Sample carrier device for measuring devices for thermal sample analysis, measuring device

The sample carrier device with a separated reference and sample unit connected by a heat flow element addresses the bulkiness and limited functionality of existing thermal analysis equipment, enabling compact, user-friendly, and versatile thermal sample analysis.

DE102024129235B3Active Publication Date: 2025-07-17NETZSCH GERATEBAU GMBH
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Patent Information

Application Number
DE102024129235
Authority / Receiving Office
DE · DE
Patent Type
Patents
Current Assignee / Owner
Filing Date
2024-10-10
Publication Date
2025-07-17
Estimated Expiration
2044-10-10

AI Technical Summary

Technical Problem

Existing thermal sample analysis equipment is bulky and limited in functionality, often requiring separate devices for different analysis techniques, and lacks a compact design suitable for mobile applications.

Method used

A sample carrier device with a main carrier structure holding a reference unit and a sample carrier unit spatially separated without direct contact, connected by a defined heat flow element, enabling dynamic differential calorimetry without a reference sample and allowing for space-saving integration in measuring devices.

Benefits of technology

Enables compact, user-friendly thermal sample analysis with simultaneous measurement capabilities, facilitating easy calibration and maintenance, and supporting multiple analysis methods in a single device.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention relates to a sample carrier device (1) for measuring devices for thermal sample analysis. This sample carrier device (1) comprises a main carrier structure (2), a reference unit (5) with a first thermocouple device (11), and a sample carrier unit (6) with a second thermocouple device (12), wherein the main carrier structure (2) is designed to keep both the reference unit (5) and the sample carrier unit (6) spatially separated from one another. A defined heat flow element (14) is also arranged between the reference unit (5) and the sample carrier unit (6). In addition, a measuring device (100) for thermal sample analysis is presented.
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Description

TECHNICAL FIELD OF THE INVENTION

[0001] The present invention relates to a sample carrier device for measuring devices for thermal sample analysis and a measuring device for thermal sample analysis. BACKGROUND OF THE INVENTION

[0002] Thermal sample analysis devices are already available in a wide variety of designs and are available on the market. To open up further fields of application for this technology, there is currently a need not only to integrate more functions into each device unit, but also to develop a more compact design, enabling mobile use in the future.

[0003] Current equipment sometimes has dimensions that could be perceived as cumbersome and hinder new fields of application. Furthermore, current equipment usually only offers a limited range of possible analysis techniques, so additional equipment would have to be purchased to provide additional analysis techniques.

[0004] In this respect, equipment is known that is suitable either exclusively for differential thermal analysis (DTA) or for dynamic differential scanning calorimetry (DSC), or for thermogravimetry (TGA). TGA is used for the temperature- or time-dependent investigation of physical processes and chemical reactions associated with mass changes.

[0005] The differences often lie in the specific handling of the respective samples. DTA and DSC, in particular, require a more complex design, as the equipment for these, for example, is usually equipped with two sample crucibles, one containing the material to be analyzed and the other containing the reference material. TGA equipment, on the other hand, generally requires only one crucible for the material to be analyzed. Essential for TGA are a balance integrated into the instrument, which detects the sample's mass changes, and temperature measurement of the sample.

[0006] When setting up for DTA or DSC, the two crucibles are then either heated or cooled in a targeted manner and under conditions that are as similar as possible. Both crucibles are measured with regard to their thermal behavior in order to determine differences in the thermal behavior of the two materials.

[0007] Simultaneous thermal analysis (STA) methods are also known, in which the DTA or DSC and TGA methods are combined.

[0008] For future devices, it would be desirable to provide a simpler design that could also enable more advanced analysis methods.

[0009] The following information is already known from the state of the art.

[0010] The document DE 11 2008 001 462 B4 shows a thermal measuring system comprising: a measuring arrangement for receiving a sample, wherein the measuring arrangement comprises an elongated cylinder, an infrared lamp arrangement arranged circumferentially around the elongated circular cylinder and comprising an infrared reflector having a cavity with a length approximately the same as that of the elongated cylinder and further comprising a base plate, a thermal resistor coupled to the measuring arrangement and having a variable thermal resistance value, wherein the thermal resistor comprises: a gas-filled gap, a plate with high thermal conductivity formed integrally with the measuring arrangement, and a heat sink surface arranged on one side of the gas-filled gap opposite the plate with high thermal conductivity, a heat sink,which is thermally coupled to the thermal resistor and to the infrared lamp assembly, wherein the heat sink has an outer portion configured to bear against the base plate, and further comprises a heat sink extension configured to extend through an opening in the base plate when the outer portion is in contact with the base plate, and further comprises a sealing assembly coupled to the measuring assembly, wherein the thermal resistor is operable to change the thermal resistance value between the measuring assembly and the heat sink during sample measurement by changing one or more of changing a total pressure within the gap from about atmospheric pressure to a vacuum and changing a composition of the gas contained in the gap, and wherein the sealing assembly is operablethat it adjusts a distance between the high thermal conductivity plate and the heat sink extension such that the gas-filled gap with a vertical height of less than a few tenths of a millimeter is created between the high thermal conductivity plate and a top surface of the heat sink extension.

[0011] The document DE 11 2018 006 122 T5 shows a heat flow measuring system including a first wire, a first heat flow sensor provided individually in the middle of the first wire, a second wire including a first end connected to the first wire at a position closer to a first end of the first wire than the first heat flow sensor, the second wire being formed of the same material as that of the first wire, a second heat flow sensor provided individually in the middle of the second wire, a first detection unit that detects a voltage between opposite ends of the first wire, and a second detection unit that detects a voltage between the first end of the first wire and a second end of the second wire. SUMMARY OF THE INVENTION

[0012] Against this background, the present invention is based on the object of providing a sample carrier device for measuring devices for thermal sample analysis and a measuring device for thermal sample analysis, which at least partially overcome the aforementioned disadvantages.

[0013] This object is achieved by a sample carrier device for measuring instruments having the features of patent claim 1 and by a measuring instrument for thermal sample analysis having the features of patent claim 16.

[0014] Accordingly, a sample carrier device for measuring instruments for thermal sample analysis is provided, comprising a main support structure, a reference unit, which does not support a reference sample, with a first thermocouple device, and a sample carrier unit with a second thermocouple device. The main support structure is designed to keep both the reference unit and the sample carrier unit spatially separated from one another. The reference unit and sample carrier unit are provided without direct contact with one another. In addition, a defined heat flow element is arranged between the reference unit and the sample carrier unit, wherein the arranged heat flow element connects the two components.

[0015] Furthermore, a measuring device for thermal sample analysis is provided, which comprises a sample carrier device according to the invention and a weight measuring device for detecting a sample mass of a sample to be examined.

[0016] One idea underlying the invention is to provide a compact sample carrier device which can be conveniently provided in measuring devices for thermal sample analysis with spatially limited possibilities, without having to accept any loss of functionality.

[0017] In particular, the invention presented allows measurements in the sense of dynamic differential scanning calorimetry (DSC) to be carried out despite a compact design with a simple reference unit that does not carry a reference sample, since the required calibration steps before a first sample analysis can be carried out simply and user-friendly using the defined heat flow element provided.

[0018] In deviation from classic definitions of the DSC method, a recent basic standard on the DTA (DTA = Differential Thermal Analysis) and DSC methods (DIN 51007:2019-04) does not speak of a “defined heat flow path”, but rather of a clear separation between Differential Thermal Analysis (DTA) for measuring the temperature difference and Dynamic Differential Scanning Calorimetry (DSC), which additionally enables the measurement of the heat flow difference between sample and reference.

[0019] Ultimately, it is important to be able to establish the calibration required to measure the heat flow difference. The proposed defined heat flow element can therefore meet this requirement and be used advantageously for these purposes without the need for a complex construction with a reference sample in an additional sample vessel (sample crucible).

[0020] The inventive sample carrier device for measuring devices for thermal sample analysis can thus be used advantageously for measuring a temperature difference and optionally a heat flow between a sample and a reference, wherein the reference is unchangeable and can be firmly connected to the respective measuring device at least temporarily via the sample carrier device.

[0021] At the same time, the inventive sample carrier device is designed, when arranged accordingly in a measuring device for thermal sample analysis, to enable a measurement of a respective temperature on a sample which is arranged, for example, in a container in the sample carrier unit.

[0022] The sample carrier device has a manageable number of components for the desired functionality, so that it can be accommodated in a measuring device for thermal sample analysis in a space-saving manner.

[0023] In this respect, the sample carrier device can be used, for example, in a surrounding measuring device for thermal sample analysis. It can be integrated into a heating and cooling device with a small interior space of a measuring device for thermal sample analysis in a space-saving manner.

[0024] The inventive sample carrier device for measuring instruments for thermal sample analysis is also designed to be used advantageously when it is necessary to calculate a heat flow from the temperature difference between the sample and the reference unit with the aid of a calibration.

[0025] In the context of the presented invention, the term "spatial" should be understood in relation to three dimensions. In other words, the reference unit and sample carrier unit are designed without direct contact with each other. Only the arranged heat flow element connects the two components in such a way that a heat flow can flow between them.

[0026] The advantages mentioned above also apply, to the extent transferable, to the presented inventive measuring device for thermal sample analysis.

[0027] According to one embodiment of the sample carrier device, it is provided that the defined heat flow element is selected from: metal wire, copper wire, platinum wire, platinum alloy wire, nickel-chromium wire, nickel alloy wire, metal sheet, copper sheet, platinum sheet, platinum alloy sheet, nickel-chromium sheet, nickel alloy sheet, metal rod, copper rod, platinum rod, platinum alloy rod, nickel-chromium rod, nickel alloy rod.

[0028] Space-saving concepts are thus particularly easy and advantageous to implement. Furthermore, the selected materials are sufficiently well-known, allowing the desired calibration steps to be carried out simply and easily.

[0029] According to a further development of the sample carrier device, it is provided that the main carrier structure is designed to hold the reference unit below the sample carrier unit.

[0030] The resulting overall size can therefore have a defined maximum size, since the two components are arranged one above the other, so that space-saving concepts can be realized, for example, by selecting the same size of the components.

[0031] According to a further development of the sample carrier device, the main support structure comprises at least a first holding element, which is designed to reversibly accommodate both the reference unit and the sample carrier unit. Since the number of required components can thus be further reduced, space-saving concepts can be implemented particularly advantageously.

[0032] According to one embodiment of the sample carrier device, it is provided that the main support structure comprises a second holding element which is designed to receive respective connecting line sections of the first and second thermocouple devices and to hold the first holding element.

[0033] A modular structure in the manner presented has the advantage that particularly user-friendly concepts can be implemented in order to facilitate, for example, maintenance work or the replacement of retained components.

[0034] According to one embodiment of the sample carrier device, it is provided that the second holding element comprises a first end region which is designed to be received by the first holding element, and a second end region, opposite the first end region, which is designed to receive a plug contact unit of the sample carrier device for connecting the respective connecting line sections of the first and second thermocouple devices to a measuring device.

[0035] In this way, the sample carrier device can be plugged into a measuring device in a user-friendly and simple manner, so that, for example, interchangeability with another sample carrier device or upcoming maintenance work in connection with replacement processes of supported components or structures can be carried out particularly easily and advantageously.

[0036] According to a further development of the sample carrier device, it is provided that the sample carrier unit comprises holding means for holding respective sample containers, which are designed to be flexibly adjustable, so that respective sample containers of different sizes and different materials can each be individually and reversibly received by the sample carrier unit.

[0037] In this respect, the sample carrier device according to the invention is designed to accommodate different containers for holding respective samples. The respective containers can be of the type commonly used in thermal analysis. In this respect, the containers can be different crucibles that differ in size, for example, with regard to an average diameter.

[0038] In general, various crucibles with different shapes can also be accommodated, as the holding means can be designed to be flexible enough for this purpose. The containers can also be made of different materials, as the holding means can be designed to be flexible enough for this purpose. Typically, the container is placed on the sample carrier device before the measurement and removed again after the measurement.

[0039] According to one embodiment of the sample carrier device, it is provided that the first holding means is made of aluminum oxide (Al2O3).

[0040] Since this material is a poor thermal conductor, the designated heat flow path can be easily implemented as intended using the defined heat flow element. Furthermore, since it is a highly heat-resistant material, this type of holding device is particularly well-suited for use in areas of a measuring device intended for heating the respective samples.

[0041] According to one embodiment of the sample carrier device, it is provided that the reference unit and the sample carrier unit are arranged one above the other without direct contact and each have a minimum diameter which essentially corresponds to at least twice the diameter of the second holding element.

[0042] This makes space-saving concepts advantageous. Various diameters are conceivable, with each component also being able to have a specific diameter. However, the minimum limit of twice the diameter must not be exceeded. This has the advantage of ensuring optimal arrangement in specific measuring devices at all times.

[0043] According to one embodiment of the sample carrier device, it is provided that the sample carrier unit can be reversibly fastened to the first holding element by means of at least one first plug connection.

[0044] Sample carrier unit exchanges can thus be carried out conveniently and within a user-friendly time interval.

[0045] According to one embodiment of the sample carrier device, it is provided that the reference unit can be reversibly fastened to the first holding element by means of at least one second plug connection.

[0046] Exchanges of reference units can thus be carried out conveniently and within a user-friendly time interval.

[0047] According to one embodiment of the sample carrier device, it is provided that the first holding element can be reversibly fastened to the second holding element by means of at least one plug connection.

[0048] In this way, an even better modular design can be promoted, so that, for example, flexible and user-friendly concepts can be provided for maintenance work or replacement of components of the sample carrier device.

[0049] According to one embodiment of the sample carrier device, it is provided that the at least one plug connection between the first and second holding element has a substantially conical shape.

[0050] This type of plug-in connection offers the advantage of providing user-friendly reversibility and ensuring reliable strength even under high temperature fluctuations, resulting in a particularly reliable and stable sample carrier device.

[0051] According to one embodiment of the sample carrier device, it is provided that the sample carrier unit is essentially made of a metal foil, wherein the metal is selected from: platinum, platinum alloy, nickel-chromium, nickel alloy, steel and similar alloys, and wherein a thickness of the metal foil is between 0.02 and 3 mm, preferably between 0.03 and 2 mm, preferably between 0.05 and 1 mm.

[0052] Space-saving concepts for the sample carrier device can thus be provided even more advantageously, since the sample carrier unit requires only a very small volume of space in order to be functional for the intended purpose.

[0053] According to one embodiment of the sample carrier device, it is provided that respective plug connections are reinforced with at least one ceramic adhesive.

[0054] This allows the sample support device to be used for applications requiring particularly high stability. For example, the ceramic adhesive used can be selected and formulated to achieve temperature resistance up to 1,700 °C. While reversibility may be limited, detachment processes can still be achieved with a certain amount of force, if necessary. Rebonding can then be performed.

[0055] According to one embodiment of the measuring device, it is provided that the measuring device is provided without a weight measuring device for detecting a sample mass of the sample to be examined. BRIEF DESCRIPTION OF THE DRAWINGS

[0056] The invention is explained below with reference to the figures of the drawings. The figures show: Fig. 1 a schematic side view of a sample carrier device for measuring instruments for thermal sample analysis; Fig. 2 shows a further schematic side view of an alternative sample carrier device for measuring instruments for thermal sample analysis; Fig. 3 is a further schematic side view of a sample carrier device for measuring instruments for thermal sample analysis; Fig. 4 a schematic plan view of a sample carrier device for measuring instruments for thermal sample analysis without a sample carrier unit; Fig. 5 a schematic representation of a measuring device for thermal sample analysis.

[0057] In the figures, the same reference symbols denote identical or functionally identical components, unless otherwise stated. DETAILED DESCRIPTION OF EMBODIMENTS OF THE INVENTION

[0058] Fig. 1 shows a schematic side view of a sample carrier device 1 for measuring devices for thermal sample analysis.

[0059] The sample carrier device 1 is shown with a main support structure 2. The main support structure 2 comprises a first and a second holding element 3, 4. In the Fig. In the embodiment shown in Figure 1, the second holding element 4 holds the first holding element by means of holding means not shown in detail.

[0060] For example, it can be a plug-in connection or a screw connection by means of which the two holding elements 3, 4 are reversibly connected to one another. In a variant embodiment not shown in detail, it is conceivable that the two holding elements 3, 4 are provided essentially as a single piece.

[0061] In the schematic side view shown, the first holding element 3 has a substantially rectangular shape, wherein, with respect to the image plane, it is provided above the second holding element 4 and spatially projects beyond the second holding element 4 in lateral regions. The main support structure 2 is provided in a substantially rotationally symmetrical manner in the embodiment variant shown. The first holding element 3 has a downwardly directed part (with respect to the image plane) which is suitable for establishing a mechanical connection with the second holding element 4. This part has larger external dimensions than the holding element 4. This makes it possible, for example, for this downwardly directed part of the holding element 3 to receive the holding element 4 by being inserted.

[0062] The retaining element 4 is depicted as a rod-shaped and essentially cylindrical shape. Alternative shapes are conceivable in embodiments not shown in detail. For example, it is conceivable that a substantially identical shape results downwards, with a rectangular shape or the like being provided instead of a cylindrical shape.

[0063] The first holding element 3 is designed to reversibly receive both a reference unit 5 shown and a sample carrier unit 6 shown of the sample carrier device 1.

[0064] In the schematic side view shown, the reference unit 5 has a substantially rectangular shape, being provided below the sample carrier unit 6 with respect to the image plane.

[0065] In the schematic side view shown, the sample carrier unit 6 also has a substantially rectangular shape, being provided above the reference unit 5 with respect to the image plane.

[0066] The sample carrier unit 6 can be reversibly fastened to the first holding element 3 by means of two first plug connections 7. For this purpose, the first holding element 3 can have respective slots into which the two first plug connections 7 can be inserted with a substantially precise fit.

[0067] The number of first plug connections 7 can vary in embodiments not shown in detail, in which case the number of slots in the first holding element 3 must be adjusted accordingly. For example, three or four first plug connections 7 can also be provided, which are located at essentially equal spacing in an outer region of the sample carrier unit 6 and equally protrude downwards (relative to the image plane) at essentially a right angle.

[0068] These two first plug connections 7 are provided on opposite lateral areas of the sample carrier unit 6 and project downwards from it essentially at right angles, wherein they are provided in the lower area plugged into the first holding element 3.

[0069] These two first plug connections 7 can, as shown, be provided as separate components that are firmly connected to the sample carrier unit 6. Alternatively, it is conceivable that the sample carrier unit 6 and the two first plug connections 7 are provided as a single piece and thus represent a structural unit. In both variants, the sample carrier unit 6 and the two first plug connections 7 can be made of the same material and have essentially the same thickness. For example, it is conceivable that they are made of a metal foil or a flexible metal plate.

[0070] In an embodiment variant not shown in more detail, it is conceivable that the two first plug connections 7 are each provided so as to be pushed through the first holding element 3 so that they protrude from the bottom of the first holding element 3 with respect to the image plane, wherein the projecting portion of the respective first plug connections 7, which can also be referred to as tabs, is then rotated or twisted, for example, by 90° or more, for example 95°, 100° or 120 to 150° or the like.

[0071] Additionally, a small amount of ceramic adhesive or the like can be applied to this respective twisted or tangled location to provide additional stability. The amount can, for example, be selected such that sufficient stability can be provided while still allowing the sample carrier unit 6 connected to the first holding element 3 to be separated under the application of force.

[0072] The reference unit is shown reversibly attached to the first holding element 3 by means of two second plug connections 8. These second plug connections 8 project downwards essentially at right angles and are each provided on an outer side of the first holding element 3.

[0073] At this outer region of the first holding element 3, they protrude beyond a longitudinal center of the first holding element 3. On the opposite side, hidden in this side view, there are portions of these second plug connections 8, which, together with the illustrated parts of the second plug connections 8, form a clamp-like structure, so that the second plug connections 8 are plugged onto the first holding element 3.

[0074] In an embodiment variant not shown in detail, it is conceivable that the second plug connections 8 are each plugged onto the first holding element 3 as shown, with respective end regions of the respective parts projecting downwards (relative to the image plane) beyond the first holding element 3.

[0075] The illustrated second plug connections 8 are also shown connected to one another, wherein a connection region 9 has the same side length as the reference unit 5 and is provided below it.

[0076] In a variant embodiment not shown in detail, it is conceivable that this connection area 9, on which the second plug connections 8 are arranged, is provided in one piece together with the reference unit 5 and the second plug connections 8. It is also conceivable that these are merely interconnected structures, with at least the reference unit 5 being provided from a different material. In this respect, it is conceivable that the connection area 9 and the second plug connections 8 together represent a material unit made of one material and that the reference unit 5 is correspondingly provided from a different material, which differs from the material of the material unit at least with regard to its heat-conducting properties.

[0077] The reference unit 5 and the sample carrier unit 6 are shown spatially separated from each other, with the main carrier structure 2 being designed specifically for this purpose.

[0078] The sample carrier unit 6 has, relative to the image plane, a total of three holding means 10 above, which are connected to a main body of the sample carrier unit 6. This connection can also be material. In other words, the respective holding means 10 can also be a fixed component of the sample carrier unit 6. The holding means 10 each protrude (relative to the image plane) essentially at right angles upwards and are provided for holding respective sample containers (not shown in detail). The holding means 10 are designed to be flexibly adjustable, so that respective sample containers (not shown in detail) of different sizes and different materials can each be reversibly accommodated individually by the sample carrier unit 6.For example, sample containers containing a sample to be measured, which have different sizes, particularly with regard to their respective average diameter, can be accommodated by the sample carrier unit 6, with the holding means 10 then ensuring a certain stability during this accommodation. For example, the holding means 10 can be provided in a flexible manner so that they can be bent toward the respective walls of the accommodated sample container in order to create corresponding holding forces, by means of which the accommodated sample container is held approximately centrally in the sample carrier unit 6.

[0079] The sample carrier device 1 for measuring instruments for thermal sample analysis is also shown with the reference unit 5 with a first thermocouple device 11 and the sample carrier unit 6 with a second thermocouple device 12. Of the first and second thermocouple devices 11, 12, only respective thermocouple wires 13 are shown in Fig. 1. The corresponding thermocouples are covered by the sample carrier unit 6 and the reference unit 5 in this side view.

[0080] Using the respective thermocouple devices 11, 12, temperatures can be measured on the sample carrier unit 6 and on the reference unit 5 if the inventive sample carrier device 1 is functionally connected to a measuring device for thermal sample analysis. Appropriate evaluation electronics can also detect the temperature difference between the two thermocouple devices 11, 12.

[0081] A defined heat flow element 14 is also shown arranged between the reference unit 5 and the sample carrier unit 6. This heat flow element 14 is particularly in this Fig. 1, arranged on the respective main bodies of the reference unit 5 and the sample carrier unit 6. In particular, the heat flow element 14 is provided so as to be firmly connected to the reference unit 5 and the sample carrier unit 6.

[0082] In other words, a connection is provided in each case that is suitable for enabling heat flow between the components. For example, it is conceivable that the respective connections are essentially equivalent to a material connection between the respective components.

[0083] The main support structure 2 comprises the second holding element 4, which is designed to accommodate respective connecting line sections, i.e., the thermocouple wires 13, of the first and second thermocouple devices 11, 12 and simultaneously hold the first holding element 3. The main support structure 2 is also designed and illustrated to hold the reference unit 5 below the sample carrier unit 6, wherein respective connecting line sections, i.e., the thermocouple wires 13, are illustrated as being guided substantially centrally in the sample carrier device 1.

[0084] The second holding element 4 has a first end region 15, which is received by the first holding element 3, and also a second end region 16, opposite the first end region 15, which is designed to receive a plug-in contact unit 17 of the sample carrier device 1 for connecting the respective connecting line sections, i.e. the thermocouple wires 13, of the first and second thermocouple devices 11, 13 to a measuring device (not shown in detail). These thermocouple wires 13 protrude in the illustration of Fig. 1 protrudes downwards (relative to the image plane). These are the same thermocouple wires 13, each of which is shown in sections between the sample carrier unit 6 and the first holding element 3.

[0085] However, it is also conceivable that these ends are arranged in the plug contact unit 17 and can then be connected to connection areas of a measuring device (not shown in detail) by means of a plug contact principle or the like.

[0086] In a further embodiment variant not shown in detail, it is conceivable that the first and second holding elements 3, 4 form a coherent material unit, i.e. as a component which has the respective functions of the first and second holding elements 3, 4.

[0087] Fig. 2 shows a further schematic side view of an alternative sample carrier device 1 for measuring devices for thermal sample analysis.

[0088] This is essentially the same sample carrier device 1 for measuring instruments for thermal sample analysis as in Fig. 1. The same reference numerals are used here, so they are not introduced again here.

[0089] A key difference between Fig. 2 and Fig. 1 is the location of the defined heat flow element 14. This defined heat flow element 14 is in Fig. 2 is also provided between the reference unit 5 and the sample carrier unit 6, but a connection point is provided on the sample carrier unit 6 via the first plug connection 7. The sample carrier unit 6 and the respective first plug connections 7 are in Fig. 2 as a material unit. In other words, it is a one-piece structural component, which is thus inherently heat-conductive. The sample carrier unit 6 with the associated respective first plug connections 7 can be designed, for example, as a metal foil or metal sheet, wherein the respective first plug connections 7 are bent downwards relative to the image plane. A connection point of the defined heat flow element 14 is thus located on the sample carrier unit 6, wherein Fig. 2, a heat-conducting path is provided via one of the plug connections 7.

[0090] Fig. 3 shows a further schematic side view of a sample carrier device 1 for measuring devices for thermal sample analysis.

[0091] This is essentially the same sample carrier device 1 for measuring instruments for thermal sample analysis as in Fig. 1. The same reference numerals are used here, so they are not introduced again here.

[0092] In the Fig. 3 is a related to the representation of Fig. 1 is shown as a side view rotated by 90°. The respective second plug connections 8 are shown plugged onto the first holding element 3, with respective end regions of the respective portions projecting downwards (relative to the image plane) beyond the first holding element 3. In this respect, the respective second plug connections 8 are not only plugged onto the first holding element 3, but rather are clamped onto it, resulting in a secure hold of the reference unit 5 on the holding element 3.

[0093] The respective connecting line sections, i.e. the thermocouple wires 13, of the first and second thermocouple devices 11, 12 projecting below beyond the plug contact unit 17 each cover a thermocouple wire 13, so that in this side view of Fig. 3 only two thermocouple wires 13 are shown at this point.

[0094] Four thermocouple wires 13 are shown above the first holding element 3, with two thermocouple wires 13 being provided for each thermocouple device 11, 12. Thus, the thermocouple wires 13 of the respective thermocouple devices 11, 12 are routed from bottom to top within the main support structure 2 and are divided according to their function above the first holding element 3.

[0095] Fig. 4 shows a schematic plan view of a sample carrier device 1 for measuring devices for thermal sample analysis without a sample carrier unit.

[0096] This can essentially be the same sample carrier device 1 for measuring instruments for thermal sample analysis as in Fig. 1. Therefore, the same reference numerals are used here, so they are not introduced again here.

[0097] The reference unit 5 is depicted as a substantially round element with a free space in its center. The first holding element 3 is depicted as having a substantially rectangular shape, with the center of the first holding element 3 providing a view into the second holding element 4. Therefore, the second holding element 4 is hollow inside, so that the thermocouple wires 13 of the respective thermocouple devices 11, 12 can be guided in this hollow space.

[0098] In Fig. 4 shows the thermocouple device 11, which measures a temperature at the reference unit 5, wherein a thermocouple 18 is connected in direct contact with a surface portion of the reference unit 5. The thermocouple 18 is enclosed by respective thermocouple wires 13 of the thermocouple device 11. These thermocouple wires 13 are provided in direct contact with the thermocouple 18. The thermocouple 18 can have a spatial extension in all directions of a few millimeters, for example in a range of 1 to 35 mm, preferably 5 to 20 mm, preferably 2 to 15 mm, preferably 3 to 7 mm.

[0099] For example, in one embodiment, the thermocouple 18 may have a dimension that exceeds the dimension of a simple thermocouple bead and is thus suitable and designed to determine a temperature profile in a region between a sample to be measured and the reference unit 5 to a certain extent.

[0100] In this respect, in the application case of the inventive sample carrier device 1, there is a defined heat flow path between a sample to be measured, which is held on the sample carrier unit 5, for example by being held in a crucible or the like, and the reference unit 5. In this respect, the sample carrier unit 6 of the sample carrier device 1 is connected to the reference unit 5 directly and with a defined thermal resistance via a material in the solid state.

[0101] The sample carrier device 1 for measuring instruments for thermal sample analysis is shown in this illustration without the sample carrier unit 6, allowing a view of the first and second holding elements 3, 4. Analogously, the sample carrier unit 6 would be connected without direct contact above the illustrated reference unit 5, with a connection being provided by means of the illustrated defined heat flow element 14.

[0102] In the first holding element 3, respective plug-in slot areas 19 are also shown at respective lateral end areas, into which the sample carrier unit 6 (not shown) can be inserted. In this illustrated embodiment, these plug-in slot areas 19 have a substantially rectangular shape.

[0103] In other embodiments not shown in detail, however, it is conceivable that they have alternative shapes, wherein they are to be selected essentially according to a shape of the first plug connections 7 of the sample carrier unit 6 (not shown), so that the plug connections 7 can be fastened to the first holding element 3 at this point with as much precision as possible.

[0104] Fig. Figure 5 shows a schematic representation of a measuring device 100 for thermal sample analysis. An inventive sample carrier device 1 for measuring devices for thermal sample analysis is shown arranged in a heating and cooling device 20 of the measuring device 100.

[0105] This can essentially be the same sample carrier device 1 for measuring instruments for thermal sample analysis as in Fig.1. The sample carrier device 1 is provided essentially centrally in the heating and cooling device 20 of the measuring device 100, wherein the sample carrier device 1 is shown functionally coupled to a connection unit 21 of the measuring device 100 via the plug-in contact unit 17.

[0106] In particular, respective thermocouple wires 13 of respective thermocouple devices 11, 12 of the sample carrier device 1 are provided coupled to the measuring device 100, so that corresponding control and measuring processes can be effected via a control device of the measuring device 100 (not shown in detail).

[0107] It is particularly possible for the measuring device 100 to contain a weight measuring device (not shown in detail), for example in the form of a scale, to which the sample carrier device 1 is connected via the plug-in contact unit 17.

[0108] This then enables the measurement of the sample mass, also as a function of temperature and time, simultaneously with the recording of the temperatures via thermocouple devices 11 and 12 and their temperature difference. The heat flow can be calculated from the temperature difference using a suitable calibration.

[0109] Due to its space-saving structure and design, the sample carrier device 1 can be arranged particularly advantageously in the measuring device 100 and can, for example, be easily maintained or even replaced. A sample to be measured in a corresponding sample container can also be easily inserted or arranged on the sample carrier device 1.

[0110] It is conceivable that the measuring device 100 has a lifting mechanism (not shown in detail) for this purpose, so that the sample carrier device 1 can be mounted or functionally coupled so that it can be moved upwards relative to the image plane. A user can then, for example, perform a replacement process or the like via an opening area 22 with cover element 23 of the measuring device 100. For example, components of the sample carrier device 1 can also be easily accessible in this way for maintenance or replacement operations, since the sample carrier device 1 has a correspondingly slim design and the arrangement of the individual components is particularly advantageous for these purposes.

[0111] For example, various thermocouple devices 11, 12 can be provided in the sense of a modular principle, whereby individual components are then provided to be easily replaceable without the measuring device 100 having to be laboriously disassembled into its individual parts. LIST OF REFERENCE SYMBOLS 1 sample carrier device 2 Main support structure 3 first holding element 4 second holding element 5 Reference unit 6 Sample carrier unit 7 first connector 8 second connector 9 Connection area 10 holding devices 11 first thermocouple device 12 second thermocouple device 13 Thermocouple wire 14 defined heat flow element 15 first end area 16 second end area 17 Plug-in contact unit 18 thermocouple 19 Slot area 20 Heating and cooling equipment 21 Connection unit 22 Opening area 23 Cover element

Claims

[1] Sample carrier device (1) for measuring instruments for thermal sample analysis comprising a main carrier structure (2), a reference unit (5) which does not carry a reference sample, with a first thermocouple device (11) and a sample carrier unit (6) with a second thermocouple device (12), wherein the main carrier structure (2) is designed to hold both the reference unit (5) and the sample carrier unit (6) spatially separated from one another, characterized by that the reference unit (5) and sample carrier unit (6) are provided without direct contact with each other and a defined heat flow element (14) is arranged between the reference unit (5) and sample carrier unit (6), wherein the arranged heat flow element (14) connects the two components (5, 6). [2] Sample support device (1) according to claim 1, wherein the defined heat flow element (14) is selected from: metal wire, copper wire, platinum wire, platinum alloy wire, nickel-chromium wire, nickel alloy wire, metal sheet, copper sheet, platinum sheet, platinum alloy sheet, nickel-chromium sheet, nickel alloy sheet, metal rod, copper rod, platinum rod, platinum alloy rod, nickel-chromium rod, nickel alloy rod. [3] Sample carrier device (1) according to claim 2, wherein the main support structure (2) is designed to hold the reference unit (5) below the sample carrier unit (6). [4] Sample carrier device (1) according to one of the preceding claims, wherein the main carrier structure (2) comprises at least one first holding element (3) which is designed to reversibly receive both the reference unit (5) and the sample carrier unit (6). [5] Sample carrier device (1) according to one of the preceding claims, wherein the main support structure (2) comprises a second holding element (4) which is designed to receive respective connecting line sections of the first and second thermocouple devices (11, 12) and to hold the first holding element (3). [6] Sample carrier device (1) according to claim 5, wherein the second holding element (4) comprises a first end region (15) which is designed to be received by the first holding element (3), and a second end region (16), opposite the first end region (15), which is designed to receive a plug-in contact unit (17) of the sample carrier device (1) for connecting the respective connecting line sections of the first and second thermocouple devices (11, 12) to a measuring device. [7] Sample carrier device (1) according to one of the preceding claims, wherein the sample carrier unit (6) comprises holding means for holding respective sample containers, which are designed to be flexibly adjustable, so that respective sample containers of different sizes and different materials can each be individually reversibly received by the sample carrier unit (6). [8] Sample carrier device (1) according to one of the preceding claims, wherein the first holding means (3) is made of aluminum oxide (Al2O3). [9] Sample carrier device (1) according to one of the preceding claims, wherein the reference unit (5) and the sample carrier unit (6) are arranged one above the other without direct contact and each have a minimum diameter which substantially corresponds to at least twice the diameter of the second holding element (4). [10] Sample carrier device (1) according to one of the preceding claims 4 to 9, wherein the sample carrier unit (6) can be reversibly fastened to the first holding element (3) by means of at least one first plug connection (7). [11] Sample carrier device (1) according to one of the preceding claims 4 to 10, wherein the reference unit (5) can be reversibly fastened to the first holding element (3) by means of at least one second plug connection (8). [12] Sample carrier device (1) according to one of the preceding claims 4 to 11, wherein the first holding element (3) can be reversibly fastened to the second holding element (4) by means of at least one plug connection. [13] Sample carrier device (1) according to claim 12, wherein the at least one plug connection between the first and second holding element has a substantially conical shape. [14] Sample carrier device (1) according to one of the preceding claims, wherein the sample carrier unit (6) is essentially made of a metal foil, wherein the metal is selected from: platinum, platinum alloy, nickel chromium, nickel alloy, steel and similar alloys, and wherein a thickness of the metal foil is between 0.02 and 3 mm, preferably between 0.03 and 2 mm, preferably between 0.05 and 1 mm. [15] Sample carrier device (1) according to one of the preceding claims 4 to 11, wherein respective plug connections are reinforced with at least one ceramic adhesive. [16] Measuring device (100) for thermal sample analysis comprising a sample carrier device (1) according to one of claims 1 to 15 and a weight measuring device for detecting a sample mass of a sample to be examined. [17] Measuring device (100) according to claim 16 without a weight measuring device for detecting a sample mass of a sample to be examined.

Citation Information

Patent Citations

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