Labormahlkörpermühle

Abstract

The invention relates to a laboratory grinding media mill (1), in particular a planetary ball mill, centrifugal ball mill or vibrating mill, comprising: a grinding vessel (8) with walls defining a grinding vessel interior (18) which can be filled with grinding material and grinding elements in order to grind the grinding material in the grinding vessel interior (18) between the grinding elements and the walls of the grinding vessel (8) by means of impact and friction effects by means of rotational and / or oscillating movements of the grinding vessel (8), a grinding vessel receiving device (216) in which the grinding vessel (8) can be clamped, a motor drive (226) for driving the rotation and / or oscillating movement of the grinding vessel receiving device (216) with the grinding vessel (8) clamped therein, a mill control device (224) which controls the grinding process of the laboratory grinding media mill (1), wherein the grinding vessel (8) comprises: a gas temperature sensor (80) which measures a gas temperature measurement value of the gas atmosphere in the grinding vessel (8) and a contact temperature sensor (110) which measures a contact temperature measurement value of one of the walls of the grinding vessel (8).

Description

Field of the InventionThe invention relates to a laboratory grinding mill for process analysis in laboratory applications, in particular a planetary ball mill, a centrifugal ball mill or a vibratory mill on a laboratory scale, in which grinding material can be finely ground in a sealed grinding vessel by permanently changing acceleration in a grinding vessel interior space between the grinding bodies and walls of the grinding vessel by impact and frictional action.BACKGROUND OF THE INVENTIONGrinding media mills on a laboratory scale are used, for example, in process analysis for grinding samples. Depending on the requirements of the sample quantity and the grinding conditions and the desired grinding result, for example the desired degree of fineness or the amount of grinding material, such laboratory grinding mill mills can be designed as planetary ball mills, centrifugal ball mills or vibrating mills, sometimes also simply referred to as ball mills. Laboratory-scale planetary ball mills are described, for example, in patent applications DE 197 12 905 A1, DE 10 2006 006 529 A1, DE 10 2006 018 325 A1, DE 10 2006 047 481 A1, DE 10 2006 047 480 A1 and DE 10 2006 047 479 A1. DE 10 2006 047 498 A1 describes a ball mill with cooling, in which cooling channels extend at least partially within the base and / or the annular wall of a cup-like receiving device. More recent planetary mills are described, for example, in DE 10 2010 044 254 A1, DE 10 2012 009 983 A1, DE 10 2012 009 985 A1, DE 10 2012 009 982 A1, DE 10 2012 009 984 A1, DE 10 2012 009 987 A1. A selection of currently available planetary mills on a laboratory scale is also found on the web page of the applicant under www.fritsch.de.In planetary (ball) mills and most centrifugal (ball) mills, grinding vessels are arranged as planets eccentrically to a sun axis, sometimes also referred to as the center axis, and on the one hand revolve on a circular path around the sun axis and on the other hand rotate about their own axis, the eccentric planetary axis. As a result of the circulation and the simultaneous rotation of the grinding cups, a changing centrifugal force directed radially outwards is exerted on the grinding material filled into the grinding cup. Typically, reusable grinding bodies, for example grinding balls, are also added to the grinding material, which grinding bodies break the grinding material with high efficiency by impact and frictional action between the grinding bodies and the walls of the grinding vessel. The grinding vessel and grinding body together form the so-called grinding assembly.With certain dimensions of the revolving parts and certain rotational speeds, flight paths for the grinding material and the grinding bodies can be produced in a planetary ball mill. The grinding material and the grinding bodies then move transversely through the grinding cup until they strike the inner wall of the grinding cup. Thereafter, the grinding material with the grinding bodies can be carried along a certain distance on the inner circumference of the grinding cup until the resulting force again ensures that the above-described transverse acceleration takes place and the grinding material and the grinding bodies execute a flight movement through the grinding cup. This is also referred to as a "throwing regime". If a ball mill operates in the throwing regime, a high grinding effect or a high energy input into the ground material can be achieved at high rotational speeds.In vibrating mills, a grinding vessel consisting of a grinding cup and a grinding cup cover is likewise set into a permanently alternating acceleration, specifically typically into an oscillatory or vibrating movement. In some vibratory mills, the grinding vessels are suspended upright on a vibratory plate as a grinding vessel receiving device. Such vibratory mills typically operate with a single or a few larger grinding bodies, e.g. ring-shaped or disc-shaped grinding bodies (grinding discs) which remain resting on the grinding cup bottom when the grinding vessel oscillates. An example of a vibrating mill, sometimes also referred to as a disk (vibrating) mill, is the Pulverisette® 9 of the applicant, cf. www.fritsch.de. However, vibrating mills are also known which optionally use smaller, typically longitudinally cylindrical, grinding vessels with grinding balls, e.g. with a grinding vessel volume of up to 50 ml, wherein the grinding vessels are clamped e.g. horizontally, e.g. in two grinding vessel receptacles vibrating horizontally in opposite directions (Boxer principle). The grinding vessels can oscillate to and fro at a defined oscillation frequency substantially along a straight or slightly curved line, substantially horizontally.Laboratory grinding mills are distinguished by rapid and effective comminution. They can be used in many applications and are ideally suitable for loss-free ultra-fine comminution, depending on the mill type, up to final finenesses in the nanometer range. Depending on the object to be achieved, the grinding can be carried out dry, in suspension or under inert gas. Laboratory grinding mills can be used not only for pure comminution processes but also for mixing, alloying, activation, amorphization or phase conversion processes.These processes can be associated with a relatively high energy input into the grinding material or the grinding vessel and optionally lead to undesired heating of the grinding material and / or the grinding vessel. Some materials are temperature sensitive that they cannot be ground to the desired quality in current laboratory grinding mills. Other materials can only be comminuted after embrittlement. The grinding vessels themselves may also be subject to thermal or pressure-related restrictions, in particular if they are joined grinding vessels. Moreover, safety measures for the operation must be taken into account.Patent DE 10 2006 047 481 describes a ball mill with a grinding vessel which comprises two measurement pickups, wherein one of the measurement pickups is a temperature sensor and the other of the measurement pickups is a pressure sensor, as well as a plate which can be positioned on the cover and carries at least one of the measurement pickups. During operation of the ball mill, the measurement pickup records at least one measurement value of the state in the interior of the grinding vessel, in particular of the pressure and / or the temperature.Patent application DE 10 2023 103 629 (not prepublished) describes a laboratory grinding mill for crushing grinding material, wherein the grinding vessel is provided, at least in a visible region on the outer side of the grinding vessel, for example with a passive thermochromic display device.GENERAL DESCRIPTION OF THE INVENTIONThe object of the invention is to provide a laboratory grinding mill which ensures a high level of safety for the user, in particular when opening or removing the grinding vessel from the grinding vessel receiving device, and protects the user from improper handling.A further aspect of the object of the invention is to provide a laboratory grinding mill which simultaneously accommodates both automation and manual operation, and which can additionally, as quickly as possible and ergonomically provide the user with information about selected parameters of the grinding material, the grinding atmosphere and / or the grinding vessels, in particular immediately after the grinding, in particular as the automation progresses.A further aspect of the object of the invention is to provide a laboratory grinding mill which is safe and ergonomic to operate for the user.A further aspect of the object of the invention is to provide a laboratory grinding mill which can at least partially automatically control the processes running in the grinding vessel under various conditions and / or can protect the grinding assembly and / or the grinding material from undesired adverse effects.Another aspect of the object of the invention is to provide a laboratory grinding mill which provides the user with additional information about the grinding process.A further aspect of the object of the invention is to provide a laboratory grinding mill which can bring the grinding time, the energy input, user- and grinding-material-protecting restrictions of the grinding vessels and requirements due to different grinding materials into agreement with one another.The object of the invention is achieved by the subject matter of the independent claims. Advantageous further developments of the invention are defined in the dependent claims.According to one aspect of the present invention, a laboratory-scale grinding mill, i.e. a laboratory grinding mill, is provided, in particular selected from planetary ball mills, centrifugal ball mills or vibrating mills on a laboratory scale or prepared for process analysis carried out in a laboratory. The laboratory grinding body mill comprises a grinding vessel with a grinding cup and a grinding cup cover for hermetically closing the grinding cup. The grinding vessel can be designed, for example, as a whole cylindrically, so that the grinding cup cover axially closes the grinding vessel at an opening on the end side with respect to the grinding cup axis. The grinding cup cover can also itself be shaped cup-like, wherein the grinding cup and the grinding cup cover can then engage in each other cup-like manner. The grinding vessel defines the grinding vessel interior, which can be filled with grinding material and grinding bodies, in particular grinding balls. By means of rotational and / or oscillatory movements, i.e. a permanently changing acceleration of the grinding vessel, wherein the direction and / or amount of the acceleration can also permanently change, the grinding material in the grinding vessel interior space between the grinding bodies and the walls, e.g. a grinding cup shell wall, a grinding cup base and / or the grinding cup cover, of the grinding vessel is ground by impact and frictional action and / or is subjected to further physicochemical reactions or processes.During operation, the grinding vessel is firmly clamped in a grinding vessel receiving device of the laboratory grinding body mill in order to transmit the rotational and / or oscillatory movements from the grinding vessel receiving device to the clamped and closed grinding vessel.An electric motor drives the rotational and / or oscillatory movement of the grinding vessel receiving device with the grinding vessel clamped therein. For example, in a planetary ball mill, the electric motor may drive the sun and planetary rotation at a certain speed ratio via a belt drive, as shown in the documents cited in the introduction, e.g. to planetary ball mills, which are hereby incorporated by reference.The laboratory grinding mill has, in particular in its stationary mill housing, a mill control device which controls the grinding process, e.g. drive parameters such as rotational speed, oscillation frequency, grinding duration etc. of the laboratory grinding mill. The mill housing also houses the moving parts of the laboratory grinding mill, such as the grinding vessel receiving device and the grinding vessel clamped therein. The mill housing preferably has an openable and closable housing cover which protects the moving parts from access during operation and, when the laboratory grinding body mill is stationary, allows access to the grinding vessel by opening the housing cover. The laboratory grinding body mill has in particular a safety circuit which ensures that the grinding process can only be started when the housing cover is closed.The grinding vessel according to one aspect of the invention comprises at least one sensor which measures a state parameter of the grinding vessel and / or of the grinding vessel interior and an electronic display device which is arranged on an outer side of the grinding vessel and which displays the state parameter measured by the sensor visibly directly on the outer side of the grinding vessel for the user.With the electronic display device directly on the grinding vessel, a special and multiple use for the user can be achieved in a laboratory grinding mill.Advantageously, the user can have the desired information about the status parameter directly in the direction of grip and viewing on the grinding vessel, namely regardless of whether the grinding vessel is still braced in the grinding vessel receiving device or whether the grinding vessel bracing device has already been opened.It is thus possible, inter alia, to prevent the user from touching the grinding vessel with bare fingers when actuating the grinding vessel clamping device if said grinding vessel clamping device exceeds a specific temperature threshold value, without the user having to do so with regard to a user interface of the laboratory grinding body mill, for example, or to another location of the mill. The same also applies to the removal of the grinding vessel from the grinding vessel receiving device or from the laboratory grinding body mill. Thus, the user has the corresponding information and warning functions exactly where he would typically intervene with the fingers and possibly threaten a risk and does not have to swerve to another location with a glance.Furthermore, during the grinding process, depending on the grinding material and the energy input, not only a high temperature but also a high gas pressure can build up in the grinding vessel. The opening of the grinding vessel is often carried out outside the mill, for example away from the mill on a laboratory table, namely when the user has already removed the grinding vessel, optionally with protective gloves. In such laboratory situations, the user can also be protected, for example, from an explosive escape of the gas atmosphere from the grinding vessel interior when the grinding vessel is opened, if the user is provided with the gas pressure directly displayed on the grinding vessel itself. The user thus always has the corresponding information and warning functions at the correct location, regardless of the type of grinding vessel handling. In addition, it may also be relevant for the user to have the gas temperature in the grinding vessel interior and / or the contact temperature of the grinding vessel outside the mill in the field of view if the grinding vessel is handled, e.g. is to be opened, outside or remote from the laboratory grinding body mill. The user therefore has the information about the measured state parameter of the grinding vessel interior at any time and independently of the grinding vessel handling in the field of view in the grip direction, even if the grinding vessel has already been removed from the laboratory grinding body mill and has been placed, for example, on a laboratory table or in a trigger in order to open it in order to remove grinding material. If necessary, the user can also draw particular conclusions on the grinding material, the gas atmosphere in the grinding vessel interior and / or the behavior when opening the grinding vessel from the presence of a plurality of items of information in combination such as gas pressure, gas temperature and / or contact temperature.If necessary, after the grinding, the user can distinguish or identify a plurality of grinding vessels from the same or from different laboratory grinding mill bodies by reading the measured state parameter on the grinding vessel. With the same weight, but different input parameters, different temperatures can develop, for example, for different grinding stock material or for wet grinding compared to dry grinding.The grinding vessel preferably comprises an energy supply for supplying the electronic display device of the grinding vessel with electrical energy, for example in the grinding cup cover.The at least one sensor is in particular a temperature sensor and / or a pressure sensor. As a result, the current temperature and / or the current pressure in the grinding vessel can be displayed, which can be safety-relevant information on the one hand when removing the grinding vessel from the laboratory grinding mill and on the other hand when opening the grinding vessel.The grinding vessel can preferably comprise a grinding cup base, a circumferential grinding cup jacket wall, in the form of an annular wall circumferentially around the grinding cup axis or grinding vessel axis, as well as the grinding cup cover, wherein the at least one sensor comprises at least one or more of the following sensors:a gas temperature sensor which measures a temperature measurement value of the gas atmosphere located in the grinding vessel interior,a contact temperature sensor which measures a temperature measurement value of a grinding vessel wall, in particular of the grinding cup base, the grinding cup shell wall or the grinding cup lid, by thermal contact,a pressure sensor which measures the gas pressure of the gas atmosphere present in the grinding vessel interior.Preferably, the grinding cup base, the grinding cup shell wall or the grinding cup cover has a measurement cavity and a connecting channel which connects the grinding vessel interior to the measurement cavity for fluid exchange and pressure equalization, so that fluid communication is ensured between the grinding vessel interior and the measurement cavity. The gas temperature sensor and / or the pressure sensor can thus be arranged in the measurement cavity, and the measurement cavity is in fluid communication with the grinding vessel interior via the connecting channel, such that the gas atmosphere in the measurement cavity is substantially the same as in the grinding vessel interior, and the pressure sensor and the temperature sensor supply the corresponding measurement values of the gas atmosphere of the grinding vessel interior.The grinding vessel preferably comprises a grinding vessel board with control electronics inherent to the grinding vessel, which has sensor reading electronics and / or a display controller, to which the at least one sensor and the electronic display device are connected and which is supplied with electrical energy by the energy supply of the grinding vessel in order to read out the at least one sensor directly on the grinding vessel and to actuate the electronic display device on the outer side of the grinding vessel, so that the state parameters measured by the at least one sensor are electronically displayed directly on the outer side of the grinding vessel. Although this can increase the energy consumption at the grinding vessel, it can simplify the communication between the grinding vessel and the stationary mill control device.The electronic display device can preferably be arranged on an outer surface of the grinding cup lid, in particular on the upper side in the clamped state. This can be advantageous since the viewing direction of the user can fall, for example, directly onto the clamped grinding vessels after the opening of the housing cover.Preferably, the grinding vessel has a central grinding vessel axis which intersects the grinding cup base and the grinding cup cover in each case centrally, wherein the grinding cup cover has an end-face outer surface and a circumferential surface running around the central grinding vessel axis, and wherein the end-face outer surface has an end-face central region and an end-face peripheral ring region around the central grinding vessel axis, wherein the electronic display device is arranged at a distance from the central grinding vessel axis. Advantageously, in many laboratory grinding body mills, the clamping device of the grinding vessel receiving device thus does not obstruct the view of the electronic display device in the clamped state of the grinding vessel.According to one exemplary embodiment, the electronic display device comprises an alphanumeric digital display with a letter and / or numerical display and displays in particular the gas temperature measurement value, the contact temperature measurement value and / or the pressure measurement value in each case as a numerical value. This data can be helpful for the user, in particular when combining various displayed state parameters, for further grinding vessel handling.The alphanumeric digital display can comprise, for example, an LCD display, a TFT display, a QLED display, an OLED display, an AMOLED display or an electronic paper display, these being controlled by the control electronics inherent in the grinding vessel.The mill control device and / or the control electronics inherent in the grinding vessel preferably have a memory which is designed to store one or more threshold values for the state parameter to be measured.According to one exemplary embodiment, the electronic display device can have at least one luminous element, for example an LED, which lights up visibly if the measured value of the state parameter measured by the at least one sensor exceeds the at least one stored threshold value.If necessary, the grinding vessel can also comprise an acoustic signal transmitter which emits an acoustic warning signal if the measured value of the state parameter measured by the at least one sensor exceeds the at least one stored threshold value, so that the user receives an acoustic warning if, for example, the pressure or the temperature in the grinding vessel are so high that special safety precautions during handling, in particular before opening, the grinding vessel could be required.According to one exemplary embodiment, the mill control device or the control electronics inherent in the grinding vessel can have a memory which is designed to store a plurality of threshold values of different height for the state parameter, wherein the electronic display device has a plurality of luminous elements, e.g. LEDs, which each successively light up in a visible manner when the threshold values of different height for the state parameter are exceeded, and / or wherein the grinding vessel comprises an acoustic signal transmitter which each successively emits different acoustic warning signals when the threshold values of different height for the state parameter are exceeded, in order to signal to the user the exceeding of threshold values of different height.According to one aspect of the invention, the laboratory grinding mill has a receiving device and the grinding vessel has a transmitting device in order to transmit the state parameters measured by the at least one sensor from the grinding vessel to the mill control device or an external computer for further processing and / or for display there.The laboratory grinding mill may also include a fluid cooling system having a stationary source of cooling fluid, e.g., a vessel containing liquid nitrogen, from which a cooling fluid, e.g., liquid nitrogen (LN 2) may be introduced to or into the moving grinding vessel to actively cool the grinding vessel with the cooling fluid. The fluid cooling system is controlled by the mill control device, wherein in particular a control circuit is formed in which the mill control device actively controls the pressure and / or the temperature in the interior of the grinding vessel in response to the state parameter measured by the at least one sensor by targeted metering of the cooling fluid.In particular, the mill control device can control the rotational or oscillation frequency of the grinding vessel receiving device, the duration of the grinding phases, the duration of the pauses between the grinding phases, the quantity of cooling fluid, the duration of the cooling phases and / or the number of alternating grinding and cooling cycles in response to the state parameter measured by the at least one sensor, in particular in response to the temperature and / or pressure measurement value measured by the at least one sensor, in particular in response to the temperature measurement value measured by the gas temperature sensor, in particular in response to the temperature measurement value of the gas atmosphere located in the grinding vessel interior measured by the gas temperature sensor. The use of the gas temperature measurement value has the advantage that it exhibits a fast response behavior, in particular can exhibit a faster response behavior than the measurement of a contact temperature.The invention also relates to the grinding vessel, prepared for the laboratory grinding mill, in particular as described above, comprising:a grinding cup and a grinding cup cover for closing the grinding cup, wherein the grinding cup defines a grinding cup interior space which can be filled with grinding material and grinding bodies,at least one sensor which measures a state parameter of the grinding vessel and / or of the grinding vessel interior, andan electronic display device which is arranged on an outer side of the grinding vessel and which displays the status parameter measured by the sensor visually directly on the outer side of the grinding vessel for the user.The invention further relates to the grinding cup cover, which is designed to be placed on the grinding cup to form a grinding vessel for the laboratory grinding body mill, in particular as described above:at least one sensor which measures a state parameter of the grinding vessel and / or of the grinding vessel interior when the grinding cup is closed with the grinding cup cover, andan electronic display device which is arranged on an outer side of the grinding cup lid and which displays the status parameter measured by the sensor directly on the outer side of the grinding cup lid so as to be visible to the user.The invention further relates to a method for controlling the laboratory grinding mill as described above, wherein the same sensor, in particular pressure, gas temperature and / or contact temperature sensor, is used to both control the laboratory grinding mill during operation with the measured state parameters and to visually display the measured state parameters to the user on the electronic display device of the grinding vessel.According to a further aspect of the invention, a laboratory grinding body mill for laboratory analysis, in particular a planetary ball mill, centrifugal ball mill or vibrating mill, is provided, which comprises a grinding vessel having walls defining and enclosing a grinding vessel interior. The walls are formed, for example, by a grinding cup base, a circumferential grinding cup shell wall and a grinding cup cover, in particular a cover plate made of the material of the grinding cup or the grinding cup pellet. The grinding cup is hermetically sealed with the grinding cup cover for the grinding operation. The grinding cup base, the grinding cup shell wall and the cover plate accordingly form the grinding vessel interior, which can be filled with grinding material and grinding bodies, in particular grinding balls, in order to grind the grinding material in the grinding vessel interior between the grinding bodies and the walls of the grinding vessel by impact and frictional action by rotational and / or oscillatory movements, in particular by permanently changing acceleration of the grinding vessel.For this purpose, the grinding vessel is clamped into a grinding vessel receiving device in order to transmit the rotational and / or oscillatory movements from the grinding vessel receiving device to the clamped and closed grinding vessel.The grinding vessel receiving device with the grinding vessel clamped therein is driven by means of an electric motor and, for example, a belt drive. For example, in a planetary ball mill, the electric motor can drive a sun disk via a V-belt, which in turn drives the planetary rotation via a toothed belt.The laboratory grinding mill further comprises a mill control device in a stationary mill housing, which controls the grinding process, e.g. drive parameters such as rotational speed, oscillation frequency, grinding duration etc. of the laboratory grinding mill. The mill housing houses, on the one hand, the mill control device as well as the moving parts of the laboratory grinding mill. The mill housing is closed by a housing cover in order to allow the user access to the grinding vessel when the mill housing is open, for example for removing the grinding vessel, and to protect the moving parts from user access when the mill housing is closed.The grinding vessel comprises a gas temperature sensor which measures a gas temperature measurement value of the gas atmosphere located in the grinding vessel interior and a contact temperature sensor which measures a contact temperature measurement value on one of the walls of the grinding vessel, that is to say, in particular, a contact temperature of the grinding cup base, the grinding cup shell wall or the lid plate by thermal contact with the wall.The gas temperature measurement and the contact temperature measurement may provide different information about the milling process. Thus, for example, during a phase conversion process, the gas temperature can increase or decrease abruptly, wherein the contact temperature changes only slowly. Thus, for example, the grinding process can be continued even if the gas temperature measurement value briefly exceeds a critical threshold, as long as the contact temperature measurement value does not measure, for example, a maximum permissible grinding cup temperature at which, for example, a joined grinding cup can damage.New findings about the chemico-physical processes running in the grinding vessel interior can also be obtained, optionally also in combination with the measured pressure value, inter alia since the gas temperature in the grinding vessel interior and the contact temperature of the grinding vessel material can have different temporal response characteristics during the grinding process.Furthermore, the contact temperature can generally be used as an input variable for the start of the grinding process. For example, the user has frequently used several grinding cups. In this case, as a result of previous processes, a temperature difference between the grinding vessels can already be present before the grinding. For example, grinding vessels may come from the dishwasher, from an autoclave or from a previous grinding process and have been cleaned by hand or grinding vessels were previously placed in a cabinet at room temperature. The resulting measured contact temperatures of the grinding vessels at the beginning of the grinding process can therefore already be significantly different. The grinding vessel temperatures at the beginning of the grinding can have an influence on the grinding process and can provide advantageous findings on the grinding process for the user, in particular in comparison with the gas temperature.Preferably, the walls of the grinding vessel comprise a grinding cup base, a grinding cup shell wall encircling the grinding vessel axis, and a grinding cup cover and the gas temperature sensor and / or the contact temperature sensor can be arranged and fastened in or on the grinding cup cover.Preferably, the grinding vessel, in particular the grinding cup lid, comprises a measuring cavity which is in fluid communication with the grinding vessel interior via connecting channels and wherein the gas temperature sensor measures the gas temperature in the measuring cavity in order to thus measure the gas temperature of the gas atmosphere located in the grinding vessel interior.The contact temperature sensor is in direct thermal contact with one of the walls of the grinding vessel and measures the contact temperature measurement value of the respective wall by means of the thermal contact.The mill control device in the mill housing is configured to receive the gas temperature measurement value and the contact temperature measurement value from the grinding vessel and to control the grinding process in response to the temperature measurement values of both sensors, i.e. in response to the gas temperature measurement value measured with the gas temperature sensor and to the contact temperature measurement value measured with the contact temperature measurement value.The mill control device can be configured in particular to compare the gas temperature measurement value and the contact temperature measurement value and to control the grinding process in response to the temperature comparison of the gas temperature measurement value and the contact temperature measurement value of the wall of the grinding vessel.The grinding vessel preferably also comprises a pressure sensor which measures the gas pressure of the gas atmosphere located in the grinding vessel and sends it to the mill control device.According to an embodiment, the stationary mill control device may be configured to compare the gas temperature measurement value and the contact temperature measurement value and to control the grinding process in response to the temperature comparison and in response to the gas pressure measurement value.The walls of the grinding vessel can comprise in particular a grinding cup base, a circumferential grinding cup shell wall and a grinding cup lid, preferably with a lid plate made of a material that resists the impact and frictional effect of the grinding bodies and the grinding material, in particular made of the material of the grinding cup or of the grinding cup inlay. The grinding cup base, the grinding cup shell wall or the grinding cup cover further comprise a measurement cavity and a connecting channel through the cover plate in order to connect the grinding vessel interior space to the measurement cavity for fluid communication, wherein the gas temperature sensor, the contact temperature sensor and / or the pressure sensor is arranged in the measurement cavity.Preferably, the grinding vessel, e.g. in the grinding vessel cover, has an energy supply and a grinding vessel plate with control electronics inherent to the grinding vessel and sensor read-out electronics, to which the gas temperature sensor, the contact temperature sensor and / or the pressure sensor and the energy supply are connected, optionally via electrical plug connectors.Furthermore, the grinding vessel can comprise an electronic display device which is supplied with electrical energy from the energy supply. The electronic display device is arranged or fastened in particular on an outer side of the grinding vessel and displays the gas temperature measurement value and / or the contact temperature measurement value visibly directly on the outer side of the grinding vessel for the user.The walls of the grinding vessel comprise in particular a grinding cup base, a circumferential grinding cup shell wall and a grinding cup cover, and the electronic display device is preferably arranged on an axially front-side or upper outer surface of the grinding cup cover.Furthermore, the grinding vessel can have a central grinding vessel axis which intersects the grinding cup base and the grinding cup cover in each case centrally, wherein the grinding cup cover has an outer face side and a circumferential or tangential circumferential surface, and wherein the electronic display device is arranged on the outer face side of the grinding cup cover.The mill control device or the grinding vessel plate may comprise a memory configured to store a first threshold value for the gas temperature measurement value and / or a second threshold value for the contact temperature measurement value.Furthermore, the stationary mill control device can be configured to stop the grinding process and / or to reduce the rotational or oscillation frequency of the grinding vessel receiving device if the gas temperature measurement value exceeds the first threshold value and / or if the contact temperature measurement value exceeds the second threshold value, wherein the first and the second temperature threshold value are different.The laboratory grinding mill preferably has a receiving device and the grinding vessel has a transmitting device in order to transmit the gas temperature measurement value, the contact temperature measurement value and / or the gas pressure measurement value from the grinding vessel or the control device inherent to the grinding vessel to the stationary mill control device or an external computer.According to one aspect of the invention, the laboratory grinding mill may comprise a fluid cooling system having a stationary cooling fluid source, e.g. a vessel containing liquid nitrogen, from which the cooling fluid is feedable to the moving grinding vessel. The cooling fluid can be introduced, for example, to or into the grinding vessel in order to actively cool the grinding vessel with the cooling fluid. Depending on requirements, however, water cooling may also be possible. The fluid cooling system is now controlled by the mill control device in particular to the effect that a control loop is formed in which the mill control device actively controls the pressure and / or the temperature in the grinding vessel by targeted metering of the cooling fluid in response to the gas temperature measurement value measured by the gas temperature sensor and / or the contact temperature measurement value measured by the contact temperature sensor, in particular in response to a comparison of the gas temperature measurement value and the contact temperature measurement value.In particular, the mill control device can control the rotational or oscillation frequency of the grinding vessel receiving device, the duration of the grinding phases, the duration of the pauses between the grinding phases, the quantity of cooling fluid, the duration of the cooling phases and / or the number of alternating grinding and cooling cycles in response to the gas temperature measurement value measured by the gas temperature sensor and / or the contact temperature measurement value measured by the contact temperature sensor, in particular in response to a comparison of the gas temperature measurement value and the contact temperature measurement value.The invention also relates to the grinding vessel, prepared for the laboratory grinding mill, in particular planetary ball mill, centrifugal ball mill or vibrating mill, in particular as described above, wherein the grinding vessel comprises the following:a grinding cup and a grinding cup cover for closing the grinding cup, wherein the grinding cup defines a grinding cup interior space which can be filled with grinding material and grinding bodies,a gas temperature sensor that measures a gas temperature measurement value of the gas atmosphere located in the grinding vessel, anda contact temperature sensor that measures a contact temperature measurement of one of the walls of the grinding vessel.The invention also relates to the grinding cup cover, which is designed to be placed on a grinding cup for forming the grinding vessel for the laboratory grinding body mill, in particular planetary ball mill, centrifugal ball mill or vibrating mill, in particular as described above, wherein the grinding cup cover comprises a control device in an electronics interior space in the grinding cup cover and a gas temperature sensor, and(i) a contact temperature sensor which measures a contact temperature measurement value of the grinding cup lid, or(ii) an electrical connector for electrically contacting a contact temperature sensor by means of a complementary electrical connector of the grinding cup in order to measure a contact temperature measurement value of one of the walls of the grinding cup with the contact temperature sensor and to read out the contact temperature sensor with the electronic control device via electrical lines and the electrical connector. The connector and the complementary connector connect in particular automatically when the grinding cup cover is placed on the grinding cup.The invention further relates to a method for controlling a laboratory grinding mill, in particular a planetary ball mill, centrifugal ball mill or vibrating mill, in particular as described above, comprising the following steps:filling a grinding cup with grinding material and optionally one or a plurality of grinding bodies,closing the grinding cup with an associated grinding cup lid to form a closed filled grinding vessel, wherein the grinding cup or the grinding cup lid has a gas temperature sensor and wherein the grinding cup or the grinding cup lid has a contact temperature sensor,inserting (before or after closing the grinding vessel) and clamping the grinding vessel into a grinding vessel receiving device of the laboratory grinding body mill,closing the mill housing,presetting grinding parameters, in particular grinding duration and / or rotational or oscillation frequency of the grinding vessel receiving device, by means of a user interface of the laboratory grinding body mill,starting the grinding operation,wherein a mill control device controls the grinding process in response to the grinding parameters preselected by the user, wherein during the grinding process both a gas temperature measurement value and a contact temperature measurement value of a wall of the grinding vessel are measured and transmitted to the mill control device, andwherein the mill control device, in response to the gas temperature measurement value and / or the contact temperature measurement value of a wall of the grinding vessel, in particular in response to a comparison of the gas temperature measurement value and the contact temperature measurement value, automatically controls the grinding process deviating from the grinding parameters preselected by the user and / or the addition of cooling fluid for the active cooling of the grinding vessel.Preferably, the mill control device interrupts the grinding process in response to the gas temperature measurement value and / or the contact temperature measurement value of a wall of the grinding vessel, in particular in response to a comparison of the gas temperature measurement value and the contact temperature measurement value, shortens the grinding duration preselected by the user, reduces the rotational or oscillation frequency of the grinding vessel receiving device preselected by the user, and / or controls the addition of cooling fluid for the active cooling of the grinding vessel.The invention is explained in more detail below on the basis of exemplary embodiments and with reference to the figures, wherein identical and similar elements are provided in part with identical reference symbols and the features of the different exemplary embodiments can be combined with one another. The following exemplary embodiments are embodied identically in many aspects, and therefore features which are described on the basis of an exemplary embodiment are also to be considered as disclosed for the other exemplary embodiments, unless this is explicitly described differently or is clearly different.Brief Description of the FiguresThe following are shown: FIG. 1 is an exploded view of an embodiment of the grinding vessel, FIG. 2 shows a cross-sectional illustration of the sealed grinding vessel from FIG. 1, FIG. 3 shows a cross-sectional representation of an exemplary embodiment of the grinding vessel in monolithic construction, FIG. 4 shows a cross-sectional illustration of an exemplary embodiment of a joined grinding vessel, FIG. 5 shows an exploded view of an exemplary embodiment of a cover measuring unit, FIG. 6 shows a cross-sectional illustration through the cover measuring unit from FIG. 5 assembled to form a structural unit, FIG. 7 is a three-dimensional view of the assembled cover measuring unit of FIG. 5 , FIG. 8 shows a three-dimensional view of a further exemplary embodiment of the grinding vessel, FIG. 9 shows a cross-sectional representation of a further exemplary embodiment of a joined grinding cup, FIG. 10 shows a three-dimensional view of the grinding cup from FIG. 9, FIG. 11 is a cross-sectional view of another embodiment of a monolithic grinding cup, FIG. 12 shows a three-dimensional view of the grinding cup from FIG. 11, FIG. 13 shows an exploded illustration of an exemplary embodiment of a grinding vessel with the grinding cup from FIG. 11, FIG. 14 shows a three-dimensional view obliquely from below when the cover measuring unit is placed on a grinding cup, FIG. 15 shows a three-dimensional view obliquely from above when the cover measuring unit is placed on a grinding cup, FIG. 16 shows a three-dimensional representation of an exemplary embodiment of a disk vibration mill, FIG. 17 shows an enlarged detail illustration from FIG. 16 , FIG. 18 is a three-dimensional representation of an embodiment of a planetary ball mill, FIG. 19 is a partially cut-away view of the planetary ball mill of FIG. 18 , FIG. 20 is a block diagram of an embodiment of the control device inherent to the grinding vessel.DETAILED DESCRIPTION OF THE INVENTIONReferring to FIGS. 1-4, the grinding vessel 8 comprises a grinding cup 10 and a grinding cup cover 12 for closing the grinding cup 10, in particular hermetically sealed. In the present example, the grinding cup cover 12 comprises an upper cover measuring unit 14 and a cover plate 16, which closes an upper axial opening 20 of the grinding cup 10 and delimits the grinding vessel interior 18 axially with respect to the lower end-face grinding cup base 54. The grinding cup cover 12 or the cover plate 16 are sealed with respect to one another by a grinding vessel seal 22, in the present example an elastomeric ring (flat) seal, when the grinding cup cover 12 is braced with the grinding cup 10. In the present example, the grinding cup cover 12 is screwed to the grinding cup 10, for example by means of screws 24 which engage in threaded bores 26 which are arranged on the upper side 10 aof the grinding cup 10 around the grinding cup opening 20. The grinding vessel 8 for the laboratory grinding mill 1 preferably has a useful volume of 2 ml to 1000 ml, preferably of 20 ml to 500 ml.The grinding vessel interior 18 is accessible to the user through the grinding cup opening 20 on the upper side 10 awhen the grinding vessel 8 is open, in order to fill in grinding material and grinding bodies (both not shown) through the grinding cup opening 20. The grinding vessel seal 22 is then placed on a grinding cup sealing edge 26, in particular a front-side grinding cup sealing edge, which runs around the grinding cup opening 20. Subsequently, the cover plate 16 closing the grinding vessel interior 18 at the end face or upwardly is placed on the grinding vessel seal 22. For this purpose, the user can individually grip the cover plate 16, for example on the grip ring 28 thereof. The cover measuring unit 14 can then be placed as a pre-assembled structural unit on the top side 10 aof the grinding cup 10 or on the grinding cup opening 20 (covered with the cover plate 16) and screwed to the grinding cup 10 by means of the screws 24, wherein the grinding vessel seal 22 is braced between the cover plate 16 and the annular grinding cup sealing surface 26 in order to hermetically close the grinding vessel. However, it is also possible for the grinding cup cover 12 comprising the cover plate 16 and the cover measuring unit 14 to be connected to one another in advance, for example connected in a clamping manner, in order to place the entire grinding cup cover 12 including the cover plate 16 as a whole on the grinding cup 10. The grinding cup cover 12 can thus be formed in multiple parts, with the cover plate, which delimits the grinding vessel interior 18 and is preferably formed from the same material as the inner walls of the grinding cup 10, and the cover measuring unit, which accommodates the electronic components of the grinding cup cover 12 and can in particular also contain plastic components. The cover measuring unit 14 is accordingly a type of measuring and electronic attachment of the grinding cup cover 12.The cover measuring unit 14 is screwed together with further screws 30 as a pre-assembled structural unit. The cover measuring unit 14 is formed in multiple parts and can comprise a cover base 32, which forms a sensor / electronics unit with the sensor and / or the grinding cup electronics, for example, an intermediate body 34, which houses the battery, for example, and / or an upper cover 36, which is visible in particular axially. The cover measuring unit 14 forms an electronics interior 38, in the present example between the cover base 32 and the intermediate body 34, which accommodates a grinding vessel plate 40 with control electronics 64 inherent to the grinding vessel. In the cover measuring unit 14, a battery holder 42 can be fastened, for example, axially above the cover base 32 in the intermediate body 34, into which a power supply 44, for example in the form of a battery 45 for the control electronics 64 inherent to the grinding vessel, is inserted. Seated on the intermediate body or battery body 34 is the axially visible cover 36 which closes off the grinding cup cover 12 axially or upwardly. An electronic display device 46 is fastened to an outer side 9 of the grinding vessel 8, in the present example on the end-face outer surface or upper side 12 aof the grinding cup lid 12, in particular the lid measuring unit 14. In the present example, the electronic display device 46 is designed as a film display 48 which is adhesively bonded to the outer side 9 of the grinding vessel 8, here to the front-side outer surface 12 aof the grinding cup lid 12 or the surface 36 aof the cover 36, for example into a central axial depression 37 (FIGS. 5, 13 ). The cover measuring unit 14 can also comprise an acoustic signal transmitter 47, which is controlled by the control electronics 64 inherent in the grinding vessel.The electronic display device 46 can have an on-off switch 48, for example in the form of a so-called "click frog" switch, with which the grinding vessel electronics and the electronic display device 46 can be switched on and off. The electronic display device 46 can have an electronic temperature display 50 on the outer side 9 of the grinding vessel 8, here on the axial upper side 12 aof the grinding cup lid 12, which in the present example is designed as a colored LED 52, which lights up when a temperature threshold value is exceeded and lies directly in the field of view for the user when looking directly at the grinding vessel. The electronic display device 46 or the electronic temperature display 50 is thus arranged directly on the outer side 9 of the grinding vessel 8, in particular of the grinding cup lid 12 or the lid measuring unit 14. The electronic display device 46 or the electronic temperature display 50 is thus arranged in a direct viewing direction onto the grinding vessel 8, namely directly on its outer side 9 or upper side 8 a, namely both when the grinding vessel 8 is inserted into the laboratory grinding body mill 1 and clamped there, and also when the grinding vessel 8 is removed from the laboratory grinding body mill 1. This can prevent, among other things, the user from touching the grinding vessel 8 after the grinding process without any protective measures, without having to turn away the view of a display arranged elsewhere, in particular in order to avoid burns or other risks.In this example, the grinding vessel 8 is substantially rotationally symmetrical about a grinding vessel axis X. The grinding cup 10 has an axially front grinding cup base 54, through which the grinding vessel axis X extends substantially centrally. At a peripheral edge 54 aof the grinding cup base 54, the latter can be connected, in particular in one piece, to the grinding cup shell wall 56, which extends axially annularly around the grinding cup axis from the grinding cup base 54 as far as the grinding cup opening 20. The annular grinding cup sealing surface 26 can form an upper axial annular end face of the grinding cup 10. The grinding cup cover 12 can have an upper face surface 12 aand a circumferential surface 12 bcircling about the grinding vessel axis X.The grinding vessel plate 40 can be clamped into the cover base 32 by an O-ring 58, for example from above. For this purpose, the cover base 32 has an inner cutout 33, which can form the electronics interior 38. A sensor device 60, in the present example a combined pressure and temperature sensor 62, 80, can be attached to the underside 40 aof the grinding vessel plate 40. The sensor device 60 is read out by the control electronics 64 inherent to the grinding vessel, for example with a microcontroller 242.In the present example, the sensor device 60 comprises a piezo-resistive pressure transmitter with an integrated microcontroller interface. For example, a sensor device 60 with a welded, oil-filled stainless steel housing 61 in which the sensor's own microcontroller interface is accommodated can be used. Such pressure transmitters have in particular a low power consumption, which is of particular advantage in the present case on account of the low space available during battery operation. The sensor device 60 is bounded on the measuring side by a pressure membrane 68. The pressure membrane 68 is in gas contact with a measuring cavity 70 in which the gas pressure and the gas temperature are measured. The sensor device 60 can be arranged in an annular sleeve 78 of the cover base 32. In the present example, the measuring cavity 70 is arranged in an interior of the grinding cup cover 12 and hermetically sealed with respect to the external atmosphere. The measuring cavity 70 is in fluid communication with the grinding vessel interior 18 via connecting channels 72, so that the pressure sensor 62 can measure the gas pressure in the grinding vessel interior 18 via the pressure membrane 68 via the fluid communication with the measuring cavity 70. The measuring cavity 70 is defined here (axially) on the grinding cup side by the top side 16 bof the cover plate 16 and on the side facing away from the grinding vessel interior by the pressure membrane 68. The connecting channels 72 extend axially through the cover plate 16, for example in the form of bores. On the side facing away from the grinding vessel interior, the measuring cavity 70 is axially sealed by an O-ring 74 on an outer circumferential edge 63 of the pressure sensor 62. The measurement cavity 70 is radially sealed by a measurement cavity sealing ring 76, which can circulate radially around the measurement cavity 70 and is designed as an O-ring in the present example. In the present example, the measurement cavity seal 76 radially seals against the annular sleeve 78 of the cover base 32, in which the sensor device 60 or the pressure sensor 62 can be arranged, and against the grip ring 28.In the present example, the sensor device 60 comprises a gas temperature sensor which measures the gas temperature in the measuring cavity 70 and thus also the gas temperature of the gas atmosphere located in the grinding vessel interior 18 via the fluid communication with the grinding vessel interior 18. In the present example, the first temperature sensor, which is designed as a gas temperature sensor 80, is thus integrated into the sensor device 60 having the pressure sensor 62. The gas temperature sensor 80 thus does not measure the material temperature of solid parts of the grinding cup lid 12 or the grinding cup 10 by means of thermal contact, but measures the gas temperature of the gas located in the measurement cavity 70 and thus, via the fluid communication, the gas temperature of the gas atmosphere located in the grinding vessel interior 18. If the gas located in the measuring cavity 70 is in sufficient fluid communication with the grinding vessel interior 18, a reliable measured value for the gas temperature of the gas atmosphere in the grinding vessel interior 18 can thus be measured. The measurement of the gas temperature is also not substantially impaired if the gas temperature sensor 80 is integrated into the sensor device 60 with the pressure sensor 62, as long as the mass and heat capacity of the pressure sensor 62 is small compared to the mass and heat capacity of the grinding vessel 8, in particular small compared to the mass of the grinding vessel 8.The pressure sensor 62 and the gas temperature sensor 80 are read by the control electronics 64 inherent to the grinding vessel, i.e. in particular within the grinding vessel which is accelerated during operation. The measured pressure and / or temperature measurement values can thus be displayed directly on the grinding vessel 8 on the electronic display device 46 (FIG. 7 ) and can be transmitted to a stationary receiving device 222 of the mill control device 224 (FIG. 19 ) by a transmitting device 65 of the control electronics 64 inherent in the grinding vessel. Thus, the pressure and temperature measurement values can be used in duplicate, namely on the one hand directly at the grinding vessel 8, wherein the user can read the pressure and / or temperature information directly at the grinding vessel 8 when the mill housing 204 (FIGS. 16 to 18 ) is open, optionally even in alphanumeric and / or luminous form, and secondly as control parameter for the control of the grinding process by the control device for controlling the laboratory grinding body mill 1.FIG. 2 shows the grinding vessel 8 with an outer mount 82, for example made of stainless steel, and an inlay 84 defining the grinding vessel interior 18, for example made of agate or ceramic, for example zirconium oxide. The cover plate 16 is preferably made of the same material as the inlay 84, but in any case of a material which resists the impact and frictional effect of the grinding material and, if appropriate, of the grinding bodies and during operation, in order to form an inner wall 86 of the grinding vessel 8, which defines and surrounds the grinding vessel interior 18, if appropriate made of a uniform material. The grinding bodies, not shown, can consist of the same material as the inlay 84 or of a different material, which is selected on the basis of the grinding task. The grinding vessel 8 and the grinding bodies together form the so-called grinding assembly.Referring to Fig. 3, a monolithic grinding vessel 8 is shown. The monolithic grinding cup 10 is made of stainless steel, for example. In this case, the cover plate 16 is also preferably monolithically manufactured from stainless steel. Otherwise, the grinding vessel 8 in FIG. 3 corresponds to that from FIG. 2, so that reference can be made to it.Referring again to FIG. 4, a joined mill vessel 8, similar to that of FIG. 2, is shown, wherein the mill vessel 8 in FIG. 4 still has a secondary or alternative measurement cavity seal 76'. The secondary or alternative measurement cavity seal 76' is designed, for example, as an elastomeric flat ring seal, and seals the cover base 32 against the cover plate 16 in a peripheral ring region.Referring to FIGS. 5-7, the electronic display device 46 may include an alphanumeric pressure indicator 88 and / or an alphanumeric temperature indicator 90 that the user may read directly on the exterior of the grinding vessel 8, preferably the grinding cup lid 12, when the mill housing 204 is opened. The alphanumeric pressure or temperature indicators 88, 90 have the advantage that the user is not only informed about the exceeding of a threshold value, but can read the actual, in particular current, pressure measurement value and / or the actual, in particular current, temperature measurement value. In the present example, the alphanumeric pressure indicator 88 indicates the pressure measurement measured by the pressure sensor 62. The alphanumeric temperature display 90 displays the measured gas temperature value measured by the first temperature sensor, i.e. the gas temperature sensor 80. The electronic pressure and / or temperature indicators 88, 90 can be controlled by the control electronics 64 inherent in the grinding vessel and / or can be supplied with electrical energy by the electrical energy supply 44 inherent in the grinding vessel, in the present example in the form of the battery 45.The grinding vessel blank 40 has an electrical (plug) connector 92 on its flat side (top side) 40 bfacing away from the grinding vessel interior. The connector 92 protrudes into or through a connector recess 94 in the intermediate body 34 and / or into or through another connector recess 96 in the cover 36. When assembled, the connector 92 is connected to the mating connector 98 of the electronic display device 46 to drive the electronic display device 46. The electrical connection through the two plug connectors 92, 98 also brings about the switching on and off of the control electronics 64 inherent in the grinding vessel by means of the switch 48.Referring to FIG. 8, the electronic display device 46 may also include a plurality of simple LEDs 102 that may have different colors and indicate the exceeding of predefined temperature measurement values.Referring to FIGS. 9-10, the grinding vessel 8 may comprise a second temperature sensor, which is configured as a contact temperature sensor 110. The contact temperature sensor 110 is in thermal contact with the material of the grinding vessel 8, in the present example the grinding cup 10. In the present example, the grinding cup 10 is joined and the holder 82 made of stainless steel has a radial bore 114, into which the contact temperature sensor 110 is inserted radially from the outside and makes thermal contact with the inlay 84. In this way, the material temperature of the grinding cup 10, here more specifically of the grinding cup inlay 84, can be measured, which have a large heat capacity. The development over time of this material temperature can have a significantly different time characteristic during the grinding process than the gas temperature in the grinding vessel interior 18 or the measurement cavity 70, which is measured with the gas temperature sensor 80. From a comparison of the gas temperature measurement value and the contact temperature measurement value measured at the large heat capacity, useful additional information about the grinding process can be obtained and / or used for controlling the laboratory grinding mill 1. The laboratory grinding mill 1 can be controlled in particular in response to a comparison of the gas temperature measurement value and the contact temperature measurement value.The contact temperature sensor 110 is connected to an electrical (plug) connector 120 via sensor connecting conductors 116, which run, for example, in a bore 118 in the interior of the grinding vessel wall. In the present example, the plug connector 120 is arranged on the open axial end face of the grinding cup 10, e.g. on an annular edge 21 surrounding the opening 20, which simplifies the connection to a complementary (plug-in) connector. Preferably, the contact temperature sensor 110 is arranged on the grinding vessel wall or grinding cup wall 56 at an axial edge region. In the present example, the contact temperature sensor 110 is arranged in an axial edge region 122 adjoining the grinding cup opening 20. Alternatively, the contact temperature sensor 110 can also be arranged on an axial edge region 124 of the grinding cup shell wall 56 adjoining the grinding cup base 54. It has been found that the positioning of the contact temperature sensor 110 away from the axial center 126 of the grinding cup shell wall 56 can have advantages with regard to the temperature distribution and the temperature profile over time during the grinding process. In principle, however, it should not be excluded to arrange the contact temperature sensor 110 in a central region 126 of the grinding cup shell wall 56, on the grinding cup base 54 or on the grinding cup cover 12, in particular on the cover plate 16, and to contact it thermally in order to measure the contact temperature of solid parts of the grinding vessel 8.Referring to Figs. 11-12, a monolithic mill cup 10 is illustrated. Here too, the contact temperature sensor 110 can be arranged in a radial bore 114 in the outer side 56 bof the grinding cup shell wall 56 and be in thermal contact therewith in order to measure directly the contact temperature of the grinding cup 10.Referring to FIGS. 13-15, the connector 120 of the contact temperature sensor 110 is electrically connected to a mating connector 128. In the present example, the electrical connection between the contact temperature sensor (plug) connector 120 on the complementary contact temperature sensor (plug) connector 128 takes place automatically when the grinding cup cover 12 is placed on the grinding cup 10.Referring to FIGS. 16-19, the laboratory grinding mill 1, according to FIGS. 16-17, for example, designed as a disk vibration mill 202 and according to FIGS. 18-19, for example, as a planetary ball mill 302, has a mill housing 204. The mill housing 204 houses, among other things, the drive motor 226 with a converter 228 for driving the oscillatory movement or rotation of the grinding vessel receiving device 216, as well as the mill control device 224. The mill control device 224 is connected to a user interface 206, wherein the user can input desired grinding parameters via an input device 208. The user interface 206 further comprises a display 210 which can display selected parameters of the grinding process, for example the grinding duration. The display 210 can also display the measured pressure and / or temperature measurement values, which are transmitted from the transmitting device 65 of the control electronics 64 inherent in the grinding vessel to the receiving device 222 of the stationary mill control device 224 in the mill housing 204. The mill control device 224 can control the grinding process, for example grinding duration and / or oscillation or rotation frequency, in response to the pressure and / or temperature measurement values transmitted by the control electronics 64 inherent to the grinding vessel. For example, the mill controller 224 may shorten the grinding time and / or reduce the oscillation or rotation frequency, e.g., when the pressure and / or temperature measurements exceed predetermined thresholds. In particular, the mill controller 224 may control the milling process in response to a comparison of the contact temperature measurement and the gas temperature measurement. If, for example, the gas temperature changes abruptly, this can be an indication of a phase transition, whereas the material temperature of the grinding vessel 8 is still within an acceptable range, for example within a range in which the quality of the joint between mount 82 and inlay 84 is not yet impaired. Furthermore, the gas temperature in the grinding vessel interior 18 at the beginning of the grinding process typically rises considerably more quickly than the material temperature of the grinding vessel 8 on account of its large heat capacity. This different temporal response behavior of the gas temperature and the contact temperature measured on the material of the grinding vessel 8 can also be used to gain knowledge about the grinding process and / or to control the grinding process. For example, phase transitions or reactions in the grinding stock during the grinding process may be better detected than when only one of the two temperatures is measured.The mill housing 204 further comprises an openable and closable housing cover 212 which, in the closed state, encloses the moving parts of the laboratory grinding mill 1 in a manner secure against access, and, in the open state, allows the user to make visual contact with the electronic display device 46 of the grinding vessel 8 and access to the grinding vessel 8 in order to remove it from the laboratory grinding mill 1 or insert it into it. The housing cover 212 thus seals the mill interior 218 in which the grinding vessel 8 is located during operation in a secure manner from access. It is obvious to the person skilled in the art that the laboratory grinding mill mills 1 can have a plurality of grinding vessel receiving devices 216, into which a plurality of grinding vessels 8 can be clamped, depending on the mill subtype. Also, a plurality of grinding vessels 8 can be clamped into the same grinding vessel receiving device 216.In the example of the oscillating disk mill 202 (FIGS. 16 to 17 ), the grinding cup 10 is inserted into the laboratory grinding mill 1 and, in the inserted state, is filled with grinding material and grinding bodies. The grinding cup cover 12 is then placed with the electronic display device 46 and clamped with a grinding vessel clamping device 214. In the case of a vibratory mill 202, the grinding vessel receiving device 216 oscillates back and forth, for example, in a circular movement or a linear movement and thus brings about the comminution of the grinding material in the grinding vessel 8.In the planetary ball mill 302 (FIGS. 18-19 ), as well as in vibrating mills with smaller grinding vessels, the grinding vessel 8 can be filled and optionally closed remote from the laboratory grinding body mill 1 and already filled and optionally closed inserted into the laboratory grinding body mill 1. Referring to FIG. 18, the planetary ball mill 302 also includes a user interface 206. In this example, the user interface 206 is designed as a touch display, so that the input device 208 is integrated into the display 210. The housing cover 212 is designed as a rotating cover in this example in order to close the mill interior 218. In the planetary ball mill 302 shown, the mill vessel receiver 216 rotates about the planetary axis which coincides with the mill vessel axis X, and the mill vessel receiver 216 rotates with the inserted mill vessel 8 about a sun axis to produce a combined planetary motion when the planetary ball mill 302 is in operation.Referring again to all types of laboratory grinding mill 1, when housing cover 212 is open, the user directly sees electronic display device 46 of grinding vessel 8 and has access to grinding vessel 8, in order to remove it from laboratory grinding mill 1 and / or open it and fill it, if necessary.The grinding process of the laboratory grinding mill 1 can be controlled in response to the pressure measurement value, gas temperature measurement value and / or contact temperature measurement value measured by the sensors 62, 80, 110 during the grinding process, i.e. during the oscillation or rotation of the grinding vessel 8. For example, the grinding duration and / or, in the case of the planetary ball mill 302, the rotational frequency of the grinding vessel receiving device 216 and / or the sun disk 220 or, in the case of a vibration mill, the oscillation frequency can be controlled in response to one or more of these measured values. In particular, the grinding parameters, such as grinding duration, rotational speed and / or oscillation frequency, can be automatically controlled by the mill control device 224 in response to one or more of these measured values, in particular to a comparison of the gas temperature measured value and the contact temperature measured value.Referring to FIG. 20, the control electronics 64 which are accelerated in operation with the grinding vessel and are inherent to the grinding vessel have a controller 242 which reads out the pressure sensor 62, the gas temperature sensor 80 and / or the contact temperature sensor 110. In the examples shown, the pressure sensor 62 and the gas temperature sensor 80 are structurally integrated in a common sensor device 60, which is arranged in the interior of the grinding cup lid 16 and forms an internal sensor device 60. In the examples shown, the contact temperature sensor 110 is arranged outside the measurement cavity 70 and forms an external sensor. The control electronics 64 inherent in the grinding vessel transmit the measured values measured by the sensors 62, 80, 110 via the (radio) transmission device 65 to the stationary receiving device 222 of the mill controller 224. The thresholds are stored in the configuration memory 244 and are read by the controller 242. The mill vessel control electronics 64 further includes a battery management module 246 and the controller is supplied with electrical power from the battery 45.When controlling the grinding process, the mill control device 224 can, in response to one or more of the measured values, possibly even overregulate the setpoint values specified by the user, for example by the grinding process being terminated prematurely or by the duration of grinding cycles being shortened or by the rotation or oscillation frequency being automatically reduced compared to the user specification. The mill control device 224 can thus automatically react to undesired or unexpected deviations of individual or several of these measured values, in particular a combination of the measured values of the gas pressure in the grinding vessel interior 18, the gas temperature and / or the contact temperature at the grinding vessel 8 from predefined parameters. Furthermore, the pressure measurement value, the gas temperature measurement value and / or the contact temperature measurement value can be displayed directly on the grinding vessel 8 in a visually visible manner for the user by means of the electronic display device 46 inherent in the grinding vessel. The user can thus obtain information about the grinding process in an ergonomically accurate manner. Furthermore, the user can be prevented from touching the grinding vessel 8 with bare fingers if this exceeds a certain temperature threshold value, without the user having to do so with regard to the user interface 206 of the laboratory grinding body mill 1 or to another location of the mill. Thus, the user has the corresponding information and warning functions exactly where a risk might threaten, which can offer a safety advantage.Furthermore, the user can also be protected, for example, from an explosive escape of the gas atmosphere from the grinding vessel interior 18 when the grinding vessel 8 is opened, if the user is provided with the gas pressure directly displayed on the grinding vessel 8 itself. This is of particular advantage if the opening of the grinding vessel 8 takes place remote from the laboratory grinding mill 1. Nevertheless, the user has the appropriate information and warning functions in the correct place. If necessary, the user thus also has the gas temperature and / or the contact temperature in the field of view when the grinding vessel is removed from the laboratory grinding mill 1 and handled, e.g. opened, away from it.The laboratory grinding mill 1, regardless of its type, may further comprise an integrated fluid cooling 230 with a stationary cooling fluid source, which supplies cooling fluid from a fluid nozzle 232 to the grinding vessel 8 during the grinding process. This is schematically illustrated in FIG. 16 using the example of a vibratory mill 202, wherein the cooling fluid, for example liquid nitrogen, can be dropped from the fluid nozzle 32 onto the grinding vessel 8 during the grinding process. Alternatively, fluid channels can also be provided, which feed the cooling fluid to the grinding vessel receiving device 216 and / or to the grinding vessel 8. The fluid cooling can be realized in a planetary ball mill, for example as described in DE 20 2005 015 897 A1, DE 10 2020 127 234 A1, DE 10 2020 127 239 A1, DE 10 2020 127 240 A1, which are hereby incorporated by reference.Also, the amount or dosage of the cooling fluid may be controlled in response to one or more of the pressure measurement, the gas temperature measurement, and / or the contact temperature measurement measured with one or more of the sensors 62, 80, 110, particularly in response to a comparison of the gas temperature measurement and the contact temperature measurement.It will be apparent to those skilled in the art that the above-described embodiments are to be understood as exemplary and the invention is not limited thereto, but can be varied in many ways without departing from the scope of the claims.It will be further understood that the features, whether disclosed in the specification, claims, figures or otherwise, individually define essential components of the invention, even when collectively described with other features. In particular, it will be apparent to the person skilled in the art that aspects of the invention relating to the two different temperature sensors and aspects of the invention relating to the electronic display device on the grinding vessel can be claimed or combined with one another independently and shall be considered to be mutually disclosed. Orientation indications such as top, bottom, left, right, front, rear etc. are related to the figures used and should not be understood as absolutely limiting. Thus, grinding vessels which are upright can also be inserted into the laboratory grinding body mill in some laboratory grinding body mills, for example horizontally, i.e. with a horizontal grinding vessel axis. The phrase "comprises" means an open enumeration, and means "comprises at least.". In particular, one or more receiving devices, e.g. 1, 2, 3, 4 or more, and one or more grinding vessels, e.g. 1, 2, 3, 4, 5, 6 or more, e.g. stacked, can be provided for each receiving device.

Claims

Laboratory grinding mill (1), in particular planetary ball mill, centrifugal ball mill or vibrating mill, comprising: a grinding vessel (8) with walls defining a grinding vessel interior (18), which can be filled with grinding material and grinding bodies in order to grind the grinding material in the grinding vessel interior (18) between the grinding bodies and the walls of the grinding vessel (8) by impact and frictional action by rotational and / or vibrating movements of the grinding vessel (8), a grinding vessel receiving device (216) in which the grinding vessel (8) can be clamped, a motor drive (226) for driving the rotational and / or vibrating movement of the grinding vessel receiving device (216) with the grinding vessel (8) clamped therein, a mill control device (224) which controls the grinding process of the laboratory grinding mill (1), wherein the grinding vessel (8) comprises: a gas temperature sensor (80) measuring a gas temperature measurement value of the gas atmosphere located in the grinding vessel (8); and a contact temperature sensor (110) measuring a contact temperature measurement value of one of the walls of the grinding vessel (8), wherein the mill control device (224) is configured to receive the gas temperature measurement value and the contact temperature measurement value from the grinding vessel (8) and to control the grinding process in response to the temperature measurement values of both sensors (80, 110).Laboratory grinding body mill according to claim 1, wherein the walls of the grinding vessel (8) comprise a grinding cup base (54), a circumferential grinding cup shell wall (56) and a grinding cup lid (12), and the gas temperature sensor (80) and / or the contact temperature sensor are arranged in or on the grinding cup lid (12).Laboratory grinding mill according to any one of the preceding claims, wherein the grinding vessel (8) comprises a measuring cavity (70) which is in fluid communication with the grinding vessel interior (18) and wherein the gas temperature sensor (80) measures the gas temperature in the measuring cavity (70).Laboratory grinding mill according to one of the preceding claims, wherein the contact temperature sensor (110) is in thermal contact with one of the walls of the grinding vessel (8) and measures the contact temperature measurement value of the wall by means of the thermal contact.Laboratory grinding mill according to any of the preceding claims, wherein the mill control device (224) is configured to compare the gas temperature measurement value and the contact temperature measurement value and to control the grinding process in response to the temperature comparison of the gas temperature measurement value and the contact temperature measurement value of the wall of the grinding vessel (8).Laboratory grinding mill according to one of the preceding claims, wherein the grinding vessel (8) comprises a pressure sensor (62) which measures the gas pressure of the gas atmosphere located in the grinding vessel (8).The laboratory grinding mill of claim 6, wherein the mill controller (224) is configured to compare the gas temperature measurement and the contact temperature measurement and to control the grinding process in response to the temperature comparison and in response to the gas pressure measurement.Laboratory grinding body mill according to one of the preceding claims, wherein the walls of the grinding vessel (8) comprise a grinding cup base (54), a circumferential grinding cup shell wall (56) and a grinding cup lid (12), and wherein the grinding cup base (54), the grinding cup shell wall (56) or the grinding cup lid (12) has a measurement cavity (70) and a connecting channel (72), wherein the gas temperature sensor (80), the contact temperature sensor (110) and / or the pressure sensor (62) is arranged in the measurement cavity (70), and the measurement cavity (70) is in fluid communication with the grinding vessel interior (18) via the connecting channel (72).Laboratory grinding mill according to one of the preceding claims, wherein the grinding vessel (8) comprises a power supply (44) and a grinding vessel plate (40) with control electronics (64) inherent to the grinding vessel, to which the gas temperature sensor (80), the contact temperature sensor (110) and / or the pressure sensor (62) are connected in order to read out the respective sensor (62, 80, 110) within the grinding vessel (8).Laboratory grinding mill according to any one of the preceding claims, wherein the grinding vessel (8) comprises an electronic display device (46) and a power supply (44) for supplying the electronic display device (46) with electrical power, and wherein the electronic display device is arranged on an outer side (9) of the grinding vessel (8) and displays the gas temperature measurement value and / or the contact temperature measurement value visibly to the user on the outer side (9) of the grinding vessel (8).The laboratory grinding mill of claim 10, wherein the walls of the grinding vessel (8) comprise a grinding cup bottom (54), a circumferential grinding cup shell wall (56), and a grinding cup lid (12), and wherein the electronic display device (46) is disposed on an outer surface (12a) of the grinding cup lid (12).Laboratory grinding mill according to claim 11, wherein the grinding vessel (8) has a central grinding vessel axis (X) which intersects the grinding cup base (54) and the grinding cup cover (12) in each case centrally, wherein the grinding cup cover (12) has an end-face outer surface (12a) and a circumferential lateral surface (12b), and wherein the electronic display device (46) is arranged on the end-face outer surface (12a) of the grinding cup cover (12).The laboratory grinding mill according to any one of the preceding claims, wherein the mill control device (224) or the grinding vessel plate (40) comprises a memory (244) adapted to store a first threshold value for the gas temperature measurement value and / or a second threshold value for the contact temperature measurement value.The laboratory grinding mill of claim 13, wherein the mill controller (224) is configured to stop the grinding process and / or reduce the frequency of rotation or oscillation of the grinding vessel receiver when the gas temperature measurement exceeds the first threshold and / or when the contact temperature measurement exceeds the second threshold.The laboratory grinding mill of claim 13 or 14, wherein the first and second thresholds are different.Laboratory grinding mill according to any one of the preceding claims, wherein the laboratory grinding mill (1) comprises a receiving device (222) and the grinding vessel comprises a transmitting device (65) for transmitting the gas temperature measurement value, the contact temperature measurement value and / or the gas pressure measurement value from the grinding vessel (8) to the mill control device (224) or to an external computer.Laboratory grinding mill according to one of the preceding claims, wherein the laboratory grinding mill (1) has a fluid cooling system (230) with a stationary cooling fluid source, from which a cooling fluid can be supplied to the grinding vessel (8) in order to actively cool the grinding vessel (8) with the cooling fluid, and wherein the fluid cooling system (230) is controlled by the mill control device (224), wherein in particular a control loop is formed in which the mill control device (224) actively controls the pressure and / or the temperature in the grinding vessel (8) by targeted metering of the cooling fluid in response to the gas temperature measurement value measured by the gas temperature sensor (80) and / or the contact temperature measurement value measured by the contact temperature sensor (110), in particular in response to a comparison of the gas temperature measurement value and the contact temperature measurement value.Laboratory grinding mill according to one of the preceding claims, wherein the mill control device (224) controls the rotation or oscillation frequency of the grinding vessel receiving device (216), the duration of the grinding phases, the duration of the pauses between the grinding phases, the amount of cooling fluid, the duration of the cooling phases and / or the number of alternating grinding and cooling cycles in response to the gas temperature measurement value measured by the gas temperature sensor (80) and / or the contact temperature measurement value measured by the contact temperature sensor (110).Grinding vessel (8) designed for a laboratory grinding body mill (1), in particular for a planetary ball mill, centrifugal ball mill or vibration mill, in particular according to one of the preceding claims, comprising: a grinding cup (10) and a grinding cup cover (12) for closing the grinding cup (10), wherein the grinding vessel (8) defines a grinding vessel interior (18), which can be filled with grinding material and grinding bodies, a gas temperature sensor (80), which measures a gas temperature measurement value of the gas atmosphere located in the grinding vessel (8), a contact temperature sensor (110), which measures a contact temperature measurement value of one of the walls of the grinding vessel (8), and sensor read-out electronics, to which the gas temperature sensor (80) and the contact temperature sensor (110) are connected.Grinding cup cover (12) designed for placement on a grinding cup (10) for forming a grinding vessel (8) for a laboratory grinding body mill (1), in particular for a planetary ball mill, centrifugal ball mill or vibrating mill, in particular according to one of the preceding claims, comprising a control device (66) inherent in the grinding cup cover and a gas temperature sensor (80) and sensor reading electronics, to which the gas temperature sensor (80) is connected, and (i) a contact temperature sensor (110), which measures a contact temperature measurement value of the grinding cup cover (12) and is connected to the sensor reading electronics, or (ii) an electrical connector (128) for electrically contacting a contact temperature sensor (110) by means of a complementary electrical connector (120) of the grinding cup (10), in order to use the contact temperature sensor (110) to measure a contact temperature measurement value of one of the walls (54, 54, 56) of the grinding cup (10) and connecting the contact temperature sensor (110) to the sensor reading electronics and reading it out with the control device (66) on the grinding cup cover via electrical lines (116) and the electrical connectors (120, 128).Method for controlling a laboratory grinding mill (1), in particular a planetary ball mill, centrifugal ball mill or vibration mill, in particular according to one of claims 1 to 18, comprising the following steps: filling a grinding cup (10) with grinding material and optionally one or a plurality of grinding bodies, closing the grinding cup (10) with an associated grinding cup lid (12) to form a closed filled grinding vessel (8), wherein the grinding cup (10) or the grinding cup lid (12) has a gas temperature sensor (80) and wherein the grinding cup (10) or the grinding cup lid (12) has a contact temperature sensor (110), inserting and clamping the grinding vessel (8) into a grinding vessel receiving device (216) of the laboratory grinding mill (1), closing the mill housing (204), presetting grinding parameters, in particular, grinding duration and / or rotational or oscillation frequency of the grinding vessel receiving device (216), starting the grinding process, wherein a mill control device (224) controls the grinding process in response to the grinding parameters preselected by the user, wherein during the grinding process both a gas temperature measurement value and a contact temperature measurement value of a wall (16, 54, 56) of the grinding vessel (8) are measured and transmitted to the mill control device (224), and wherein the mill control device (224) automatically, in response to the gas temperature measurement value and the contact temperature measurement value of the wall of the grinding vessel (8), in particular in response to a comparison of the gas temperature measurement value and the contact temperature measurement value, the grinding process, optionally deviating from the grinding parameters preselected by the user and / or controlling the addition of cooling fluid for the active cooling of the grinding vessel.Method according to claim 21, wherein the mill control device (224), in response to the gas temperature measurement value and / or the contact temperature measurement value of a wall (16, 54, 56) of the grinding vessel (8), in particular in response to a comparison of the gas temperature measurement value and the contact temperature measurement value, aborts the grinding process, shortens the grinding duration preselected by the user, reduces the rotational or oscillation frequency of the grinding vessel receiving device preselected by the user and / or controls the addition of cooling fluid for the active cooling of the grinding vessel (8).

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