Measuring instrument equipped with an electrothermal converter for adjusting thermal resistance, and method of operation

Abstract

To provide a measuring instrument for thermal analysis that has an efficient and dynamic heat flux. [Solution] A measuring instrument (100) for thermal analysis of a sample is described, which comprises i) a sample container (120) for containing a sample, ii) a heating device (110) for raising the temperature of the sample container (120), iii) a cooling device (130) for lowering the temperature of the sample container (120), and a heat transfer element (140) having thermal resistance, the heat transfer element being positioned between the heating device (110) and the cooling device (130) such that a heat flux between the heating device (110) and the cooling device (130) is possible through the heat transfer element (140). The measuring instrument (100) further comprises v) an electrothermal converter (150), which is positioned between the heat transfer element (140) and the cooling device (130) such that the operation of the electrothermal converter (150) adjusts the heat flux passing through the heat transfer element (140).

Description

【Technical Field】 【0001】 The present invention relates to a measuring device for thermal analysis, in particular for (thermal) differential measurements. Furthermore, the present invention relates to a method of operating the measuring device. Furthermore, the present invention relates to a special use of a Peltier element. 【0002】 Thus, the present invention can be in the technical field of measuring devices for thermal analysis. In particular, the present invention can be in the technical field of measuring devices for differential scanning calorimeters or differential thermal analysis. 【Background Art】 【0003】 Measuring devices for thermal analysis are known in principle and include, for example, differential scanning calorimeters (DSC) and differential thermal analysis (DTA). Such measuring devices generally include a furnace in which two sample containers are present, one of the sample containers being supplied with a sample and the other sample container being provided with a control (this control may simply be an empty sample container). This structure enables the measurement of various physical properties associated with temperature changes. For example, when a phase transition or phase change occurs within the sample, a temperature difference is formed between the sample container with the sample and the sample container with the control (with the same amount of heat supplied by the furnace). In this case, the temperature difference or heat flux between the sample and the control is measured by a sensor, thereby enabling inferences about the type of phase transition or phase change. 【0004】 Generally, such measuring devices include a heating system having an electric heater for heating the furnace according to a time-temperature profile. However, in the case of thermal measurements, not only the heating curve (rising temperature profile) but also the cooling curve (falling temperature profile) is important. For many measurement applications, simply switching off the electric heater is not sufficient to achieve the required rapid cooling rate. For this reason, active cooling by a cooling system is necessary. 【0005】 In the case of heating by a heating system, on the one hand, it must be ensured that too much heat is not released from the furnace to the cooling system, otherwise the heating rate cannot be maintained. On the other hand, on the other hand, heat must be transferred sufficiently quickly towards the cooling system during each cooling process. To address this problem, it is known in the prior art to place a so-called thermal resistor as a connection between the heating system and the cooling system. 【0006】 However, due to the generally compact structure of calorimeters, the electric heater in the heating system has limitations in its output. That is, if the thermal resistance is too low, the heating system will heat up too slowly and / or fail to reach its target temperature. Conversely, if the thermal resistance is too high, the heat cannot be transferred sufficiently quickly towards the cooling system during the cooling process. 【0007】 In other words, thermal resistance has the disadvantage of removing too much heat from the heating system during the heating phase and too little heat during the cooling phase. However, thermal resistance is a fixedly mounted element, and this element is preferably made of a particularly thermally conductive metal. [Overview of the Initiative] [Problems that the invention aims to solve] 【0008】 The object of the present invention is to provide a measuring instrument for thermal analysis that has an efficient and dynamic heat flux (in particular, the thermal resistance should be as high as possible during the heating phase and as low as possible during the cooling phase). [Means for solving the problem] 【0009】 This problem is solved by subject matter having the features of the independent claim. Other embodiments are shown in the dependent claims. 【0010】 According to one aspect of the present invention, a measuring instrument for the thermal analysis of a sample (e.g., a differential scanning calorimeter) is described, the measuring instrument comprising: i) a sample housing (or sample chamber or measuring chamber) for housing a sample (and especially a control); ii) a heating device for raising the temperature of the sample housing (especially for providing a temperature profile); iii) a cooling device for lowering the temperature of the sample housing (especially for providing a temperature profile); and iv) a heat transfer element having thermal resistance (or high thermal conductivity) and a heat flux between the heating device and the cooling device via a heat transfer element. The device comprises a heat transfer element (e.g., an element having a particularly thermally conductive metal) positioned between the heating device and the cooling device so as possible, and a thermoconverter (e.g., a Peltier element, which can operate in heating mode and cooling mode) positioned between the heat transfer element and the cooling device so that the operation (e.g., control or adjustment) of the thermoconverter adjusts (selectively and to suit the purpose) the heat flux passing through the heat transfer element (or adjusts (selectively and to suit the purpose) the thermal resistance of the heat transfer path passing through the heat transfer element and the thermoconverter. 【0011】 Another aspect of the present invention describes a method of operating a measuring instrument for thermal analysis (particularly as described above), comprising a heating device and a cooling device, wherein the heating device and the cooling device are connected to each other by heat flux via a heat transfer element. The method includes i) preparing an electrothermal converter between the heat transfer element and the cooling device; ii) operating the electrothermal converter in heating mode (particularly controlled or adjusted) or switching off the electrothermal converter in order to reduce the heat flux passing through the heat transfer element (or increase the thermal resistance of the heat transfer path passing through the heat transfer element and the electrothermal converter) (particularly when a temperature rise (with respect to a sample) is provided); and iii) operating the electrothermal converter in cooling mode (particularly controlled or adjusted) in order to increase the heat flux passing through the heat transfer element (or decrease the thermal resistance of the heat transfer path passing through the heat transfer element and the electrothermal converter) (particularly when a temperature drop (with respect to a sample) is provided). 【0012】 According to another aspect of the present invention, the use of a Peltier element is described in a measuring instrument for thermal analysis to adjust (to suit the purpose) the heat flux passing through a heat transfer element (placed) between a heating device and a cooling device (in particular, the spatial arrangement of the Peltier element makes direct contact between the heat transfer element and the cooling device impossible). 【0013】 According to another aspect of the present invention, a computer program product is described which is configured to perform a method of operating a measuring instrument for thermal analysis (as described above) when the computer program product is run on a computer (particularly of a control unit, and even more particularly of a measuring instrument). [Modes for carrying out the invention] 【0014】 In this document, the concept of “measuring instrument” can refer to an apparatus specifically designed to measure the physical properties of a sample. Preferably, physical properties are thermal properties or properties observable over changes in ambient temperature. Examples of such properties may include melting temperature and glass transition temperature (particularly for plastics), kinetic considerations of chemical reactions, specific heat capacity, and determination of the purity of a substance (based on melting point changes caused by impurities). 【0015】 In this document, the concept of “sample container” can refer to a device suitable for containing a sample to be measured, either in contact with or within a measuring instrument. In particular, the sample container may have at least one sample container (e.g., a crucible) in which the sample for measurement is provided. If the measuring instrument is to perform differential measurement, for example, two sample containers are provided, one for the sample and the other for the control (the control container may be empty). Furthermore, the sample container may have known sensors to detect, for example, temperature changes in the sample container / temperature changes inside the sample container during measurement. The acquired data may be transferred to a control unit and / or evaluation unit. 【0016】 In this document, the concept of “heating device” can refer to a device suitable for providing a temperature rise (or heating) to a sample container or measurement chamber. A heating device may therefore have one (or more) heating elements. For example, a heating device may include an electric heating element particularly suited to releasing heat into the surroundings when electrical energy is supplied. The heating element may include, for example, a heating wire, a heating cable, a heating sheet, or a heating surface. The heating element may be implemented, for example, by a copper lane. The heating device may be controlled (or tuned) to provide a time-dependent temperature transition (or temperature profile) to the sample container (as described above). The heating device may be directly connected to the sample container or spatially separated from it. For example, the heating device may be located below the sample container or localized in a circular pattern around the sample container. 【0017】 In this document, the concept of “cooling device” can refer to a device suitable for providing a temperature drop (or cooling) around the sample container. In a simple embodiment, the cooling device may be a heat pipe or heat sink that transfers or decouples heat in a known manner. In another embodiment, the cooling device may have a cavity in which a cooling medium is stored or circulated. The cooling medium may be, for example, cold air, liquid nitrogen, helium, or other known cooling mediums. Furthermore, a known cryostat may be used. Furthermore, the cooling device may have a Peltier element used in cooling mode. Within the cooling device, a Peltier element operating (exclusively) in cooling mode should not be confused with the electrothermal converter described below. The cooling device may be controlled (or tuned) to provide a time-dependent temperature transition (or temperature profile) to the sample container (as described above). Advantageously, the cooling device may be positioned at least partially around the heating device and / or the sample container. In particular, the cooling device may be positioned spatially separated from the sample container. Preferably, the heating device is spatially closer to the sample containment area than the cooling device. 【0018】 In this document, the concept of a “heat transfer element” can refer, in particular, to an element (component) that has specific heat capacity or specific heat resistance and can be installed for the purpose of providing heat transfer or heat flux. For example, a heat transfer element may be provided between a heating device and a cooling device so that a heat flux is generated between the two devices via the heat transfer element. In principle, heat transfer elements may be provided in any shape and size. Possible embodiments are shown, for example, at the bottom of Figure 3. Preferably, the heat transfer element has a particularly thermally conductive material. This material may be a metal or a metallic alloy in particular. For example, nickel or copper (as an alloy) may be used. In principle, and more particularly, thermally conductive materials such as functional ceramics or carbon similar to diamond may also be considered. 【0019】 In this document, the concept of an electric thermoconverter can refer, in particular, to an element that provides a temperature difference when an electric current is flowing, and conversely, provides an electric current when a temperature difference is present. Thus, an electric thermoconverter can operate in cooling mode and (when the direction of the current is reversed) can be used in heating mode. Thus, a predetermined desired operating mode can be provided by operation (control or adjustment) by power supply. By connecting with a heat transfer element (as described above), the thermal resistance of this electric thermoconverter can be adjusted dynamically to suit the purpose. For this purpose, it is preferable that the electric heating element be positioned spatially close to the heat transfer element (especially so as to be in direct contact). Particularly preferable, the electric heating element is positioned between the heat transfer element and the cooling device such that contact between the cooling device and the heat transfer element is prevented by the electric heating element. It has become clear that operation of the electric thermoconverter in heating mode or switching off the electric thermoconverter can increase the thermal resistance of the heat transfer path between the heating device and the cooling device to suit the purpose, and operation of the electric thermoconverter in cooling mode can decrease the thermal resistance of the heat transfer path to suit the purpose. 【0020】 According to one embodiment, the thermal resistance (R) of the heat transfer element thThe formula (=l / λ·A) is, in principle, the same or unchanging. However, the thermal resistance of the thermotransmitter, and consequently the thermal resistance of the heat transfer path passing between the heat transfer element and the thermotransmitter, may be affected / modulated. In this document, the concept of a "heat transfer path" can specifically refer to the components (e.g., the heat transfer element and the thermotransmitter) located between the heating device and the cooling device. The thermal resistance of the heat transfer element may be, for example, 3K / W to 9K / W. The thermal resistance of the thermotransmitter may be, for example, -90K / W to +50K / W. 【0021】 According to one embodiment, the heat flux passing through the heat transfer element can be increased or decreased as follows, particularly due to the temperature difference between the heating device and the cooling device. Heat flux / heat flow (watts, heat output): Q=ΔT / R th Therefore, the operation of the electrothermal converter adjusts the heat flux passing through the heat transfer element. 【0022】 According to one embodiment, "adjustment" can be performed as follows: The thermal resistance of a heat transfer path (or the heat flux passing through the heat transfer element) can be increased or decreased, or the range of values ​​of the thermal resistance of the heat transfer path can be adjusted to a desired value. 【0023】 In particular, the "adjustment" of the thermal resistance (or heat flux passing through the heat transfer element) of the heat transfer path consisting of a heat transfer element and an electrothermal converter can be performed by causing the electrothermal converter to operate as a heat pump in a direction opposite to or in the direction of the temperature gradient (between the heating device and the cooling device) through the heat transfer path. 【0024】 In particular, the thermal resistance of the heat transfer path (or the heat flux passing through the heat transfer element) can be adjusted to a desired value by changing the heat pump output of the electric thermoconverter. For example, a Peltier element based on BiTe can be used as the electric thermoconverter, in which case both the operating current and the polarity of the operating voltage can be freely selected to achieve the effects described above. 【0025】 According to an exemplary embodiment, the present invention is based on the idea that when the electric heat converter is provided between the heat transfer element and the cooling device such that the operation suitable for the purpose of the electric heat converter dynamically adjusts the heat flux passing through the heat transfer element (or the thermal resistance of the heat transfer path passing through the heat transfer element and the electric heat converter), a measuring device for thermal analysis having an efficient and dynamic heat flux can be provided. In this manner, a thermal resistance is provided in the measuring device that can be made as high as possible during the heating period and as low as possible during the cooling period. 【0026】 Conventionally, with respect to the heat flux in a measuring device such as a calorimeter, the heat transfer member is provided such that the thermal resistance of the heat transfer member is an average value (or a compromise value) and is invariant, thereby providing a compromise between heating and cooling (the heat transfer member is usually a static member made of metal or ceramic). 【0027】 However, the inventor has surprisingly recognized that when an electric heat converter (e.g., a Peltier element) is attached between the heat transfer element and the cooling device, an adjustable (and thus dynamically operable) heat flux (or thermal resistance) suitable for the purpose can be realized in an effective and yet simple manner. 【0028】 The measuring device according to the present invention provides a heating rate and a cooling rate that are substantially faster than those of conventional measuring devices, and thus provides a particularly effective mode of operation. Furthermore, the described structure can be incorporated into an existing system in a simple and flexible manner. 【0029】 It might be considered known to use a Peltier element as an additional heating device or an additional cooling device in a measuring device. However, the fundamental idea of ​​the present invention is to use the electrothermal converter not as an additional heating or cooling device, but solely for the purpose of dynamically adjusting the thermal resistance in the heat flux between the heating and cooling devices to suit the required conditions. Thus, the electrothermal converter in the measuring instrument described in the claims satisfies a completely different technical problem from the prior art. Therefore, the electrothermal converter in the measuring instrument described in the claims is positioned in a completely different manner, namely directly between the cooling device and the heat transfer element. 【0030】 Furthermore, additional exemplary embodiments of the apparatus and method will be described. 【0031】 According to one embodiment, the electric thermoconverter can operate in both heating and cooling modes. This offers the special advantage of enabling highly efficient dynamic adjustment of thermal resistance in a simple manner. Electric thermoconverters having the described functional mode can be realized in a variety of ways. 【0032】 In particular, the electric thermoconverter may be embodied (efficiently and directly) using a known Peltier element, which is especially preferable. In principle, any series and / or parallel connection of Peltier elements may be used to realize the electric thermoconverter. In one embodiment, the Peltier element is constructed asymmetrically (this Peltier element is located on the characterized low-temperature side), and the low-temperature side may be oriented toward both the heat transfer element and the cooling device in order to change the thermal resistance. Thus, the Peltier element may have a high-temperature side, and the high-temperature side may be oriented toward both the heat transfer element and the cooling device in order to change the thermal resistance. 【0033】 In another embodiment, the electrothermal converter is positioned between the heat transfer element and the cooling device such that direct contact between the heat transfer element and the cooling device is impossible. In other words, the positioning of the electrothermal converter prevents direct physical contact between the cooling device and the heat transfer element. This results in the advantage that the controllability of the thermal resistance (of the heat transfer element) is independent of the direct influence of the cooling device and, consequently, more effectively possible. Without this physical separation, the cooling provided by the cooling device would undesirably affect the thermal resistance of the heat transfer element. 【0034】 In one embodiment, the separation of the heating device from the cooling device (at a high temperature in the sample chamber) results in a small amount of heating of the cooling device due to its high thermal resistance compared to the case of low thermal resistance. When the heating device is switched off at high temperatures and the thermal resistance is adjusted to a small value, the full cooling capacity of the (unheated) cooling device is immediately available. 【0035】 In another embodiment, the sample container has two sample containers, and the measuring instrument is configured to perform differential measurements on the two sample containers. In this configuration, the described advantageous measuring instrument can be directly used for industrial measurements. 【0036】 In an exemplary example, an encapsulated sample container containing a sample, such as an aluminum crucible, and a second sample container (control) without contents are subjected to the same temperature program. In this case, a temperature change occurs compared to the empty sample container as a result of the sample's heat capacity and the exothermic or endothermic processes or phase changes such as melting or evaporation, and the thermal energy then flows into or out of the corresponding processes. 【0037】 In other embodiments, the measuring instrument is a differential scanning calorimeter or differential thermal analyzer. In this form as well, the advantageous measuring instruments described can be used directly for industrial measurements. DSC and DTA are (as described above) generally known and can be carried out particularly efficiently using the measuring instruments described. 【0038】 In another embodiment, the heating device is configured to provide a temperature transition that increases over time. Additionally or separately, the cooling device is configured to provide a temperature transition that decreases over time. Thus, the heating and / or cooling devices are not used solely for heating / cooling themselves, but rather to heat / cool as intended to provide a predetermined temperature (time) profile for the sample to be measured. 【0039】 In other embodiments, the cooling device comprises at least one of the following: a heat pipe, a heat sink, a cryostat, a Peltier element, and a heat exchanger. This has the advantage of directly embodying a known and established cooling system. In particular, the cooling device is configured as a closed unit that can be spatially separated from other components of the measuring instrument (heat transfer element, heating device) using an electrothermal converter. 【0040】 In one embodiment, the thermal energy transferred from the low-temperature side of the Peltier element is re-released on the high-temperature side of the Peltier element. Preferably (especially with respect to the efficiency and protection of the Peltier element), the high-temperature side of the Peltier element is cooled, for example, by direct air cooling. In one embodiment, the pure surface of the Peltier element is not sufficient to transfer energy, and a heat exchanger can be used, for example. An example of this type of heat exchanger is a known thin-film heat sink. 【0041】 According to another embodiment, the measuring instrument is configured such that the operation of the electrothermal converter involves controlling or adjusting the thermal resistance of the heat transfer path. This has the advantage of allowing for dynamic (particularly stepless) adaptation of the thermal resistance. 【0042】 This control / adjustment can be performed automatically using the control unit of the measuring instrument. For example, a corresponding computer program for this purpose may be stored in the data carrier. In special embodiments, the control unit may have artificial intelligence (e.g., by a neural network) that further improves the control / adjustment by a self-learning algorithm. Furthermore, the control / adjustment may be performed manually by the user (especially during measurement). The operation of the electrothermal converter, particularly the Peltier element, can be performed in known manner. 【0043】 In another embodiment, the measuring instrument is configured such that the operation of the thermotransmitter in heating mode (or the switching off of the thermotransmitter) reduces the heat flux passing through the heat transfer element (or increases the thermal resistance of the heat transfer path). Additionally or separately, the measuring instrument is configured such that the operation of the thermotransmitter in cooling mode increases the heat flux passing through the heat transfer element (or decreases the thermal resistance of the heat transfer path). 【0044】 Increased thermal resistance prevents much of the generated heat from being transferred from the heating device. Simultaneously, the increased thermal resistance acts as a shield against the cooling device. Reduced thermal resistance allows for rapid transfer of heat from the heated sample container. At the same time, the cooling action of the cooling device is no longer blocked. 【0045】 This preferred embodiment enables the following operation method. (i) Step of preparing the sample in the sample container of the measuring instrument. ii) a step of increasing the thermal resistance of the heat transfer path when increasing the temperature of the sample containment section, and / or iii) a step of decreasing the thermal resistance of the heat transfer path when decreasing the temperature of the sample containment section. 【0046】 In another embodiment, the measuring instrument is configured such that the operation of the thermotransmitter in cooling mode allows for lower temperatures within the instrument (particularly below -20°C, even more specifically below -30°C, and even more specifically below -40°C) than when the thermotransmitter is not operating in cooling mode. This can have the advantage of enabling particularly efficient cooling and lower minimum temperatures in the sample chamber, in addition to the dynamic adjustment of thermal resistance. 【0047】 An electrothermal converter can be used to lower the temperature as low as possible when using a cooling device. In this manner, significantly lower temperatures (down to -40°C) can be achieved in the measurement chamber during normal cooling (e.g., air cooling). The use of the described measuring instrument increases the possible rate of temperature change, making it possible to achieve a minimum temperature lower than that of the cooling device itself. 【0048】 In another embodiment, the heat transfer element has a metal (e.g., nickel or nickel alloy, copper or copper alloy, aluminum or aluminum alloy, functional ceramic). This can have the advantage of producing an effective and robust heat flux through established and verified materials. [Brief explanation of the drawing] 【0049】 [Figure 1] This shows a measuring instrument according to an exemplary embodiment of the present invention. 【0050】 [Figure 2] This shows a measuring instrument according to another exemplary embodiment of the present invention. 【0051】 [Figure 3] This shows another exemplary embodiment of a measuring instrument according to the present invention. [Examples] 【0052】 Before describing the drawings in detail, some specific embodiments of the present invention are described below. 【0053】 According to exemplary embodiments, it is advantageous for dynamic temperature control if the thermal resistance between the sample chamber (sample housing) and the cooling system (cooling device) is high during heating (or when a high temperature needs to be maintained) and low during cooling (or when a low temperature needs to be achieved). This problem is solved by using a Peltier element as a variable thermal resistance, which is advantageous for the dynamic and thermal design of the entire measuring instrument. In this case, the Peltier element does not provide additional heating or cooling to the furnace (heating device). 【0054】 In another embodiment, the Peltier element is heated (or switched off) during the heating phase of the measuring instrument, resulting in high thermal resistance. During the cooling phase, the Peltier element is cooled, resulting in low thermal resistance (use of the Peltier element as a variable thermal resistance between the heating and cooling devices). When the Peltier element is not energized or is heated, the thermal resistance between the heating and cooling devices increases. 【0055】 Figure 1 schematically shows the structure of a measuring instrument 100 according to an exemplary embodiment of the present invention. The measuring instrument 100 comprises a sample container 120 for accommodating one or more samples (e.g., two sample containers for differential measurement). Below the sample container 120, a heating device is positioned to raise the temperature of the sample container 120. Preferably, the heating device 110 is configured to provide a time-dependent temperature progression (i.e., temperature profile) with respect to the sample. Below the heating device 110, a heat transfer element 140 having thermal resistance (or specific heat capacity) is positioned. In one embodiment, the heat transfer element has a nickel alloy. The measuring instrument 100 further comprises a cooling device 130 to lower the temperature of the sample container 120 (or to lower the temperature inside the measuring instrument 100). Preferably, the cooling device 130 is configured to provide a time-dependent temperature progression (i.e., temperature profile) with respect to the sample. The heating device 110 and the cooling device 130 are spatially separated from each other. Nevertheless, the heat flux between the heating device 110 and the cooling device 130 is made possible by the heat transfer element 140. However, the heat transfer element 140 is not directly coupled to the cooling device 130. Instead, an electrothermal converter 150 (e.g., a Peltier element) is directly positioned between the heat transfer element 140 and the cooling device 130 so that direct spatial (physical) contact (or touch) between the cooling device 130 and the heat transfer element 140 is impossible. In this case, the electrothermal converter 150 is positioned so that its operation can dynamically adjust the heat flux passing through the heat transfer element 140 (or the thermal resistance of the heat transfer path passing through the heat transfer element 140 and the electrothermal converter 150) to suit the purpose. Operation of the electrothermal converter 150 in heating mode (or switching off the electrothermal converter 150) causes a decrease in heat flux (or an increase in the thermal resistance of the heat transfer path 140, 150). Therefore, this mode is used when the temperature of the sample containment section 120 needs to be increased. Due to the increased thermal resistance, less of the generated heat is transferred from the heating device. At the same time, the increased thermal resistance acts as a shield against the cooling device.In contrast, the operation of the electric thermoconverter 150 in cooling mode causes an increase in the heat flux passing through the heat transfer element 140 (or a decrease in the thermal resistance of the heat transfer paths 140 and 150). Therefore, this mode is used when it is necessary to lower the temperature of the sample container 120. The reduced thermal resistance allows the heat from the heated sample container to be rapidly transferred. At the same time, the cooling action of the cooling device is no longer blocked. 【0056】 Figure 2 schematically shows the structure of a measuring instrument 200 according to another exemplary embodiment of the present invention. Unlike Figure 1, two cooling devices 130 are provided, each of which is positioned to the side of the heat transfer element 140 or the heating device 110. Thus, two electrothermal converters 150 are used, each of which is inserted between the heat transfer element 140 and the cooling device 130. Alternatively, it may be shown that a single cooling device 130 surrounds the heat transfer element 140 or the heating device 110. 【0057】 Figure 3 shows an embodiment of the measuring instrument 300 schematically described in Figure 2, according to an exemplary embodiment of the present invention. Along the main axis A, from top to bottom, are arranged a sample housing section 120 (measuring chamber), a heating device 110, a first portion 141 of the heat transfer element 140, a second portion 142 of the heat transfer element 140, and an insulating base 180. The first portion 141 of the heat transfer element 140 is formed in a tubular (cylindrical) shape and connects the heating device 110 to the second portion 142 of the heat transfer element 140, which is formed in a flange or disc shape. While the illustrated embodiment of the heat transfer element 140 has been found to be energy-engineerally preferable, numerous other (preferred) embodiments of the heat transfer element 140 are also possible. A thermal coupling element 145 is fixed around the first portion 141 and the second portion 142 of the heat transfer element 140, and this thermal coupling element is, in principle, also the heat transfer element 140 (e.g., made of copper). The thermal coupling element 145 is optional and, in the illustrated example, is used for effective fixation (of the cooling device 130). A Peltier element 150, used as an electrothermal converter, is fixed along the heat transfer element 140 (particularly outside the thermal coupling element 145) to adjust the thermal resistance of the heat transfer element 140 to suit the purpose. The cooling device 130 has two heat sinks, which are mounted laterally to the heat transfer element 140 (or perpendicular to the main axis A). As already described earlier, the Peltier element 150 is directly fixed (sandwiched) between the heat transfer element 140 and the cooling device 130, thereby preventing any physical (spatial) contact between the heat transfer element 140 and the cooling device 130. 【0058】 It should be noted that “having” does not exclude other elements or steps, and “one” or “one” does not exclude multiple elements or steps. Furthermore, it should be noted that any feature or step described with reference to one of the above embodiments may be used in combination with other features or steps of another embodiment described above. The reference numerals in the claims are not considered limiting. [Explanation of symbols] 【0059】 100, 200, 300 measuring equipment 110 Heating device 120 Sample storage section 130 Cooling device 140 Heat transfer elements 141 Heat transfer element of the first part 142 Heat transfer element of the second part 145 Thermal coupling element 150 Electrical heating converters, Peltier elements 180 base

Claims

[Claim 1] In a measuring instrument for thermal analysis of a sample, the measuring instrument is: A sample storage section for accommodating the aforementioned sample, A heating device for raising the temperature of the sample containment section, A cooling device for lowering the temperature of the sample containment section, A heat transfer element having thermal resistance and positioned between the heating device and the cooling device such that a heat flux between the heating device and the cooling device is possible via the heat transfer element, The operation of the electric thermoconverter adjusts the heat flux passing through the heat transfer element, and the electric thermoconverter is positioned between the heat transfer element and the cooling device. A measuring instrument equipped with a function for thermal analysis of a sample. [Claim 2] The aforementioned electric heating converter can be operated in heating mode and / or cooling mode. The measuring instrument according to claim 1. [Claim 3] The aforementioned electric heating converter has a Peltier element. The measuring instrument according to claim 1 or 2. [Claim 4] The electric heat converter is positioned between the heat transfer element and the cooling device such that direct contact between the heat transfer element and the cooling device is impossible. A measuring instrument according to any one of claims 1 to 3. [Claim 5] The sample storage unit has two sample containers, and the measuring instrument is configured to perform difference measurements between the two sample containers. A measuring instrument according to any one of claims 1 to 4. [Claim 6] The measuring instrument is a differential scanning calorimeter or a differential thermal analysis measuring instrument. A measuring instrument according to any one of claims 1 to 5. [Claim 7] The heating device is configured to provide a temperature progression that increases over time, and / or The cooling device is configured to provide a temperature transition that decreases over time. A measuring instrument according to any one of claims 1 to 6. [Claim 8] The cooling device comprises at least one of the following: a heat pipe, a heat sink, a cryostat, a Peltier element, and a heat exchanger. A measuring instrument according to any one of claims 1 to 7. [Claim 9] The measuring instrument is configured such that the operation of the electrothermal converter includes controlling or adjusting the thermal resistance of the heat transfer path. A measuring instrument according to any one of claims 1 to 8. [Claim 10] The aforementioned measuring instrument is The operation of the electric heat converter in heating mode or the switching off of the electric heat converter increases the thermal resistance of the heat transfer path passing through the heat transfer element and the electric heat converter, and decreases the heat flux passing through the heat transfer element. and / or The operation of the electric thermoconverter in cooling mode reduces the thermal resistance of the heat transfer path passing between the heat transfer element and the electric thermoconverter, and increases the heat flux passing through the heat transfer element. A measuring instrument according to any one of claims 1 to 9. [Claim 11] The measuring instrument is configured such that the operation of the electric thermotransmitter in cooling mode allows for lower temperatures within the instrument, particularly below -40°C, than when the electric thermotransmitter is not operating in cooling mode. A measuring instrument according to any one of claims 1 to 10. [Claim 12] The heat transfer element has a metal, particularly nickel or a nickel alloy, or a functional ceramic. The measuring instrument according to any one of claims 1 to 11. [Claim 13] In a method of operating a measuring instrument for thermal analysis, comprising a heating device and a cooling device that are interconnected with respect to heat flux by a heat transfer element, the method of operating the measuring instrument for thermal analysis is: The steps include preparing an electric thermoconverter between the heat transfer element and the cooling device, To reduce the heat flux passing through the heat transfer element, the steps include operating the electric heat converter in heating mode or switching off the electric heat converter. The steps include: operating the electric thermoconverter in cooling mode in order to increase the heat flux passing through the heat transfer element; A method of operating measuring instruments for thermal analysis, including the operation of such instruments. [Claim 14] The operating method of the measuring instrument for the aforementioned thermal analysis is as follows: The steps include preparing a sample in the sample storage section of the measuring instrument, When raising the temperature of the sample containment section, the steps include increasing the thermal resistance of the heat transfer path passing through the heat transfer element and the electrothermal converter, When lowering the temperature of the sample containment section, the steps include reducing the thermal resistance of the heat transfer path passing through the heat transfer element and the electrothermal converter. A method for operating a measuring instrument for thermal analysis according to claim 13, further comprising one or more of the following: [Claim 15] The use of a Peltier element to adjust the heat flux passing through a heat transfer element between a heating device and a cooling device within a measuring instrument for thermal analysis to suit a specific purpose. [Claim 16] A computer program for causing a computer, particularly a control unit, to perform the method of operating a measuring instrument for thermal analysis according to claim 13 or 14.

Images