Classifications

• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
  • F27—FURNACES; KILNS; OVENS; RETORTS
  • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
  • F27D3/00—Charging; Discharging; Manipulation of charge
• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
  • F27—FURNACES; KILNS; OVENS; RETORTS
  • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
  • F27D19/00—Arrangements of controlling devices
• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
  • F27—FURNACES; KILNS; OVENS; RETORTS
  • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
  • F27D3/00—Charging; Discharging; Manipulation of charge
  • F27D2003/0001—Positioning the charge
• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
  • F27—FURNACES; KILNS; OVENS; RETORTS
  • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
  • F27D19/00—Arrangements of controlling devices
  • F27D2019/0003—Monitoring the temperature or a characteristic of the charge and using it as a controlling value
• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
  • F27—FURNACES; KILNS; OVENS; RETORTS
  • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
  • F27D19/00—Arrangements of controlling devices
  • F27D2019/0096—Arrangements of controlling devices involving simulation means, e.g. of the treating or charging step

Definitions

• the invention relates to a method for determining temperature distribution data and providing position arrangement data, arranging one or more samples in one or more ovens, and determining one or more samples out of the heat-treated samples. Furthermore, the invention also relates to a cathode, an oven arrangement, and the use of one or more ovens for heat treatment of two or more samples.
• Calcining is a thermal treatment process characterized by the controlled application of heat to a material, typically in the absence or limited presence of air, leading to the removal of volatile components, phase transformations, or the activation of desired chemical reactions. This technique is widely utilized in various industries, including chemistry, to enhance material properties and achieve specific chemical outcomes.
• this disclosure relates to a method for determining temperature distribution data associated with a temperature distribution inside an oven having inside spatially distributed sample positions, the method comprising: providing calibration temperature values at the sample positions for predetermined setpoint temperature values of the oven; providing a selected setpoint temperature value of the oven from a continuously adjustable setpoint temperature value; determining the temperature distribution data based on the calibration temperature values and/or the selected setpoint temperature value, wherein for the selected setpoint temperature value, the temperature distribution data includes a determined temperature value at each sample position.
• This approach is particularly advantageous, as calculating local temperature value at different position allows predicting which temperature samples may experience, and thus, providing foundation for an optimization approach as described herein. Additionally or alternatively, it is beneficial, as it provides basis for monitoring and/or checking that a given oven is behaving the same as when calibration data were gathered.
• Predetermined setpoints are intended to refer to predetermined setpoints from, for instance, a calibration and/or training data, which may be collected in advance of a synthesis to be performed.
• Selected setpoint temperature is intended to refer to a temperature chosen for a material synthesis in question.
• the disclosure relates to a method for providing position arrangement data associated with arranging one or more samples in one or more ovens at spatially distributed sample positions, the comprising: providing a target temperature value for each sample; determining temperature distribution data for a given oven according to aforementioned method; providing position arrangement data associated with a sample of the one or more samples, wherein the sample is to be arranged at a sample position dependent on the target temperature value of sample and/or the determined temperature distribution data.
• the disclosure relates to a method for providing position arrangement data associated with arranging one or more samples in one or more ovens at spatially distributed sample positions, the comprising: providing a target temperature value for each sample; providing a selected setpoint temperature of a given oven; determining temperature distribution data for a given oven according to aforementioned method; providing position arrangement data associated with a sample of the one or more samples, wherein the sample is to be arranged at a sample position dependent on the target temperature value of sample and/or the determined temperature distribution data.
• This approach is particularly beneficial, as it allows achieving of pre-determined experimental conditions rather than relying on a fixed oven setpoint with the expectation that each sample experiences a temperature close to the desired one. This eliminates the need for trial-and-error methods, resulting in increased efficiency and more informative experimental studies. Furthermore, it provides greater control over the experimental conditions, ensuring that each sample experiences the specific temperature required by the experimental plan, which is advantageous, as it eliminates the uncertainty and variability that can occur when relying solely on a fixed oven setpoint. Ultimately this makes experimental studies more efficient and informative.
• the disclosure relates to a method for arranging one or more samples in one or more ovens at assigned sample positions based on the position arrangement data generated according to the aforementioned method. This is advantageous, as it allows for the maximization of each oven's sample capacity, which may be achieved by utilizing the pre-determined experimental conditions, which optimizes the use of available resources while maintaining the accuracy and reliability of results.
• the disclosure relates to a method for determining one or more samples out of heat-treated samples, the method comprising: Arranging samples in one or more ovens according to the method for arranging one or more samples in one or more ovens as recited herein; performing a firing run by a given oven of the one or more ovens; and determining one or more samples out of the heat-treated samples based on at least one performance parameter.
• This approach is advantageous, as it allows optimization of laboratory resources by minimizing number of materials that need to be synthesized, which reduces need for extensive synthesis processes, saving time, energy and materials.
• the disclosure relates to a cathode comprising at least partially a material of the determined heat-treated sample obtained by the method for determining one or more samples out of the heat-treated samples as recited herein.
• This approach is beneficial, as, for instance, it minimizes the number of electrochemical cells that need to be built and tested.
• the disclosure relates to a computer program for performing at least one of the aforementioned methods, such as method for determining temperature distribution data and method for providing position arrangement data.
• a computer program for performing at least one of the aforementioned methods, such as method for determining temperature distribution data and method for providing position arrangement data.
• the disclosure relates to an oven arrangement having an oven and a computing device configured to execute at least one of the aforementioned methods, such as method for determining temperature distribution data and method for providing position arrangement data.
• a computing device configured to execute at least one of the aforementioned methods, such as method for determining temperature distribution data and method for providing position arrangement data.
• the disclosure relates to a use of one oven for heat treatment of two or more samples arranged at spatially distributed sample positions, wherein at least two of the samples demand heat treatment temperatures differing from each other.
• This approach is particularly advantageous, as it allows to dispense with multiple firing runs to perform such experiments. Consequently, this approach is beneficial, as it allows treating multiple samples using only a single firing run, thus requiring less energy and time.
• any disclosure, embodiments and examples described herein relate to the method for determining temperature distribution data, the method for providing position arrangement data, a method for arranging one or more samples in one or more ovens, a method for determining one or more samples out of the heat-treated samples, a cathode, the computer program, the oven arrangement and the use of one oven lined out above and below.
• the benefits provided by any of the embodiments and examples equally apply to all other embodiments and examples.
• the disclosure relates to a method for determining temperature distribution data associated with a temperature distribution inside an oven having inside spatially distributed sample positions, the method comprising: providing calibration temperature values at the sample positions for predetermined setpoint temperature values of the oven; providing a selected setpoint temperature value of the oven from a continuously adjustable setpoint temperature value; determining the temperature distribution data based on the calibration temperature values and/or the selected setpoint temperature value, wherein for the selected setpoint temperature value, the temperature distribution data includes a determined temperature value at each sample position.
• an oven setpoint temperature and a sample position in the oven can be chosen such that the temperature acting on the sample is as close as possible to the demanded target temperature of the sample. This prevents an unwanted variation in the material quality of heat-treated samples.
• the at least partially prevailing temperature heterogeneities inside the oven can be utilized to the effect that several samples demanding for treatment temperatures at least partially different from each other, can be heat treated in a single oven.
• the disclosure relates to a method for providing position arrangement data associated with arranging one or more samples in one or more ovens at spatially distributed sample positions, the comprising: providing a target temperature value for each sample; determining temperature distribution data for a given oven according to aforementioned method; providing position arrangement data associated with a sample of the one or more samples, wherein the sample is to be arranged at a sample position dependent on the target temperature value of sample and/or the determined temperature distribution data.
• a method for providing position arrangement data wherein the position arrangement data is determined based on the demanded target temperatures of the samples and the determined temperature distribution data, for samples to be heat treated at least an oven setpoint temperature and sample positions in the oven are suggested such that the temperature acting on the respective sample is as close as possible to the demanded target temperature of this sample. Heat treatment of several samples in one oven run increases the sample throughput and therefore saves time.
• the temperature distribution data may be associated with a collection of data regarding the temperature distribution inside an oven.
• the temperature distribution may be indicative of the variation of temperature inside the oven over a specific area of the oven interior.
• the temperature distribution may refer to a plurality of determined temperatures at sample positions spatially distributed over the specific area of the oven interior.
• the specific area may be the entire oven interior.
• the temperature distribution may relate to the setpoint temperature and the calibration temperature values.
• the temperature distribution may be an output of an interpolating function, which is generated by fitting a temperature distribution model to the calibration temperature values for a given setpoint temperature of the oven.
• the temperature distribution may be an output of an interpolating function, which is generated by fitting a temperature distribution model to the calibration temperature values for multiple setpoints temperature of the oven.
• the oven may be a firing oven, in particular a calcination oven.
• the oven may have sample positions and a heating source, which are arranged immovable to each other during a firing run.
• the oven may have means for transporting the samples in relation to the heating source during a firing run, such as a conveyor belt.
• the heating source may be heating elements or a hot air blower.
• the oven may have cooling means at the front door. In particular based on the interaction of the heating means and the cooling means the oven has inside a temperature distribution.
• the sample to be heat treated may be a so-called P-CAM (precursor cathode active material).
• the P-CAM may be a composition of educts for producing cathode materials (CAM) of batteries as end products.
• the respective educt is in form of a powder.
• the respective composition of educts may include at least one of the following: a Nickel Cobalt Manganese hydroxide (NCM) precursor, a lithium salt and a at least one dopant.
• the lithium salt may be lithium hydroxide (LiOH).
• the dopant may be provided in a quantity of 0 to 5 mol%, such as 0 to 3 mol%, such as 2.5 mol%.
• the respective dopant may be zirconium (Zr), titanium (Ti), magnesium (Mg) and/or aluminum (Al).
• the educts are mixed in order to obtain the powdery composition of educts and then the composition is filled into a crucible.
• the crucibles may be arranged on a tablet that is inserted into the oven interior.
• the crucibles may be chessboard-like arranged on the tablet.
• the composition of educts gas in particular oxygen, may be fed to the oven interior.
• the calibration temperature values may be associated with temperature values that are determined based on measured temperatures inside the oven at spatially distributed positions during a calibration run of the oven for a given setpoint temperature value of the oven. For measuring the temperatures there may be provided fewer temperature sensors inside the oven than sample positions inside the oven. The determination of the calibration temperature values at the sample positions may be performed by interpolating the measured temperatures. The calibration temperature is dependent on the sample position and the temperature at this sample position that is dependent on at least one of the measured temperatures.
• the setpoint temperature value of the oven may be associated with the temperature value to which the entire oven is set. Despite that the set point temperature is set, inside the oven a temperature distribution may be prevailing having at least one determined temperature that differs from the setpoint temperature.
• the set point temperature may depend on the use of the oven.
• the use of the oven may be for calcining cathode materials of batteries. For said use the set point temperature may be in the range of about 700 to 900 degrees Celsius.
• the determined temperature may be associated with the temperature at a respective sample position for a respective setpoint temperature of the oven.
• the determined temperature may be related to the setpoint temperature and the calibration temperature values.
• the determined temperature for a setpoint temperature may be interpolated based on the calibration temperature values.
• Determining one or more samples out of the heat-treated samples is associated with choosing that respective sample that has for an intended use a predetermined quality indicated by reaching a threshold by the at least one performance parameter.
• a heat-treated sample is chosen that is suitable for usage as a cathode material in a battery.
• the calibration temperature values are determined based on temperature measurements in the oven during calibration runs of the oven for given setpoint temperature values of the oven.
• calibration runs of the oven may be performed.
• the oven setpoint temperature may be varied in several temperature steps across a relevant range.
• the relevant range may be depending on the intend use of the oven.
• the intended use may be calcining cathode materials of batteries.
• the relevant range may be about 700 to 900 degrees Celsius.
• the temperatures may be measured inside the oven by temperature sensors at spatially distributed positions. The measured temperatures may be used to calculate, in particular interpolate, the calibration temperatures at the sample positions.
• the temperature distribution data depends additionally on the sample position in the oven. Since the temperature distribution data includes for each setpoint temperature a determined temperature at each sample position, the determined temperature also depends on the following temperatures: the respective setpoint temperature, the calibration temperature and in particular the sample position.
• this temperature for each oven is determined using the calibration temperatures and in particular the target temperatures and/or at least a constant.
• an interval having an upper bound and a lower bound is determined, wherein the setpoint temperature is arranged in the interval, and wherein the bounds are each dependent on at least one of following: the target temperatures, the calibration temperatures, at least a constant and the maximum reachable temperature of the given oven.
• the bounds are dependent each on the target temperatures, the calibration temperatures and in particular the constant.
• the upper bound is either a highest calibration temperature or a sum of a highest target temperature and a constant; whichever is lower, and the lower bound is a lowest calibration temperature or a sum of a lowest target temperature and a further constant; whichever is lower.
• said setpoint temperature is varied in the interval in order to minimize a loss function.
• the Nelder-Mead method known in the state of the art may be used.
• the loss function may be provided depending on the respective target temperature and the respective temperature distribution data.
• the determined temperature vector is subtracted from the target temperature vector, wherein this difference is squared and summed up over all samples.
• an initial value of this setpoint temperature is uniformly distributed within the interval. In more simple words, if there are multiple setpoints to be determined, these may be spaced on a uniform grid within a given interval. If only a single setpoint is to be determined, this may be put at the center point.
• the setpoint temperature value may be varied in the interval to minimize a loss function depending on the target temperature value and/or the temperature distribution data. Additionally or alternatively, for varying the at least one setpoint temperature an initial value of this setpoint temperature is uniformly distributed within the interval. Furthermore, for minimizing the loss function each of the samples may be consecutively assigned to a given sample position in the given oven, at which the target temperature value is closest to the determined temperature value of the temperature distribution data.
• the respective samples one after the other are assigned to that respective sample position in the respective oven, at which the target temperature is closest to the determined temperature of the temperature distribution data and at which no sample has already been assigned to.
• the target temperature is closest to the determined temperature of the temperature distribution data and at which no sample has already been assigned to.
• the setpoint temperature is chosen that minimizes the loss function at least in a local minimum.
• Fig. 1 shows an oven arrangement 10 according to the invention, which comprises two firing, in particular calcination, ovens 12, 13 and a computing unit 14 in form of a cloud server.
• Ovens 12, 13 or a given oven 12, 13 may be a heat treatment device according to the disclosure of WO 2023/198804 A1 .
• the computing unit 14 is communicatively connected to two personal computers 16 each being arranged with an end user.
• On the computing unit 14 a software back end is implemented, wherein the assigned software front end is accessible for an end user via each personal computer 16.
• the methods according to the invention are executed on the computing unit 14. Via a personal computer 16 an end user has access separated from each other to the computing unit 14 as well as to a control unit of a given oven 12,13.
• x ijk is a variable, which is 1 if the position j in firing run i is occupied by a sample (for instance, a material to be calcinated) and otherwise 0.
• a sample for instance, a material to be calcinated
• This approach allows improvements of planned calcination temperatures of each material subject to practical constraints, such as allowing each position of the oven to be occupied by only a single crucible.
• a next step S17 the assignment 26, 28 of samples to the sample positions 18 and the ovens 12, 13 (see Fig. 6 ) are shown to the end user.
• the sample ID 22, the determined temperature T exp 30 and the temperature difference 24 between the determined temperature T exp and the target temperature T targ is visualized to the end user.
• Fig. 7 depicts a method 300 for arranging one or more samples in one or more ovens.
• step S28 Thereafter in a step S28 according to the assignment data the end user arranges the samples in the respective oven 12, 13. It is also conceivable that this arrangement is done by an arm of a robot.
• steps S30 to S38 the method for arranging samples in one or more ovens is performed according to steps S20 to S28.Thereafter the user parameterizes the ovens, in particular sets the setpoint temperature, via a personal computer 16 and starts the firing runs.
• the samples may be lithiated, which means that lithium goes from LiOH into the crystal structure, and/or the hydroxide groups may be removed from the sample material.
• the structure itself of the material can also change (different crystal phases can be achieved for example).
• posttreatment may be done, which involves mechanically breaking up the heat-treated sample material (CAM) so it can be processed more easily, and/or coat the heat-treated sample material to improve the properties of the particle surfaces.
• CAM heat-treated sample material
• the heat-treated sample material is mixed with a solvent, carbon and binder to make a slurry, which in a next step 42 can be applied to an aluminum part in order to obtain a cathode.
• this cell is tested in a device to measure at least one performance parameter of the cell, for example the capacity (how much charge does it hold and can be transferred), the energy density and/or the lifetime.
• a next step 45 based on the respective performance parameter a decision is made about which materials are worth pursuing in research and are potentially sent to customers.

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• General Engineering & Computer Science (AREA)
• Investigating Or Analyzing Materials Using Thermal Means (AREA)

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Citations (3)

• 2024
  • 2024-08-02 EP EP24192564.3A patent/EP4686902A1/de not_active Withdrawn

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