Heat treatment device

Abstract

Heat treatment device for materials and a method for heat-treating materials that is carried out using the device according to the invention. Based on the invention, measurement data can be acquired with a high level of accuracy, it being significant that the device and the method are operated at very high temperatures. The method is preferably operated at a temperature > 773.15 K (500°C). Besides the very high level of accuracy, the method also provides the option of acquiring and storing the measurement data while the method is carried out, and then expressing said measurement data in relation to performance data that are determined during downstream characterizations of the materials.

Description

[0001] Heat treatment device

[0002] Field of the invention

[0003] The invention relates to a device for the heat treatment of materials and to a method for the thermal treatment of materials, which is carried out using the device according to the invention. The materials are located in spatially confined areas. The material confined in an area, which additionally possesses a material property, is referred to hereinafter as a sample. In a preferred embodiment of the method according to the invention, the samples are heat-treated simultaneously at different temperature levels in order to specifically influence the material property. One goal is to investigate whether the heat treatment leads to an increase in the efficiency of desired material properties and then to specifically optimize these properties.Based on the invention, measurement data can be recorded with a high degree of accuracy during the thermal treatment of materials, whereby it is important that the heat treatment device and the method are operated at high temperatures. The method is preferably operated at a temperature > 773.15 K (> 500°C). In addition to the very high accuracy with regard to the treatment temperature of the samples, the method also offers the possibility of relating the measurement data during the process and also the possibility of comparing the measurement data with performance data determined during subsequent characterization of the materials. One aspect when carrying out the method according to the invention is also how the temperature of a sample is determined if the number of temperature measuring points differs from the number of samples.

[0004] Background of the invention

[0005] The use of high-temperature furnaces for the thermal treatment of materials is state-of-the-art, both in laboratory operations and in production processes. Some examples of this technology are presented below.

[0006] DE 103 48 811 A1 describes a muffle furnace for the thermal treatment of materials. During the simultaneous thermal treatment of materials in the muffle furnace, the problem can arise that volatile substances are released in the individual material samples, which can precipitate into the other substances and thus cause uncontrolled contamination. To prevent contamination, the samples are arranged on a common perforated plate, which is positioned with spacers above the floor in the interior of the furnace. Heat-resistant plates are arranged on top of the perforated plate, which divide the furnace interior into individual chambers. The materials are arranged in the different chambers. The furnace has at least one duct located outside the furnace and forming a connection to the interior of the furnace, wherein the duct is connected to a fan.Air will be extracted from the furnace interior through the duct. Any volatile substances released will be removed from the furnace chamber by the extraction system.

[0007] DE 10 2011 077 005 B4 describes a continuous furnace for the thermal treatment of substrates, which is equipped with a measuring system for recording measurement data. The continuous furnace has openings on two opposite sides, which represent an inlet side and an outlet side. A carrier system is arranged on the bottom side of the interior, which runs through the furnace and enables the transport of substrates through the furnace chamber. The measuring system for recording measurement data can be positioned either on the inlet side or the outlet side of the furnace. The measuring system is equipped with a measuring sensor located at the top of the measuring system. The measuring sensor is connected to a movable drive and can be positioned at different locations within the interior of the furnace to record the measured values.A shield is provided in the area between the measuring sensor rod and the sensor tip to protect the drive from thermal radiation escaping from the furnace interior. Furthermore, the sensor tip is attached to a telescopic extension, allowing the sensor tip to be positioned at different locations toward the furnace interior.

[0008] Another approach to thermal treatment of materials is described in US Pat. No. 10,562,098 B2, which describes a process for the high-throughput synthesis of multicomponent materials based on microsystems. The materials are introduced into the various positions of honeycomb-shaped containers, which are then treated with microwave radiation. Very rapid heating rates can be achieved using microwave radiation.

[0009] EP 3 256 804 B1 discloses a sintering furnace for treating dental components.

[0010] EP 752 568 B1 discloses an electric oven and its use.

[0011] DE 103 61 099 B3 discloses a method and apparatus for analyzing a sample plate on which at least two samples are arranged. An impedance spectrum is measured for each of the samples in the process. In response to the measured impedance spectrum, a structure corresponding to each circuit, comprising at least one electronic device, is determined. An error minimization calculation is performed to determine starting values ​​for the components of the respective circuit equivalent. When minimizing the errors of at least one of the samples, a theoretical impedance spectrum is considered based on the measured impedance spectrum of the sample, and initial values ​​for the heating elements and heating element fit values ​​for the calculated switching network equivalent are determined. Validation of the calculated values ​​is then determined, and a theoretical impedance spectrum analysis is determined by comparing at least one of the device fit values ​​for the parameter with a reference value.The invention relates to a device for analyzing a sample plate according to the preamble of claim 1 and to a method for analyzing a more precisely defined sample plate type.

[0012] DE 10 2012 101717 A1 discloses a method for treating at least one substrate in a process chamber of a reactor housing, specifically using metal-organic vapor deposition (MOCVD). In this method, several substrates arranged on a susceptor are heated. Heating is achieved via a surface heating system with several heating elements arranged beneath the susceptor. The device has optical temperature sensors arranged outside the process chamber, which measure the temperatures of the surface zones. The measured values ​​are fed to a control device that regulates the heating power of the heating elements.

[0013] CN 203 132 346 U discloses a shuttle kiln for calcining quartz ceramic articles. The kiln chamber comprises a relative wall and a kiln crown on both sides, wherein the side wall forms a unit with the kiln crown and encloses it for holding and setting up. The shuttle kiln further comprises: the temperature sensing mechanism comprises a plurality of temperature sensing units, and the temperature sensing units are arranged in a matrix shape and penetrate the two side walls and extend to the inner sides of the two side walls; the fire hole mechanisms comprise fire holes with the same number as the temperature sensing units, the fire holes are arranged in a matrix shape and are arranged in the two side walls.

[0014] RO 132 883 A0 discloses an array of temperature sensors for characterizing the homogeneity of food heating. This allows the performance of a microwave oven or an oven for uniformly heating food to be characterized. According to the invention, the array of temperature sensors consists of a plurality of temperature sensors, each comprising a transducer mounted in a metallic penetration head. The temperature sensors are fixed in a matrix in a mounting plate. The individual temperature sensors each have a penetration head. The penetration head, which is designed to penetrate the heated food, has a tip with a movable cutting device that is tapered at a given angle. For the measurement, the food to be heated is removed from the oven.With the aid of the arrangement according to the invention, the temperature can be measured simultaneously at different positions within the food at previously selected positions.

[0015] DE 10 2011 109332 A1 discloses a device and a method for treating at least one laboratory sample using a laboratory device, and a computer program product for implementing the method. The invention relates to a laboratory device for treating laboratory samples, in particular a laboratory device for mixing and / or tempering a liquid sample in a medical, biological, or biochemical laboratory. The invention also relates to a method for treating such laboratory samples.

[0016] EP 3 539 660 A1 discloses a device and a method for storing samples at a target temperature. In particular, EP 3 539 660 A1 relates to an incubator for storing cell cultures.

[0017] DE 101 43 517 A1 discloses a device and a method in which a base plate with a matrix arrangement is provided, above which a thermal camera is arranged. DE 101 43 517 A1 describes a device for analyzing a fluid medium that is passed over at least one microsensor. During the analysis, the changes in properties are monitored using a thermographic detector arranged such that the focus of the detector is located above the microsensors. DE 101 43 517 A1 discloses that aluminum oxide moldings are impregnated with different metal salts, whereby a total of 94 different impregnated moldings are produced. The impregnated moldings are arranged in the holes of a reactor plate, whereby the reactor plate has 96 holes arranged in a matrix.Different gas mixtures are passed over the molded bodies, with the thermal properties of the sample molded bodies being observed using an infrared thermal camera. One of the objects underlying the invention is to provide a device and a method for the thermal treatment of materials that makes it possible to monitor the thermal treatment. At the same time, the method according to the invention should also run automatically, if possible.

[0018] Summary of the invention

[0019] The subject matter of the present invention relates to a device for the heat treatment of materials as well as a method for the thermal treatment of materials according to the independent claims, further embodiments of the invention are embodied in the appended claims.

[0020] The object underlying the invention is achieved by providing a device for the heat treatment of materials, which device comprises a temperature-controlled interior, a sensor matrix, a positioning system for receiving containers, a plurality of containers and a measuring and control unit, wherein the sensor matrix comprises a plurality of temperature sensors arranged at different points within the temperature-controlled interior of the device and the number of temperature sensors is > 4, preferably the number of temperature sensors is > 6, more preferably the number of temperature sensors is > 8. The term temperature sensor refers to a transducer that detects the temperature and converts it into an electrical signal. The signal processing and storage takes place using data processing and storage technology.

[0021] The device according to the invention is advantageous for conducting screenings. This means that the device is designed so that a large number of samples are heat-treated simultaneously. In a preferred embodiment, the positioning device has a number of receiving positions in the range of 4 to 256; preferably, the number of receiving positions is in the range of 9 to 128, particularly preferably in the range of 16 to 96.

[0022] The heat treatment device according to the invention is designed as a lockable device. A lockable device has at least one thermally insulated door equipped with a folding or sliding mechanism. The sliding mechanism comprises, for example, sliding elements. The invention preferably relates to a lockable heat treatment device. The heat treatment device according to the invention is preferably used for thermal treatment at high temperatures, and the shielding of the interior of the heat treatment device from the exterior can exclude external interference better than in a continuous device due to the lockable door.

[0023] It is preferred that the temperature sensors are arranged in a symmetrical group or at least partially in a flat surface. Preferably, temperature sensors are arranged in a rectangular group in the room. Furthermore, the temperature sensors are preferably arranged in a cubic group. Even more preferably, the temperature sensors are arranged in a flat surface. Furthermore, the temperature sensors are preferably arranged below the positioning system. The temperature mapping is more accurate if the spatial points in the interior are recorded evenly. With regard to the temperature sensors, it should be noted that they are preferably Ni / Cr / Ni or Pt thermocouples. Hereinafter, the spatial arrangement of the temperature sensors is referred to as a sensor matrix. The temperature sensors are preferably arranged in a regular arrangement in the room, in particular preferably in a flat arrangement.The position of the temperature sensors can be clearly specified by specifying a column and a row index.

[0024] Regarding the dimensioning of the heat treatment device, it should be noted that this is characterized by the dimensions of the interior. The width of the interior is preferably in the range of 10 to 100 cm, more preferably in the range of 20 to 80 cm; the height of the interior is preferably in the range of 5 to 50 cm, more preferably in the range of 10 to 40 cm; the depth of the interior is preferably in the range of 10 to 100 cm, more preferably in the range of 20 to 80 cm.

[0025] In a preferred embodiment, the invention relates to a device for heat treatment which comprises a temperature-controlled interior space, wherein the device is closable and has at least one thermally insulated door which is equipped with a folding or sliding mechanism, wherein the temperature-controlled interior space has a width in the range of 20 to 80 cm, a height in the range of 10 to 40 cm and a depth in the range of 20 to 80 cm.

[0026] A device for the heat treatment of materials, which has a temperature-controlled interior, is also referred to in the description as a furnace. Such a device is also referred to as a laboratory furnace. In general, a device for the heat treatment of materials has one or more heating elements, at least one temperature sensor, and a temperature controller. The device elements are connected to one another. The actual temperature is determined using the temperature sensor. A target temperature can be specified using the temperature controller, whereby the temperature controller is designed to supply the heating elements with electrical power required to control the temperature-controlled interior to a predetermined target temperature. A furnace is formed from a box-shaped housing that has wall surfaces as well as a floor and ceiling surface.The surfaces can be divided into those surfaces that are in contact with the exterior of the device and those surfaces that are in contact with the temperature-controlled interior of the device. The housing is constructed in such a way that the interior wall surfaces as well as the floor and ceiling surfaces of the temperature-controlled interior are equipped with heating elements, with one or more layers of insulating material being arranged in the area between the interior and exterior walls. With regard to the heating elements, it should be noted that they are arranged in such a way that a plurality of surfaces of the temperature-controlled interior can be temperature-controlled with heating elements at the same time, so that several wall surfaces, together with the floor and ceiling surfaces, are connected to one or more heating elements.

[0027] The device according to the invention has an advantage over the devices known from the prior art, in which temperature is measured by measuring instruments arranged outside the furnace chamber. In the case of a thermal camera or optical sensors in the form of pyrosensors, radiation-permeable windows must be located in the ceiling surface of the device. The production of a device with outside temperature measurement in conjunction with radiation-permeable windows is associated with a very high level of effort. Heating conductors cannot be attached to the locations where the radiation-permeable windows are installed. This reduces the heat input in the area of ​​the ceiling surface, which can lead to malfunctions at high temperatures, since a horizontal temperature gradient can occur in the temperature-controlled interior.An extreme or maximum horizontal temperature gradient occurs when the temperature control of a reaction chamber is only achieved via the bottom surface of a chamber, as is the case, for example, in MOCVD apparatus used to coat substrate surfaces.

[0028] Another advantage of the device according to the invention is that the temperature sensors do not have to be arranged in the containers containing the material samples, which would require considerable technical effort, since otherwise each individual sample material or sample container would have to be contacted with a temperature sensor. With the device according to the invention, susceptor disks also do not need to be set in a rotating motion to achieve uniform temperature control of the surface. The sensor matrix and the positioning system, or sample containers, form an independent arrangement arranged in the temperature-controlled interior and are variable and flexible. In a preferred embodiment of the invention, the sensor matrix and the positioning system, or sample containers, are decoupled. Defective temperature sensors can be easily replaced.The positioning system can be equipped with containers of different dimensions and are interchangeable. Alternatively, a positioning system designed as a tray with recesses of a specific size can be exchanged for another positioning system.

[0029] The positioning system (13) comprises a tray with recesses or a tray with markings. The tray can be equipped with containers. The recesses or containers have an inner diameter in the range of 1-10 cm; the surface of the positioning system comprises a measuring system, whereby the surface areas or surface points of the positioning system can be located and identified. Also conceivable are embodiments in which the containers can be arranged in the recesses of the positioning system 13 or the materials for treatment can be introduced directly into the recesses.

[0030] The positioning system is suitable for being arranged in the temperature-controlled interior of the device, using one or more elements from the group of holder, rail, support, blocks.

[0031] The heat treatment device according to the invention comprises a measuring and control unit having an electrical control device with a database, preferably a data processing device, more preferably a computer processor, wherein the database stores the information describing the properties of the positioning system and which is selected from the group consisting of the total area (dimensioning) of the positioning system, the trough position and trough diameter, the position and diameter of individual containers, and the identifier numbers of individual containers. Furthermore, the control device has a connection to the individual temperature sensors of the sensor matrix.

[0032] Thus, the device according to the invention also has the advantages of improved manageability and improved accuracy compared to devices known from the prior art.

[0033] In a preferred embodiment, the heat treatment device is equipped with one or more additional temperature control elements, which enable targeted heating or targeted cooling of a part of the interior. In a further preferred embodiment, the additional temperature control element is an element for specifically cooling a part of the interior. In an even more preferred embodiment, the additional temperature control element comprises a cooling fluid selected from the group consisting of gases or liquids, with inert gases being preferred. Suitable liquids can be, for example, silicone oil or water. Furthermore, the additional temperature control element can be present in an embodiment in which a liquid is used which evaporates on its way through the cooler and absorbs energy during evaporation.

[0034] The provision of one or more additional temperature control elements also means that these additional temperature control elements are equipped with a separate temperature controller, whereby the additional temperature control element(s) are controlled independently of those temperature control elements that maintain the temperature-controlled interior at a predetermined target temperature.

[0035] In a preferred embodiment, the heat treatment device has a door or a hinged door, wherein it is further preferred that the additional temperature control elements are arranged in the door of the heat treatment device. For example, the door of the heat treatment device can contain a temperature control element in the form of temperature control lines through which a temperature control fluid is passed. For example, the door equipped with temperature control lines can be cooled with water as the temperature control fluid. In a preferred embodiment, the temperature control element arranged in the door is designed for cooling. Preferably, the door is equipped with sealing elements that can be cooled by the temperature control element. Sealing elements are important for controlling the gas atmosphere in the interior of the device.

[0036] The effect achieved with the additional temperature control element is that a temperature gradient is imposed on the interior of the heat treatment device, which extends from the temperature control element to a point opposite the temperature control element. For example, the additional temperature control element can be configured such that the temperature gradient has a value in the range from 10 to 100 K, more preferably the value is in the range from 20 to 95 K. The temperature gradient indicates the relative temperature difference that exists in the interior of the heat treatment device between the temperature control element and the opposite point. At the same time, it is preferred that the temperature of the heat treatment device is greater than or equal to 573.15 K, more preferably greater than or equal to 773.15 K.

[0037] The additional temperature control element can be rod-shaped or sheet-shaped, wherein it is preferred that the temperature control element has a parallel orientation with respect to the sensor matrix, wherein it is also preferred that the temperature control element is positioned in a lateral arrangement if it is rod-shaped. It should be noted that the combination of the additional temperature control element and the sensor matrix for the precise spatial detection of the temperature values ​​within the treatment zones results in a synergistic effect that enables the device and method to be used with great flexibility in terms of high accuracy in thermal treatment and a controlled achievement of thermal differences when treating individual samples located at different positions.The lateral positioning of the additional temperature control element is advantageous because mounting the additional temperature control element in the side area is technically easy to carry out and because the field of the temperature gradient runs from one side to the opposite side with respect to the base area of ​​the device.

[0038] In a preferred embodiment, the device according to the invention comprises one or more suction lances and an analysis device, wherein the suction lances are connected to the analysis device by lines and wherein the end points of the suction lances are arranged in the interior of the device. Preferably, the suction lances have a capillary tip, more preferably the suction lances are fixed and made of a high-temperature-resistant material. The analysis device serves to characterize the gas flow that is transferred by means of the suction lances from the regions of the interior of the device to the analysis device. For example, the analysis device can be a mass spectrometer, a gas chromatograph, or an FTIR spectrometer. Preferably, the end points of the suction lances are positioned near the various containers, wherein it is further preferred that the number of suction lances approximately corresponds to the number of sample containers.This allows the gas atmosphere in the direct spatial proximity to the material to be characterized, and the data for analyzing the gas composition can be correlated with the heat treatment of the respective samples. It will be clear to those skilled in the art that the term "analyzer" can also refer to a group of multiple analyzers. In a preferred embodiment, the connections between the suction lances and the analyzer comprise one or more multiport valves. It is further preferred that the analyzer and the multiport valves are coupled to the program control of the device and operated at least partially automatically by the latter. This device is for heat treatment and for online analytical characterization of the heat treatment process.Thus, the heat treatment device not only offers the advantages of flexibility and accuracy of thermally treating a large number of samples at different temperatures, but also the advantage of monitoring the thermal treatment process locally with respect to individual samples through analytical characterization of the gas atmosphere.

[0039] In a further embodiment, the device according to the invention for the heat treatment of materials, in combination with online analytical characterization of the treatment, is surrounded by a protective housing that can be filled with an inert gas, so that the heat treatment device can be operated in the absence of oxygen. In a preferred embodiment, the protective housing is designed such that the furnace chamber is formed by metal walls, and the door is provided with sealing means, thus preventing uncontrolled entry or exit of gas.

[0040] In addition, separation walls can be arranged on the positioning system, forming individual compartments in which the containers are positioned. The separation walls that form the individual compartments prevent the exchange of the gas atmosphere between the individual containers. In a preferred embodiment, the ends of the individual suction lances are each arranged in the compartments so that the gas atmosphere extracted by the suction lance is not contaminated by the gas atmosphere of the adjacent sample containers. Further preferably, the gas flow can be exchanged in the furnace. For example, gas can be supplied via the floor area of ​​the interior of the device and discharged via the ceiling area of ​​the interior. The separation walls are made of a temperature-resistant material. Designs for shielding samples in the interior of a heat treatment device are given in DE 10348 811 A1.

[0041] The invention relates to a device and a method for the heat treatment of materials, wherein the materials are examined in subsets, each of which is assigned an individual identifier, and wherein a single subset of material is then referred to as an individual sample. Each sample can be assigned an identifier so that a distinction can be made between the different samples. The positioning system used to hold the samples is adapted to the dimensions of the respective interior space of the heat treatment device. In a preferred embodiment, the containers in the holder of the positioning system have a tolerance that is less than or equal to 10%, more preferably the tolerance is less than or equal to 5%, and furthermore preferably the tolerance is less than or equal to 2.5%.For example, this means that an individual container with a diameter in the range of 20 to 40 mm has a total tolerance of 1 mm. If the container has a diameter of 20 mm, the tolerance is 5%. If the container has a diameter of 40 mm, the tolerance is in the range of 2.5%. This enables precise spatial positioning of the containers within the positioning system. At the same time, the positioning system can also be arranged with a high degree of accuracy in the interior of the heat treatment device. The accuracy with which the positioning system is arranged in the interior of the heat treatment device is preferably higher than 20 mm, more preferably the accuracy is higher than 10 mm, and furthermore preferably the accuracy is higher than 5 mm.

[0042] Preferably, there is a holder for receiving the positioning system in the interior of the heat treatment device.

[0043] An essential aspect of the invention is that a plurality of temperature sensors are arranged within the heat treatment device. The temperature sensors, and thus the temperature measuring points, are preferably arranged in rows and columns below the positioning system. This arrangement of the measuring points results in a matrix arrangement. By specifying the row and column, a temperature sensor is uniquely addressed. The sensor matrix comprises at least 2x1, i.e. a total of two temperature sensors. In a preferred embodiment, the sensor matrix is ​​integrated into parts of the holder. For example, in the form of cylindrical rods that are arranged in the interior of the device, preferably below the positioning system. The cylindrical rods provide mechanical protection for the temperature sensors.

[0044] The heat treatment device according to the invention also comprises a measuring and control device with which the method is carried out. Thus, the invention also relates to a method for the thermal treatment of materials in a heat treatment device. In one embodiment, the method is carried out such that the different materials are treated under uniform thermal conditions. This is achieved by carrying out the method according to the invention without applying a temperature gradient in the interior of the heat treatment device. The temperature field within the interior of the heat treatment device is recorded by means of the sensor matrix. Since the temperature sensors are preferably arranged in a flat surface, the temperature field is spatially determined for a two-dimensional region located below the positioning system.In a preferred embodiment, the sensor matrix has more than four temperature sensors; preferably, the temperature sensors form a matrix selected from the group consisting of 3x3 temperature sensors, 4x4 temperature sensors, 2x3 temperature sensors, 2x4 temperature sensors, 2x5 temperature sensors, and 3x5 temperature sensors. The detection of the temperature field further provides for the measured values ​​from each individual temperature sensor to be recorded as a function of time. The detection of the measured values ​​from the individual temperature sensors involves mapping, both in terms of location and over time. In a further step, the individual measured values ​​from neighboring temperature sensors at a given point in time are related to one another, with the spatial areas between neighboring temperature sensors being assigned a temperature value that results from the relationship.

[0045] The invention also relates to a method for heat treating materials in a device having one of the embodiments described here and connected to a database for recording and analyzing process parameters, the method comprising the following steps:

[0046] - Placing the materials in containers;

[0047] - Positioning of the filled containers in the receiving positions of the positioning system;

[0048] - Transfer of the positioning system equipped with containers in the thermal treatment zone of the device;

[0049] - Storage of the positioning system in the thermal treatment zone;

[0050] - Recording of test parameters, including information on the individual materials in the form of sample identification numbers and their spatial arrangement in relation to the respective recording positions within the positioning system; wherein, when the positioning system or the samples are stored in the treatment zone, measurement data on the temperature of the individual temperature sensors are recorded as a function of time using the sensor matrix.

[0051] In a preferred embodiment, the method for heat treating materials comprises the following steps:

[0052] - Storing information on the positions of the individual temperature sensors within the temperature-controlled interior in the database; - Storing information on the positioning system in the database, whereby this information includes the position of the individual surface of the positioning system and the dimensions of the individual containers;

[0053] - storing the positioning system in the thermal treatment zone with the interior temperature controlled at a temperature in the range of 473.15 to 2073.15 K (200 to 1800°C) for a selected period of time, wherein the interior temperature control is carried out by means of a single control unit in such a way that the device is temperature controlled at a uniform target temperature with respect to the surface of the positioning system;

[0054] - Registration of the temperature measurements determined by the individual temperature sensors in the database together with the position and time during the temperature control process;

[0055] - Allocation of the local temperature measurements to the individual containers whose surface area overlaps with the local temperature sensors or where the temperature sensors are located nearby, whereby the temperature measurements are adjusted during the allocation if adjacent temperature measurements show a temperature difference, and the temperature measurements assigned to the containers are assigned to the materials contained in the containers, whereby the values ​​are stored in the database under an identification number which is characteristic of the respective container and the material arranged therein.

[0056] Preferably, the heat treatment is carried out at a temperature in the range of 473.15 to 2073.15 K, more preferably the heat treatment is carried out at a temperature in the range of 773.15 to 1773.15 K, and further preferably the heat treatment is carried out at a temperature in the range of 873.15 to 1473.15 K. The process is particularly advantageous at temperatures in the range of more than 873.15 K, since it is more difficult to precisely control the thermal conditions in heat treatment devices having the above-mentioned dimensions than at temperatures < 873.15 K.

[0057] The method according to the invention is preferably carried out at temperatures > 500°C, which means that the device for the heat treatment of materials is designed such that it is operated at temperatures > 500°C. The invention preferably relates to a device for the heat treatment of materials which is operated at temperatures > 500°C. Further preferably, the invention relates to a device in which the surfaces of the temperature-controlled interior are equipped with ceramic plates. The sensor matrix is ​​a spatial arrangement of the temperature sensors in the temperature-controlled interior of the device, wherein the temperature sensors are preferably located in a regular arrangement or in a planar arrangement. The position of a temperature sensor can be clearly specified by specifying a column and a row index.

[0058] The positioning system is a support plate or a holder, preferably designed as a surface, wherein the positioning system is arranged in the temperature-controlled interior of the device. Since the dimensions of the temperature-controlled interior are specified, the area of ​​the positioning system arranged in the temperature-controlled interior can also be derived from this information, wherein the area of ​​the positioning system is preferably in the range of 400 - 6400 cm 2 (or 0.04 - 0.64 m 2 or 4 - 64 dm 2 ) lies.

[0059] The sensor matrix is ​​preferably a spatial arrangement of temperature sensors, preferably in a plane or in an area below the positioning system. The temperature sensors are preferably arranged in metal tubes that provide mechanical protection. The metal tubes are preferably arranged so that they are easily accessible in the temperature-controlled interior and can be easily replaced. This is because the temperature sensors are sensitive objects that are subject to wear. A particularly advantageous aspect of the device according to the invention is the flexibility in replacing the individual temperature sensors of the sensor matrix, since they are arranged in an easily accessible manner in the temperature-controlled interior. In a preferred embodiment, the sensor matrix or the temperature sensors are at a distance from the positioning system that 50 mm, preferably the distance from the sensor matrix or the temperature sensors to the positioning system 20 mm, furthermore preferably the distance from the sensor matrix or the temperature sensors to the positioning system is 10 mm, even more preferably the distance from the sensor matrix or the temperature sensors to the positioning system is 10 mm, even more preferably

[0060] 5 mm.

[0061] In this method, it is preferred that the measurement data determined by the sensor matrix be correlated, whereby the values ​​in the space between adjacent temperature sensors are determined mathematically. The measured data from the temperature sensors are assigned to the receiving positions and the containers arranged in the receiving positions. This method is particularly advantageous because the positioning element is interchangeable and can be replaced with a positioning element with a different number of receiving units. However, it is not necessary to adjust the number of temperature sensors, since the thermal values ​​can be determined with high accuracy based on the database and comparison.

[0062] Based on the measured values ​​and the calculated intermediate values, the temperature field inside the heat treatment device can be determined with high temperature accuracy as a function of the thermal treatment location, expressed by the coordinates of the matrix. The recording of the temperature and the determination of the intermediate values ​​between the individual temperature sensors are registered in the program control. This also provides information about the temporal temperature profile to which the individual sample materials were exposed at the respective locations. The individual temperature values ​​on the surface of the temperature field are assigned to the materials located in the immediate vicinity in the containers. This means that the treatment temperatures can be assigned to the individual materials with very high accuracy.

[0063] During the thermal treatment of different materials under conditions that are not thermally equivalent, a temperature gradient is generated in the interior of the heat treatment device by means of the additional temperature control element. This temperature gradient extends in the plane of the sensor matrix. Based on the temperature gradient, a temperature field is generated that has a distribution of different temperature zones.

[0064] In a preferred embodiment of the method, the thermal treatment zone of the device is heated or cooled by means of the additional tempering element, preferably the thermal treatment zone is cooled by means of the additional tempering element, wherein the measurement data of the individual temperature sensors have temperature deviations of < 5 K (< 5 ° C), further preferably the measurement data of the individual sensors have temperature deviations of < 1 K (< 1 ° C).

[0065] The procedure for treating materials under non-equivalent thermal conditions is analogous to that for treating materials with thermally equivalent conditions. Under non-equivalent thermal conditions, the temperature of the temperature field is determined, and the individual sample materials arranged in the containers are assigned a temperature value based on the determination of the measured and calculated temperature values.

[0066] One advantage of implementing the method according to the invention is that a given number of materials can be treated simultaneously at different temperature levels. Using the method according to the invention, the tempering of materials can be accelerated, since simultaneous tempering means that multiple devices do not have to be operated in parallel or that processing does not have to be carried out in multiple runs. Using the method according to the invention can save energy due to the improved efficiency. It is also clear that the method according to the invention for tempering materials is limited to laboratory scale.

[0067] In a further step, the process is improved by measuring the temperature field of the furnace using the sensor matrix under a given set of parameters. The measurement and control program then calculates the temperature or the temporal temperature profile at the position of all containers, including the samples contained therein, in the case of the containers being loaded with samples.

[0068] Thus, based on the method according to the invention, it is possible to record the accuracy of the heat treatment temperature of the individual containers and the materials contained therein in a highly precise and reproducible manner. The recorded measured values ​​are stored in the program control system. The storage of measured values ​​also provides the user with values ​​for the accuracy of the heat treatments based on comparative values.

[0069] Based on an optimization algorithm, the device and method are capable of providing the user with process information regarding the accuracy of the process, which is recorded in the database, or the device and method can suggest parameters to the user that lead to an improvement in the accuracy of the thermal treatment. For example, the improved accuracy can be achieved by determining, for a specific parameter space relating to the heat treatment of materials, those positions within the positioning system that have a high level of accuracy and the suitable diameters of containers to achieve the desired accuracy. Preferably, the diameter of an individual container is small in relation to the temperature gradient running through this container, wherein the temperature gradient and diameter of the containers are selectable.For example, the temperature gradient can be in the range of 0.5 to 2 K / cm. In the direction of the gradient, the temperature increases along the section of the furnace surface in which the containers with the samples are positioned.

[0070] The device according to the invention is characterized in that a temperature field is recorded with high accuracy by means of a sensor matrix in the interior of the device. With regard to the implementation of the method, a synergistic effect is achieved, based on the fact that the method according to the invention includes the integration of calibration data, or the integration of test data used as calibration data, or both calibration data and test data.

[0071] A heat treatment device is characterized by an operating range determined by the performance characteristics of the heating elements and control electronics. The operating range determines the minimum and maximum temperature values ​​reached in the thermal treatment zone. To perform calibration, the interior of the device or the thermal treatment zone is maintained at different temperature values ​​(hereinafter also referred to as set values ​​or target values) that cover the range between the minimum and maximum temperature values. The local temperature is then recorded using temperature sensors as a function of the selected set value.For example, a heat treatment device may be characterized by an operating range of 773.15 to 1273.15 K (500 °C to 1000 °C). Temperature data are recorded by the program control system within the operating range at a total of eleven predefined setpoint temperatures, each at intervals of 50 K, and stored in the associated database. Preferably, the interval between the setpoints for recording the temperature data during calibration is < 50 K, in particular < 20 K, more particularly < 10 K, and even more preferably < 5 K.

[0072] In a preferred embodiment, the heat treatment device also comprises an additional tempering element with which a thermal gradient field or a temperature gradient can be generated within the thermal treatment zone. The terms thermal gradient field and temperature gradient are used synonymously here. In a preferred embodiment, calibration is carried out in the presence of a thermal gradient field. The size or the range of the thermal gradient field depends on the individual configuration of the device, which is determined by the respective setpoint temperature and performance characteristics of the additional tempering element. Preferably, the thermal gradient field across the treatment zone has a value that is > 10 K, in particular > 25 K, further in particular

[0073] > 50 K, even more preferably > 60 K.

[0074] The additional temperature control element is not specified in any way regarding its specific design. Preferably, the additional temperature control element is characterized by a simple structure and robustness. A simple structure is characterized by low control dynamics. Regarding the additional temperature control element, it should be noted that the additional temperature control element can comprise liquid cooling.

[0075] Preferably, the method includes recording calibration data in the presence of a temperature gradient. For example, the additional temperature control element is operated at a defined cooling capacity, while simultaneously adjusting the setpoint temperature to different temperatures within the device's operating range in order to record the corresponding local temperature data with the sensor matrix using the program control and store it in the database.

[0076] During the process, thermal measurement data can also be recorded by the program control during the thermal treatment of samples and stored in the database, which is then used as calibration data. The distinction between the terms measurement data and calibration data is that calibration data is recorded more systematically, with the entire operating range being set for all temperatures. Measurement data can be recorded within a narrower temperature range, which only applies to temperatures within a selected operating range. In principle, the temperature measurement data is recorded with high accuracy for the various specified parameters and stored in the database.

[0077] The method preferably comprises an optimization algorithm and a program control which selects parameters from the group consisting of the number of samples to be subjected to thermal treatment, the quantity of samples, the (absolute) value of the target temperature at which the thermal treatment is to be carried out, and the level of accuracy, wherein the accuracy is given by AK or delta in Kelvin. In a further embodiment, the method also comprises specifying the temperature range if the samples are to be treated simultaneously in a thermal gradient field at different temperatures. The program control analyzes the measurement data contained in the database and, using the optimization algorithm, determines the experimental parameters required to carry out the method in order to implement the parameters selected by the user.

[0078] The positions to be selected to achieve the desired accuracy and the required furnace setting temperature can be predicted by the optimization algorithm for any (even previously unused) positions (configurations).

[0079] Accuracy can also be improved by suggesting suitable temperature settings for the temperature control system or the additional temperature control element. The suggestion can be made by providing a selection. In a preferred embodiment, the program control is designed to provide a selection through which the accuracy can be specified by a user, or the program control can make suggestions to the user. The temperature control system includes setting the temperature of the device as well as setting the temperature or the required cooling capacity of the additional temperature control element.

[0080] The prediction does not depend on the number and positions of previously defined containers, but can be extended to other arrangements and sizes of containers by appropriate correlation.

[0081] In a preferred embodiment, the method comprises the following steps: positioning the samples at a position determined from the data in the database or from the measured values ​​of the sensor matrix in order to thermally treat a single sample or a plurality of samples at a desired temperature.

[0082] In a preferred embodiment, the method comprises the following steps: temporally staggered positioning of the samples at a plurality of positions determined from the data in the database or from the measured values ​​of the sensor matrix in order to thermally treat a single sample or a plurality of samples at a desired temperature and a temporally staggered temperature profile.

[0083] Preferably, the measurement data determined by the sensor matrix are correlated, whereby the values ​​in the space between adjacent temperature sensors are determined mathematically, and the measured data from the temperature sensors are assigned to the receiving positions and the containers arranged in the receiving positions. An embodiment of the method according to the invention is illustrated in the workflow shown in Figure 10. Thus, the invention also relates to a workflow that is implemented in combination with the device according to the invention, wherein it is preferred that the workflow be integrated into the program control.

[0084] The method can comprise a database containing fixed and variable structural parameters of the device. The fixed structural parameters include the size of the surface of the positioning system, the number of temperature sensors on the sensor matrix arranged in the plane of the positioning system, the position of the individual temperature sensors, and possibly an additional temperature control element. The surface of the positioning system is assigned to a coordinate system, whereby the surface is divided into individual surface elements and the position of the individual surface elements is stored in the database, for example, in the form of index numbers for rows and columns. The variable structural parameters include the size of the individual containers and the amount of sample material stored in a single container during thermal treatment.In addition, the database may include process data, where the process data are temperature values ​​generated and measured under specified operating parameters.

[0085] In a preferred embodiment of the method, the program controller provides the user with a selection of process parameters, and the user can select the desired process parameters. The process parameters are preferably provided via a graphical user interface. In a preferred embodiment of the method, the selection option also allows the user to specify a configuration for implementing the method for thermally treating materials.

[0086] A preferred aspect of the method is that the evaluation further comprises comparison with data or information taken from a database that was not obtained during the implementation of the method or during a previous implementation of the method. In a further preferred embodiment, the evaluation is carried out using a computer system equipped with an intelligent search system that proposes independent analysis suggestions for optimizing materials during the evaluation. Preferably, the device comprises a computer program for implementing a method, which is also linked to a relational database. Preferably, the method also comprises a program having an algorithm that is capable of comparing the collected data. It is preferred that the device and the method are integrated into a digital infrastructure of the user.

[0087] With regard to optimizing the accuracy of the device according to the invention, it is also considered that the plate of the positioning system is constructed from a material with a medium thermal conductivity. Preferably, the steel comprises 50 Wnr'K' 1 , Iron 117 Wnr 1 K' 1 , Corundum Ceramic 49 Wnr 1 K' 1 with a thermal conductivity of 40-100 Wnr'K' 1 .

[0088] In a preferred embodiment, the device and the method are used to produce materials from the group of catalysts, battery materials, high-performance ceramics, inorganic semiconductor materials.

[0089] With regard to the containers, it should be noted that these are crucibles or vessels made of metal or ceramic, or that contain metal or ceramic as a component. Both metal and ceramic may also be included.

[0090] These and other features are explained in the following figure description.

[0091] Short description of the characters

[0092] Fig. 1 shows a schematic representation of a heat treatment device in an embodiment with a flap door 21 equipped with closure elements, wherein a sensor matrix 3 is arranged in the interior of the furnace chamber;

[0093] Fig. 2 shows a schematic representation of a positioning system 13 equipped with thirty-six containers 15 arranged in a 6x6 matrix; several temperature sensors 4, 4', 4" are shown below the positioning system;

[0094] Fig. 3 shows a schematic representation in which the positioning system equipped with containers is arranged in the interior of a heat treatment device;

[0095] Fig. 4 shows a schematic representation of a portion of a heat treatment apparatus, showing the interior and attachments;

[0096] Figure 5 shows a schematic representation of the method, in which the device according to the invention is connected to a computer control system and database and integrated into a process flow. The process parameters during calibration and during the execution of the method are recorded in the database and made available to the user as part of an optimization cycle for subsequent process executions.

[0097] Fig. 6. a shows a schematic representation in the form of a sectional drawing, the orientation of which is parallel to the floor surface of the furnace interior, showing an overlay of the positioning system with a 5x5 matrix and a sensor matrix with 4x4 temperature sensors;

[0098] Fig. 6.b shows a schematic representation of the sectional drawing shown in Fig. 6.a, but with the positioning system equipped with 6x6 recording positions;

[0099] Fig. 7. a shows a schematic representation of a sectional drawing of the open interior analogous to the representation given in Fig. 6. a, but containing an additional tempering element 27 which is arranged laterally of the positioning system 13;

[0100] Fig. 7.b shows a schematic representation of a sectional view of the open interior, similar to the representation shown in Fig. 6.b, but including an additional temperature control element 27 arranged to the side of the positioning system. Fig. 8.a shows a schematic representation of a temperature field of the open interior with the determined / measured temperature values ​​determined for the individual fields of the 6x5 matrix.

[0101] Fig. 8.b shows a schematic representation of the temperature field of the furnace interior, which is shown in Fig. 8.b, in which the positions of temperature sensors or intermediate temperatures are also shown;

[0102] Fig. 9 shows a schematic representation in the form of a three-dimensional representation of the temperature curve in the z-axis compared to the surface fields of the temperature field in the x,y-plane on which the containers with the samples are positioned;

[0103] Fig. 10. a shows the calibration curves for the interior of the device at different measuring points: during the calibration, the temperature was increased in increments of 20 K, with nine different target temperatures set on the x-axis (horizontal axis) in the range from 1003.15 K to 1163.15 K, adjusted via the device's central temperature sensor; in the vertical direction (y-axis), the measured temperature is plotted for four different positions in the interior of the device (temperatures are given in Kelvin);

[0104] Fig. 10.b shows a close-up of a single position of one of the calibration curves shown in Fig. 10.b in a specific temperature window. (Temperature is given in Kelvin units.)

[0105] Further features and advantages of the method and device according to the invention will become apparent from the figures and the associated descriptions. It is understood that the features mentioned above and those to be explained below can be used not only in the respective combinations specified, but also in other combinations or on their own, without departing from the scope of the present invention. Exemplary embodiments of the invention are illustrated in the figures and are described in detail below.

[0106] Detailed description of exemplary embodiments

[0107] Figure 1 shows the device 1 for heat treatment according to the invention in the form of a high-temperature furnace 6, which has a hinged door 21 in the open state. The temperature sensors 3 are contained in four metal rods or metal tubes. The four metal rods or metal tubes are arranged above the base surface and form a sensor matrix with a planar orientation. The metal tubes protect the temperature sensors from damage. At the same time, the device has an additional temperature control element 7 arranged parallel to the metal rods. In the present case, the additional temperature control element 7 is designed as a cooling element through which a cooling fluid is passed. The supply lines for the coolant and the temperature sensors are designated by reference numerals 9 and 11 in the outer area.

[0108] Figure 2 shows a schematic representation of a positioning system 2 with containers, with the base plate designated by reference numeral 2 and the containers designated by reference numeral 15. Below the base plate of the positioning system 13, the temperature sensors 4, 4', 4" are shown, which here have a symmetrical matrix arrangement. Figure 2 shows a sensor matrix with 4x4 temperature sensors, thus 16 temperature sensors, and 6x6 sample containers, thus 36 sample containers.

[0109] Figure 3 shows a combination of the elements from Figures 1 and 2, with the positioning system 2 located in the heat treatment zone of the furnace chamber. As shown in Figure 2, the device comprises a sensor matrix with 16 temperature sensors and a positioning system with 36 sample containers.

[0110] Figure 4 shows a section of the device shown in Figure 1, showing the details of the front side of the device.

[0111] Figures 6.a and 6.b show schematic representations of the arrangement of the sensor matrix and positioning system in superimposed images. Figure 6.a shows a positioning system for 25 sample containers, and Figure 6.b shows a positioning system for 36 sample containers. In both cases, the device is equipped with a symmetrical sensor matrix comprising 4x4 temperature sensors, thus 16 temperature sensors.

[0112] Figures 7.a and 7.b show the schematic representations also shown in Figures 6.a and 6.b. The devices also have additional temperature control elements 27, which create the temperature gradient in the plane of the positioning system. This results in the temperature zones for certain rows of sample containers being almost identical and the temperature of the successive rows either rising or falling. Figure 7.a shows a drop in temperature along the rows, which is caused by the additional temperature control element 27 heating, which decreases as a function of the distance from the heat source. Figures 8.a and 8.Figure 8b shows schematic representations of a temperature sensor matrix with 5x5 measuring points or temperature values, which were achieved in conjunction with a temperature gradient of 60 K, with the total temperature from minimum to maximum temperature value in the range of 730 K to 790 K. It should be emphasized that a large number of samples can be treated at very different temperature values. In this case, five samples each at five different temperature values. Figure 8b illustrates that the accuracy is also influenced by the interaction of the various parameters. For example, by the number of temperature sensors in the sensor matrix and by the size of the respective sample containers. In addition, the magnitude of the temperature gradient also plays a role.

[0113] Examples of how to perform a calibration of the device.

[0114] Tests were conducted using the device according to the invention to calibrate the interior of the device. The device used here was equipped with a temperature control element in the form of a cooling device located in the door area of ​​the device. A sensor matrix with 4x4 temperature sensors (a total of 16 temperature sensors) was positioned in the interior of the device, arranged at defined points in the plane of the positioning system. The sensor matrix was connected to a process computer. The temperature control element was connected to a water-operated cooling thermostat. In this case, the cooling thermostat used was equipped with its own control system. The cooling thermostat is preferably connected to the process computer.During calibration, the device is set to different temperature levels, with cooling fluid being passed through the temperature control element at the same time, creating a temperature gradient in the form of a temperature drop towards the temperature control element. During calibration, the device was set to nine different set temperatures, and the temperatures at the sixteen temperature sensors were recorded. In the example, the set temperature was increased by 20 K in each case. Calibration data for the temperature range from 1003.15 K to 1163.15 K are shown in Figure 10.a, with the increase in the set temperature visible on the x-axis. Figure 10.a shows the measured data for four different positions inside the device.A graphical representation of all temperature values ​​at all sixteen positions would be too confusing due to the large amount of measured data. At a target temperature of 1003.15 K, the temperature gradient within the interior of the device is 65 K, and at a target temperature of 1163.15 K, the temperature gradient within the interior of the device is 41 K. Figure 10.b shows an enlarged detail for a single spatial position within the interior of the device for a target temperature of 1043.15 K. The basic elements of a heat treatment device also include heating elements, controllers, and at least one base temperature sensor. The basic elements are preferably integrated into the process control of the device according to the invention. The base temperature sensor(s) serve to regulate the base temperature of the device.Depending on the device's design, the base temperature sensor is a temperature sensor that forms a temperature sensor in the sensor matrix. The target temperature specification here refers to the temperature of the base temperature sensor, which serves as the central measuring sensor for adjusting or regulating the device's heating elements. Therefore, the base temperature sensor is also referred to as the central temperature sensor.

[0115] The furnace's temperature control causes a control noise of + / -1 K, meaning that temperatures fluctuate by a maximum of + / - 1 K over time. This control noise propagates to the individual spatial positions. Temperature measurements were detected with a precision of <0.1 K and correlated to the respective expected value with a statistical correlation coefficient of R>0.99. The expected value is calculated from the modeling of the calibration data.

[0116] Examples of thermal treatment of samples.

[0117] In two runs, sample materials in 25 containers and in 36 containers were subjected to thermal treatment, with the containers and the samples contained therein being exposed to different temperatures simultaneously. This was done in different runs for the sample materials in the 25 containers and the sample materials in the 36 containers. The duration of the thermal treatment was chosen to be 10 hours. The sample materials were powdered precipitates of mixed oxides, which form a Krista II structure upon thermal treatment. Mixed oxide powder compositions were selected in which the size of the crystallites formed depends on the temperature of the thermal treatment to which the sample materials are subjected.After completion of the thermal treatment, the sample materials were subjected to analytical characterization, in which the crystallite sizes of the individual samples were determined using an X-ray analytical method, namely by structure refinement with the Rietveld method using standards. Both internal reflections and samples prepared independently of the procedure described here served as standards. The achieved crystallite sizes show a correlation with the target temperature and corresponding reference samples. The achieved crystallite sizes show a correlation with the target temperature. A statistical evaluation of the data showed that the crystallite sizes of the samples correlated with the measured data from the thermal treatment with a correlation coefficient R. 2 > 0.95 could be correlated.

[0118] This example illustrates some of the advantages of the invention: with just a few runs, a large number of sample materials could be thermally treated simultaneously at different temperatures. The accuracy of the thermal treatment could be controlled very precisely, with the measurement data being recorded by the process control system and used as information for future measurements. These advantages are particularly interesting in the field of high-throughput research, where it is important to efficiently produce a large number of samples simultaneously.

[0119] List of reference symbols:

[0120] 1 device for heat treatment

[0121] 2 Positioning system with containers

[0122] 3 Sensor matrix

[0123] 4, 4', 4" temperature sensor

[0124] 5 Plug-in device

[0125] 6 Housing device for heat treatment

[0126] 7 additional temperature control device

[0127] 9 Supply line / connection line to temperature sensors

[0128] 11 Supply line to the additional temperature control device

[0129] 13 Positioning system

[0130] 14 Position for container

[0131] 15 containers

[0132] 21 Folding door

[0133] 23 mechanical locking system

[0134] 25 Measuring and control device in the form of a computer

[0135] 27 Level measuring device

[0136] 51 Tip of a temperature sensor

[0137] 53 Temperature at measuring position

[0138] 55 interpolated line, linearly interpolated in this case

Claims

Patent claims 1. Device for the heat treatment of materials, which is lockable and which has at least one thermally insulated door (21) equipped with a hinged or sliding mechanism, and which comprises a temperature-controlled interior, a sensor matrix (3) of temperature sensors, and a measuring and control unit, wherein the sensor matrix (3) comprises a plurality of temperature sensors (4, 4', 4,") arranged at different points within the temperature-controlled interior of the device and the number of temperature sensors is > 4.

2. Device for the heat treatment of materials according to claim 1, wherein the temperature-controlled interior has a width in the range of 10 to 100 cm, a height in the range of 5 to 50 cm and a depth in the range of 10 to 100 cm.

3. Device for heat treatment of materials according to claim 1 or claim 2, wherein the device has a positioning system (13) for receiving containers, the number of containers being in the range of 4 to 256, or the positioning system (13) has a number of recesses being in the range of 4 to 256.

4. Device for the heat treatment of materials according to any of the aforementioned claims 1 to 3, characterized in that the temperature sensors are arranged in a symmetrical group or at least partially in a planar surface.

5. Device for the heat treatment of materials according to any of the preceding claims 1 to 4, wherein the device has an additional temperature control element by means of which at least a partial area of ​​the thermal treatment zone is heated or cooled.

6. Device for the heat treatment of materials according to any one of claims 1 to 5, wherein the device has one or more suction lances and an analyzer, wherein the suction lances are connected to the analyzer by lines and wherein the endpoints of the suction lances are arranged inside the device.

7. Device for the heat treatment of materials according to one of the preceding claims 5 or 6, wherein the additional tempering element is designed in the form of a rod or a planar shape. Method for the heat treatment of materials in a device constructed according to any one of claims 1 to 7 above and connected to a database for recording and analyzing process parameters, wherein the method comprises the following steps: - Placing the materials into containers; - Positioning of the filled containers in the receiving positions of the positioning system; - Transfer of the positioning system equipped with containers into the thermal treatment zone of the device; - Storage of the positioning system in the thermal treatment zone; - Acquisition of test parameters, wherein information on the individual materials in the form of sample identification numbers and their spatial arrangement with respect to the respective recording positions within the positioning system is included; wherein, when the positioning system is stored in the treatment zone, measurement data on the temperature of the individual temperature sensors are recorded as a function of time using the sensor matrix. A method for the heat treatment of materials according to claim 8, comprising the following steps: - Storing information on the positions of the individual temperature sensors within the temperature-controlled interior space in the database; - Storing information about the positioning system in the database, including the position of each surface of the positioning system and the dimensions of each container; - Storage of the positioning system in the thermal treatment zone with temperature control of the interior at a temperature in the range of 473.15 to 2073.15 K for a selected period of time, wherein the temperature control of the interior is carried out by means of a single control unit in such a way that the device is temperature-controlled at a uniform target temperature with respect to the surface of the positioning system; - Recording of the temperature measurements, which are determined by means of the individual temperature sensors, in the database together with position and time information during the execution of the temperature control; - Assignment of local temperature measurements to individual containers whose surface area overlaps with the local temperature sensors or where the temperature sensors are located nearby, whereby an adjustment of the tem- Temperature measurements are taken when adjacent temperature measurements show a temperature difference, and the temperature measurements assigned to the containers are assigned to the materials contained in the containers, with the values ​​being stored in the database under an identification number that is characteristic of the respective container and the material arranged in it.

10. A method for the heat treatment of materials according to claim 9, wherein the method comprises an optimization algorithm and a program control, and the program control provides a selection of parameters from the group consisting of the number of samples to be subjected to thermal treatment, the quantity of samples, the value of the target temperature at which the thermal treatment is to be carried out, and the magnitude of the accuracy is determined on the basis of at least one parameter, wherein the accuracy is given by AK or Delta in Kelvin.

11. Method for the heat treatment of materials according to claim 10, wherein the measurement data determined by means of the sensor matrix are related, wherein the values ​​in the space between adjacent temperature sensors are determined computationally and the determined measurement data of the temperature sensors are assigned to the recording positions and the containers arranged in the recording positions.

12. Method for the heat treatment of materials according to any one of claims 8 to 11, wherein a heat treatment device according to claim 5 is used and wherein the thermal treatment zone is heated or cooled by means of the additional temperature control element, wherein the additional temperature control element is controlled by a separate control element which is connected to the measuring and control unit of the device and thus also to the data storage device; the additional temperature control element causes the generation of a temperature gradient field in the interior of the device, preferably the temperature gradient field is aligned parallel to the surface of the positioning system, wherein in the method the containers are stored in the receiving positions of the positioning system at different temperature values, wherein the measurement data of the individual temperature sensors have temperature deviations of < 5K.

13. Method for the heat treatment of materials according to claim 12, wherein the temperature-controlled interior is heated to a target temperature and a gradient field is generated by means of the additional temperature control element; wherein the temperature readings measured at the individual temperature sensors are combined with the set Control and regulation parameters are stored in the database, wherein the respective configuration of target temperature in combination with control and regulation parameters determines the structure of the temperature gradient field within the temperature-controlled interior space, wherein the gradient field surface preferably has a monotonic profile and is characterized by a linear rise or fall.

14. A method for the heat treatment of materials according to claim 13, wherein the quantity and number of materials and the temperature levels at which the tempering is to be carried out are specified, and the method comprises a computer program which uses the values ​​stored in the database to determine a program sequence for carrying out the method, wherein the specification of parameters preferably also includes a specification of the temperature fluctuation which is not to be exceeded, wherein the slope of the temperature gradient is related to the diameter of the bottom surface of a single container, which is preferably 5 K, wherein the computer program is preferably also able to specify the appropriate container size to be used for carrying out the temperature control.

15. Method for the heat treatment of materials according to any one of claims 8 to 14, wherein the method comprises the following steps: the materials obtained by the heat treatment are characterized with respect to their performance properties and the parameters characterizing the performance properties are recorded in the database.

16. A method for the heat treatment of materials according to any one of claims 8 to 15, wherein the method comprises the evaluation of the data relating to the performance characteristics according to claim 10 and wherein the evaluation further comprises the comparison with data and / or information obtained from a database that was not obtained during the execution of the method or in a previous execution of the method.

17. A method for the heat treatment and characterization of materials according to any one of claims 8 to 16, wherein the method relates to the production of materials from the group consisting of catalysts, battery materials, high-performance ceramics, and inorganic semiconductor materials, wherein the materials from the group mentioned herein are subjected to a temperature treatment during the production process, wherein the Information on the type of materials and the treatment is stored in the database, with each treatment step being recorded in such a way that the treated material receives a corresponding identification number, which is stored in the database. A computer program for controlling a heat treatment device having the features according to any one of claims 1 to 7. A computer program for carrying out a method according to any one of claims 8 to 17.

Images