detection unit further includes a sample-side thermoelectric device for generating a sample-side voltage signal between two terminal parts of the sample-side thermoelectric device, and a reference-side thermoelectric device for generating a reference-side voltage signal between two terminal parts of the reference-side thermoelectric device. The sample-side voltage signal is indicative of heat flow across a sample-side measurement area, the reference-side voltage signal is indicative of heat flow across a reference-side measurement area, and the sensing unit further includes a sample-side electric heater device below the sample-side pan support area and a reference-side electric heater device below the reference-side pan support area.

[0006] Preferably, the sensing units are formed in a thermodynamically symmetric arrangement with respect to a plane perpendicular to the disk-shaped substrate and intersecting with a center point of the disk-shaped substrate, in this embodiment, the center point of the disk-shaped substrate is the center point of the sensing units.

[0007] Preferably, the sample side measurement region and the reference side measurement region are arranged in the outer peripheral region of the disk-shaped substrate.

[0008] Preferably, the thermoelectric device is located within the measurement area. The heat source can be controlled independently of the sample side and / or reference side electric heater devices.

[0009] The sample side or reference side pan support area, respectively, preferably extends beyond the lower portion of the sample or reference pan, respectively.

[0010] The presence of sample-side and reference-side electric heater devices enables the use of a power compensation mode in a differential scanning calorimeter, where both the sample and the reference are located in the same volume, the temperature of which is controlled by the same heat source, which is preferably a furnace.

[0011] The sample and reference side electric heater arrangement further enables to increase the time resolution of the sensor assembly including the sensing unit.

[0012] In one embodiment, the sample side measurement area surrounds the sample side pan support area and the reference side measurement area surrounds the reference side pan support area.

[0013] The different "areas" of the sensing unit are characterized by their areas and locations with respect to the sensing unit, and extend through the thickness of the sensing unit. The term "surrounding" should be understood in a broad sense to allow for overlap. In the embodiment at hand, for example, the measurement area may have the shape of a hollow cylinder with inner and outer radii, and the bread support area may have the shape of a cylinder with an outer radius. The measurement area and the bread support area may be arranged concentrically. In such an embodiment, the measurement area surrounds the bread support area as long as the outer radius of the measurement area is larger than the outer radius of the bread support area, regardless of the inner radius of the measurement area.

[0014] Since the measurement area surrounds the respective pan support area, the sensing unit according to the present invention has a greater tolerance with respect to the placement of the sample pan and the placement of the reference pan. Therefore, the combination of the measurement area surrounding the pan support area and the electric heater device allows for exceptionally robust and repeatable measurements over a wide range of time resolutions.

[0015] It is noted first of all that the expression "heat source" as used herein is preferably also to be interpreted to include low heat sources, whereby the present specification applies to the heating mode of operation and also to the cooling mode of operation of a differential scanning calorimeter. Furthermore, the temperature control of the heat source may include isothermal operation, where the temperature is constant, or dynamic operation, where the temperature is oscillating according to a predetermined temperature program as a function of time, in particular a linear temperature ramp, or in particular in the form of a moderated linear temperature ramp.

[0016] The heat flow in the sample side and reference side, respectively, is proportional to the temperature gradient along the flow path according to Fourier's Law, and the sample side and reference side voltage signals generated by the sample side and reference side thermoelectric devices, respectively, thus indicate the heat flow between the heat source and the sample side and reference side pan support areas, respectively.

[0017] In one embodiment, one terminal portion of the sample-side thermoelectric device is connected to one terminal portion of the reference-side thermoelectric device having the same polarity. In the following, these terminal portions that are at the same potential during use will be referred to as "first terminal portions". In this embodiment, a differential voltage signal, which is a voltage signal indicating the rate of differential heat flow between the sample side and the reference side, is available between two terminal portions of the sample side and the reference side thermoelectric device that are not connected to each other. In the following, these terminal portions will be referred to as "second terminal portions", even though the potentials of the terminal portions may differ during use.

[0018] In a preferred embodiment, the first terminal portions of the sample and reference side thermoelectric devices are connected to each other and to the same thermoelectric material, while the sample and reference side thermoelectric junctions include the same combination of thermoelectric materials.

[0019] The sensing unit is preferably used in a power compensation mode of operation. In this embodiment, the sample and reference side electric heater devices are energized to operate the differential scanning calorimeter in a power compensation mode of operation. In this mode of operation, the energization is controlled to bring the differential heat flow signal close to zero. This can be achieved, for example, by applying a differential voltage signal to the input of a proportional controller, which feeds the heater device from the output side of the proportional controller.

[0020] Preferably, the differential voltage signal is measured between the second terminal portions of the sample-side and reference-side thermoelectric devices, while the first terminal portions of the sample-side and reference-side thermoelectric devices having the same polarity are connected to each other. In another embodiment, the differential voltage signal is derived from the sample-side and reference-side voltage signals, inter alia, by calculating the difference.

[0021] In power compensation mode, the power provided to the sample-side and reference-side electric heater devices is detected and used to determine the heat flow to or from the sample. In a preferred embodiment, the differential thermoelectric voltage is detected as well and taken into account in determining the heat flow to or from the sample.

[0022] The sensing unit is preferably used in a heat flux mode of operation. In this embodiment, a differential thermoelectric voltage, which is the difference between the sample side thermoelectric voltage and the reference side thermoelectric voltage, is detected. In the heat flux mode of operation, the sample side and reference side electric heater devices are either not energized at all or the electric heater devices are energized according to a predetermined temperature program.

[0023] The disc-shaped substrate of the sensing unit is preferably a circular disc, preferably made from an aluminium oxide ceramic material, preferably having a diameter of more than 20 mm, preferably 24 mm or more.

[0024] Preferably, the disk-shaped substrate has an essentially flat upper side on which the various structural elements of the sensing unit are provided, preferably by using multi-layer thick film technology, at least the thermoelectric and electric heater devices, both on the sample and reference side.

[0025] Preferably, the sensing unit comprises a multi-layer structure arranged on a disc-shaped substrate. Starting from the disc-shaped substrate, the multi-layer structure preferably comprises the following layers in a given order: a layer of an electric heater device, an insulating layer, a second layer of a thermoelectric device, an insulating layer, a first layer of a thermoelectric device, and an insulating layer. Preferably, these layers are applied using a mulit-layer thick film technique. Preferably, furthermore, the insulating layer comprises an electrically conductive material for establishing through-contact connections between the first and second layers of the thermoelectric device, and between the layer of the electric heater device and the connector pads on the upper surface of the sensing unit, and between at least one of the layers of the thermoelectric arrangement and the connector pads on the upper surface of the sensing unit.

[0026] According to another aspect of the invention, the thickness of the disk-shaped substrate is reduced below the respective sample-side and reference-side measurement regions, and preferably the thickness is also reduced below the respective sample-side and reference-side pan support regions as well.

[0027] In particular, the thickness reduction below the sample-side and reference-side measurement areas, respectively, causes heat to flow across the measurement areas along a measurement path that is confined between the upper surface of the disk-shaped substrate and the recessed lower surface of the disk-shaped substrate, resulting in better detection of the heat flow by a thermoelectric device positioned in the measurement area.

[0028] Thermally conductive contact between the disk-shaped substrate and the temperature-controlled heat source is preferably established by engagement between the upper end face of the furnace, which serves as the heat source, and the disk-shaped substrate, particularly in the area where the thickness of the disk-shaped substrate is greater than below the measurement areas on the sample and reference sides, respectively.

[0029] Due to the high thermal conductivity through the materials of the furnace and the disk-shaped substrate, the sample or reference is heated primarily by the heat flow, trough, the measurement area. The heat flow through the measurement area can be detected by a thermoelectric device.

[0030] In a preferred embodiment, the upper end surface of the furnace comprises a layer of material, for example glass ceramic, with a thermal conductivity between 0.5 W / (mK) and 5 W / (mK), preferably between 1 W / (mK) and 2 W / (mK). Such a layer protects the sensing unit from undesired rapid temperature changes, while the conductivity of the layer at the same time ensures that the heat flow through the measurement area is the dominant heat flow path.

[0031] The sensing unit and the overall geometry of the sensor assembly including the sensing unit are ideally configured for thermodynamic symmetry so that the conditions for heat to flow between the sample side and reference side pan support areas, respectively, and the heat source are identical.

[0032] In a preferred embodiment of the sensing unit, each of the sample-side and reference-side thermoelectric devices includes a plurality of thermoelectric junctions, each formed by a first thermoelectric material in contact with a second thermoelectric material, the thermoelectric junctions of any of the thermoelectric devices being connected in series and alternately positioned at locations that are differently spaced from each other from the respective pan support area.

[0033] This can be specifically achieved when both the sample side and reference side pan support areas have outer circular boundaries and the differently spaced locations are located on an inner circle and on an outer circle. The inner circle is located concentrically with respect to the outer circular boundary and in close proximity to the outer circular boundary as well as radially outside the outer circular boundary. The outer circle is located concentrically with respect to the inner circle. The outer circle has a larger radius than the inner circle. The thermoelectric junctions on the inner circle are preferably equally spaced in the circumferential direction. Similarly, the thermoelectric junctions on the outer circle are equally spaced in the circumferential direction in this embodiment.

[0034] As the first thermoelectric material, gold (Au) is preferably used, and as the second thermoelectric material, a gold-palladium alloy (AuPd) is preferably used. The number of thermoelectric junctions on each of the inner and outer circles in a given layer of the thermoelectric device is preferably greater than 30, specifically equal to 34.

[0035] By arranging pairs of junctions on concentric circles, preferably always one radially outside the other, and connecting the junctions in series, an improved measurement signal results. Thermoelectric junctions using gold and gold-palladium alloys can be produced in a reliable manner by thick film technology. By arranging 30 to 34 junctions on each circle, a reliable production is possible.

[0036] It is further preferred that successive junctions in said series connection of junctions are interconnected in pairs by alternating traces of said first and second thermoelectric materials respectively.

[0037] Preferably, each thermoelectric junction in the outer circle is positioned radially outward relative to one of the thermoelectric junctions in the inner circle. Each of these pairs of thermoelectric junctions is connected by a radially extending trace of one of the respective first and second thermoelectric materials. The trace of the other of the thermoelectric materials establishes a connection circumferentially to halfway between adjacent inner junctions, then radially outward to halfway between adjacent outer junctions, and then circumferentially to an adjacent outer junction. The latter is not the case for terminal junctions in series, where the traces of the first and second thermoelectric materials are instead open ended at the outer circle to be connected to terminal portions for tapping off voltage signals.

[0038] This embodiment minimizes the length of traces required to form a suitable thermoelectric device and is therefore more reliable. Preferably, the measurement area is the area between the inner circle and the outer circle. Preferably, each of the sample side and reference side thermoelectric devices has their thermoelectric junctions distributed in at least two layers arranged one on top of the other with an electrically insulating layer between them, and the series connection is through-contacted through the insulating layer.

[0039] Thus, the number of thermoelectric junctions in the overall series connection can be increased to be the sum of the junctions in each of the individual layers, and the sensitivity of the sensing unit, and therefore of the sensor assembly including the sensing unit, is thereby increased.

[0040] Preferably, the total number of thermoelectric junctions is therefore between 60 and 68. In an advantageous embodiment, each of the sample side and reference side electric heater devices includes a resistive heating trace that meanders between a central portion and a peripheral portion of the sample side and reference side pan support area, respectively.

[0041] Specifically, the serpentine trace extends between an outer limit circle concentrically positioned within and near the outer circular boundary of each of the sample-side and reference-side pan support regions, and an inner limit circle concentrically positioned radially inwardly of and relative to the outer limit circle. The serpentine turnaround region and the outer and inner limit circles, respectively, are tangent at positions equidistant from one another in the circumferential direction of the circle. This serpentine pattern advantageously achieves uniform heating of the pan support region.

[0042] Another advantageous embodiment further includes sample side and reference side absolute temperature measuring devices below said sample side and reference side pan support areas respectively.

[0043] These absolute temperature measurement devices allow absolute temperature measurements in the immediate vicinity of the sample and reference pans, respectively. The temperature measurements can be used to estimate the thermal resistance in the sensor assembly.

[0044] A sensing unit including a sample-side and a reference-side absolute temperature measuring device can be used to measure the temperature of the sample. To measure the temperature of the sample, the sensing unit is placed inside the temperature-controlled heat source of the differential scanning calorimeter. The sample is placed in a pan-shaped sample pan on the sample-side pan support area. The signal of the sample-side absolute temperature measuring device is used to determine the temperature of the sample. Preferably, the sample-side thermoelectric voltage and / or the power provided to the sample-side electric heater device are also used to determine the temperature of the sample.

[0045] The absolute temperature measuring device is placed in very close proximity to the sample. Therefore, the signal generated by the absolute temperature measuring device is a good estimate of the actual temperature of the sample, especially in near-steady-state conditions. In transient conditions, the heat flow generated by the sample, the heat source, and / or the electric heater device may directly heat or cool the absolute temperature measuring device, causing a deviation between the sample temperature and the signal generated by the absolute temperature measuring device. This deviation can be corrected by taking into account the sample-side thermoelectric voltage and / or the power provided to the sample-side electric heater device.

[0046] In an advantageous embodiment, the sample side and reference side absolute temperature measurement devices each include a temperature sensitive resistive trace that snakes in a pattern that is symmetrical about a central axis that intersects the sample side and reference side pan support area, respectively.

[0047] Specifically, the pan support area has a circular perimeter and an axis of symmetry defines a diameter of the circular perimeter. The legs of the serpentine extending between turn regions located near the perimeter and near the axis of symmetry are perpendicular to the axis of symmetry. The resistive traces can be dimensioned to have resistances ranging between, illustratively, 20 Ω at -150°C and 175 Ω at 700°C.

[0048] Preferably, the sample-side and reference-side absolute temperature measuring devices are further structural elements of the sensing unit, provided by using multi-layer thick film technology.

[0049] Preferably, the sample-side and reference-side absolute temperature measuring devices are included in a multi-layer structure. The multi-layer structure of the sensing unit according to this embodiment includes an additional electrical insulation layer and a layer of the absolute temperature measuring device. The layer of the absolute temperature measuring device is arranged between the upper side of the disc-shaped substrate and the layer of the electric heater device. The additional electrical insulation layer is arranged between the layer of the electric heater device and the layer of the absolute temperature measuring device.

[0050] Starting from a disk-shaped substrate, the multi-layer structure of this embodiment preferably includes successive layers in a given order: a layer of an absolute temperature measurement device, an insulating layer, a layer of an electric heater device, an insulating layer, a second layer of a thermoelectric device, an insulating layer, a first layer of a thermoelectric device, and an insulating layer.

[0051] Preferably, further, the insulating layer comprises an electrically conductive material for establishing through contact connections between the first and second layers of the thermoelectric device, as well as between the layer of the electric heater device and the connector pad on the upper surface of the sensing unit, between at least one of the layers of the thermoelectric device and the connector pad on the upper surface of the sensing unit, and between the layer of the absolute temperature measuring device and the upper surface of the sensing unit.

[0052] In a further embodiment, the sensing unit comprises a pan support. The pan support is a thin layer applied on top of the topmost electrically insulating layer, but only locally on the sample side and reference side pan support areas. In a preferred embodiment, the diameter of the pan support in the sample side and reference side pan support areas and / or in the sample side or reference side pan support areas is slightly larger than the diameter of the lower part of the pan.

[0053] Small depressions, either in the pan support and / or in the multi-layer structure, can be located at the center points of the sample and reference pan support areas. With pans that contain centering pins, such depressions can aid in manual positioning of the pan on the sensing unit.

[0054] Preferably, the pan support compensates for local surface waviness, which may be caused for example by the underlying structure, and provides a particularly flat surface, thus allowing reduced thermal contact between the pan and the sensing unit.

[0055] The method for manufacturing the sensing unit comprises the steps of providing a disk-shaped substrate and depositing, successively on the disk-shaped substrate, the following layers: - a layer of electric heater devices; - an electrical insulating layer, - a second layer of a thermoelectric device; - an electrical insulating layer, a first layer of a thermoelectric device; and - Electrical insulation layer and providing the

[0056] Preferably the layer is applied using thick film techniques, especially screen printing techniques. The electric heater device layer includes conductive traces which form the electric heater devices, connector pads for the electric heater devices, and connector pads for lower layers, if any.

[0057] The electrically insulating layer is electrically insulating with the only exception being the area of ​​the connector pads on the layer below it. The second layer of thermoelectric devices includes traces that form at least a portion of the thermoelectric junctions of the sensing unit, connector pads for the second layer of thermoelectric devices, and connector pads for the lower layer.

[0058] The first layer of the thermoelectric device includes traces that form at least a portion of the thermoelectric junctions of the sensing unit, connector pads for the first layer of the thermoelectric device, and connector pads for the lower layer.

[0059] In a preferred embodiment, a layer of an absolute temperature measuring device and an electrical insulating layer are disposed between the disk-shaped substrate and the layer of the electrical heater device.

[0060] The absolute temperature measurement device layer includes conductive traces that form the absolute temperature measurement device and connector pads for the absolute temperature measurement device.

[0061] In a preferred embodiment, the material for the pan support is applied locally onto the sample side and reference side support areas.

[0062] Fabricating the sensing unit by application of the above layers allows for efficient and reliable manufacturing, especially if thick film techniques such as screen printing are used.

[0063] In a preferred embodiment, the sensing unit further includes a plurality of connector pads adapted to receive external wiring.

[0064] Preferably, the connector pad is positioned on a central circle having a center point equal to the center point of the sensing unit and a diameter smaller than the difference between the distance between the center points of the sample side and reference side pan support areas and the diameter of one of the outer circles.

[0065] These connector pads serve to establish electrical communication between electrical signals emanating from or applied to the sensing unit and external circuitry for the sensing unit.

[0066] Specifically, a first one of the connector pads has one of the terminal portions of each of the sample side and reference side thermoelectric devices connected together to the first one, the connected ones of the terminal portions having the same polarity, while the other ones of the terminal portions of each of the sample side and reference side thermoelectric devices are separately connected to second and third ones of the connector pads.

[0067] Therefore, the difference between the voltage signals from the sample side and reference side thermoelectric devices, respectively, is available between the second and third connector pads, while individual voltage signals from the sample side and reference side thermoelectric devices are available between the first and second connector pads, and between the first and third connector pads, respectively.

[0068] Further, advantageously, a fourth one of the connector pads has one of the power supply terminals of the sample side and the reference side heater arrangements connected together thereto, while the other one of the power supply terminals of the sample side and the reference side heater arrangements are connected separately to the fifth and sixth ones of the connector pads.

[0069] Thus, the sample side and reference side heater devices, respectively, can be individually energized by applying power to the fourth and fifth connector pads or to the fourth and sixth connector pads, respectively.

[0070] Moreover, conveniently, seventh and eighth ones of said connector pads are connected to respective opposed ends of said resistive traces of said sample-side absolute temperature measuring device.

[0071] Thus, the absolute temperature at the sample side pan support area can be measured by connecting corresponding circuitry to the seventh and eighth connector pads.

[0072] In a preferred embodiment, there are no similar connections and pads provided on the reference side. The reference side absolute temperature measurement device in this embodiment is in fact provided merely for thermal symmetry, but is not used for temperature measurement.

[0073] According to another aspect of the invention, a sensor assembly includes a sensing unit and an elongated member extending along a longitudinal axis, one of the axial end portions of the elongated member including an electrical contact device to form a plug member for being brought into electrical contact with a complementarily formed socket member of the differential scanning calorimeter, the electrical contact device being electrically connected to the connector pad of the sensing unit.

[0074] Preferably, external wiring establishes an electrical connection between electrical contact devices and connector pads of the sensing unit.

[0075] In particular, the plug member may be configured to connect with the receptacle member in an interlocking and / or force-fit manner, thereby contacting all of the connector pads at once in a particularly easy manner. In a preferred embodiment, the electrical contact device is located on the tip portion which includes a guiding surface. The guiding surface is asymmetric in the circumferential direction, ensuring a predefined orientation of the plug member relative to the receptacle. In addition, the tip portion protects the contact device during insertion of the plug member.

[0076] Preferably, the sensor assembly further comprises a tensioning wire, which is used to fix the sensing unit in the calorimeter by mechanical tension and to ensure a well-defined thermal contact between the furnace and the sensing unit, preferably the disk-shaped base of the sensing unit. The tensioning wire, which is preferably two small openings arranged side by side inside the central circle, is looped. The tensioning wire passes through the elongated member and leaves the elongated member at the tip portion of the elongated member, ending in a loop. A fixing element of the calorimeter can engage with this loop. Preferably, the fixing element exerts a spring force on the tensioning element, thus ensuring that the disk-shaped base of the sensing unit is pressed with a constant force onto the upper end surface of the furnace.

[0077] In a preferred embodiment, the elongate member and the sensing unit of the sensor assembly do not contact each other when the sensor assembly is installed. Preferably, the taut wire is selected to have a diameter of 0.2 mm or less to minimize heat transfer between the sensing unit and the fixing element.

[0078] Preferably, the longitudinal axis is a central axis of symmetry for the entire sensor assembly, whereby, in particular, the sample side and reference side pan support areas are positioned symmetrically on either side of the axis, while the multiple connector pads are positioned on a circle centered about this axis.

[0079] Preferably, the elongated member has a cylindrical outer periphery and the electrical contact device includes elongated contact lugs extending parallel to the longitudinal axis, spaced apart from one another in the circumferential direction and connected to the connector pads by connecting wires disposed in axially extending hollow spaces formed in the elongated member.

[0080] Preferably, the connecting wires form the external wiring. Finally, a preferred embodiment of the sensing unit further comprises at least one positioning tab formed at the outer peripheral edge of the disc-shaped substrate, the positioning tab being configured to be brought into a positive fit with a complementarily formed locating recess in said calorimeter.

[0081] Thus, the angular orientation of the sensing unit with respect to the body of the calorimeter is precisely defined.Preferably, two diametrically opposed positioning tabs are provided.

[0082] In one embodiment, the sensing unit is used to simultaneously determine heat flow to a first and a second sample, whereby the first sample is placed in a sample pan disposed on a sample-side pan support area and the second sample is placed in a reference pan disposed on a reference-side pan support area. The heat flow to the first sample is determined using at least the sample-side voltage signal. The heat flow to the second sample is determined using at least the reference-side voltage signal.

[0083] Preferably, the heat flow to the first sample is additionally determined using the power provided to the sample-side electric heater device. Preferably, the heat flow to the second sample is additionally determined using the power provided to a reference electrical heater device.

[0084] The ability of the sensing unit to determine both the sample-side voltage signal and the reference-side voltage signal allows it to distinguish between heat flow to and from the sample side and heat flow to and from the reference side. Placing a second sample on the reference side increases throughput, which is useful especially if a large number of samples are to be compared with each other.

[0085] In one embodiment, the sensing unit is used to determine at least one of the parameters describing the complex heat capacity of the sample, preferably the phase angle of the complex heat capacity. In this embodiment, the sample is placed in a sample pan that is placed on the sample side pan support area, and a reference pan is placed on the reference side pan support area. The heating power is controlled as a function of time to be modulated by a selected periodic power modulation, to vary gradually, or to follow a constant baseline. A sample side voltage signal, a reference side voltage signal, and a temperature signal are measured. A functional relationship between the sample side voltage signal, the reference side voltage signal, and the temperature signal is evaluated to determine the desired parameter.

[0086] Periodic power modulation of the heating power induces periodic heat flow to or from the sample without phase transition. The situation can be described when the response of a component to an alternating current or voltage is characterized by impedance, and a functional relationship can be derived by analogy with a DC electric circuit. Complex heat capacity is a complex function that describes the temperature of a sample in response to an alternating heat flow. It may depend on the average temperature and the frequency of the power modulation. The phase angle describes the difference in phase between the heat flow to and from the sample and the temperature of the sample in response to a sinusoidal heating power modulation. The parameters of the complex heat capacity are the real and imaginary parts of the complex heat capacity, the phase angle, and the absolute value.

[0087] Preferably, the reference pan is empty, however, in another embodiment, a familiar reference is placed in the reference pan.

[0088] Preferably, here, and in all other disclosed embodiments, the sample pan and reference pan are of the same pan type and therefore of the same size, shape, and material.

[0089] By evaluating both the sample and reference side voltage signals, it is possible to determine the complex heat capacity of the reference side sensing unit components and the pan of the pan mold separately from the sample side sensing unit components and the sample pan containing the sample. Hence, the complex heat capacity of the sample can be estimated by subtracting the effects of the sensing unit and the pan.

[0090] In a preferred embodiment, a gradually varying or constant baseline of heating power is provided at least in part by a heat source, while a periodic power modulation is provided by sample-side and reference-side electric heater devices. Preferably, temperature signals are detected by and in the sample-side and reference-side absolute temperature measurement devices. The sample-side and reference-side voltage signals detect the heat flow to and from the sample and reference.

[0091] Further features, advantages and details result from the following description in which the invention will be explained in more detail with reference to the drawings. In the drawings: [Brief description of the drawings]

[0092] [Figure 1] Figure 1a is a perspective overall view of an exemplary embodiment of a sensor assembly according to the present invention, and Figure 1b is an enlarged partial view of a plug formed by an axial end portion of an elongated element of the sensor assembly of the embodiment shown in Figure 1a. [Diagram 2]Figure 2a is a top view of the embodiment of Figure 1a, and Figure 2b is a corresponding view of Figure 2a visualising the superimposed layers below the top layer shown in Figure 2a. [Diagram 3] Figure 3a is a top view of a first layer of thermoelectric devices positioned below the top layer illustrated in Figure 2a, and Figure 3b is a top view of a second layer of thermoelectric devices positioned below the first layer of thermoelectric devices illustrated in Figure 3a. [Figure 4] FIG. 3c is a top view of a layer of electric heater devices including resistive heaters and positioned below the second layer of thermoelectric devices illustrated in FIG. 3b. [Diagram 5] FIG. 5 is a top view of a layer of an absolute temperature measuring device placed below the layer of an electric heater device illustrated in FIG. 4. [Figure 6] FIG. 6 is a schematic partial cross-sectional view of one of the measurement areas in a plane perpendicular to the layer plane of FIGS. 2 to 5. [Figure 7] FIG. 6 is a schematic partial cross-sectional view of the sensor assembly in a plane perpendicular to the layer planes of FIGS. 2 to 5. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0093] As illustrated in Fig. 1a, an embodiment of the sensor assembly according to the invention comprises a sensing unit 1 having an essentially planar upper surface 2 which is aligned horizontally when the sensor assembly is mounted for a measurement operation in a manner that is in thermally conductive contact with a temperature-controlled heat source of a differential scanning calorimeter. The sensing unit 1 has essentially the shape of a circular disk with two positioning tabs 3 projecting radially from a circular periphery 4 of the disk. These positioning tabs 3 are in positive engagement with complementary recesses in the tubular wall of a furnace. The furnace forms the heat source of the calorimeter. At the same time, when a disk-shaped substrate is placed in the recess, an annular area of ​​the lower surface of the sensing unit 1, surrounding the sample-side and reference-side measurement areas, is kept in thermally conductive contact with the upper end surface of the tubular furnace wall of the heat source.

[0094] As can be seen in more detail in FIG. 2a, arc-shaped indicators 5 for the sample side pan support area S and the reference side pan support area R are provided on the upper surface 2 of the sensing unit 1, said pan support areas S, R being positioned diametrically and symmetrically with respect to the center point of the circular periphery 4 of the sensing unit 1. Each of the sample side and reference side pan support areas S, R has a circular shape with a respective center point. The center points of the sample side and reference side pan support areas lie on a straight line passing through the center point of the sensing unit 1 and are equidistant to the center point of the sensing unit 1. Small depressions 7, 8 positioned at the center points of the respective pan support areas S, R are provided in the top layer of the sensing unit 1. The user may utilize pans that include a centering pin on the bottom of the pan that corresponds to one of the small depressions 7, 8. If such a pan is used, the depressions 7, 8 assist in correct positioning of the pan on the sensing unit.

[0095] The upper surface 2 is the exposed side of the thin electrically insulating layer, the oppositely positioned lower surface of which is adjacent to the superposition of further layers, which for illustration purposes are shown as semi-transparent in Fig. 2b to clearly show the spatial relationship between the structures of the further layers, said thin electrically insulating layer and said further layers forming a multi-layer structure.

[0096] The topmost layer of this multi-layer structure is a first layer 9 of a thermoelectric device as shown in Figure 3a, and a similar second layer 10 of a thermoelectric device as shown in Figure 3b is positioned below the first layer of Figure 3a with a thin insulating layer between the first and second layers. Within these first and second layers 9, 10 of the thermoelectric device, a plurality of thermoelectric junctions 11a, 11b, each formed by contact between a first thermoelectric material 12 and a second thermoelectric material 13, are positioned on a pair of inner and outer circles 14, 15 centered near the center points of the sample-side and reference-side pan support areas S, R, respectively. In each pair of inner and outer circles 14, 15, the thermoelectric junctions 11a, b are distributed in the circumferential direction and spaced radially between the inner and outer circles 14, 15 pair-wise. The thermoelectric junctions 11 a,b are formed as overlapping traces of first and second thermoelectric materials 12, 13 applied by thick film techniques. The traces of the first thermoelectric material 12 extend radially between radially opposed thermoelectric junctions 11 a,b of the inner and outer circles 14, 15, while the traces of the second thermoelectric material 13 each extend from junction 11 a on the inner circle 14, circumferentially about the inner circle 14, halfway to its neighboring thermoelectric junction 11 a′, and then radially outwardly to halfway between opposed thermoelectric junctions 11 b, 11 b′ on the outer circle 15, and along the periphery of the outer circle 15 to their respective neighboring thermoelectric junctions 11 b′ on the outer circle 15. Thus, the arrangement of traces of thermoelectric material 12, 13 forms and connects, in series, thermoelectric junctions 11b, 11a, 11b', 11a' arranged alternately on inner and outer circles 14, 15. First and second terminal portions of the series connection are formed by terminal traces 18, 19 that extend outward from neighboring thermoelectric junctions 11b at the periphery in a region near center point 6 of sensing unit 1. Connection traces 18a, 19a and a set of feedthrough contacts 20 are used to continue the series connection between first layer 9 and second layer 10 of the thermoelectric device.

[0097] Within a central region located between the outer circles 15 of the sample-side and reference-side measurement regions, a plurality of connector pads 16 are positioned equidistantly on a central circle 17 centered about the central point 6 of the sensing unit 1. A first one of the connector pads 16 are of the same electrical polarity and are connected together to terminal traces 18 from the sample-side and reference-side thermoelectric series connections in the first layer 9 of the thermoelectric element, thereby forming a central tab for the entire series connection. In both the first layer 9 and the second layer 10, connection traces 18a and 19a, respectively, extend from respective traces of the thermoelectric material 12, 13 to respective sample or reference side feedthrough contacts 20 on both the sample and reference sides. Sample-side and reference-side terminal traces 19 are located within the second layer 10 of the thermoelectric device, and the terminal traces 19 are connected to second and third respective ones of the connector pads 16.

[0098] Underneath the second layer 10 of the thermoelectric element and separated therefrom by an electrical insulating layer is a layer 21 of the electric heater device illustrated in FIG. 4. The layer 21 of the electric heater device includes a symmetrically configured sample side and reference side pattern of resistive heating traces 22 formed by thick film technology. The heating pattern is confined within a reference side and sample side outer heating circle, respectively, and a sample side and reference side inner heating circle, respectively. The diameters of the sample side and reference side outer heating circle are close to, but less than, the diameter of the inner circle 14 of the thermoelectric junction 11a in the first and second layers 9, 10 of the thermoelectric device. Each of the resistive heating traces meanders between the respective inner and outer heating circles in that the inner and outer turning portions are tangent to the inner and outer heating circles at points equidistant in the circumferential direction, while the corresponding ends of the turning portions are connected by essentially straight portions extending essentially radially. In each of the sample side and reference side patterns, one of the outward turning portions near the central location of the connector pads 16 is broken to form two power supply terminals 23, 24. One of the sample side and reference side power supply terminals 23, respectively, is connected together to a fourth one of the connector pads 16 by a trace 25, while the other sample side and reference side power supply terminal 24 is separately connected to the fifth and sixth ones of said connector pads 16 by a sample side and reference side trace 26, respectively.

[0099] Positioned below the electric heater device layer 21 and separated therefrom by an electrical insulating layer is an absolute temperature measurement device layer 27 illustrated in FIG. 5. Identical sample-side and reference-side patterns of temperature-dependent resistive traces are formed near the center points of the sample-side and reference-side pan support areas, respectively. Each trace of each of the sample-side and reference-side patterns meanders with a configuration that is symmetrical about a straight line passing through the center points of the sample-side pan support area, the reference-side pan support area, and the sensing unit. The meanders are made up of equidistant linear sections 28 connected in pairs by inward and outward turning sections 29 and 30, respectively. The outward turning section 30 extends along the inner circle 14 of the thermoelectric junction 11a, while the inward turning section 29 extends along a line having an approximately semicircular portion centered near the center point of the sample or reference side pan support area, respectively, and partially following the inner heating circle, and two linear sections that merge with the semicircular portion and extend radially outward from the semicircular portion parallel to a center line passing through the center points of the sample side pan support area, the reference side pan support area, and the detection unit. The radially outermost linear section 28' facing away from the center point 6 extends across the linear line of symmetry, thereby connecting the outermost turning sections 30', 30" of the serpentine. The oppositely positioned outermost turning sections 30a, 30b facing the center point 6 are connected to the seventh and eighth connector pads 16 by correspondingly configured traces on the sample side, while the corresponding turning sections 30a, 30b on the reference side ultimately terminate in dead ends.

[0100] The above-described superposition of layers 9, 10, 21 and 27 is formed on the upper side of a disk-shaped substrate 31 (FIG. 1a) in such a way that the sample-side pan support area, the reference-side pan support area and the center point of the sensing unit of each layer are positioned on respective axes perpendicular to said upper side. Among these axes, the one passing through the center point of the sensing unit is the main axis of symmetry of the sensing unit 1. The sample-side and reference-side axes passing through the sample-side and reference-side center points, respectively, are the axes of symmetry of the circular sample-side and reference-side pan support areas, respectively, which are positioned in the inner circle 14. The sample-side and reference-side axes passing through the sample-side and reference-side center points, respectively, are in turn the axes of symmetry of the sample-side and reference-side measurement areas, respectively, which are positioned between the inner circle 14 and the outer circle 15.

[0101] As can be seen in Figures 1a and 1b, an elongated member 32 is disposed at the lower side of the disk-shaped base plate 31, but is not directly attached thereto. The elongated member 32 has a mainly cylindrical outer surface, the longitudinal axis of which coincides with the central axis of symmetry of the sensing unit 1. The axial end portion 34 of the elongated member 32, which is in opposing relation to the sensing unit 1, is formed as a plug having axially extending contact lugs 35 located in circumferentially equidistant recesses formed in the outer surface 33. The outermost end is formed with an axially extending flat guide surface 36 to aid in the introduction of the calorimeter in the correct angular orientation into a complementary formed socket member.

[0102] Inside the axially extending hollow space formed in the elongated member 32, connecting wires are accommodated which connect the contact lugs 35 of the plug-in member to corresponding connector pads 16 of the sensing unit 1. It should be noted that the repeating pattern of connector pads 16 on the various superimposed layers of the multi-layer structure is what forms the through contact connection.

[0103] A tension wire 37 is used to mount the sensing unit 1 to the elongated member 32 and to allow an axially tensioning engagement with the anchoring place in the calorimeter. The tension wire 37 is looped through two small openings 6a, b close to the center point of the sensing unit 1. The two small openings 6a, 6b are both located in the central circle 17 onto which the connector pad 16 is located. The tension wire 37 is housed in an axially extending hollow space of the elongated member 32. The tension wire 37 leaves the elongated member 32 on the tip of the axial end portion 34. In the illustrated embodiment, the tension wire 37 forms a loop in which an anchoring element of the calorimeter can get caught and stay. In use, the anchoring element pulls the sensing unit 1 against the upper end face of the furnace, thus ensuring a constant and reliable thermal contact between the heat source, which in this embodiment is a furnace, and the sensing unit 1.

[0104] FIG. 6 illustrates diagrammatically one of the pan support areas R,S in a cross section perpendicular to the upper surface 2 of the sensing unit 1 and on which an empty pan 38 is placed. The sensing unit 1 shown in this embodiment includes a pan support 41 but does not include an absolute temperature measuring device 27. The pan support 41 is merely a locally applied additional layer in the pan support area R,S and reduces the thermal resistance between the lower part of the pan and the uppermost electrically insulating layer of the multi-layer structure. In this highly schematic illustration, the radially inner and outer small circles represent the thermoelectric junctions 11a and 11b of the inner and outer circles 14 and 15, respectively, which define the radial extent of the measurement area between the inner and outer circles 14 and 15. Furthermore, the resistive heating pattern 22 below the lower part of the pan 38 is illustrated only in a highly schematic manner. The curved arrows 39 visualize the path of heat flow from the furnace to the pan 38, while the straight arrows 40 visualize the flow of heat from the electric heater device, realized by the resistive heating traces 22, to the pan 38 and further to any sample material (not shown) within the pan.

[0105] FIG. 7 shows a sensor assembly including the sensing unit 1 and the elongated member 32 connected by a taut wire 37 in a cross section perpendicular to the upper surface 2 of the sensing unit 1. The sensing unit 1 includes a disk-shaped substrate 31 that varies in thickness. The disk-shaped substrate 31 has a reduced thickness 31b below the sample side and reference side measurement area and below the sample side and reference side pan support area, and the disk-shaped substrate 31 has a greater thickness 31a outside the measurement and pan support area. The resistive heating traces 22 are disposed below the sample side and reference side pan support area and above the disk-shaped substrate 31. The thermoelectric devices with the junctions 11a, 11b are disposed above the resistive heating traces 22 and in the measurement area. The pan supports 41 are disposed on top of the layer including the thermoelectric devices but within the respective pan support areas.

[0106] The sensing unit 1 includes sample-side and reference-side pan support areas S, R, both of which are equipped with pan supports 41. In the embodiment shown in Figure 7, a sample pan 38a and a reference pan 38b are disposed on the respective pan supports 41.

[0107] One of the two openings 6a is shown in Figure 7. A tensioning wire 37 and a connecting wire connecting the respective contact lugs 35 and connector pads 16 at the axial end portions 34 of the elongated member 32 run through the inside of the elongated member 32. The tensioning wire 37 ends in a loop in which a fixing element, not shown, can hook and lodge within to pull the sensing unit 1 towards the upper end of the furnace.

[0108] 7 shows the symmetry of the sensor assembly about a plane passing through the center point of the sensing unit, perpendicular to a straight line passing through the sample side pan support area, the reference side pan support area, and the center point of the sensing unit. Symmetry about this plane is broken only by a few details in the wiring between the connector pads 16 and the structural elements on the sample and reference sides. [Explanation of symbols]

[0109] 1 Detection unit 2 Upper surface 3 Positioning tab 4 Circular perimeter 5 Arc shape indicator S, R Sample side, reference side pan support area 6 Center point of the detection unit 6a, b Openings (for tension wires) 7, 8 Center point of sample side / reference side 9 First layer of thermoelectric device 10 Second layer of thermoelectric device 11a, 11a', 11b, 11b' thermoelectric junction 12 The first thermoelectric material 13 The second thermoelectric material 14, 15 Inner / outer circle (measurement area) 16 Connector Pads 17 Center Circle 18, 19 Terminal Trace 18a, 19a Connection trace 20 Feed-through contacts (connections between layers of thermoelectric devices) 21 Electric Heater Device Layer 22 Resistive Heat Trace 23, 24 Power supply terminal 25 Trace 26 Trace 27 Absolute Temperature Measuring Device Layer 28, 28' Linear section 29 Inward turning section 30, 30', 30”, 30a, 30b Outer turning section 31 Disk-shaped substrate 32 Long and thin members 33 Outer surface 34 Axial end section 35 Contact Lag 36 Guide Surface 37 Tension Wire 38 Bread 39 Curved Arrow 40 Straight Arrow 41 Pan Support

Claims

1. A detection unit (1) for a differential scanning calorimeter, comprising a disc-shaped substrate (31), wherein the disc-shaped substrate (31) is mounted in such a manner that it is in thermal conduction contact with a temperature-controlled heat source of the differential scanning calorimeter, and the detection unit (1) is - A sample-side pan support region and a reference-side pan support region (S, R), wherein the sample-side pan support region and the reference-side pan support region (S, R) are adapted to receive the lower parts of the sample pan and the reference pan (38) in a manner that they are in thermal conduction contact with the sample-side pan support region and the reference-side pan support region (S, R), respectively. - A sample-side thermoelectric device and a reference-side thermoelectric device, wherein between the two terminal portions of the sample-side thermoelectric device and the reference-side thermoelectric device, a sample-side voltage signal and a reference-side voltage signal are provided to indicate the flow of heat across the sample-side measurement area and the reference-side measurement area, respectively. In the detection unit (1), which includes, - Below the sample-side pan support region and the reference-side pan support region (S, R), respectively, the sample-side electric heater device and the reference-side electric heater device, - Below the sample-side pan support region and the reference-side pan support region (S, R), respectively, a sample-side absolute temperature measuring device and a reference-side absolute temperature measuring device, A detection unit (1) characterized by including the following.

2. The detection unit (1) according to claim 1, wherein the thickness of the disc-shaped substrate (31) is reduced below the sample-side measurement area and the reference-side measurement area, respectively.

3. The detection unit (1) according to claim 1, wherein each of the sample-side electric heater device and the reference-side electric heater device includes a resistance heating trace (22) that meanders between the central and peripheral portions of the sample-side pan support region and the reference-side pan support region (S, R), respectively.

4. A multilayer structure disposed on the disc-shaped substrate, wherein the multilayer structure starts from the disc-shaped substrate, Layers of electric heater device, insulating layer, The second layer of the thermoelectric device, insulating layer, First layer and insulating layer of the thermoelectric device Includes, The layer of the absolute temperature measuring device is positioned between the upper side of the disc-shaped substrate and the layer of the electric heater device. The detection unit (1) according to claim 1, wherein an additional electrical insulating layer is disposed between the layer of the electric heater device and the layer of the absolute temperature measuring device.

5. The detection unit (1) according to claim 1, wherein each of the sample-side absolute temperature measuring device and the reference-side absolute temperature measuring device includes a temperature-sensitive resistance trace (28, 29, 30) that meanders in a pattern symmetrical with respect to a central axis crossing the sample-side pan support region and the reference-side pan support region (S, R), respectively.

6. The detection unit (1) according to claim 1 further includes a plurality of connector pads (16) adapted for the connection of external wiring.

7. A sensor assembly comprising a detection unit (1) as described in claim 1, and an elongated member (32) that extends along its longitudinal axis, wherein the axial end portion (34) of the elongated member includes an electrical contact device and forms an insertion member such that it is in electrical contact with a complementary receiving member of the differential scanning calorimeter, and the electrical contact device is electrically connected to a connector pad (16) of the detection unit (1).

8. The sensor assembly according to claim 7, wherein the elongated member (32) has a cylindrical outer peripheral portion (33), and the electrical contact device includes an elongated contact lug (35) that extends parallel to the longitudinal axis, is spaced apart from one another in the circumferential direction, and is connected to the connector pad (16) by a connecting wire arranged in an axially extending hollow space formed within the elongated member (32).

9. The detection unit (1) according to claim 1, further comprising at least one positioning tab (3) formed on the outer peripheral edge (4) of the disc-shaped substrate (31) and configured to be reliably fitted with a complementary positioning recess of the calorimeter.

10. A method for manufacturing a detection unit according to any one of claims 1 to 6 and claim 9, a) A step of preparing a disc-shaped substrate, b) On the disc-shaped substrate, preferably by using a thick film technique, in particular a screen printing technique, the following layers are continuously applied, i.e., - A layer of the absolute temperature measuring device, comprising the conductive trace forming the absolute temperature measuring device and the connector pad of the absolute temperature measuring device, wherein an electrical insulating layer follows, the electrical insulating layer being electrically insulating, with the sole exception being the area of ​​the connector pad in the lower part of the layer, - The layer of the electric heater device, comprising a conductive trace forming the electric heater device, a connector pad for the electric heater device, and a connector pad of the lower layer, wherein an electrical insulating layer follows, the electrical insulating layer being electrically insulating, with the sole exception being the area of ​​the connector pad of the lower layer, - The second layer of the thermoelectric device, comprising a trace forming at least a portion of the thermoelectric junction of the sensing unit, a connector pad for the second layer of the thermoelectric device, and a connector pad for the lower layer, followed by an electrical insulating layer, the electrical insulating layer being electrically insulating, with the sole exception being the area of ​​the connector pad for the lower layer, - The first layer of the thermoelectric device, comprising a trace forming at least a portion of the thermoelectric junction of the sensing unit, a connector pad for the first layer of the thermoelectric device, and a connector pad for the lower layer, followed by an electrical insulating layer, the electrical insulating layer being electrically insulating, with the sole exception being the area of ​​the connector pad for the lower layer, - Preferably, locally on the sample-side support region and the reference-side support region, the material to be applied for the pan support. The step of granting and Methods that include...

11. Use of the detection unit according to any one of claims 1 to 6 and claim 9 in power compensation operation mode, The sample-side heater and the reference-side electric heater are energized in a manner controlled to bring the differential heat flow signal close to zero. Preferably, the controlled method for energizing the electric heater device is achieved by applying a differential voltage signal to the input of a proportional controller, the proportional controller using a sensing unit that feeds the heater device from the output side of the proportional controller.

12. Use of the detection unit according to any one of claims 1 to 6 and claim 9 in a heat flux operation mode, thereby, The use of a detection unit that detects a differential thermoelectric voltage, which is the difference between the sample-side thermoelectric voltage and the reference-side thermoelectric voltage.

13. A use of a detection unit according to any one of claims 1 to 6 and 9 for simultaneously determining the heat flow to a first sample and a second sample, a) The first sample is placed in the sample pan which is positioned on the sample-side pan support region, b) The second sample is placed in the reference pan which is positioned on the reference-side pan support region, c) Thus, the heat flow to the first sample is a. At least the sample-side voltage signal, b. And preferably, the power supplied to the sample-side electric heater device Determined using, d) Thus, the heat flow to the second sample is a. At least the reference voltage signal, b. And preferably, the power supplied to the reference side electric heater device The use of the detection unit is determined using [the specified method / tool].

14. A use of a detection unit according to any one of claims 1 to 6 and 9 for determining at least one parameter, preferably a phase angle, that describes the complex heat capacity of a sample, thereby a) The sample is placed in the sample pan which is positioned on the sample-side pan support region, b) The reference pan is placed on the reference-side pan support region, c) The heating power is controlled as a function of time, modulated by selected periodic power modulation, gradually changing, or following a constant baseline. d) The detection unit is a. The sample-side voltage signal, b. The reference voltage signal, c. And preferably, a temperature signal representing the temperature associated with the heat source. Used to measure, e) Use of a sensing unit in which the functional relationship between the sample voltage signal, the reference voltage signal, and the temperature signal is evaluated to derive the at least one parameter describing the complex heat capacity.

15. A use of a detection unit according to any one of claims 1 to 6 and 9 for measuring the temperature of a sample, a) The detection unit is placed inside the temperature-controlled heat source of the differential scanning calorimeter. b) Placing the sample in the pan-shaped sample pan on the sample-side pan support region, c) To determine the temperature of the sample, use the signal from the sample-side absolute temperature measuring device, and preferably the sample-side thermoelectric voltage and / or the power supplied to the sample-side electric heater device. Use of a detection unit.

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